Synthesis, Structure, and Weakly Coordinating

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Synthesis, Structure, and Weakly Coordinating Nature of New Carborane Anions C hi-W ing T SA N G

A thesis subm itted in partial fu lfillm en t o f the requirem ents for the degree o f D octor o f Philosophy in C h em istry © The C hinese U niversity o f Hong K ong July 2000

Supervisor: Prof. Z uow ei Xie

T he C hin ese University o f Hong K ong h olds the copyright o f this thesis. Any person(s) intending to using a part o r w h o le o f the m aterials in the thesis in a proposed publication m ust seek copyright release from the Dean o f the G ra d u ate School.


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To My Family.


Thesis Committee Prof. Kevin. W in g Por LEUNG (C hairm an ) Prof. H ung-kay LEE Prof. Zuowei X IE (Supervisor) Prof. C hak-po Lau (A dditional E xternal Examiner, H ong K ong Polytechnic U niversity) Prof. C h ristop h er A. Reed

(E xternal

Exam iner, U n iversity

C alifornia, R iverside)


of

Acknowledgement I would like to express my sincere thanks to my supervisor Prof. Zuowei Xie for his guidance, help and continuous encouragement during the course of my study and preparation of this thesis.

Thanks are also due to Prof. Qingchuan Yang, Prof. Zeying Zhang, Dr. Feng Xue, Prof. Zhongyuan Zhou and Prof. Thomas C. W. Mak for their help in the determination of single-crystal X-ray structures, and Prof. Dominic T. W. Chan and Dr. Eric Tung-Po Sze for their help in the determination of anion masses by negativeion MALDI mass spectroscopy.

I am also grateful to my groupmates, Dr. Zhixian Liu, Dr. Chaoguo Yan, Dr. Baiquan Wang, Dr. Shaowu Wang, Mr. Ka-yue Chiu, Mr. Kwoli Chui, Mr. Guofu Zi, Ms. Hoi-shan Chan and Mr. Haiping Wang for their helpful discussion and suggestions. I also thank my friends and officers of Department of Chemistry and Graduate School for their help and supports during the course of my study.

I am greatly indebted to the Hong Kong Research Grants Council for the financial support.

July 2000 Chi-Wing TSANG Department of Chemistry The Chinese University of Hong Kong

I


Abstract Direct halogenation of I-CH 3-CB 11H 11' or C-methylation of I-H-CB 11H5X6 ' gave several weakly coordinating anions l-CH3-CBnX6' (X = Cl, Br, I) which show to have better solubility than their parent anion in various organic solvents. Their silver(I) salts were prepared and structurally characterized by X-ray crystallography. A common feature for the solid-state structures of these silver(I) carborane complexes is that the carborane acts as a bridging ligand to give an alternating cation-anion zigzag chain which is maintained in one-dimension throughout the lattice. For comparison, several silver(I) salts of cobalt bis(dicarbollide) ions have also been prepared. Their solid-state structures exhibit both monomeric and one-dimensional coordination polymeric structures. A new methodology (sealed-tube reaction) has been developed for the synthesis of highly halogenated carborane anions, which led to the isolation and structural characterization of a series of new weakly coordinating anions including 1H-CBnXu', 1-CH3-CBuXh", I-H-CB 9X 9 , 1-NH2-CB9X9' and I-H-CBhYjX*' (X, Y = Cl, Br, I). Their weakly coordinating nature was approached by comparing the 29Si NMR data of compounds Pr'3Si(carborane) and structural data of complexes Ag(carborane). These findings suggest that the coordinating ability of these anions depend mainly upon the nature o f the substituents at 7 - 12 positions, and the contribution from the substituents o f the upper belt (2-6 positions) is relatively small. The structural studies on silver(I) salts of these per-halo and mixed-halo carborane anions indicate the rich coordination chemistry of this type of compounds, varying from monomeric through one-dimensional polymeric to three-dimensional polymeric structures.

II


This newly-developed method also led to the preparation of several peralkylated carborane anions including 1-H-CBuRn' (R = Me, Et), l-H-CBgMe^ and l,2-Cl2-CBi0Meio. The features of this method are clean, economical, quantitative yield and organic solvent-free. It may be the best synthetic route to peralkylated carborane anions ever reported in the literature. Treatment of the silver(I) salts of carborane anion with HCl(aq) in CH 2CI2 gave several hydronium salts of carborane anions. They are weighable and stable at room temperature. However, the water molecules of the hydronium salts can be removed under high temperature and high vacuum conditions to afford highly acidic species that can protonate organic solvents such as DMF, OEt2 and acetic acid, and olefin such as cyclohexene. The molecular structures of the hydronium salts and protonated organic solvents were all confirmed by single-crystal X-ray analyses.

Ill


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Contents Acknowledgment

I

A bstract (in English)

II

A bstract (in Chinese)

IV

Contents

VI

List of Com pounds

IX

List of Figures

XII

C hatper 1 Introduction

1

1.1 Carborane Anions: A New Class of Weakly Coordinating Anions

1

1.2 Aims

9

C hapter 2 Synthesis and Characterization of I-CH 3-CB 11H5X6 ' Anions. Crystal Structure o f A g(l-CH 3-CBnH 5X6) (X = H, Cl, Br, 0

10

2.1 Synthesis

10

2.2 Structure of AgO-CHj-CBuHsX*) (X = H, Cl, Br, I)

13

C hapter 3 Synthesis and Structural Characterzation of Highly Chlorinated, Brominated, Iodinated Icosahedral Carborane Anions: 1 -H -C B uX if, I-CH 3-C B 11X 11' (X = Cl, Br, I); l-B r-C B n Brn -

25

3.1 Attempted Synthesis of Per-halo Icosahedral Carborane Anions

26

3.2 Synthesis of Highly Halogenated Carborane Anions

27

3.3 Conclusion

40

C hapter 4 Weakly Coordinating Nature of Different Halogen Atoms on an Icosahedral Cage. Synthesis and Structural Characterization o f Mixed-halo Icosahedral Carborane Anions, H-1-CBUYsX^

42

4.1 Synthesis of Mixed-halo Icosahedral Carborane Anions, 1-H-CBhY 5X6’

43

VI


4.2 Coordinating Ability

48

4.3 Polymeric vs Monomeric Structures of Silver(I) Salts of Per-halo and Mixed-halo Icosahedral Carborane Anions 4.4 Conclusion

49 60

C h ap ter 5 Synthesis and Structural Characterization of Highly Chlorinated, Brominated, Iodinated, and Methylated Carborane Anions, H-I-CB 9X 9 -, NH 2-I-CB 9X9 ' (X = Cl, Br, I), and H-l-CBsCCHsV

63

5.1 Synthesis and Structural Characterization

63

5.2 Coordinating Ability

72

5.3 Conclusion

73

C h ap ter 6 Alkylation o f C B n H n ', CB9 H 10', and C2 B 10H 12

77

6.1 Attempted Synthesis of l-H-CBu(CH 3)n" from 1-H-CBnIn'

77

6.2 Synthesis o f Peralkylated Carborane Anions

78

6.3 Synthesis of Pentamethytlated Carborane Anions, l-H-2,3,4,5,6(CH3)5-7,8,9,10,ll,12-X6-CBu' (X = Cl, Br) 6.4 Synthesis of l,2-Cl2-l,2-C2BioMei0

80 81

C h ap ter 7 Synthesis, Structure, and Reactivity of Hydronium Salts of Weakly Coordinating Anions

84

7.1 Synthesis and Structural Characterization 7.1.1 Hydronium Salts

84

7.1.2 Protonated Organic Molecules

90

7.2 Reactivity

93

7.3 TGA (Thermal Gravimetric Analysis)

93

C h ap ter 8 Monomeric and Polymeric Structures of Silver Salts of Cobalt(III) Bis(dicarbollide) ions

98

VII


8.1 Synthesis of Cobalt(III) Bis(dicarbollide) Anions and Their Silver Salts

98

8.2 Crystal Structures

100

8.3 Conclusion

104

C hapter 9 Experimental Section

105

References

151

Appendix I. Publications Based on the Research Findings

160

II. Table of Crystal Data and Refinements

161

III. Table of Atomic Coordinates and Thermal Parameters; Bond Distances and Angles.

VIII


175

List of Compounds Compound No.

Anion/Compound Formula

Page No.

(II- 2 )

l-CHs-CBnHsCI*

11

(U-3)

1-CH3-CB 1, H 5 Br6'

12

(II-4)

1-CH3-CB„H 5I6

12

(II-5)

(r/2 -benzene)Ag(l-CH 3-CB„Hu )

14

(II- 6 )

( rjl -mesity lene)Ag( 1 -CH 3-CB 11HsC16)

19

(U-7)

A g(l-C H 3-C B „H 5Br6)

20

(H- 8 )

Ag(l-CH3-CB„H 5l6)

21

(III-l)

l-CH 3- C B „ a ,r

27

(IU- 2 )

1-CH3-CB 11Bri 1

30

(IU-3)

I-CH 3-CB 11I11

27

(III-4)

1-H-CBnCln'

35

(in -5 )

1-H-CBiiBrn

31

(III- 6 )

1-H-CBiiIn

35

(III-7)

1-Br-CBi 1Br 11

32

(III-8 )

[Me3N H][l-CH 3-CB„Cln ]

28

(III-9)

(p-xy lene)Ag( 1-CH3-CB11 HBrl0)

29

(IH - 1 0 )

Ag[ 1-CH3-CB 11 Bri 1]

30

(IU-11)

[Me3NH][l-Br-CBu Brii]

32

(IH-12)

Cs[l-H -CBn Brn ]

33

(IV-1)

H -l-C B uB r 5Cl6'

43

(IV-2)

l-H -C B „C l 5 Br6

44

(IV-3)

l-H-CBiiBr 5 I6"

43

a v -4 )

l-H-CBuIsBr^

44


(IV-5)

l-H -CBn I5a 6-

44

(IV-6)

( /72-mesity lene)2Ag( 1-H-

50

CB 11 Br5Cl6 )(mesity lene) (IV-7)

( rjl-mesity lene)Ag( 1-H-

51

CBi iCl5Br6)(mesitylene) (IV-8)

(C6H5N)2Ag(l-H-CB11Br5 l 6 )(C 6H5N)

51

(IV-9)

Ag2(CB, IBr6I5)(CH3CN) 2

53

(IV -10)

(f71-mesitylene)Ag(CH3CN X l-H -CBu Bri,)

54

(IV-11)

( >72-/>-xylene)2Ag( 1-H-CB 11 Cl 11)

55

(IV -12)

A g(l-C H 3-CBi ,Cli i)

56

(IV -13)

C s[l-H -C B „B r5I6][THFl

57

(IV -14)

[Me3NH][l-H-CBi,Cl5Br6]M e 3N H C lH 20

59

(V -l)

H-1-CB9C19'

67

(V-2)

benzyl-1-CB9C19'

68

(V-3)

H -l-CB9Br9

63

(V-4)

H-1-CB9I9

68

(V-5)

n h 2- i -c b 9c i 9

69

(V-6)

NH2-l-C B 9Br9'

63

(V-7)

NH2-1-CB9I9'

69

(V-8)

H -l-C B ^C H sV

70

(V-9)

(r72-benzene)Ag(H-1-CB9Br9)

64

(V-10)

(?72-benzene)(

65

-benzene )Ag3 [ 1-H-

CB9Br9]2[N 0 3](THF) (V -ll)

Cs(l-H-CB9Br9XH20)o^

66


(V-12)

[(C6H5CH2)NMe3][C6H5CH2-l-CB9a 9 ]

68

(VI-1)

l-H-CBu(CH3)u

78

(VI-2)

1-C H 3-C B „(C H 3) m

77

(VI-3)

l-H -C B u (CH2CH3) ir

79

(VI-4)

l-H -CBlI(CH3)6l5

78

(VI-5)

1-H-CB11 MesCV

80

(VI-6)

1-H-CBj i Me5Br6

80

(VI-7)

1,2-Cl2-1^ -C 2B ioMe io

81

(VII-1)

[H30 ][l-C H 3-CBiiBr,]

85

(VU-2)

[H30 +(H20 )] [ 1-H-CBi i BrsCle]

85

( v ii-3 )

[H502][l-H-CB,il5Br6]

85

(VII-4)

[H9 0 4 ][l-H -C B,iBrn ]

85

(VII-5)

[H9O4 ] [ 1-H-CB9Br9]

89

(VII-6)

[(CH3>2NCHO--H- -OH2][1-H -C B i iQ n ]

90

(VII-7)

[(DMF) -H- OH 2 ][l-H-CBnCI5Br6]

91

(v n -8 )

[Et20 - H • OH2][l-H -C BnIu]

92

(VII-9)

[(CH3CO O H ) 2 H ][l-H -C B n a „ ]

92

(V III-l)

(/72-/)-xylene)Ag[Co(C2B9Hi 0 2]

98

(VIII-2)

(rf-p-xy lene)Ag[8,8 ’-^-1,2-C6H4-

98

Co(C2B9H 10)2] •1.5(p-xy lene) (VUI-3)

[(CH3CN)4Ag][Co(C2B9H8Br3)2]

98


List of Figures Fig. No.

Description

Page No.

2.1

Proton-coupled UB NMR spectra of compounds A g(lCH 3 -CBiiHsX 6 )(X = H, Cl, Br, I) in ^-acetone

15

2.2

Perspective view of the coordinating sphere around the silver atom in ( rj2-benzene)Ag( 1-CH3-CB u H n ) (U-5)

18

2.3

Perspective view of the coordinating sphere around the silver atom in ( r;1-mesitylene)Ag( 1-CH3-CB 11H5CI6 ) (H- 6 )

19

2.4

Perspective view of the coordinating sphere around the silver atom in Agfl-CHs-CBuHsB^) (U-7)

20

2.5

Perspective view o f the coordinating sphere around the silver atom in A g(l-C H 3-CBuH 5l6) (H-8 )

22

2 .6

Stereoscopic view of (r 72-benzene)Ag(l-CH 3-CBnH u) (H5).

22

2.7

Stereoscopic view of (i 71-mesitylene)Ag[l-CH3C B „H 5C16] (U-6 )

23

2 .8

Stereoscopic view of A g[l-C H 3-CBuH 5 Br6 ] (U-7)

23

2.9

Stereoscopic view of A g(l-C H 3-CBuH 5 I6) (U-8 )

24

3.1

Perspective view of I-CH 3-CB 11CI11' in [Me3NH][l-CH 3CB„C1„ ] (UI-8 )

28

3.2

Perspective view of Q?-xylene)Ag( 1 -CH3-CB 11HBri0) (HI9)

30

3.3

Perspective view of the coordinating sphere around the silver atom in A g[l-C H 3-CBuBru] (III- 1 0 )

31

3.4

Progress of the reaction of Cs[l-H-CBuBru] with Br2 followed by n B {'H} NMR.

34

3.5

Crystallographically independent molecule in the unit cell of [Me 3NH][l-Br-CBnBru] (IU-11)

32

3.6

Perspective view of the coordinating sphere around the Cs cation in Cs[l-H-CBuBrn] (HI-12)

35

3.7

Proton-coupled n B NMR spectra of compounds [Me3NH][l-CH 3-C B „X n] (X = H, Cl, Br, I) in d6- acetone

39


3.8

Proton-coupled llB NMR spectra of compounds [Me3N H ][l-H -CBuX n ] (X = H, Cl, Br, I) in Ag[II-2]> Ag[II-3]> Ag[II-4]. In general, they are quite soluble in polar organic solvents such as acetone, acetonitrile and ethers, insoluble in nonpolar organic solvents. Ag[ll-1] and Ag[II-2] are soluble in arenes like benzene, toluene, xylene, mesitylene, and slightly soluble in CH2CI2 and hot water. Ag[II-3] and Ag[II-4] are slightly soluble in arenes and insoluble in hot water. 11B NMR is an extremely useful technique for the characterization of boron compounds. Figure 2.1 shows the proton-coupled UB NMR spectra of compounds Ag(lCH3-CB 11H5X 6) (X = H, Cl, Br, I) in r/6-acetone. Due to the electron-donating effect of the substituted methyl group at the C position, the chemical shift of six boron atoms at 712 positions in II-l become almost identical. Anions II-2 —II-4 all exhibit typical 1:5:5 splitting pattern which is consistent with Csv symmetry and 7,8,9,10,11,12 regioselective pattern of electrophilic substitution of II-l. 2.2 Structure of Agd-CHa-CBuHsX*) (X = H, Cl, Br, I) The coordination geometries of the silver(I) salts of anions I I - l —II-4 are shown in Figures 2.2 - 2.5, respectively. Figures 2.6 - 2.9 show the stereoscopic view of their crystal packing. Selected bond distances are listed in Table 2.1. Similar to other known silver salts of carborane anions, a common feature to all four compounds is that the carborane acts as a bridging ligand to give an alternating cation-anion zigzag chain which is maintained in one-dimension throughout the lattice. The silver(I) salts of II-l and U-2 are coordinated with arene molecules, while those of II-3 and II-4 are unsolvated

13


although they were crystallized from toluene and benzene, respectively. The coordination details are unique to each structure. In (r 72 -benzene)Ag[II-l] (U-5), silver is bound to one benzene molecule in re fashion and two carborane anions via B(8 )-H(8 ) and B(9A)-H(9A) bonds, respectively, in a trigonal geometry (Figure 2.2). The formal coordination number of silver is three. In contrast, the silver atom in (r;l-benzene)Ag(CBnHi2 ), a closely related analogue to (rfbenzene)Ag[Il-l] (11-5), is r;1-bound to benzene and is coordinated to two B-H bonds from the 7-position of one cage and the 12-position of

14


A

X = Ci

-A

x = ar

;

X=

r 5

0 -5

-10

-15

-20

-25

ppm

Figure 2.1 Proton-coupled n B NMR spectra of compounds Ag(l-CH3-CBnH 5X6 ) (X= H, Cl, Br, I) in d6-acetone.

15


Table 2.1 Selected Bond Distances (A) Compound (ry2-benzene)Ag[H-I] (II1-5) A g(l) - B(8 )

2.671(1)

A g(l) - B(9A)

2.613(1)

A g(l) - C(4)

2.698(1)

Ag(l) - C(3)

2.460(1)

Compound ( r; 1-mesitylene)Ag[II-2] (III-6 ) Cl(7) - B(7)

1.757(5)

Cl(8 ) - B(8 )

1.805(7)

Cl(9) - B(9)

1.796(7)

Cl(10) - B(10)

1.765(6)

C l(ll) - B ( ll)

1.798(6)

Cl(12) - B(12)

1.776(6)

A g(l) - C( 6 )

2.495(6)

A g(l) - Cl(8 )

2.683(2)

A g(l) - Cl(12)

2.874(2)

A g(l) - Cl(27)

2.763(2)

A g(l) - Cl(28)

2.732(2)

Cl(27) - B(27)

1.829(5)

Cl(28) - B(28)

1.806(6)

CI(29) - B(29)

1.801(7)

Cl(30) - B(30)

1.819(6)

Cl(31) - B(31)

1.797(6)

16


Cl(32) - B(32)

1.802(7)

Ag(2) - C(15)

2.422(5)

Ag(2) - Cl(30)

2.729(2)

Ag(2) - Cl(32)

2.867(2)

Ag(2) - Cl(10)

2.745(2)

Ag(2) - C l(ll)

2.780(2)

Compound Ag[ll-3] (111-7) Br(4) - B(4)

1.951(12)

Br(5) - B(5)

1.958(9)

Br(6 ) - B(6 )

1.952(8)

A g (l)-B r(5 )

2.852(1)

A g(l) - Br(6 )

2.733(1)

A g(l) - Br(12)

2.990(1)

A g(l) - Br(5A)

2.852(1)

A g(l) - Br(6 A)

2.733(1)

A g(l) - Br(12A)

2.990(1)

Compound Ag[lI-4] (IU- 8 ) 1(7) - B(7)

2.188(11)

1(8) -B ( 8 )

2.184(9)

1(9)-B (9)

2.192(10)

1(10) - B(10)

2.177(10)

1(11) - B (ll)

2.172(11)

1(12) - B(12)

2.160(9)

17


A g(l) - 1(7)

2.798(2)

A g(l) - 1(12)

2.872(2)

A g(l) - I(9A)

2.822(2)

A g(l) - I(10A)

2.848(2)

the other one, respectively . 10 It should be pointed outthat B(12), Le. antipodaltothe cage carbon,

theso-called most electron-rich site in theicosahedral

cage , 10’113does

not

coordinate to the silver in compound ( r72 -benzene)Ag[II-l ] (H-5), suggesting the electronic effect of the methyl group. It is surprising that the methyl substituent at the carbon position of the icosahedral cage has such a large effect in the solid-state structure of the silver(I) salt of the icosahedral carborane anion, which is also reflected in the n B NMR of ( r f - benzene)Ag[II-l] (II-5). The asymmetric rf

C4

Figure 2.2 Perspective view of the coordinating sphere around the silver atom in ( rjzbenzene)Ag(l-CH 3-C B uH n) (II-5) showing a portion of the infinite Ag—[anion]—Ag—[anion] polymeric chain.

18


fashion o f benzene bonding, with Ag-C bond distances of 2.460(1) and 2.698(1) A, is typical o f many silver-arene complexes . 15,32’46 The 2.671(1) A of the Ag(l)-B( 8 ) distance and the 2.613(1) A of the Ag(l)-B(9A) distance are close to the values of 2.682(5) and

2.581(6) A found in ( ^ 1-benzene)Ag(CBnHi 2 ) . 10 The solid-state structure of compound (rz'-mesityleneJAglll^] (II- 6 ) is shown in Figure 2.3. The asymmetrical unit in the unit cell is [(r71-mesitylene)Ag[II-2 ] ] 2 in which each of two five coordinate silver atoms is in a distorted square pyramidal arrangement of one f^-mesitylene and two bidentate bridging l-CHs-CBnHsCV anions. The Ag-C bonds are not exactly perpendicular to the hexagonal ring planes, but tilted outward by 3.2° for A g(l) and 0.7° for Ag(2), respectively. The Ag-C bond

C22

Figure 2 3 Perspective view of the coordinating sphere around the silver atom in (rjlmesitylene)Ag(l-CH 3-CBuH 5 Cl6) (II-6 ) showing a portion of the infinite Ag—[anion]—Ag—[anion] polymeric chain.

19


distances of 2.495(6) and 2.422(5) A are typical of those found in many silver-arene n complexes . 15'3*’46 The Ag-Cl distances range from 2.683(2) to 2.874(2) A which are comparable to those found in ( 772 -p-xylene)Ag(CB 11H6 CU) 44 or in dichloroalkane complexes of silver(I) . 30,47' 50 The average B-Cl distance, 1.795(7) A, is similar to the 1.789(3) A average in (r72 -/?-xylene)Ag(CBuH 6Cl6). It is noted that the bond distance between the silver(I) and the most electron-rich chlorine atom (Cl(12) or 0 (3 2 )) is the longest one, rather than the shortest one among all four Ag-Cl distances, and the coordination geometry of the silver atom in the C-methylated hexachlorocarborane salt differs from that in (arene)Ag(CB: i HeCls) . 44 The solid-state structure of Ag[H-3] (II-7) is almost identical with that of Ag^BnHfiBrg ) . 44 As shown in Figure 2.4, the anion (U-3) occupies a site of symmetry m, and the silver atom sits at an inversion center. The six coordinate octahedral geometry about silver is very similar to that found in the complex ion [Ag(CBnH 6 Br6)i ] \ 12 with the metal atom bonding to three bromine atoms from

Figure 2.4 Perspective view of the coordinating sphere around the silver atom in Ag(lCH 3-CBnH 5Br6) (U-7) showing a portion of the infinite Ag—[anion]—A g—[anion] polymeric chain. 20


each of two bridging l-CH 3 -CBuH 5 Br6' ions. The bromine atom attached to B(12) is shared by two silver ions. Both the average Ag-Br distance of 2.858 ( 1 ) A and the average B-Br distance of 1.954 (14) A are close to those found in Ag(CBnH 6 Br6 ). These results imply that unlike the previous two cases, the methyl group on hexabromocarborane cage does not affect the coordination geometry of silver atom in the silver(I) salt of hexabromocarborane anion. In the solid-state structure of Ag[H-4] (11-8) the silver atom is complexed by four iodine atoms from two bidentate bridging anions 11*4 in a distorted-tetrahedral arrangement (Figure 2.5). However, in the molecular structure of the closely related analogue, Ag(CBuH 6 l 6 ), the silver atom is coordinated to five iodine atoms in a distorted-square-pyramidal geometry .44 It again shows the effect of methyl substituent on the solid-state structure of the silver(I) salt of hexaiodocarborane anion. The bond formed from 1(12) to silver is the longest, rather than the shortest among four Ag-I bond distances. The Ag-I distances vary from 2.798(2) to 2.872(2) A which fall in the range 2.777(4) - 3.306(5) A for Ag(CBnH 6 l 6 ) and diiodoalkane complexes of silver(I ) . 49' 51 The average B-I distance of 2.178(11) A is very close to that of 2.179(30) A in Ag(CBnH 6 l6 )-

21


Figure 2.5 Perspective view of the coordinating sphere around the silver atom in Ag(lC H 3-C B iiH sI6) (H- 8 ) showing a portion of the infinite Ag-••[anion] ••-Ag-••[anion] polymeric chain. In summary, C-methylation of the icosahedral carborane anions can result in a change not only in the solubility but also in the molecular structure of silver(I) salts of carborane anions.

Figure 2.6 Stereoscopic view of (rfJ-benzene)Ag(l-CH 3-CBnHn) (II-5). 22


Figure 2.7 Stereoscopic view of (rj 1-niesitylene)Ag[ 1 -CH3-CBj iHsC16] (H-6).

Figure 2.8 Stereoscopic view of A g[l-C H 3-CBnH 5 Br6 ] (U-7).

23


Figure 2.9 Stereoscopic view of Ag(l-CH3-CBuH5l6) (H- 8 ).

24


Chapter 3 Synthesis and Structural Characterization o f Highly Chlorinated, Brominated, Iodinated Icosahedral Carborane Anions: 1-H-CBnXn', l-C H j-C B nX n' (X = Cl, Br, I); 1-Br-CBiiBru' It has been well-documented that the 7-12 hexahalogenated derivatives, CBiiH6X6‘ (X = Cl, Br, I), are larger, more thermodynamically stable, more chemically inert, less coordinating and less nucleophilic than the parent CBuHta' ion.15 They play a very important role in stabilizing coordinatively unsaturated cations such as the silylium ion (R3Si+),IS21 the four-coordinate tetraphenylporphyrinatoiron(III) ion (Fe(tpp)+),12 fullerene cation (C 76+) , 41 hydronium ion (Hq04+)»“ and in enhancing the reactivity of organolanthanide cations.43 However, these anions along with the very recently reported polyfluorinated32'33 and permethylated25 analogues are still not the ideal weakly coordinating anions in terms of the coordinating ability18'21'32 and the stability towards oxidant-5'"6 or extremely strong electrophiles.43 Therefore, the search for the most stable, the least coordinating and soluble anion is of great interest and a challenging target. It has been known that the halogenation of CB 11H 12' leads to not only increased stability but also decreased nucleophilicity . 15-38 The origin of this less coordinating ability may lie in a steric effect, that is, the five halogen atoms in the pentagonal belt (7-11 positions) can prevent the coordination of the most basic one (the *

t S 18 ^ I 3 8

the cation. '

'

1 2 -halo

substituent) to

From this point of view, it seemed logical that the highly halogenated

icosahedral carborane anions might be the more stable and even less coordinating anion than other derivatives. On the other hand, highly iodinated carboranes are a new class of X-ray contrast agents .52 All of these features have driven us to initiate a program to carry

25


out the systematic studies on the halogenation of carborane anions and to search for the least coordinating anions. We report here the systematic studies on highly chlorination, bromination, and iodination of icosahedral carborane anions CBnHia" and I-CH3C B „H „\

3.1 Attempted Synthesis o f per-Halo Icosahedral Carborane Anions Perchlorinated, perbrominated or periodinated polyhedral boranes are known and were readily prepared from the reaction of the polyhedral analogues with an excess amount of N-chlorosuccinimide, iV-bromosuccinimide, or iodine, respectively.53 Under similar or more vigorous reaction conditions, however, the chlorination or bromination of C B uH n' did not proceed to completion, giving a mixture of polyhalocarborane anions. For example, treatment of C B u H ^ ’ with large excess amounts of chlorine gas in glacial acetic acid or CCI2 HCCI2H at 90 - 120°C for 1 month afforded a mixture of nona-, decaand undeca-chlorocarborane anions, CBnCl*Hi2 -x’ (X = 9-11), in approximate 3:5:2 ratio based on analyses of the negative-ion MALDI MS spectra. Addition of the Lewis acid catalyst such as AICI3 into the reaction system or extension of the reaction time can only slightly change the molar ratio of each component, but cannot result in the completion of this reaction. Similarly, reaction of CB 11H 12' with large excess amounts of bromine in reflux glacial acetic acid or CCI2 HCCI2 H or triflic acid for 4 weeks gave a mixture of hepta-, octa-, and nona-bromocarborane anions CBiiBrxH 12 -x' (X = 7-9), in approximate 4:6:1 ratio based on analyses of the negative-ion MALDI MS spectra. This reaction did not proceed to completion even with the aid of A1C13 or an UV lamp. However, treatment of C B uH n' with large excess amounts of IC1 in CCLHCCLH at 150°C produced 1-HC B nIu' in 56% yield ; 52 reaction of CBuHu ’ with the diluted F2 gas at room temperature

26


afforded 1-H-CBnFn ' . 34 it seems that both the halogenation reagents and halogen substituents on the cage could affect the results of these halogenation reactions. On one hand, the electron-withdrawing nature of the halogen atoms can reduce the electron density of the cage so as to slow down or perhaps inhibit the electrophilic substitution reactions of the remaining B-H bonds of the carborane anion; on the other hand, the stronger halogenation reagent can promote such electrophilic substitution reactions. In case of the halogenation reagent being identical, the overall electronic effect of substituents on the carborane cage plays an important role in the halogenation of carborane anions. It is therefore logical to introduce an electron-donating group onto the cage to balance the electronic effects caused by the halogen substituents in order to promote the electrophilic substitution reactions of B-H bonds. 3.2 Synthesis of per-halo Carborane Anions Direct chlorination o f I-CH3-CB11H11" in glacial acetic acid at 85-90°C for one week led to the isolation of the single product l-CH 3-C B n C lif (IU -i) in 85% yield.

Methylation of the C-H bonds of polychlorocarborane anions C B uC lxHi2-x' (X = 9-11) using the general procedure for C-alkylation 16 and followed by the direct chlorination can also generate the single product 111*1 in high yield. These results indicate that the

presence of methyl group on the carborane cage is critical for converting all BH to BCl vertices, probably due to its electron donating ability that can increase the overall electron density of the cage and activate the B H vertices closer to the CH vertex. Similarly, treatment of I-CH 3-CB 11H 11' with an excess amount of IC1 in triflic acid at 150°C for 10 days afforded I-CH3-CB11I11' (IH-3) in 64% yield. If CCI2HCCI2H was used as a solvent

instead, the above iodination reaction proceeded slowly.

27


The structure of III-l in [Me3N H ][U I-l] (111-8) is shown in Figure 3.1. This anion has crystallographically imposed C 3 symmetry which prohibited differentiation of the carbon atom from the boron atoms within the cage. The exohedral CH 3 group is thus completely mixed up with the eleven chlorine atoms of the cage anion. The average B-Cl bond distance of 1.767(10)

A

is shorter than the 1.803(9)

A

average in Pr^SiO-H-

CBhH 6C16) .21 The distances between the centers of pairs of the antipodal chlorine atoms (Cl—Cl diameters) fall in a narrow range 6.937 to 6.947

A.

A with an average value of 6.942

indicating that I II -l has an almost perfect spheroidal shape. With 1.75

der Waals radius o f Cl, 54 the average C l—Cl diameter of III-l is 10.422

A for the van

A. This size

is

comparable to that of the C«) molecule which has an average C—C diameter of 7.074 or 10.474 A after adding the van der Waals radii of its C atoms.53

Figure 3.1 Perspective view of III-l in [Me 3NH][IU-l] (III- 8 ). Note that the C and B atoms of the icosahedral cage are indistinguishable, and the exohedral methyl group is completely scrambled with the eleven Cl atoms. The Cs salt of III-l has high thermal stability, with no decomposition up to 260°C. It is highly soluble in donor solvents such as acetone, acetonitrile, ether, and water 28


a n d is

also somewhat soluble in arenes. Like its parent I-CH3-CB11H11' ion, 25 Cs[III-l]

s h o w s no

oxidation wave up to 2.0 V in acetonitrile ([Bu4 N][PF6]; Pt; ferrocene, 0.45 V)

(CBuMeu': 1.6 V in acetonitrile) . 25 Unlike the chlorination and iodination reactions, under similar or more vigorous reaction conditions, bromination of l-CH3-CBnH u did not proceed to completion, giving a mixture of octa-, nona-, deca-bromocarborane anions l-CH 3-CBuBrxHu-x~(X = 8-10), in approximate 1:6:2 ratio based on analyses of the mass spectra. The results show that the electron-donating methyl group can only help to put one more bromine atom onto the carborane cage as compared to the bromination of its parent CBuHn" ion. Lewis acid catalyst such as AICI3 does not promote the reaction to give a single product. In order to prepare l-CH 3-CBu B rif, a stronger bromination reagent and/or the even more vigorous reaction conditions are needed. Fractional crystallization of Ag(l-CH 3-CBnH u-nBrn) (n = 8-10) from a hot pxylene solution containing a very small amount of MeCN gave X-ray-quality crystals of (p-xylene)Ag(l-CH 3-CBuHBrio) (HI-9) which may be the least soluble salt among the others so as to crystallize out first. (/>-xylene)Ag( 1-CH 3-CB 11 HBrio) (UI-9) has a fivecoordinate silver atom in a propeller arrangement of one rj2-p-xylene and two bidentate bridging I-CH 3-CB 11HBrio’ ions (Figure 3.2), which is similar to the solid-state structure of (r72-p-xylene)Ag(CBnH 6 Cl6 ) .44 The asymmetric r f fashion of p-xylene bonding, with Ag-C bond distances of 2.485 (5) and 2.514 (5)

A,

is typical of many silver-arene

complexes.IS,32,44,46a The Ag-Br distances range from 2.818 (2 ) to 2.972 ( 2 ) average value of 2.889 (2 )

A

A

with an

which can be compared with those found in the silver(I)

salts of brominated carborane anions. 12,30'44 Among four Ag-Br bond distances, the Ag-

29


Br(12) is the shortest one, perhaps reflecting that this bromine atom is still the most basic one .44 Reaction of I-CH 3-CB 11H 11' with an excess amount of bromine in triflic acid in a sealed tube at 250°C for 2 days surprisingly produced an exclusive compound I-CH 3C B uB ru' (UI-2) in almost quantitative yield according to n B NMR. This new

C4

B r9

Br12

C5

Bril Ag1 Br7A

C1A C2A

Figure 3.2 Perspective view of (p-xylene)Ag(l -C H 3 -C B 11HBrt0) (UI-9). synthetic method is so powerful, we then extend this methodology to the parent carborane anion CB uH n’. Recrystallization of Ag[III-2] (III-10) from chlorobenzene at room temperature gave X-ray-quality single crystals. Figure 3.3 shows the coordination around silver in the solid-state structure of Ag[UI-2] (III-10). Like the other silver(I) salts of icosahedral carborane anions, 10' 111’15' 16’32’44 it is a one-dimensional coordination polymer with undecabromocarborane anion acting as bridging ligands. The silver atom sits at a two-fold axes and its six-coordinate geometry is very similar to that found in Ag^BnHgBre ) 44 and in the complex ion Ag(CBnH 6 Br6 )2 \ 12 with the metal atom bonding to three bromine atoms from each of two bridging l-CH 3 -CBnBrn*. The anion has crystallographically imposed

30


C 2 symmetry which prohibits differentiation of the carbon atom from the boron atoms within the cage. The exohedral CH 3 group is thus completely mixed up with the eleven bromine atoms of the cage anion. Therefore it is not possible to distinguish the BBr vertice antipodal to carbon from other vertices. Unlike the solid-state structure of Ag(CBnH 6 Br6)44 where the most basic bromine atom attached to B(12) antipodal to carbon is shared by two silver ions, there is no bromine atom shared by silver ion in Ag[III-2] (IH-10), perhaps reflecting the steric effect and/or there is no significantly

*5 Figure 3.3 Perspective view of the coordinating sphere around the silver atom in Ag[l(111-10) showing a portion of the infinite Ag—[IH-2]—Ag—[111-2] polymeric chain. Note that the C and B atoms of the icosahedral cage are indistinguishable and the exohedral methyl group is completely scrambled with the 11 Br atoms.

C H 3- C B n B r n ]

A

is

average in Ag(CBnH 6 Br6) and the 2.879 (3)

A

electron rich bromine atom on the cage. The average Ag-Br distance of 2.848 (5) slightly shorter than the 2.862 (2 )

A

average in Ag(CBnH 6 Br6) 2' , 12 but lies in the range found in dibromoalkane complexes of silver(I): 2.816 (2 ) - 3.081 (2 ) range 1.92 - 2.05

A .30 The

average B-Br distance, 1.948 ( 8 )

A,

falls in the

A normally observed in the complexes of CBnHeBre’ anion. 12,19' 20,44

Under the sealed tube reaction conditions, treatment of CB 11H 12’ with an excess amount of bromine in triflic acid at 200°C for 4 days generated 1-H-CBuBrn

31


(IH-5)

exclusively. If the reaction temperature was increased up to 250°C and kept at this temperature for

6

days, the C-H bond in IH-5 was also brominated to give a

perbrominated carborane anion l-Br-CBnBru‘ (HI-7). Figure 3.4 shows the progress of this reaction followed by llB NMR. Interestingly, treatment of CBnBrn" with an aqueous solution of AgNCb at room temperature gave l-H -CBnBru ' quantitatively according to 11B NMR. The mechanism of this debromination reaction is not clear. But it may involve a redox reaction. The X-ray-quality crystals of [Me3NH][HI- 7 ] (IU -I1) were grown from a saturated diethyl ether solution at room temperature. There are two crystallographically

Figure 3.5 Crystallographically independent molecule in the unit cell of [Me3NH][l-Br-

CBuBrn] (IU-11). independent molecules in the unit cell as shown in Figure 3.5. The carbon and boron atoms of the icosahedral cage in 1-Br-CBuBrif anion are indistinguishable due to the

32


crystallographically imposed m symmetry, and they are represented by three independent boron atoms B(l), B(2) and B(4). The average B-Br distances (2.926 (5) and 2.924 (5) and B-B distance (1.781 (7) and 1.784 (7)

A)

A)

all fall in the range normally observed in

the 12-vertex brominated carborane anions . 15*16,18' 21,44 This anion has an almost perfect spheroidal shape with an average Br-Br diameter of 7.24

A, or

11.14

A

after adding the

van der Waals radius of Br .54 The X-ray-quality crystals were obtained from the slow evaporation of a water/acetone solution of Cs[III-5] (111*12) at room temperature. Figure 3.6 shows the coordination around Cs cation in the solid-state structure of Cs[III-5] (IH-12). Again, the carbon and boron atoms of the icosahedral cage in 1-H-CBnBrn* anion are indistinguishable due to the crystallographically imposed C 3 symmetry, and they are represented by four independent boron atoms B(l) to B(4). The C-H bond is thus completely mixed up with the eleven B-Br bonds of the cage anion. The average B-Br distance of 1.924 (4)

A

can be compared to those normally observed in the

1 2 -vertex

brominated carborane anions. 15"16,18*21,44 The Cs atom is disordered over two sets of positions with 0.5:0.5 occupancies. It coordinates to the six bromine atoms from three carborane cages with the Cs-Br interatomic distances ranging from 3.708 (1) to 3.757 ( 1 )

A

that are similar to those found in Cs(12-Br-l-CBnH u ) . 16 Thus Cs[IU-5] (111*12) is

best described as a simple ionic salt.

33


l-Br-C3|,3.-;,'

i------ i--- r •5 -10 -15 -20 -Z5 pprr* Figure 3.4 Progress o f the reaction of Cs[l-H -CB nBrn ] with Br2 followed by n B NMR. 10

5

0

34


B r2 c

C s t ^ ''" Br39 Br3

Br2a

Br1 Br4 ,Br2

Figure 3.6 Perspective view of the coordinating sphere around the Cs cation in Cs[l-HCBuBrn] (III-12). Note that the C and B atoms of the icosahedral cage are indistinguishable and the H atom is completely scrambled with the 11 Br atoms. Under the similar reaction condition, a mixture of CB 11H 12', an excess amount of IC1 and triflic acid was sealed in a pyrex tube and then heated at 200°C for 2 days to give an unprecedented product 1-H-CBuCln' (IU-4) in high yield, which offers a new method to prepare undeca-chlorocarborane anion. On the other hand, in the absence of triflic acid, the same reaction gave the sole product 1-H -C BnIu' (III- 6 ). Similarly treatment of 1CH3-CBhH u‘ with an excess amount of IC1 in a sealed tube at 220°C for 2 days produced a pure compound l-CH 3-C B u Iif (III-3). If this reaction was performed in a triflic acid solution for 2 days, a major compound of

1 -CH3-CBuC 16 Is'

plus a small

amount of 1 -CH3-CB hC 1u.xIx' (x = 4, 3) were detected by the negative-ion MALDI MS

35


spectroscopy. To gain some insight into these reactions, treatment of l-H -C B nlu' with an excess amount of IC1 in triflic acid under the same reaction condition mentioned above produced compound IU-4 exclusively. On the basis of the above results, a mechanism may be proposed. The electrophilic substitution of CB 11H 12’ with IC1 gives the intermediate 1-H-CBuIu', followed by the nucleopbilic substitution to generate 1-HCBnClii' which is promoted by the strong triflic acid. In case of I-CH 3-CB 11H 11', the electron-donating methyl group could slow down the nucleophilic substitution reaction so that the partially substituted products were detected. The reaction condition of lithiation of 1-H-CBuXn’ is just as well as that of the parent CBu Hi2" ion . 16 For example, compound 1-H -C B uC lif can be easily lithiated with /z-BuLi, and treatment of the lithio species with CH 3 I leads to C-methylated product 1CH 3-CB 11CIH' (III-l). In principle, C-alkylated product of the type 1-R -C B nG u’ could be prepared in the same manner. Since the solubility of these anions is dependent upon the substituent R, thus a variety of new weakly coordinating anions with different solubility would be available for various purposes. All of the above synthetic routes for highly halogenated carborane anions are summarized in scheme 3.1. These highly chlorinated, brominated and iodinated icosahedral carborane anions were fully characterized by ‘H, i3C, llB NMR, negative-ion MALDI MS and IR spectroscopy. Some were further confirmed by single-crystal X-ray analyses. They are quite thermally stable, no decomposition up to 250°C. They are also stable in very strong acid such as triflic acid and strong base such as NaOH. No new peak was detected by llB NMR if treatment of l-CH 3 -CBuXn' with a saturated aqueous solution of NaOH at 90°C for 24 hours.

36


The silver salts of various carborane anions were readily achieved by treatment of their sodium salts with 1.2 equiv of AgNC>3 in water solution or a mixture of water/acetone. The solubility of these silver(I) salts in various solvents are similar to those of hexahalocarborane analogues . 15 n B NMR is an extremely useful technique for the characterization of boron compounds. Figure 3.7 shows the proton-coupled UB NM R spectra of

compounds

[MejNHjfl-CHa-CBnXn] (X = Cl, Br, I) and [Me3N H ][l-C H 3-CBiiH u l in d6- acetone. Both proton-coupled and proton-decoupled IlB NMR spectra of l-CH 3-CBnX n' are identical, and they all exhibit typical 1:5:5 splitting pattern, which are consistent with undeca-halocarborane anions and Csv symmetry. The complete conversion of BH vertices into B X vertices is also indicated by the absence of the characteristic B-H absorption (ca. 2600 cm '1) in their IR spectra. The presence of the CH 3 substituent on the cage is clearly shown by !H and proton-coupled 13C NMR spectra as well as the negative-ion MALDI MS spectra.

37


Scheme 3.1 Synthetic routes for highly halogenated carborane anions

HI-6

m-7 ICI/CF3 SO 3H 200°C, 2 d sealed tube.

IC1 ' 200°C, 2 d sealed tube

2/ c f 3 s o 3h 250°C, 6 d sealed tube

ICI/CF3 SO 3H — -— ■-----------------200°C, 2 d sealed tube

AgNQ 3

Br2/CF 3S 0 3H 200°C, 4 d sealed tube 1) nBuLi 2) CH 3 I

1) nBuLi 2) CH3 I c i 2/ c h 3 c o 2h 90°C, lweek. CH

III-5

BrVCF3 S 0 3H W 250°C, 2 d sealed tube ICI/CF3 SO 3H 150°C, 10 d, or IC1, 220°C, 2 d sealed tube

1) nBuLi 2) CH 3 I

CH

K

Cl,,

m-i

HI-2 III-3

38


X= H

^

jvj

A.

X»f

JU I

i

i

i

10

5

0

-5

V_/ 1------- 1-------- 1-------- 1 -10

-15

-20

-25 ppm

Figure 3.7 Proton-coupled UB NMR spectra of compounds [Me3NH][l-CH 3-CBuX u] (X = H, Cl, Br, I) in de- acetone.

39


As expected for undeca-halocarborane anions 1-H-CBnXn' (X = Cl, Br, I), both proton-coupled and proton-decoupled

11B NMR

spectra are identical with typical 1:5:5

splitting pattern (Figure 3.8). lH, proton-coupled I3C NMR, IR and negative-ion MALDI MS spectra all support the composition of 1-H -CBnX n’. By comparing Figures 3.6 and 3.7, it is interesting to note that after converting CH vertice into CCH 3 vertice, the 11B chemical shifts of ten BH vertices from 2 -1 1 positions in I-CH 3-CB 11H 11' become identical. Consequently, the differences in n B chemical shifts between two pentagonal belts in l-CH3-C B nX if are smaller than those in 1-H-CBnXif, indicating the electrondonating effect of CH3 group. Similar results are also observed in their 13C NMR spectra. 3 3 Conclusion The syntheses of highly chlorinated, brominated and iodinated icosahedral carborane anions were achieved via the sealed tube reactions or by introducing an electron-donating group into the carborane cage (for compound III>1). The sealed tube method can force the halogenation reactions of the parent carborane anion C B n H a' to proceed to completion, shorten the reaction time and increase the reaction yield. This is a very convenient and useful new method, and may be applicable to other carboranes or polyhedral boron clusters. Like the parent carborane anion CB1 1 H 1 2 ", 1-H-CBnXn' (X = Cl, Br, I) can be lithiated with butyllithium, and treatment of the lithio species with alkyl halides leads to C-alkylation in 1-R-CBnXn* derivatives. By the combination of both C- and Bderivatization, a variety of icosahedral carborane anions could be generated.

40


I 10

1--------1-------- i--------i 5

0

-5

-10

i-------- i--------1 -15

-20

-25 ppm

Figure 3.8 Proton-coupled UB NMR spectra of compounds [Me3NH][l-H-CBuXu] (X = H, Cl, Br, I) in d6- acetone.

41


Chapter 4 Weakly Coordinating Nature of Different Halogen Atoms on an Icosahedral Cage. Synthesis and Structural Characterization o f Mixed-halo Icosahedral Carborane Anions, H-l-CBuYjX* During these years, various derivatives of C B uH u' and CB9 H 1 0 anions (Bhalogenated, B-alkylated and B-hydroxylated) have been made 15 l6,:u' M J 2 ' 35’37’45,52’56' S9 in order to search for the most useful and the least coordinating anion. As mentioned in the previous chapters, they are playing a very important role in olefin polymerization 39 and stabilizing highly reactive cation.12' 14-‘s-22-24-35-36-38-40^ 1-43 These anions are all prepared by electrophilic substitution of B-H bonds of the carborane cage. Since the CBu or CB 9 cage is polarized, substitution occurs preferentially at the boron end of the cluster. Therefore, partially substituted carborane anions have been known for many years while full substitution has only been accomplished very recently. In all known fully substituted ones , 25-26'34,37,4552’573 each of them consists of only one kind of B-X vertexes. Those anions with more than one type of B-X vertexes have remained largely unexplored .27*’42,60 An effective methodology for the preparation of perhalocarborane anions has been developed in our laboratory,57* which makes it possible for us to synthesize mixed-halo carboranes. It has been suggested that in the perhalocarborane anions such as 1-HCBiiX if, halogen atoms at the lower part (7-12 positions) are more coordinating than those at the upper belt (2 - 6 positions),57* and their coordinating ability follows the order: F < Cl < Br < I.57* What is the possible coordinating site in a mixed-halo carborane anion such as l-H-CBuYsX^’? I herein report the synthesis, structural characterization, and

42


weakly coordinating nature of several mixed-halo carborane anions, l-H-2,3,4,5,6-Ys7,8,9,10,11,12-X6-CB u " (X, Y = halogen atoms). 4.1 Synthesis of Mixed-halo Icosahedral Carborane Anion, l-H-CBnYsX* The preparation of perhalogenated c/oso-carborane anions, 1-R-CBuXn' has been described in Chapter 3 by using a newly-developed sealed tube method .573 This method can also be employed to make mixed-halo carborane anions after some modifications. A mixture of l-H-CBuHsCU’, excess Br2 , and triflic acid was sealed in a Pyrex tube and then heated at 220°C for 2 days to give a sole product H-l-CBuBrsCV (IV-1). Under similar reaction conditions, however, bromination of I-H-CB 11H5 I6 ' led to a 1:1 mixture of l-H -CBuBrn ‘ and 1-Br-CBnBru" on the basis o f spectroscopic analyses ,573 and the final product of 1-Br-CBuBrn' would be isolated after a prolonged reaction (vide supra). In the absence of triflic acid, this reaction resulted in the formation of a mixture of l-H -C BnBrxIii-x‘ (x =

6

- 9) based on the analyses o f MS spectroscopic data. It

suggested that triflic acid could enhance the reactivity of Br2 and/or activate the carborane anion leading to a complete replacement of all B-H and B-I bonds by B-Br bonds. This may also imply that the solvent could play an important role in this type of reactions. In order to prepare the mixed-halo anion of l-H -C B nB r 5 I6' (IV-3), a suitable solvent is desirable. After many experiments, it was found that CHCI2CHCI2 was the best choice. Treatment of I-H-CB 11H5 I6 ' with excess Br2 in CHCI2 CHCI2 in a sealed tube at 180°C for 3 days yielded the anion IV-3 in high yield. Treatment of l-H-CBuHsBr6* with excess IC1 in triflic acid or in the absence of triflic acid in a sealed tube at 220°C for 2 days gave the sole product l-H-CBnClsBre"

43


(IV-2) in high yield. No l-H -C B nl 5 Br6’ was isolated. Under the same reaction conditions, reaction of l-H-CBuHsCV with excess IC1 generated undecachlorocarborane anion of l-H -C B n C lu \ and no iodo species was isolated either. It is noteworthy that treatment of l-H -C B u H if with excess IC1 afforded 1-H-CBuCln' in triflic acid or 1-HC B n Iif in the absence of triflic acid .571 In these reactions, 1-H-2,3,4,5,6-I5 -CBuX6' may serve as an intermediate, followed by nucleophilic substitution to give 1-H-2,3,4,5,6 -CI5CBnX 6 as the final product.571 The electrophilicity of iodine can be greatly enhanced in triflic acid under a sealed tube condition.(vide infra in Chapter 5) Accordingly, l-H -C B nl 5 Br6' (IV-4) and 1-HCBiiIsC16‘ (IV-5) were prepared in high yield by treatment of l-H -C B n H5 Br6' or 1-HCBnHsCl6" with excess I2 in triflic acid in a sealed tube at 220°C for 4 days. Reaction of IV-4 or IV-5 with excess IC1 in triflic acid in a sealed tube at 220°C for 2 days afforded IV-2 or 1-H-CBuCln', respectively, which supports previously proposed reaction pathway. Although l-H-CBiiClsBr6' (IV-2) was prepared by reaction of l-H-CBuHsBre’ with excess IC1 in a sealed tube at 220°C, treatment of l-H -C B nH sV with excess IC1 in triflic acid or in the absence of triflic acid always gave perchlorinated species, 1-HCBuClu . Direct chlorination of l-H-CBnHsk* with excess CI2 in glacial acetic acid or with excess NCS (N-chlorosuccinamide) in CHCI2 CHCI2 resulted in a mixture of products containing B-Cl, B-I and B-H bonds on the basis of NMR, IR and MS analyses. All attempts to prepare I-H-CBiiCIsV anion failed. Scheme 4.1 summarizes all transformations described in this chapter.

44


These mixed-halo carborane anions were fully characterized by lH, l3C, and UB NMR, negative ion MALDI MS, and IR spectroscopy. Some were further confirmed by single-crystal X-ray analyses. They are thermally very stable, with no decomposition up to 250°C. They are also stable in very strong acids such as triflic acid and strong bases such as NaOH. The silver salts of various carborane anions were readily prepared by treatment of their sodium salts with slightly excess amounts of AgNC>3 in aqueous solution or a mixture of water/acetone. The solubilities of these salts in various solvents are similar to those of perhalogenated analogues, and follow the order: Cl > Br > I. On the other hand, the solubilities of the silver(I) salts depend mainly on the lower-belt substituents, i.e. the solubility of AgJH-l-CBuBrsCk] resembles that of Ag[H-l-CBnClu ] or Ag[H-lCBnH 5CI6] but it is better than that of Ag[H-l-CBnCl 5 Br6 ], Ag[H-l-CBu Bru] or Ag[Hl-C B nH sBr6]. Figures 4.1, 4.2 and 4.3 show the proton-coupled n B NMR spectra of [Me3NH][l-H-CB„X 5Cl6] (X = H, Cl, Br, I), [Me3NH][l-H-CBnX 5Br6] (X = H, Cl, Br, I) and [Me3NH][l-H-CBnXsl 6 ] (X = H, Br, I) in acetone-rf6 >respectively. As expected, both proton-coupled and proton-decoupled UB NMR spectra of these anions are identical. From these spectra, it is very clear that the UB NMR spectra are very sensitive to the substituents on the carborane cage. Therefore, these halogenation reactions can all be monitored by n B NMR. Since the complete conversion of B-H vertexes into B-X vertexes is also indicated by the absence of the characteristic B-H absorption (ca. 2600 cm'1) in the IR spectra, IR is another useful tool to follow these reactions. The

45


composition of new anions is further supported by the lH and

C NMR as well as MS

spectroscopy.

A

A_

X= c I

X = 3r

10

5

0 - 5

-10

-15

-20

-25

ppm

Figure 4.1 Proton-coupled UB NMR spectra of [Me3 NH][l-H-CBuXsCl6] (X = H, Cl, Br, I) in acetone-d6-

46

Reproduced with permission o f the copyright owner. F urth er reproduction prohibited without permission

X = H

A

X = Cl

J lj

X = Br

X=

10

3

0

10

-15

-20

Figure 4.2 Proton-coupled UB NMR spectra of [Me3N H ][l-H -CBuX 5 Br6 ] (X = H, Cl, Br, I) in acetone-^-

X= H

l'f

X = Br

X= I

J\__ I 10

1

!

i

I

I

i

I

5

0

-5

-10

-15

-20

-25

ppm

Figure 4.3 Proton-coupled n B NMR spectra of [Me3NH][l-H-CBnX 5 I6] (X = H, Br, I)in acetone-t/6.

47


4.2 Coordinating Ability It has been documented that the 29Si shift of compound RsSiY is very sensitive to the coordinating nature of the counterion y*.18'21'34 We probed the weakly coordinating nature of 1-H-CB„C1„' (III-4), l-H -CBnBr5Cl6- (IV-i), l-H -CB,,CI5Br6- (IV-2), 1-HCBu l 5 Br6"(IV-4) and l-H-CBuBrsIe' (IV-3) by generating Pr'3Si(carborane) in tolueneds following the literature procedures.18*21 Within a period of 24 h at room temperature, the “9Si resonance for Pr^SiH at Cl > F; and (3) the coordinating ability of various mixed-halo carborane anions 1-HCBnYsXo* are mainly dependent upon the nature of the substituents at 7 - 12 positions, namely X atoms, and the contributions from the substituents Y are relatively small. The slightly more downfield 29Si chemical shift of Pr'3Si(l-H-CBn Br5Cl6) than that of Pr'3Si(l-H-CBnCl[i) may be rationalized in terms of solvation energy difference of these two anions in toluene solution and/or anion replacement by toluene molecule.

48


Table 4.1 Downfield 29Si Chemical Shifts Compound

Solvent

3](THF) (V-10) by X-ray analysis. X-ray analyses reveal that it is a one-dimensional coordination polymer with both nonabromocarborane and nitrate anions acting as bridging ligands. Each asymmetric unit consists of two H-l-CB 9Br9‘ anions, one NO 3 ' anion, two benzene, one THF, and three Ag+ cations. Each Ag has a unique coordination environment although they are all fivecoordinated (Figure 5.2). The A gl is in a propeller arrangement of one //-benzene and two bidentate bridging H -l-CB 9 Br9’ ions. The Ag2 is bound to one bidentate H -lCB9 Br9' ion, one bidentate N O 3 ' ion and oxygen atom of the coordinated THF molecule in a distorted-square-pyramidal geometry. The Ag3 adopts a highly distorted-squarepyramidal arrangement of one ^ ‘-benzene, one bidentate H-l-CB 9 Br9‘ and one bidentate N 0 3‘ ion. It is not common for a silver(I) complex to have both rf- and //-benzene coordination .65 The average A gl-C (//-benzene) distance of 2.563(6) than the Ag3-C (//-benzene) distance of 2.510(6)

A.

A is slightly longer

The average Ag-Br distance of

3.140(2) A and B-Br distance of 1.923(5) A can be compared to the corresponding values found in (//-benzene)Ag(H-l-CB 9Br9) (V-9). It is very interesting to note that the bromine atom from the upper tetragonal belt such as B rl4 can also coordinate to Ag+ ion, which is a brand new coordination mode that has never been observed before in the silver(I) salts of any carborane anions.

65


Figure 5.2 Perspective view of the coordinating sphere around the Ag atom in (r f benzene)( r; 1-benzene)Ag 3(H -l -CB9 Br9>2(N 0 3 XTHF) (V-10). X-ray-quality crystals were obtained from slow evaporation of a saturated CH2CI2 solution of Cs[V-3] at room temperature. Figure 5.3 shows the coordination around the Cs cation in the solid-state structure of Cs[V-3](H 2O)0j (V -ll). Water molecule exhibits positional disorder and is assigned half site occupancy. Therefore, one half of the Cs atoms in the solid-state structure coordinate to the eight bromine atoms from three carborane cages, and other half Cs atoms have one additional water coordination with a formal coordination number of 9. The Cs-Br interatomic distances range from 3.783(1) to 3.936(1)

A

with an average value of 3.879(2)

A,

which is longer than those found in

Cs(H -l-CBnBrn) (III-12 ) 57 and Cs(12-Br-l-CBnHn ) 16 probably due to the higher coordination number of the Cs atom in the present compound.

66


Treatment of H-I-CB9H9’ with excess IC1 in triflic acid or in the absence of triflic acid in a sealed tube at 220°C for 3 days gave the same product H-I-CB9CI9' (V -l); no HI-CB9I9' was isolated, which differ significantly from the H -l-C BnH if case .21,52,57 It is noted that reaction of H -l-C BnH if with neat IC1 in a sealed tube afforded an iodinated product H-l-CBnlii* (HI-6).3 These results may imply that

Br3

Br7A

Figure 5.3 Perspective view of the coordinating sphere around the Cs cation in Cs(l-HCB9Bry)(H20 )o^ (V -ll).

H-I-CB9I9' is more susceptible to nucleophilic attack than H-l-CBnIu' (III-6). This hypothesis is supported by following experiments. Treatment of H-I-CB9H9' with excess IC 1 in triflic acid or CHCI2CHCI2 at 150°C for one week also generated a single product H-I-CB9CI9' (V-l). This reaction was monitored by UB NMR, IR and MS. The results

67


showed that at about 120°C, a mixture of partially iodinated and chlorinated carborane species were detected while some of the B-H bonds had not yet been converted to B-X (X = Cl, I) bonds. As the temperature was increased and the reaction time was prolonged, the chlorination was close to completion. C-alkylated product of the type R-I-CB9X9' could be prepared in a manner which is similar to that of R-l-CBuHu"-16'57 For example, reaction of H-I-CB9CI9' with n-BuU in THF, followed by treatment with benzylbromide led to the C-benzylated product benzyl-I-CB9CI9' (V-2) in high yield. It is noted that the C-lithiated species Li[Li-lCB9CI9] is very soluble in THF while Li[Li-l-CBnClu] is only sparely soluble. A cationic exchange reaction in a mixed solvent of acetone/water afforded [(C6H 5CH 2)NMe3][V-2 ] (V-12) in 90 % yield. X-ray-quality crystals were grown from a saturated CH2C12 solution by n-hexane vapor diffusion at room temperature. The solidstate structure of [(C6 H5CH 2)(CH 3)3N][V-2 ] is shown in Figure 5.4. This is an ordered structure with normal B-B, B-Cl and C-B distances. For example, the average B-Cl distance of 1.777(4) A is comparable to the 1.767(10) A in [Me3NH][CH3- 1-CBi 1Cl 11 ] (IU- 8 ) . 45 To prepare periodinated species, a new method is definitely needed. It has been reported that I2 is a relatively weak iodinating agent and exhaustive iodination of H -lC B iiH if with I2 led only to the 7,12-diiodo species. 17 The electrophilicity of iodine could be greatly enhanced in triflic acid under the sealed tube condition. Accordingly, we found that treatment of H-I-CB 9 H 9" with excess I2 in triflic acid in a sealed tube at 180°C for 4 days led to almost quantitative yield of the H-I-CB 9 I9' (V-4) anion. The H-l-CBuIu* (III- 6 ) anion could also be prepared under the same reaction condition. This is probably

68


the most convenient and effective method to prepare periodocarborane anions. The corresponding perchloro and periodo carborane anions, NH2-I-CB9CI9' (V-5) and NH2-ICB9I9' (V-7), could be prepared under similar reaction conditions mentioned above. Under proper reaction conditions, deamination of NH2-I-CB9X9' could be achieved. Reaction of NIU-l-CBgHg’ with NaNOj/HCl at 0 °C, followed by treatment with H3PO2 led to a quantitative yield of H-I-CB9H9'. However, the deamination of NH2I-CB9X9' (X = Cl, Br) was more difficult than its parent anion NH2-I-CB9H9', which led only to a mixture of NH2-I-CB9X9" and H-I-CB9X9' in a ratio of 3:2 for X = Cl and 7:3 for X = Br, respectively, according to n B NMR and the negative ion MALDI mass spectroscopy. We have previously proposed that the formation of H-I-CB9CI9' (V -l) may be through the electrophilic substitution of H-I-CB9H9' with T giving H-I-CB9I9' (V-4 ), followed by a nucleophilic substitution with Cl'. Indeed, treatment of H-I-CB9I9' (V-4 ) with NaCl/triflic acid in a sealed tube at 220°C gave a single product H-I-CB9CI9' (V -l).

>03 as-

)CU

CI9! D 3l

C17

Figure 5.4 Perspective view of [(CeHsO^NM esKCfiHsC^-l-CBgCl,] (V-12).

69


We then examined other nucleophiles. Reaction of H-1-CB 9 I9‘ (V-4) with NaF/DMF or Me3NHF/triflic acid in a sealed tube did not proceed at 100°C or below. As the temperature was increased to 120°C, the carborane cage began to be degraded and after workup, boric acid was formed as a final product on the basis of n B NMR. It is noteworthy that the B-I bonds in H-I-CB 9 I9' remained intact if the mixture of H-1-CB9 I9 and neat CH3MgBr or CH 3MgBr/CH 3OCH 2CH 2OCH 2CH 2OCH 3 was heated at 180°C in a sealed tube for 1 week. Such reaction, however, could be promoted by Pd catalyst .58,59,1’66 Treatment of H-I-CB 9I9' with excess MeMgBr in THF in the presence of bis(triphenylphosphine)palladium(lI)

dichloride

and

copper(I)

iodide

at

reflux

temperature for 1 week gave H-l-CB 9(CH 3 )3 l 6‘ as a major product on the basis of MS and 11B NMR analyses. This reaction was then continued by adding more (Ph 3P)2PdCl2 and MeMgBr for another week, leading to a good yield of permethylated species H -lCB 9(CH3)9' (V- 8 ). It could also be achieved via a sealed tube reaction. Treatment of H -lCB 9 I9' with excess MeMgBr/THF in the presence of (Ph3 P)2 PdCI2 and Cul in a sealed tube at 25 ~ 220°C for

10

days, after workup, afforded H- 1 -CB 9(CH 3)9' in good yield.

The reaction temperature should be slowly increased and carefully controlled, otherwise the yield would be lower because the destruction of the catalyst maybe facile at high temperature. All transformations described in this section are summarized in Scheme 5.1. These highly chlorinated, brominated, iodinated, and methylated carborane anions were fully characterized by lH, I3C, and UB NMR, negative-ion MALDI MS, and IR spectroscopy. They are quite thermally stable, with no decomposition up to 240°C. They

70


are also stable in very strong acids such as triflic acid and strong bases such as NaOH or MeMgBr. Scheme 5.1 NH 2

V-7 I9 Wtriflic acid ICl/triflic acid

Br->/triflic acid

V-5

V-6

H9 NaNOVHCI/ h 3 p o 2"

H

ICl/triflic acid V-l

V-3 Brq

Br2/triflic acid 1) n-BuLi] 2) BzBr NaCl\triflic acid

I2/tnflic acid H MeMgBr (Ph3P)2PdCl2/ Cul

V-8 Me«

BF,

V-4

71


The silver salts o f various carborane anions were readily prepared by treatment of their sodium salts with slightly excess amounts of AgNC>3 in aqueous solution or a mixture of water/acetone. Excess AgNC>3 may result in the formation of a 2:1 adduct of Ag(carborane) and AgNC>3 such as Ag2(H-l-CB 9 Br 9)rA gN 0 3 (V-10). (vide supra) The solubilities of these silver(I) salts in various solvents are better than those of H -lC B nX ii' analogues.57 11B NMR is an extremely useful technique for the characterization of boron compounds. Figures 5.5 and 5.6 show the proton-coupled llB NMR spectra of [Me3NH][H-l-CB9X9] (X = H, Cl, Br, I, Me) and [Me3NH][NH2-l-CB9X9] (X = H, Cl, Br, I) in acetone-cf6, respectively. Both proton-coupled and proton-decoupled 11B NMR spectra of perhalocarborane anions are identical. Due to the different substituents on the carbon atom of the carborane cage, the differences in the chemical shifts of the lower and the upper belt boron atoms in the anions H-1-CB9X9‘ and NH2-1-CB9X9" are not the same. It is noted that the n B NMR spectrum of H -l-C B9Me9’ (V-8) exhibits a 1:4:4 splitting pattern while that of H-1-CB9I9' (V-4) displays a 1:8 splitting pattern. Therefore, the transformation from H-1-CB9I9" (V-4) to H -l-C B 9Me9‘ (V-8) can be closely monitored by n B NMR. The 13C NMR spectrum of H -l-C B9Me9' is very characteristic, showing broadening and upfield shifted resonances due to the close proximity of carbon nuclei to both n B and 10B, two nuclei with electric quadruple moment.663,67 The complete conversion of B-H vertexes into B-X vertexes is also indicated by the absence of the characteristic B-H absorption (ca. 2600 cm"1) in their IR spectra. The !H, 13C, UB NMR, IR and MS spectra all support the composition of new carborane anions. 5.2 Coordinating Ability

72


It has been documented that the 29Si shift of compound R3SiY is very sensitive to the coordinating nature of the counterion Y . 18' 2134 We probed the weakly coordinating nature

of

C6 H5CH 2 -I-CB 9 CI9 '

(V-2)

and

H-l-CBgBry'

(V-3)

by

generating

Pr'3Si(carborane) in toluene-rf8 following the literature procedures . 18"21 Within a period of 24 h at room temperature, the 29Si resonance for Pr^SiH at 6 12.1 decreased in intensity and a new 29Si resonance appeared at 8 106.0 for C 6H 5 CH 2-I-CB 9 CI9" (V-2) and 8 100.9 for H-l-CB 9 Br9' (V-3), respectively. No other 29Si resonance was observed, indicating that no halide abstraction reaction occurred or these carborane anions are stable in the presence of the strong electrophile such as cationic silicon center. Comparison of the above measured values with the Cl„N

CuiH|.iB||Brii)Ag

C2HiB||BriiAg

GiHiuBiiNBru

CHB||Bri|Cs

crystal size (mm)

0.20 x 0.20 x 0.20

0.35 x 0.25 x 0.08

0.45 x 0 .2 4 x 0 .1 4

0.22 x 0.20 x 0.16

0.27 x 0.38 x 0.52

fw

582.2

1160.09

1132.83

1149.96

1143.85

crystal system

rhombohedral

orthorhombic

orthorhombic

orthorhombic

rhombohedral

space group

K3c

/*na2|

C222,

fm m m

Zt3

a, A

12.119(1)

14.053(1)

13.986(3)

17.743(1)

9.824(1)

b, A

12.119(1)

10.895(1)

24.201 (5)

17.760(1)

9.824(1)

c, A

29.726 (2)

17.931 (1)

9.369(1)

17.767(1)

22.098 (4)

V, A3

3782 (2)

2745(1)

3171(1)

5598(1)

1847.1(5)

162

Mo K« (0.71073) Mo K« (0.71073) Mo K« (0.71073) Mo K« (0.71073) Mo K« (0.71073) radiation (k), A Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.


crystal system

triclinic

monoclinic

ntonoclinic

triclinic

space group

/'(-l)

in tic

Cc

l \ - 1)

a, A

10.207(2)

16.709(7)

10.353(6)

10.689(3)

b, A

13.402(3)

12.168(6)

23.959(1)

11.002(3)

c, A

16,351(3)

18.138(1)

15.535(9)

13.971(2)

«, dcg

90.64(3)

90.00

90.00

87.53(2)

A dcg

96.46(3)

90.17(4)

91.72(1)

79.02(1)

ft dcg

97.43(3)

90.00

90.00

74.460(9)

v, A-1

2203.1(8)

3688(4)

3851.6(4)

1553.9(6)

z

2

4

4

2

Oulcd, Mg/m1

1.828

2.048

2.825

3.341

radiation (A), A

Mo K« (0.71073)

Mo K« (0.71073)

Mo K« (0.71073)

Mo Kn (0.71073)

20 range, dcg

2 .5 -5 1 .4

4.0 - 50.0

3 .4 -5 6 .0

2 .9 -5 0 .0

H, ram'1

5.378

7.426

10.538

13.948

^(000)

1168

2144

2912

1370

no. of obsd reflns

3916

6507

6567

3769

no. of params refnd

461

380

380

289

goodness of fit

1.111

0.907

1.037

1.079

3262(1) 3084(3) 1947.8(4)

0.060

1842.5(2)

0.036

3360.4(7)

0.054 0.078


triclinic monoclinic monoclinic orthorhombic crystal system Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.

0.042 0.084 0.085 0.058 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.

Mo K« (0.710 73)

Mo K« (0.710 73) n|niujoj

radiation (A), A

Ntc


828 3469 no. of obstl rcflns Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.


CH(,B||BrjjO

Mo K« (0.71073)

formula

radiation (A), A

Mo K« (0.71073)

Cj.1j1H4BjoiMBry21Clf1.7fi

Mo K« (0.71073)

CHhBnBrJ^Oi

Mo Ka (0.71073)

CICBuBrnO

17.118(3) 17.784(1) 27.362(6) 13.595(9) 17.595(6)

2581 3916 501 1682 no. ofohstl refills


3069.1(11) 2589.6(3) 3823.2(1) 4821.8(5) 2311.2(2) Reproduced with permission of the copyright owner. Further reproduction prohibited without permission.


2086

o

r*

K/-. rs

r-* 3C c o

i/-. rr CM C

no. of observed reflections

2085

4515

XT'.

i/-.

^


Appendix III. Table of Atomic Coordinates and Thermal Parameters; Bond Distances and Angles. C hapter 2 Com pound 11-5 Atomic coordinates and thermal parameters X

Ag(l) C(l) C(2) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B(11) B(12) C(3) C(4) C(5) C(6) C(7) C(8)

38444(3) 1558(1) 496(1) 983(1) 1860(1) 3105(1) 2995(1) 1694(1) 2291(1) 3603(1) 4313(1) 3440(1) 2191(1) 3819(1) 1709(1) 2022(1) 2827(1) 3310(1) 2977(1) 2197(1)

y 11149(3) -3084(1) -3877(1) -1844(1) -1611(1) -2818(1) -3790(1) -3204(1) -704(1) -1300(1) -2646(1) -2903(1) -1691(1) -1342(1) 1644(1) 2850(1) 3583(1) 3110(1) 1900(1) 1175(1)

z

14763(3) 1854(1) 1266(1) 2440(1) 1481(1) 1462(1) 2407(1) 3008(1) 2474(1) 1877(1) 2448(1) 3402(1) 3420(1) 3077(1) 488(1) 759(1) 263(1) -493(1) -748(1) -261(1)

U(eq) 926(1) 39(1) 57(1) 43(1) 40(1) 36(1) 39(1) 44(1) 44(1) 40(1) 40(1) 44(1) 46(1) 45(1) 59(1) 70(1) 70(1) 67(1) 74(1) 69(1)

Bond lengths Ag(l)-B(8) Ag(l)-C(3) Ag(l)-C(4) Ag(l)-B(9A) C(l)-C(2) C(l)-B(2) C(l)-B(3) C(l)-B(4) C(l)-B(5) C(l)-B(6) B(2)-B(3) B(2)-B(6) B(2)-B(7) B(2)-B(l 1) B(3)-B(4) B(3)-B(7) B(3)-B(8) B(4)-B(5) B(4)-B(8) B(4)-B(9) B(5)-B(6) B(5)-B(9)

B(5)-B( 10) B(6)-B(10) B (6)-B (ll) B(7)-B(8) B(7)-B( 11) B(7)-B(12) B(8)-B(9) B(8)-B(12) B(9)-B(10) B(9)-B(12) B(9)-Ag(lA) B (10)-B (ll) B(10)-B(12) B (ll)-B (12) C(3)-C(4) C(3)-C(8) C(4)-C(5) C(5)-C(6) C(6)-C(7) C(7)-C(8)

2.671(1) 2.460(1) 2.698(1) 2.613(1) 1.526(2) 1.723(2) 1.711(2) 1.715(2) 1.710(1) 1.713(2) 1.778(2) 1.780(2) 1.765(1) 1.763(2) 1.779(1) 1.775(2) 1.762(1) 1.766(2) 1.785(2) 1.771(2) 1.763(2) 1.773(1)

1.767(2) 1.762(1) 1.777(2) 1.773(2) 1.775(2) 1.777(1) 1.770(2) 1.774(2) 1.774(2) 1.783(2) 2.613(1) 1.784(1) 1.792(2) 1.775(2) 1.376(2) 1.365(2) 1.391(2) 1.374(2) 1.377(2) 1.363(2)

175


Bond angles

B(8)-Ag(l)-C(3) B(8)-Ag(l)-C(4) C(3)-Ag( 1)-C(4) B(8)-Ag(l)-B(9A) C(3)-Ag( 1)-B(9 A) C(4)-Ag( 1)-B(9 A) C(2)-C(l)-B(2) C(2)-C(l)-B(3) B(2)-C(l)-B(3) C(2)-C(l)-B(4) B(2)-C(l)-B(4) B(3)-C(l)-B(4) C(2)-C(l)-B(5) B(2)-C(l)-B(5) B(3)-C(l)-B(5) B(4)-C(l)-B(5) C(2)-C(l)-B(6) B(2)-C(l)-B(6) B(3)-C(l)-B(6) B(4)-C(l)-B(6) B(5)-C(l)-B(6) C(l)-B(2)-B(3) C(l)-B(2)-B(6) B(3)-B(2)-B(6) C(l)-B(2)-B(7) B(3)-B(2)-B(7) B(6)-B(2)-B(7) C (l)-B (2)-B (ll) B(3)-B(2)-B(l 1) B(6)-B(2)-B(l 1) B(7)-B(2)-B(ll) C(l)-B(3)-B(2) C(l)-B(3)-B(4) B(2)-B(3)-B(4) Q l)-B(3)-B(7) B(2)-B(3)-B(7) B(4)-B(3)-B(7) C(l)-B(3)-B(8) B(2)-B(3)-B(8) B(4)-B(3)-B(8) B(7)-B(3)-B(8) C(l)-B(4)-B(3) C(l)-B(4)-B(5) B(3)-B(4)-B(5) C(l)-B(4)-B(8) B(3)-B(4)-B(8) B(5)-B(4)-B(8) C(l)-B(4)-B(9) B(3)-B(4)-B(9) B(5)-B(4)-B(9) B(8)-B(4)-B(9) C(l)-B(5)-B(4) C(l)-B(5)-B(6)

B(4)-B(5)-B(6) C(l)-B(5)-B(9) B(4)-B(5>B(9) B(6)-B(5)-B(9) C(l)-B(5)-B(10) B(4)-B(5>B(10) B(6)-B(5)-B( 10) B(9)-B(5)-B(10) C(l)-B(6)-B(2) C(1)-B(6>B(5) B(2)-B(6)-B(5) C(l)-B(6)-B(10) B(2)-B(6>B(10) B(5)-B(6)-B(10) C (l)-B (6)-B (ll) B(2)-B(6>B(11) B (5)-B(6)-B (ll) B(10)-B(6)-B(ll) B(2)-B(7)-B(3) B(2)-B(7)-B(8) B(3)-B(7)-B(8) B (2)-B(7)-B (ll) B (3)-B(7)-B (ll) B(8)-B(7)-B(ll) B(2)-B(7)-B( 12) B(3)-B(7)-B( 12) B(8)-B(7)-B(12) B( 11)-B(7)-B( 12) Ag(l)-B(8)-B(3) Ag(l)-B(8)-B(4) B(3)-B(8)-B(4) Ag(l)-B(8)-B(7) B(3)-B(8)-B(7) B(4)-B(8)-B(7) Ag(l)-B(8)-B(9) B(3)-B(8)-B(9) B(4)-B(8)-B(9) B(7)-B(8)-B(9) A g(i)-B (8)-B (l2) B(3)-B(8)-B(12) B(4)-B(8)-B(12) B(7)-B(8)-B(12) B(9)-B(8)-B(12) B(4)-B(9)-B(5) B(4)-B(9)-B(8) B(5)-B(9)-B(8) B(4)-B(9)-B( 10) B(5)-B(9)-B( 10) B(8)-B(9)-B(10) B(4)-B(9)-B( 12) B(5)-B(9)-B(12) B(8)-B(9)-B( 12) B(10)-B(9)-B(12)

105.3(1) 133.0(1) 30.5(1) 115.4(1) 135.6(1) 105.1(1) 118.5(1) 117.4(1) 62.3(1) 117.5(1) 113.9(1) 62.6(1) 119.1(1) 113.4(1) 113.5(1) 62.1(1) 119.5(1) 62.4(1) 113.6(1) 113.4(1) 62.0(1) 58.5(1) 58.5(1) 107.3(1) 105.3(1) 60.1(1) 108.4(1) 105.3(1) 108.1(1) 60.2(1) 60.4(1) 59.2(1) 58.8(1) 108.3(1) 105.4(1) 59.6(1) 108.8(1) 105.5(1) 107.7(1) 60.6(1) 60.2(1) 58.6(1) 58.8(1) 107.6(1) 104.3(1) 59.2(1) 107.6(1) 104.9(1) 107.2(1) 60.2(1) 59.7(1) 59.1(1) 59.1(1)

108.6(1) 105.0(1) 60.0(1) 107.8(1) 105.3(1) 108.6(1) 59.9(1) 60.1(1) 59.1(1) 58.9(1) 108.2(1) 105.5(1) 108.1(1) 60.2(1) 105.1(1) 59.4(1) 108.5(1) 60.5(1) 60.3(1) 107.8(1) 59.6(1) 59.7(1) 107.7(1) 107.6(1) 107.9(1) 107.7(1) 60.0(1) 59.9(1) 102.6(1) 146.4(1) 60.2(1) 81.6(1) 60.3(1) 108.6(1) 148.8(1) 108.0(1) 59.8(1) 108.4(1) 104.3(1) 108.4(1) 108.5(1) 60.2(1) 60.4(1) 59.8(1) 60.6(1) 108.0(1) 108.1(1) 59.8(1) 108.2(1) 108.7(1) 108.3(1) 59.9(1) 60.5(1)

176


B(4)-B(9)-Ag( 1A) B(8)-B(9)-Ag( 1A) B( 10)-B(9)-Ag( 1A) B( 12)-B(9)-Ag( 1A) B(5)-B(10)-B(6) B(5)-B(10)-B(9) B(6)-B(10)-B(9) B(5)-B(10)-B(ll) B(6)-B(10)-B(ll) B(9)-B(10)-B(ll) B(5)-B( 10)-B( 12) B(6)-B( 10)-B( 12) B(9)-B(10)-B(12) B(11)-B(10)-B(12) B(2)-B(l 1)-B(6) B(2)-B(ll)-B(7) B(6)-B(l 1)-B(7) B(2)-B(ll)-B(10) B(6)-B(ll)-B(10) B(7)-B(l 1)-B(10) B(2)-B(ll)-B(12) B(6)-B(ll)-B(12) B(7)-B(ll)-B(12) B( 10)-B( 11 )-B( 12) B(7)-B(12)-B(8) B(7)-B(12)-B(9) B(8)-B(12)-B(9) B(7)-B(12)-B(10) B(8)-B(12)-B(10) B(9)-B( 12)-B( 10) B(7)-B(12)-B(ll) B(8)-B(12)-B(ll) B(9)-B(12)-B(l 1) B(10)-B(12)-B(l 1) Ag( 1)-C(3)-C(4) Ag(l)-C(3)-C(8) C(4)-C(3)-C(8) Ag(l)-C(4)-C(3) Ag( 1)-C(4)-C(5) C(3)-C(4)-C(5) C(4)-C(5)-C(6) C(5)-C(6)-C(7) C(6)-C(7)-C(8) C(3)-C(8)-C(7)

142.1(1) 154.8(1) 78.2(1) 106.7(1) 60.0(1) 60.1(1) 107.9(1) 108.0(1) 60.2(1) 107.5(1) 108.1(1) 107.8(1) 60.0(1) 593(1) 60.4(1) 59.8(1) 108.0(1) 107.9(1) 59.3(1) 108.2(1) 108.1(1) 107.9(1) 60.1(1) 60.5(1) 59.9(1) 107.6(1) 59.7(1) 107.8(1) 107.2(1) 59.5(1) 60.0(1) 107.6(1) 107.5(1) 60.0(1) 84.4(1) 92.6(1) 119.8(1) 65.1(1) 102.0(1) 119.5(1) 120.5(1) 118.6(1) 121.2(1) 120.3(1)

B(5)-B(9)-Ag( 1A)_____________ 96.3(1)


Compound 11-6 Atomic coordinates and thermal parameters. X

Ag(l) Ag(2) CI(1) Cl(2) Cl(3) C!(4) Cl(5) Cl(6) Cl(7) Cl(8) Cl(9) CI(10) C I(ll) CI(12) C (ll) C(12) C(21) C(22) C(31) C(32) C(33) C(34) C(35) C(36) C( 37) C(38) C(39) C(41) C(42) C(43) C(44) C(45) C(46) C(47) C(48) C(49) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12) B(22) B(23) B(24) B(25)

1082(1) 1435(1) 2043(1) 1340(1) 2435(1) 1209(1) 1102(1) 1853(1) 691(1) 160(1) 503(1) 1218(1) 1298(1) 1405(1) 2645(1) 2345(1) -154(2) 158(2) 991(1) 701(2) 847(3) 1274(2) 1546(2) 1384(2) 248(2) 1417(3) 1694(2) 1495(2) 1791(2) 1712(2) 1318(2) 1007(2) 1085(1) 2231(2) 1241(3) 748(2) 2492(2) 2126(2) 1854(2) 2044(2) 2442(2) 2241(2) 1951(1) 1590(1) 1642(2) 2028(2) 1706(1) 466(2) 94(2) 41(2) 378(2)

y 3767(1) 8689(1) 9218(2) 6707(1) 6202(2) 9022(2) 5996(1) 4282(1) -712(1) 1352(2) 4302(1) 1827(1) 4009(1) 918(1) 7505(7) 7357(5) 2372(7) 2248(5) 2420(4) 3157(6) 3909(7) 4018(8) 3321(6) 2501(6) 3088(9) 4933(11) 1749(6) 7241(5) 7850(5) 8754(6) 9017(6) 8356(6) 7486(4) 7525(7) 9991(8) 6784(7) 7696(6) 8565(6) 7572(5) 6122(5) 6230(6) 6721(6) 5734(5) 6566(5) 8125(4) 8147(6) 6953(5) 1063(7) 1182(6) 2636(7) 3453(6)

z -1887(1) -5062(1) -3725(1) -3704(1) -4087(1) -1785(2) -1046(1) -2495(1) -4304(1) -2659(2) -3272(1) -3249(1) -5257(2) -5890(1) 158(5) -844(4) -6866(4) -6062(5) -402(4) 135(4) 846(5) 1022(4) 501(4) -253(4) -126(11) 1775(7) -773(6) -6455(6) -6954(4) -7651(4) -7935(5) -7443(6) -6709(4) -6778(5) -8665(6) -6270(8) -2127(5) -1351(5) -464(3) -751(5) -1680(5) -2879(6) -2074(3) -1413(5) -1750(4) -2670(5) -2702(5) -6057(6) -5111(7) -4844(5) -5574(8)

U(eq) 83(1) 85(1) 106(1) 82(1) 112(1) 105(1) 77(1) 79(1) 84(1) 107(1) 90(1) 74(1) 90(1) 72(1) 92(2) 70(1) 101(2) 89(2) 65(1) 97(2) 116(2) 100(2) 87(2) 87(2) 148(4) 131(4) 90(2) 82(2) 76(2) 95(2) 85(2) 92(2) 66(1) 99(2) 123(3) 122(3) 81(2) 75(2) 60(1) 67(2) 74(2) 77(2) 57(1) 64(1) 61(1) 80(2) 67(1) 81(2) 89(2) 78(2) 95(3)


B(26) 644B(29) B(26)-B(25)-B(30) C(22)-B(25)-B(30) B(24)-B(25)-B(30) B(29)-B(25)-B(30) B(30)-B(26)-C(22) B(30)-B(26)-B(25) C(22)-B(26)-B(25) B(30)-B(26)-B(31) C(22)-B(26)-B(31) B(25)-B(26)-B(31) B(30)-B(26)-B(22) C(22)-B(26)-B(22) B(25)-B(26)-B(22) B(31)-B(26)-B(22) B(28)-B(27)-C1(7) B(28)-B(27)-B(32) Cl(7)-B(27)-B(32) B(28)-B(27)-B(23) Cl(7)-B(27)-B(23) B(32)-B(27)-B(23) B(28)-B(27)-B(22) Cl(7)-B(27)-B(22) B(32)-B(27>B(22) B(23)-B(27)-B(22) B(28)-B(27)-B(31) Cl(7)-B(27)-B(31) B(32)-B(27)-B(31) B(23)-B(27)-B(31) B(22)-B(27)-B(31) B(27)-B(28)-B(23) B(27)-B(28)-B(32) B(23)-B(28)-B(32) B(27)-B(28)-B(24) B(23)-B(28)-B(24) B(32)-B(28)-B(24) B(27)-B(28)-B(29) B(23)-B(28)-B(29) B(32)-B(28)-B(29) B(24)-B(28)-B(29) B(27)-B(28)-C1(8) B(23)-B(28)-CI(8) B(32)-B(28)-C1(8) B(24)-B(28)-CI(8) B(29)-B(28)-C1(8) B(24)-B(29)-B(25) B(24)-B(29)-B(28) B(25)-B(29)-B(28) B(24)-B(29)-B(32) B(25)-B(29)-B(32) B(28)-B(29)-B(32) B(24)-B(29)-CI(9) B(25)-B(29)-C1(9) B(28)-B(29)-CI(9) B(32)-B(29)-C1(9)

59.6(3) 108.2(5) 121.9(4) 117.7(4) 122.2(4) 119.2(4) 121.1(4) 108.1(4) 123.9(4) 119.3(3) 61.1(3) 107.2(4) 123.5(4) 108.9(4) 58.8(3) 120.2(3) 60.1(3) 58.4(3) 61.9(3) 121.1(3) 107.8(4) 108.7(4) 57.2(4) 60.9(4) 104.3(5) 105.8(5) 56.8(3) 109.0(5) 108.0(5) 103.1(4) 60.9(4) 60.4(3) 58.0(4) 106.8(5) 58.4(4) 62.6(4) 106.6(5) 107.5(4) 108.7(4) 106.4(4) 61.2(4) 58.3(3) 62.0(4) 59.1(4) 110.6(5) 106.8(4) 109.4(4) 60.1(4) 107.3(5) 59.5(4) 108.6(4) 60.5(3) 58.9(4) 103.9(5) 58.6(4) 103.4(5)

106.9(5) 60.8(4) 55.4(3) 105.5(5) 108.8(5) 61.6(4) 116.6(4) 66.2(4) 61.6(4) 65.2(3) 113.7(5) 119.0(5) 117.2(4) 60.7(4) 113.9(5) 62.7(4) 122.4(4) 61.2(3) 122.4(4) 59.3(4) 121.9(4) 108.0(4) 105.7(4) 122.2(4) 107.3(4) 58.0(4) 107.7(4) 123.0(3) 60.4(3) 105.3(5) 58.7(3) 62.4(3) 60.9(3) 110.2(4) 108.3(4) 57.9(4) 108.1(4) 109.6(4) 106.8(5) 61.1(3) 59.0(3) 121.4(4) 124.7(4) 117.9(4) 123.7(4) 119.0(4) 59.1(4) 60.5(3) 107.8(5) 107.6(4) 108.6(5) 59.0(3) 124.3(4) 122.7(4) 122.2(5) 119.7(4)

182


B(24)-B(29)-B(30) B(25)-B(29)-B(30) B(28)-B(29)-B(30) B(32)-B(29)-B(30) CI(9)-B(29)-B(30) B(26)-B(30)-B(31) B(26)-B(30)-B(25) B(31)-B(30)-B(25) B(26)-B(30)-Cl(l 1) B(31)-B(30)-CI( 11) B(25)-B(30)-C1(11) B(26)-B(30)-B(32) B(31)-B(30)-B(32) B(25)-B(30)-B(32) Cl( 11)-B(30)-B(32) B(26)-B(30)-B(29) B(31)-B(30)-B(29) B(25)-B(30)-B(29) Cl(ll)-B(30)-B(29) B(32)-B(30)-B(29) B(26)-B(31)-B(30) B(26)-B(31)-B(22) B(30)-B(31)-B(22) B(26)-B(31)-B(32) B(30)-B(31)-B(32) B(22)-B(31)-B(32) B(26)-B(31)-B(27) B(30)-B(31)-B(27) B(22)-B(31)-B(27) B(32)-B(31)-B(27) B(26)-B(31)-C1(12) B(30)-B(31)-CI( 12) B(22)-B(31)-CI( 12) B(32)-B(31)-CI( 12) B(27)-B(31)-Cl( 12) Cl( 10)-B(32)-B(28) Cl( 10)-B(32)-B(27) B(28)-B(32)-B(27) Cl(10)-B(32)-B(31) B(28)-B(32)-B(31) B(27)-B(32)-B(31) C!( 10)-B(32)-B(30) B(28)-B(32)-B(30) B(27)-B(32)-B(30) B(31)-B(32)-B(30) Cl( 10)-B(32)-B(29) B(28)-B(32)-B(29) B(27)-B(32)-B(29) B(31)-B(32)-B(29) B(30)-B(32)-B(29)

105.9(5) 59.6(3) 106.3(4) 60.2(3) 121.9(4) 59.2(4) 58.4(4) 108.0(4) 128.5(4) 121.8(3) 123.6(4) 105.6(4) 60.4(3) 108.0(4) 118.3(3) 103.5(4) 107.6(4) 58.8(4) 120.6(4) 60.2(3) 55.6(3) 60.5(4) 107.4(4) 103.8(4) 61.6(3) 108.2(4) 106.2(4) 108.8(4) 60.9(3) 59.4(3) 128.4(4) 122.0(3) 122.9(4) 119.1(3) 119.4(4) 124.3(4) 122.1(4) 58.0(3) 122.2(3) 105.1(4) 60.2(3) 122.2(3) 106.4(4) 106.7(4) 58.1(3) 123.7(4) 59.8(3) 106.2(3) 105.3(4) 59.6(3)


Compound 11-7 Atomic coordinates and thermal parameters.

Ag(l) Br(4) Br(5) Br(6) Br(12) C(l) C( 2) B (l) B(2) B(3) B(4) B(5) B(6) B(12)

X

V

50000 25894(12) 30526(9) 37682(8) 47718(10) 756(9) -396(9) 1678(10) 1467(7) 1166(7) 2266(9) 2459(6) 2791(6) 3270(10)

0

z 50000 20548(11) 38639(9) 66476(7) 41690(10) 5231(7) 5519(10) 6229(8) 5423(6) 4123(6) 3584(10) 4408(7) 5720(7) 4574(9)

25000 -2902(9) 8196(9) 25000 2500 2500 2500 1221(7) 1691(8) 2500 1213(8) 1695(8) 2500

U(eq) 879(5) 565(5) 562(4) 479(3) 425(4) 44(1) 61(1) 41(1) 42(1) 42(1) 39(1) 37(1) 34(1) 31(1)

Bond lengths Ag(l)-Br(5) Ag(l)-Br(6) Ag(l)-Br(12) Ag(l)-Br(5A) Ag(l)-Br(6A) A g(l)-Br(lA) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6) Br(12)-B(12) Br(12)-Ae(lA) C(1)'C(2) C (l)-B (l) C(l)-B(2) C(l)-B(3) C(1)-B(2A) C(1)-B(3A) B(l)-B(2) B(l)-B(6)

2.852(1) 2.73(1) 2.990(1) 2.852(1) 2.733(1) 2.990(1) 1.951(12) 1.958(9) 1.952(8) 1.959(12) 2.990(1) 1.495(16) 1.702(15) 1.703(10) 1.729(11) 1.703(10) 1.729(11) 1.765(10) 1.783(14)

B(1)-B(2A) B(1)-B(6A) B(2)-B(3) B(2)-B(5) B(2)-B(6) B(3)-B(4) B(3)-B(5) B(3)-B(3A) B(4)-B(5) B(4)-B(12) B(4)-B(3A) B(4)-B(5A) B(5)-B(6) B(5)-B(12) B(6)-B(12) B(6)-B(6A) B(12)-B(5A) B(12)-B(6A)

1.765(10) 1.783(14) 1.746(11) 1.779(12) 1.788(12) 1.786(13) 1.751(12) 1.806(18) 1.783(12) 1.768(17) 1.786(13) 1.783(12) 1.772(12) 1.775(11) 1.793(13) 1.797(17) 1.775(11) 1.793(13)

85.6(1) 81.4(1) 83.9(1) 180.0(1) 94.4(1) 98.6(1) 94.4(1) 180.0(1) 96.1(1) 85.6(1)

Br(5)-Ag( 1)-Br( 1A) Br(6)-Ag( 1)-Br( 1A) Br(12)-Ag(l)-Br(lA) Br(5A)-Ag(l)-Br(lA) Br(6A)-Ag( 1)-Br( 1A) Ag(l)-Br(5)-B(5) Ag(l)-Br(6)-B(6) Ag(l)-Br(12)-B(12) Ag( 1)-Br( 12)-Ag( 1A) B( 12)-Br( 12)-Ag( 1A)

98.6(1) 96.1(1) 180.0(1) 81.4(1) 83.9(1) 93.4(2) 94.6(2) 90.2(1) 137.8(1) 90.2(1)

Bond angles Br(5)-Ag(l)-Br(6) B r(5)-Ag( 1)-Br( 12) Br(6)-Ag( 1)-Br( 12) Br(5)-Ag(l)-Br(5A) Br(6)-Ag(l)-Br(5A) Br(12)-Ag(l)-Br(5A) Br(5)-Ag(l)-Br(6A) Br(6)-Ag( 1)-Br(6A) Br(12)-Ag(l)-Br(6A) Br(5 A)-Ag( 1)-Br(6A)

184


C(2)-C(l)-B(l) C(2)-C(l)-B(2) B(l)-C(l)-B(2) C(2)-C(l)-B(3) B(l)-C(l)-B(3) B(2)-C(l)-B(3) C(2)-C(1)-B(2A) B(1)-C(1)-B(2A) B(2)-C(1)-B(2A) B(3)-C(1)-B(2A) C(2)-C(1)-B(3A) B(1)-C(1)-B(3A) B(2)-C(1)-B(3A) B(3)-C(1)-B(3A) B(2A)-C( 1)-B(3A) C(l)-B(l)-B(2) C(l)-B(l)-B(6) B(2)-B(l)-B(6) C(1)-B(1)-B(2A) B(2)-B(1)-B(2A) B(6)-B(1)-B(2A) C(1)-B(1)-B(6A) B(2)-B(1)-B(6A) B(6)-B(1)-B(6A) B(2A)-B(1)-B( 6 A) C(l)-B(2)-B(l) C(l)-B(2)-B(3) B(l)-B(2)-B(3) C(l)-B(2)-B(5) B(l)-B(2)-B(5) B(3)-B(2)-B(5) C(l)-B(2)-B(6) B(l)-B(2)-B(6) B(3)-B(2)-B(6) B(5)-B(2)-B(6) C(l)-B(3)-B(2) C(l)-B(3)-B(4) B(2)-B(3)-B(4) C(l)-B(3)-B(5) B(2)-B(3)-B(5) B(4)-B(3)-B(5) C(1)-B(3)-B(3A) B(2)-B(3)-B(3A) B(4)-B(3)-B(3A) B(5)-B(3)-B(3A) Br(4)-B(4)-B(3) Br(4)-B(4)-B(5) B(3)-B(4)-B(5) Br(4)-B(4)-B(12) B(3)-B(4)-B(12) B(5)-B(4)-B(12) Br(4)-B(4)-B(3A) B(3)-B(4)-B(3A) B(5)-B(4)-B(3A) B( 12)-B(4)-B(3A) Br(4)-B(4)-B(5A)

119.1(8) 118.5(5) 62.5(4) 118.8(7) 112.3(7) 61.1(4) 118.5(5) 62-5(4) 113.9(8) 113.1(7) 118.8(7) 112.3(7) 113.1(7) 63.0(7) 61.1(4) 58.8(4) 106.1(6) 60-5(5) 58.8(4) 107.9(7) 108.8(7) 106.1(6) 108.8(7) 60.5(7) 60.5(5) 58.8(5) 60.2(5) 108.6(6) 105.9(6) 107.7(7) 59.6(5) 105.8(6) 60.2(6) 107.8(6) 59.6(5) 58.7(4) 105.6(6) 109.4(7) 106.0(6) 61.1(5) 60.5(5) 58.5(3) 107.5(4) 59.6(3) 107.7(4) 122.0(6) 122.4(5) 58.8(5) 122.2(7) 107.0(7) 60.0(5) 122.0(6) 60.7(7) 107.2(7) 107.0(7) 122.4(5)

B(3)-B(4)-B(5A) B(5)-B(4)-B(5A) B(12)-B(4)-B(5A) B(3A)-B(4)-B(5A) Br(5)-B(5)-B(2) Br(5)-B(5)-B(3) B(2)-B(5)-B(3) Br(5)-B(5)-B(4) B(2)-B(5)-B(4) B(3)-B(5)-B(4) Br(5)-B(5)-B(6) B(2)-B(5)-B(6) B(3)-B(5>B(6) B(4)-B(5)-B(6) Br(5)-B(5)-B( 12) B(2)-B(5)-B(12) B(3)-B(5)-B(12) B(4)-B(5)-B(12) B(6)-B(5)-B(12) Br(6)-B(6)-B(l) Br(6)-B(6)-B(2) B(l)-B(6)-B(2) Br(6)-B(6)-B(5) B(l)-B(6)-B(5) B(2)-B(6>B(5) Br(6)-B(6)-B(12) B( 1)-B(6)-B( 12) B(2)-B(6)-B(12) B(5)-B(6)-B(12) Br(6)-B(6)-B(6A) B( 1)-B(6)-B(6A) B(2)-B(6)-B(6A) B(5)-B(6)-B(6A) B(12)-B(6)-B(6A) Br(12)-B(12)-B(4) Br(12)-B(12)-B(5) B(4)-B(12)-B(5) Br(12)-B(12)-B(6) B(4)-B( 12)-B(6) B(5)-B(12)-B(6) Br( 12)-B( 12)-B(5 A) B(4)-B(12)-B(5A) B(5)-B( 12)-B(5A) B(6)-B( 12)-B(5 A) Br( 12)-B( 12)-B(6A) B(4)-B(12)-B(6A) B(5)-B( 12)-B(6A) B(6)-B( 12)-B(6A) B(5 A)-B( 12)-B(6A)

107.2(7) 107.3(8) 60.0(5) 58.8(5) 121.3(5) 123.1(5) 59.3(5) 122.8(6) 108.1(6) 60.7(5) 119.3(5) 60.5(5) 108.3(6) 108.6(6) 120.9(5) 108.5(6) 108.2(6) 59.6(5) 60.7(5) 122.5(5) 124.3(5) 59.3(5) 123.0(5) 107.2(6) 60.0(4) 120.7(6) 107.2(6) 107.3(6) 59.7(5) 120.0(2) 59.7(3) 107.2(4) 107.7(4) 59.9(3) 120.8(7) 121.8(5) 60.4(5) 122.1(6) 108.4(7) 59.6(5) 121.8(5) 60.4(5) 108.1(8) 107.7(7) 122.1(6) 108.4(7) 107.7(7) 60.1(7) 59.6(5)


Compound II-8 Atomic coordinates and thermal parameters.

A g(l) 1(7) 1(8) 1(9) 1(10) 1(11) 1(12) C(l) C(2) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12)

X

y

24594(17) 19387(8) -10441(7) 4542(8) 43894(8) 52400(7) 19031(8) 2639(9) 2817(10) 3260(10) 1596(10) 1207(9) 2640(10) 3930(10) 2228(9) 926(9) 1587(10) 3261(9) 3652(10) 2209(9)

99771(9) 93952(5) 77159(6) 57570(5) 61825(6) 84311(6) 82825(5) 6227(7) 5665(9) 7305(8) 7134(8) 6152(7) 5711(8) 6457(8) 7958(8) 7230(7) 6385(8) 6554(7) 7538(8) 7498(7)

z -15993(10) 3991(5) -6281(6) -24139(6) -24632(6) -7407(6) -26127(5) 853(7) 1843(8) 885(8) 924(8) 161(7) -318(8) 1 2 1 (8 )

80(8) -371(7) -1128(7) -1155(8) -424(8) -1209(7)

U(eq) 973(5) 449(2) 544(3) 508(2) 556(3) 524(2) 471(2) 40(1) 57(1) 35(1) 37(1) 31(1) 37(1) 39(1) 34(1) 32(1) 37(1) 33(1) 36(1) 29(1)

Bond lengths Ag(l)-I(7) Ag(l)-I(12) Ag(l)-I(9A) Ag(l)-I(10A) 1(7)-B(7) I(8)-B(8) I(9)-B(9) I(9)-Ag(lA) I( 10)-B(10) I(10)-Ag(lA) K ll)-B (ll) I( 12)-B(12) C(l)-C(2) C(l)-B(2) C(l)-B(3) C(l)-B(4) C(l)-B(5) C(l)-B(6) B(2)-B(3) B(2)-B(6) B(2)-B(7) B(2)-B(l 1)

2.798(2) 2.872(2) 2.822(2) 2.848(2) 2.188(11) 2.184(9) 2.192(10) 2.822(2) 2.177(10) 2.848(2) 2.172(11) 2.160(9) 1.527(15) 1.721(15) 1.732(15) 1.702(13) 1.692(14) 1.717(14) 1.756(14) 1.762(15) 1.747(14) 1.791(14)

B(3)-B(4) B(3)-B(7) B(3)-B(8) B(4)-B(5) B(4)-B(8) B(4)-B(9) B(5)-B(6) B(5)-B(9) B(5)-B(10) B(6)-B(10) B (6)-B (ll) B(7)-B(8) B (7)-B (ll) B(7)-B(12) B(8)-B(9) B(8)-B(12) B(9)-B(10) B(9)-B(12) B (10)-B (ll) B(10)-B(12) B (ll)-B (12)

1.789(15) 1.784(15) 1.782(14) 1.769(14) 1.754(14) 1.763(14) 1.807(15) 1.781(15) 1.792(15) 1.760(14) 1.765(16) 1.804(14) 1.764(15) 1.797(14) 1.749(15) 1.806(13) 1.764(14) 1.773(16) 1.771(15) 1.774(14) 1.771(13)

96.1(1)

I(7)-Ag(l)-I(9A)

137.1(1)

Bond angles I(7)-Ag(l)-I(12)


I(12)-Ag(l)-!(9A) I(7)-Ag(l)-I(10A) I(12)-Ag(l)-I(10A) I(9A)-Ag( 1)-I( 10A) Ag(l)-I(7)-B(7) B(9)-I(9)-Ag(lA) B(10)-I(10)-Ag(lA) Ag( 1)-I( 12)-B( 12) C(2)-C(l)-B(2) C(2)-C(l)-B(3) B(2)-C(l)-B(3) C(2)-C(l)-B(4) B(2)-C(l)-B(4) B(3)-C(l)-B(4) C(2)-C(l)-B(5) B(2)-C(l)-B(5) B(3)-C(l)-B(5) B(4)-C(l)-B(5) C(2)-C(l)-B(6) B(2)-C(l)-B(6) B(3)-C(l)-B(6) B(4)-C(l)-B(6) B(5)-C(l)-B(6) C(l)-B(2)-B(3) C(l)-B(2)-B(6) B(3)-B(2)-B(6) C(l)-B(2)-B(7) B(3)-B(2)-B(7) B(6)-B(2)-B(7) C (l)-B (2)-B (ll) B(3)-B(2)-B(l 1) B(6)-B(2)-B(l 1) B (7)-B(2)-B(ll) C(l)-B(3)-B(2) C(l)-B(3)-B(4) B(2)-B(3)-B(4) C(l)-B(3)-B(7) B(2)-B(3)-B(7) B(4)-B(3)-B(7) C(l)-B(3)-B(8) B(2)-B(3)-B(8) B(4)-B(3)-B(8) B(7)-B(3)-B(8) C(l)-B(4)-B(3) C(l)-B(4)-B(5) B(3)-B(4)-B(5) C(l)-B(4)-B(8) B(3)-B(4)-B(8) B(5)-B(4)-B(8) C(l)-B(4)-B(9) B(3)-B(4)-B(9) B(5)-B(4)-B(9) B(8)-B(4)-B(9) C(l)-B(5)-B(4) C(l)-B(5)-B(6) B(4)-B(5)-B(6)

107.0(1) 115.1(1) 103.7(1) 94.2(1) 95.2(3) 96.8(3) 96.1(3) 94.0(3) 117.0(8) 115.2(8) 61.2(6) 117.9(8) 113.1(7) 62.8(6) 119.7(9) 115.0(7) 115.2(7) 62.8(6) 120.2(8) 61.7(6) 112.8(8) 114.5(7) 64.0(6) 59.7(6) 59.1(6) 109.5(7) 106.2(7) 61.2(6) 108.1(7) 105.0(7) 109.2(7) 59.6(6) 59.8(6) 59.1(6) 57.8(6) 107.3(7) 104.1(7) 59.1(6) 107.4(7) 103.2(7) 107.5(7) 58.8(6) 60.8(6) 59.4(6) 58.3(6) 108.7(7) 105.6(7) 60.4(6) 109.0(7) 104.4(7) 107.7(7) 60.6(6) 59.6(6) 58.8(6) 58.7(6) 107.0(7)

C(1)-B(5>B(9) B(4)-B(5)-B(9) B(6)-B(5)-B(9) C(l)-B(5)-B(10) B(4)-B(5)-B( 10) B(6)-B(5)-B( 10) B(9)-B(5)-B( 10) C(l)-B(6)-B(2) C(l)-B(6)-B(5) B(2)-B(6)-B(5) C(l)-B(6)-B(10) B(2)-B(6)-B(10) B(5)-B(6)-B( 10) C (l)-B(6)-B(ll) B(2)-B(6)-B(ll) B(5)-B(6)-B(ll) B( 10)-B(6)-B( 11) I(7)-B(7)-B(2) I(7)-B(7)-B(3) B(2)-B(7)-B(3) I(7)-B(7)-B(8) B(2)-B(7)-B(8) B(3)-B(7)-BC(6) C(5)-C(6)-C(7) C(5)-C(6)-C(10) C(7)-C(6)-C(10) C(6)-C(7)-C(8) Q3)-C(8)-Q7)

74.7(2) 120.2(2) 73.1(1) 107.7(1) 119.7(2) 120.0(2) 119.0(2) 120.9(2) 120.2(2) 119.7(2)

201


Compound III-11 Atomic coordinates and thermal parameters. y 5000 3915(1) 5000 3276(1) 3275(1) 3913(1) 5000 4491(3) 5000 4194(3) 4177(3) 4496(3) 2500 2035(7)

X

Br(l) Br(2) Br(3) Br(4) Br# 1-B(3)-B(5)#5 B(5)-B(3)-B(5)#5 B(3)#5-B(3)-Br(3) B(6)-B(3)-Br(3) B(6)#l-B(3)-Br(3) B(5)-B(3)-Br(3) B(5)#5-B(3)-Br(3) B(l)-B(4)-B(l)#2 B( 1)-B(4)-B(2)#2 B(l)#2-B(4)-B(2)#2 B(l)-B(4)-B(2) B( 1)#2-B(4)-B(2) B(2)#2-B(4)-B(2) B( 1)-B(4)-B(4)#4 B( 1)#2-B(4)-B(4)#4 B(2)#2-B(4)-B(4>#4 B(2)-B(4)-B(4)#4 B(l)-B(4)-Br(4) B(l)#2-B(4)-Br(4) B(2)#2-B(4)-Br(4) B(2)-B(4)-Br(4) B(4)#4-B(4)-Br(4) B(5)#2-B(5)-B(6) B(5)#2-B(5)-B(6)#6 B(6)-B(5)-B(6)#6 B(5)#2-B(5)-B(3) B(6)-B(5)-B(3) B(6)#6-B(5)-B(3) B(5)#2-B(5)-B(3)#5 B(6)-B(5)-B(3)#5 B(6)#6-B(5)-B(3)#5 B(3)-B(5)-B(3)#5 B(5)#2-B(5)-Br(5) B(6)-B(5)-Br(5) B(6)#6-B(5)-Br(5) B(3)-B(5)-Br(5) B(3)#5-B(5)-Br(5) B(5)#2-B(6)-B(5) B(5)#2-B(6)-B(6)#l B(5)-B(6)-B(6)#l B(5)#2-B(6)-B(3)#2 B(5)-B(6)-B(3)#2

59.3(2) 121.8(2) 121.8(2) 122.0(2) 122.0(2) 122.16(14) 108.2(2) 108.2(2) 59.9(3) 60.8(2) 59.0(2) 107.2(3) 60.8(2) 107.2(3) 59.0(2) 108.4(3) 123.01(14) 120.5(3) 120.5(3) 122.5(2) 122.5(2) 61.0(3) 108.7(3) 60.0(2) 60.0(2) 108.7(3) 107.8(3) 107.1(2) 107.1(2) 59.4(2) 59.4(2) 122.0(3) 122.0(3) 121.4(2) 121.4(2) 122.03(14) 60.8(2) 60.8(2) 108.5(3) 108.9(2) 60.2(2) 107.1(3) 108.9(2) 107.1(3) 60.2(2) 58.3(3) 123.6(2) 122.5(2) 122.5(2) 119.8(3) 119.8(3) 58.5(3) 108.7(2) 108.7(2) 60.8(2) 107.5(3)

B(6)#l-B(6)-B(3)#2 B(5)#2-B(6)-B(3) B(5)-B(6)-B(3) B(6)#l-B(6)-B(3) B(3)#2-B(6)-B(3) B(5)#2-B(6)-Br(6) B(5)-B(6)-Br(6) B(6)#l-B(6)-Br(6) B(3)#2-B(6)-Br(6) B(3)-B(6)-Br(6) C (l)#7-N (l)-C (l)#8 C (l)#7-N (l)-C (l)#9 C (l)#8-N (l)-C (l)#9 C (l)#7-N (l)-C (l) C (l)#8-N (l)-C (l) C (l)# 9 -N (l)-a i)

60.1(2) 107.5(3) 60.8(2) 60.1(2) 107.9(3) 120.8(3) 120.8(3) 122.6(2) 122.1(2) 122.1(2) 110.6(10) 105.6(10) 112.3(10) 112.3(10) 105.6(10) 110.6(10)

203


Compound III-12 Atomic coordinates and thermal parameters. X

Brfl) Br(2) Br(3) Br(4) B(l) B(2) B(3) B(4) Cs(l) Cs(2)

9313(1) 11507(1) 12258(1) 10890(1) 11311(6) 12402(6) 12817(5) 12243(5) 6667 6667

y 3703(1) 7290(1) 2628(1) 4822(1) 5188(6) 7000(5) 4815(4) 5850(5) 13333 13333

z -2138(1) -3123(1) -1495(1) -507(1) -1976(3) -2421(3) -1673(2) -1207(2) 538(1) -832(1)

U(eq) 55(1) 55(1) 50(1) 48(1) 74(2) 49(2) 26(1) 33(2) 61(1) 79(1)

Bond lengths Br(l)-B(l) Br(l)-Cs(2)#l Br(l)-Cs(l)#2 Br(2)-B(2) Br(2)-Cs(l)#3 Br(3)-B(3) Br(3)-Cs(l)#2 Br(3)-Cs(2)#4 Br(4)-B(4) Br(4)-Cs(2)#l B(l)-B(3) B(l)-B(2) B(l)-B(2)#5 B(l)-B(3)#6 B(l)-B(4) B(2)-B(3)#6 B(2)-B(l)#6 B(2)-B(2)#6 B(2)-B(2)#5 B(3)-B(2)#5 B(3)-B(4) B(3)-B(4)#5 B(3)-B(l)#5

1.802(5) 3.778(2) 4.2729(10) 1.873(6) 3.7077(9) 1.973(4) 3.7574(11) 4.2876(10) 1.959(4) 3.7151(8) 1.821(9) 1.838(7) 1.848(8) 1.850(7) 1.885(8) 1.731(7) 1.848(8) 1.932(10) 1.932(10) 1.731(7) 1.727(7) 1.774(6) 1.850(7)

B(4)-B(4)#6 B(4)-B(4)#5 B(4)-B(3)#6 Cs(l)-Cs(2) Cs(l)-Br(2)#7 Cs(l)-Br(2)#8 Cs(l)-Br(2)#9 Cs(l)-Br(3)#10 Cs(l)-Br(3)#ll Cs(l)-Br(3)#12 Cs(l)-Br(l)#lO Cs(l)-Br(l)#12 C s(l)-B r(l)#n Cs(2)-Br(4)#13 Cs(2)-Br(4)#14 Cs(2)-Br(4)#15 Cs(2)-Br(l)#13 Cs(2)-Br(l)#14 Cs(2)-Br(l)#15 Cs(2)-Br(3)#16 Cs(2)-Br(3)#17 Cs(2)-Br(3)#18

1.673(7) 1.673(7) 1.774(6) 3.029(2) 3.7077(9) 3.7078(9) 3.7078(9) 3.7574(11) 3.7575(11) 3.7575(11) 4.2729(10) 4.2729(10) 4.2729(9) 3.7151(8) 3.7151(8) 3.7151(8) 3.778(2) 3.778(2) 3.778(2) 4.2876(10) 4.2876(10) 4.2876(10)

110.2(2) 100.6(2) 124.87(2) 109.5(2) 110.06(12) 100.55(13) 125.01(2) 112.8(2) 125.2(3) 123.3(4) 104.6(3)

Br(l)-B(l)-B(2)#5 B(3)-B(l)-B(2)#5 B(2)-B( 1)-B(2)#5 Br(l)-B(l)-B(3)#6 B(3)-B(l)-B(3)#6 B(2)-B(l)-B(3)#6 B(2)#5-B( 1)-B(3)#6 Br(l)-B(l)-B(4) B(3)-B(l)-B(4) B(2)-B(l)-B(4) B(2)#5-B(l)-B(4)

122.7(4) 56.3(3) 63.2(4) 127.0(4) 100.2(3) 56.0(3) 103.9(3) 127.1(4) 55.5(3) 101.6(3) 100.8(4)

Bond angles B( 1)-Br( 1)-Cs(2)# 1 B( 1)-Br( 1)-Cs( 1)#2 Cs(2># 1-Br( 1)-Cs( 1)#2 B(2)-Br(2)-Cs( 1)#3 B(3)-Br(3)-Cs( 1)#2 B(3)-Br(3)-Cs(2)#4 Cs( 1)#2-Br(3)-Cs(2)#4 B(4)-Br(4)-Cs(2)#l Br(l)-B(l)-B(3) Br(l)-B(l)-B(2) B(3)-B(l)-B(2)


B(3)#6-B( 1)-B(4) B(3)#6-B(2)-B(l) B(3)#6-B(2)-B(l)#6 B(l)-B(2)-B(l)#6 B(3)#6-B(2)-Br(2) B(l)-B(2)-Br(2) B( 1)#6-B(2)-Br(2) B(3)#6-B(2)-B(2)#6 B( I )-B(2)-B(2)#6 B( 1)#6-B(2)-B(2)#6 Br(2)-B(2)-B(2)#6 B(3)#6-B(2)-B(2)#5 B( 1)-B(2)-B(2)#5 B( 1)#6-B(2)-B(2)#5 Br(2)-B(2)-B(2)#5 B(2)#6-B(2)-B(2)#5 B(2)#5-B(3)-B(4) B(2)#5-B(3)-B(4)#5 B(4)-B(3)-B(4)#5 B(2)#5-B(3)-B(l) B(4)-B(3)-B(l) B(4)#5-B(3)-B(l) B(2)#5-B(3)-B(l)#5 B(4)-B(3)-B( 1)#5 B(4)#5-B(3)-B( 1)#5 B(l)-B(3)-B(l)#5 B(2)#5-B(3)-Br(3) B(4)-B(3)-Br(3) B(4)#5-B(3)-Br(3) B(l)-B(3)-Br(3) B(l)#5-B(3)-Br(3) B(4)#6-B(4)-B(4)#5 B(4)#6-B(4)-B(3) B(4)#5-B(4)-B(3) B(4)#6-B(4)-B(3)#6 B(4)#5-B(4)-B(3)#6 B(3)-B(4)-B(3)#6 B(4)#6-B(4)-B( 1) B(4)#5-B(4)-B(l) B(3)-B(4)-B(l) B(3)#6-B(4)-B(l) B(4)#6-B(4)-Br(4) B(4)#5-B(4)-Br(4) B(3)-B(4)-Br(4) B(3)#6-B(4)-Br(4) B(l)-B(4)-Br(4) Cs(2)-Cs(l)-Br(2)#7 Cs(2)-Cs(l)-Br(2)#8 Br(2)#7-Cs( 1)-Br(2)#8 Cs(2)-Cs( 1)-Br(2)#9 Br(2)#7-Cs(l)-Br(2)#9 Br(2)#8-Cs( 1)-Br(2)#9 Cs(2)-Cs( 1)-Br(3)# 10 Br(2)#7-Cs(l)-Br(3)#10 Br(2)#8-Cs( 1)-Br(3)#l 0 Br(2)#9-Cs(l)-Br(3)#10

56.7(3) 62.4(3) 61.1(3) 113.6(5) 128.7(4) 120.0(3) 121.4(3) 104.3(2) 108.4(3) 58.1(3) 119.4(2) 105.2(2) 58.6(3) 108.0(3) 118.7(2) 60.0 112.5(3) 110.8(3) 57.1(3) 62.6(3) 64.1(3) 110.9(3) 61.6(3) 110.6(3) 62.6(3) 114.3(4) 118.7(3) 121.8(2) 121.2(3) 118.7(2) 116.8(3) 60.0 110.2(3) 62.9(4) 60.1(3) 108.0(3) 107.1(3) 111.4(2) 112.6(3) 60.4(3) 60.7(3) 122.3(2) 121.8(3) 120.3(3) 122.1(3) 116.5(3) 78.74(2) 78.74(2) 116.282(12) 78.74(2) 116.281(12) 116.280(12) 139.89(2) 62.24(2) 125.57(2) 109.41(2)

Cs(2)-Cs( 1)-Br(3)# 11 Br(2)#7-Cs(l)-Br(3)#l 1 Br(2)#8-Cs( 1)-Br(3)#l 1 Br(2)#9-Cs( 1)-Br(3)#l 1 Br(3)#10-Cs( 1)-Br(3)#l 1 Cs(2)-Cs( 1)-Br(3)# 12 Br(2)#7-Cs(l)-Br(3)#12 Br(2)#8-Cs( 1)-Br(3)#l 2 Br(2)#9-Cs(l)-Br(3)#12 Br(3)#10-Cs(l)-Br(3)#12 Br(3)#l 1-Cs(l)-Br(3)#12 Cs(2)-Cs(l)-Br(l)#10 Br(2)#7-Cs(l)-Br(l)#10 Br(2)#8-Cs(l)-Br(l)#10 Br(2)#9-Cs( 1)-Br( 1)#10 Br(3)#10-Cs(l)-Br( 1)#10 Br(3)#l 1-Cs(l)-Br(l)#10 Br(3)#12-Cs(l)-Br(l)#10 Cs(2)-Cs(l)-Br(l)#12 Br(2)#7-Cs( 1)-Br( 1)#12 Br(2)#8-Cs( 1)-Br(l)#12 Br(2)#9-Cs(l)-Br(l)#12 Br(3)#10-Cs(l)-Br(l)#12 B r(3)#ll-C s(l)-Br(l)#12 Br(3)#12-Cs(l)-Br(l)#12 Br(l)#10-Cs(l)-Br(l)#12 C s(2)-Cs(l)-Br(l)#l 1 Br(2)#7-Cs(l)-Br(l)#l 1 Br(2)#8-Cs(l )-Br( 1)#11 Br(2)#9-Cs(l)-BT(1)#11 Br(3)#10-Cs(l)-Br(l)#ll B r(3)#ll-C s(l)-B r(l)#ll Br(3)#12-Cs(l)-Br(l)#l 1 B r(l)#10-C s(l)-B r(l)#ll B r(l)#12-C s(l)-B r(l)#ll Cs(l)-Cs(2)-Br(4)#13 Cs(l)-Cs(2)-Br(4)#14 Br(4)#13-Cs(2)-Br(4)#14 Cs(l)-Cs(2)-Br(4)#15 Br(4)#13-Cs(2)-Br(4)#15 Br(4)#14-Cs(2)-Br(4)#15 Cs(l)-Cs(2)-Br(l)#13 Br(4)#13-Cs(2)-Br(l)#13 Br(4)#14-Cs(2)-Br( 1)#13 Br(4)#15-Cs(2)-Br( 1)#13 Cs(l)-Cs(2)-Br(l)#14 Br(4)#13-Cs(2)-Br(l)#14 Br(4)#14-Cs(2)-Br( 1)#14 Br(4)#15-Cs(2)-Br( 1)#14 Br( 1)# 13-Cs(2)-Br( 1)#14 Cs(l)-Cs(2)-Br(l)#15 Br(4)#13-Cs(2)-Br(l)#15 Br(4)#14-Cs(2)-Br(l)#l5 Br(4)#15-Cs(2)-Br( 1)#15 Br(l)#13-Cs(2)-Br(l)#15 Br(l)#14-Cs(2)-Br(l)#15

139.89(2) 109.41(2) 62.24(2) 125.57(2) 67.82(2) 139.89(2) 125.57(2) 109.41(2) 62.24(2) 67.82(2) 67.82(2) 109.86(2) 56.342(10) 77.623(10) 165.39(2) 56.32(2) 55.189(14) 110.24(3) 109.86(2) 77.624(10) 165.39(2) 56.342(10) 55.189(14) 110.24(3) 56.32(2) 109.08(2) 109.86(2) 165.39(2) 56.341(10) 77.622(10) 110.24(3) 56.31(2) 55.189(14) 109.08(2) 109.08(2) 78.86(3) 78.86(3) 116.36(2) 78.86(3) 116.36(2) 116.36(2) 139.81(2) 61.99(2) 109.49(2) 125.36(3) 139.81(2) 125.36(3) 61.99(2) 109.49(2) 67.96(3) 139.81(2) 109.49(2) 125.36(5) 61.99(2) 67.96(3) 67.96(3)


Cs(l)-Cs(2)-Br(3)#16 Br(4># I3-Cs(2)-Br(3># 16 Br(4># 14-Cs(2)-Br(3># 16 Br(4)#15-Cs(2)-Br(3)#16 Br(l)#13-Cs(2)-Br(3)#16 Br(l)#14-Cs(2)-Br(3)#16 Br(l)#15-Cs(2)-Br(3)#16 Cs( 1)-Cs(2)-Br(3)#17 Br(4)#13-Cs(2)-Br(3)#17 Br(4># 14-Cs(2)-Br(3)#l 7 Br(4)#15-Cs(2)-Br(3)#17 Br( 1)# 13-Cs(2)-Br(3)# 17 Br( 1)#14-Cs(2)-Br(3)#l 7 Br( l)#15-Cs(2)-Br(3)#17 Br(3)#16-Cs(2)-Br(3)#17 Cs( 1)-Cs(2)-Br(3)#18 Br(4)#13-Cs(2)-Br(3)#18 Br(4)#14-Cs(2)-Br(3)#18 Br(4)#15-Cs(2)-Br(3)#18 Br(l)#13-Cs(2)-Br(3)#18 Br(l)#14-Cs(2)-Br(3)#18 Br( l)#15-Cs(2)-Br(3)#18 Br(3># 16-Cs(2)-Br(3)#18 Br(3>#17-Cs(2)-Br(3>#18

109.96(2) 77.137(12) 56.747(12) 165.65(3) 54.94(2) 56.39(2) 110.22(4) 109.96(2) 56.747(12) 165.65(3) 77.137(12) 56.39(2) 110.22(4) 54.94(2) 108.98(2) 109.96(2) 165.65(3) 77.137(12) 56.747(12) 110.22(4) 54.94(2) 56.39(2) 108.98(2) 108.98(2

206


C hap ter 4 Com pound IV-6 A tom ic coordinates and thermal parameters.

A g(l) C(l) C (ll) C(12) C(13) C(14) C(15) C( 16) C(17) C(1S) C(19) C(21) C(22) C(23) C(24) C(25) C(26) C(27) C(28) C(29) C(31) C(32) C(33) C(34) C(35) C(36) C(37) C(38) C(39) Br(2) Br(3) Br(4) Br(5) Br(6) Cl(7) Cl(8) Cl(9) Cl(10) C I(ll) Cl( 12) B(2) B(3) B(4) B(5) B(6) B(7) B(S) B(9)

X

V

-2868(1) 160(6) -4479(7) -5521(6) -5924(6) -5340(7) -4297(6) -3834(7) -6262(8) -2741(8) -5909(9) -1731(6) -2961(7) -3477(7) -2801(7) -1631(8) -1029(7) -3634(9) 319(7) -3353(9) -8233(8) -7620(7) -6620(8) -6198(8) -6717(8) -7781(8) -9380(9) -5954(8) -6213(11) 1322(1) 2438(1) 446(1) -1856(1) -1259(1) -19(2) -544(2) -3133(2) -4192(2) -2262(2) -3317(2) 125(7) 604(8) -353(8) -1463(7) -1152(°) -486(7) -761(7) -2041(7)

-2416(1) -2614(4) -1385(4) -2044(4) -1956(5) -1267(5) -605(5) -669(4) -2796(5) 90(5) -1186(6) -3457(4) -3929(4) -3594(5) -2848(5) -2413(5) -2681(5) -4813(5) -2270(7) -2581(7) -2133(5) -2961(5) -3043(5) -2200(5) -1350(5) -1313(5) -2148(7) -3980(6) -437(7) -4699(1) -2345(1) -347(1) -1467(1) -4128(1) -4332(1) -1689(1) -1187(1) -3496(2) -5457(1) -3630(1) -3803(4) -2656(5) -1727(5) -2253(5) -3531(5) -3626(5) -2356(5) -2094(5)

z -549(1) 3275(4) -286(4) -619(5) -1461(4) -1908(4) -1541(5) -721(5) -80(6) -370(5) -2795(5) -1281(4) -1614(4) -2355(4) -2749(4) -2398(4) -1682(4) -1217(5) -1358(5) -3594(5) -4503(4) -4582(4) -5037(5) -5464(4) -5442(5) -4931(5) -3978(5) -5108(6) -5869(6) 3147(1) 2120(1) 2744(1) 4189(1) 4452(1) 918(1) 684(1) 1970(1) 2974(1) 2354(1) 867(1) 2793(5) 2306(5) 2594(4) 3270(4) 3408(5) 1749(4) 1635(5) 2252(4)

U(eq) 81(1) 67(2) 85(3) 86(3) 74(2) 86(3) 89(3) 87(3) 127(4) 114(3) 136(4) 68(2) 79(2) 90(3) 83(2) 95(3) 79(2) 136(3) 143(4) 152(4) 93(3) 93(3) 99(3) 103(3) 108(3) 106(3) 154(4) 139(4) 179(5) 108(1) 102(1) 116(1) 119(1) 114(1) 84(1) 67(1) 101(1) 109(1) 97(1) 79(1) 69(2) 76(3) 61(2) 67(2) 82(3) 61(2) 60(2) 63(2)

207


B(10) -2558(8) -3223(6) 2734(5) 77(3) B (ll) -1594(7) -4182(5) 2440(4) 60(2) B(12)________________-2096(8)______________-3256(5)_____________ 1719(5)_____________ 73(3) Bond lengths Ag(l)-C(21) Ag( 1)-C( 11) Ag(l)-CI(12) Ag(l)-C(22) Ag(l)-C(16) Ag(l)-CI(8) C(l)-B(3) C(l)-B(4) C(l)-B(6) C(l)-B(2) C(l)-B(5) C(11)-C(16) C(11)-C(12) C(12)-C(13) C(12)-C(17) C(13)-C(14) C(14)-C(15) C(14)-C(19) C(15)-C(16) C(16)-C(18) C(21)-C(22) C(21)-C(26) C(22)-C(23) C(22)-C(27) C(23)-C(24) C(24)-C(25) C(24)-C(29) C(25)-C(26) C(26)-C(28) C(31)-C(32) C(31)-C(36) C(31)-C(37) C(32)-C(33) C(33)-C(34) C(33)-C(38) C(34)-C(35) C(35)-C(36) C(35)-C(39)

2.328(6) 2.352(6) 2.889(2) 2.644(6) 2.661(6) 2.986(2) 1.698(11) 1.728(9) 1.731(10) 1.764(8) 1.784(10) 1.348(9) 1.351(8) 1.401(9) 1.529(10) 1.309(9) 1.372(9) 1.510(10) 1.378(10) 1.468(9) 1.381(8) 1.397(8) 1.369(9) 1.485(9) 1.352(9) 1.324(9) 1.498(10) 1.335(9) 1.452(9) 1.355(10) 1.367(10) 1.526(12) 1.343(11) 1.383(10) 1.513(11) 1.319(11) 1.448(12) 1.478(12)

Br(2)-B(2) Br(3)-B(3) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6) Cl(7)-B(7) Cl(8)-B(8) Cl(9)-B(9) Cl(10)-B(10) C l(ll)-B (ll) Cl(12)-B(12) B(2)-B(3) B(2)-B(7) B (2)-B (ll) B(2)-B(6) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(4)-B(8) B(4)-B(9) B(4)-B(5) B(5)-B(9) B(5)-B(10) B(5)-B(6) B(6)-B(l 1) B(6)-B(10) B(7)-B(8) B(7)-B(12) B (7)-B (ll) B(8)-B(12) B(8)-B(9) B(9)-B(12) B(9)-B(10) B(10)-B(12) B (10)-B (ll) B (ll)-B (12)

1.872(7) 1.923(8) 1.924(6) 1.933(7) 1.901(7) 1.790(7) 1.823(8) 1.784(7) 1.750(9) 1.754(6) 1.782(8) 1.778(10) 1.780(10) 1.790(10) 1.803(12) 1.767(11) 1.769(9) 1.770(11) 1.755(10) 1.755(10) 1.759(10) 1.727(10) 1.757(10) 1.795(10) 1.782(10) 1.804(12) 1.769(9) 1.772(11) 1.789(10) 1.719(10) 1.804(10) 1.768(10) 1.762(10) 1.777(11) 1.808(11) 1.803(10)

130.3(2) 96.55(14) 120.51(17) 62.2(4) 111.8(4) 110.6(5) 61.8(4) 112.4(4) 62.1(4)

B(3)-C(l)-B(5) B(4)-C(l)-B(5) B(6)-C(l)-B(5) B(2)-C(l)-B(5) Q 16)-C (ll)-C (12) C(ll)-C(12)-C(13) C(ll)-C(12)-C(17) C(13)-C(12)-C(17) C(14)-C(13)-C(12)

111.1(5) 60.1(4) 61.4(4) 112.2(4) 123.3(7) 116.7(6) 120.6(7) 122.6(6) 122.4(6)

Bond angles C(22)-Ag( 1)-C( 16) C(22)-Ag( 1)-C1( 12) C( 16)-Ag( 1)-CI(12) B(3)-C(l)-B(4) B(3)-C(l)-B(6) B(4)-C(l)-B(6) B(3)-C(l)-B(2) B(4)-C(l)-B(2) B(6)-C(l)-B(2)

208


C(13)-C(14)-C(15) C( 13)-C( 14)-C( 19) C( 15)-C( 14 )-C( 19) C( 14)-C( 15)-C( 16) C(ll)-C(16)-C(15) C(11)-C(16)-C(18) C( 15)-C( 16)-C( 18) C (ll)-C (16)-A g(l) C( 15)-C( 16)-Ag( 1) C( 18)-C( 16)-Ag( 1) C(22)-C(21)-C(26) C(23)-C(22)-C(21) C(23)-C(22)-C(27) C(21)-C(22)-C(27) C(23)-C(22)-Ag( 1) C(21)-C(22)-Ag( 1) C(27)-C(22)-Ag( 1) C(24)-C(23)-C(22) C(25)-C(24)-C(23) C(25)-C(24)-C(29) C(23)-C(24)-C(29) C(24)-C(25)-C(26) C(25)-C(26)-C(21) C(25)-C(26)-C(28) C(21)-C(26)-C(28) C(32)-C(31)-C(36) C(32)-C(31)-C(37) C(36)-C(31)-C(37) C(33)-C(32)-C(31) C(32)-C(33)-C(34) C(32)-C(33)-C(38) C( 34)-C(33 )-C(38) C(35)-C(34)-C(33) C(34)-C(35)-C(36) C(34)-C(35)-C(39) C(36)-C(35)-C(39) C(31)-C(36)-C(35) B( 12)-Cl( 12)-Ag( 1) C(l)-B(2)-B(3) C(l)-B(2)-B(7) B(3)-B(2)-B(7) C(l)-B(2)-B(l 1) B(3)-B(2)-B(l 1) B(7)-B(2)-B(l 1) C(l)-B(2)-B(6) B(3)-B(2)-B(6) B(7)-B(2)-B(6) B(11)-B(2)-B(6) C(l)-B(2)-Br(2) B(3)-B(2)-Br(2) B(7)-B(2)-Br(2) B(11)-B(2)-Br(2) B(6)-B(2)-Br(2) C(l)-B(3)-B(8) C(l)-B(3)-B(7) B(8)-B(3)-B(7)

118.9(6) 118.4(6) 122.5(7) 121.4(6) 117.3(6) 124.6(7) 117.9(6) 62.0(4) 107.0(4) 104.8(4) 121.9(6) 117.0(6) 121.8(6) 121.0(6) 105.7(4) 61.5(3) 104.8(4) 121.5(6) 119.1(6) 121.7(7) 119.1(6) 124.6(7) 115.9(6) 123.3(7) 120.6(6) 116.1(7) 120.6(7) 123.3(7) 126.0(7) 116.1(7) 124.6(7) 119.3(8) 123.8(8) 117.0(7) 123.3(9) 119.6(8) 121.0(7) 111.5(3) 57.3(4) 104.2(4) 59.6(4) 104.5(5) 106.8(5) 60.1(4) 58.1(4) 105.0(5) 106.7(5) 59.5(4) 122.4(4) 123.1(5) 125.2(5) 124.0(4) 121.3(5) 106.7(5) 107.5(5) 60.1(4)

C(l)-B(3)-B(4) B(8)-B(3)-B(4) B(7)-B(3)-B(4) C(l)-B(3)-B(2) B(8)-B(3)-B(2) B(7)-B(3>B(2) B(4)-B(3)-B(2) C(l)-B(3)-Br(3) B(8)-B(3)-Br(3) B(7)-B(3)-Br(3) B(4)-B(3)-Br(3) B(2)-B(3)-Br(3) C(l)-B(4)-B(8) C(l)-B(4)-B(9) B(8)-B(4)-B(9) C(l)-B(4)-B(5) B(8)-B(4)-B(5) B(9)-B(4)-B(5) C(l)-B(4)-B(3) B(8)-B(4)-B(3) B(9)-B(4)-B(3) B(5)-B(4)-B(3) C(l)-B(4)-Br(4) B(8)-B(4)-Br(4) B(9)-B(4)-Br(4) B(5)-B(4)- Br(4) B(3)-B(4)-Br(4) B(9)-B(5)-B(10) B(9)-B(5)-B(4) B( 10)-B(5)-B(4) B(9)-B(5)-B(6) B(10)-B(5)-B(6) B(4)-B(5)-B(6) B(9)-B(5)-C(l) B(10)-B(5)-C(l) B(4)-B(5)-C(l) B(6)-B(5)-C(l) B(9)-B(5)-Br(5) B( 10)-B(5)-Br(5) B(4)-B(5)-Br(5) B(6)-B(5)-Br(5) C(l)-B(5)-Br(5) C (l)-B (6)-B (ll) C(l)-B(6)-B(5) B(11)-B(6)-B(5) C(l)-B(6)-B(10) B( 11 )-B(6)-B( 10) B(5)-B(6)-B( 10) C(l)-B(6)-B(2) B(ll)-B(6)-B(2) B(5)-B(6)-B(2) B(10)-B(6)-B(2) C(l)-B(6)-Br(6) B(ll)-B(6)-Br(6) B(5)-B(6)-Br(6) B(10)-B(6)-Br(6)

59.7(4) 593(4) 108.0(5) 60.9(4) 109.0(5) 60.3(4) 109.8(6) 120.4(5) 124.8(5) 122.3(5) 122.6(4) 117.8(5) 106.0(4) 107.7(5) 61.9(4) 61.5(4) 108.5(5) 58.9(4) 58.1(4) 60.2(4) 110.0(5) 109.0(5) 119.5(4) 124.3(4) 123.8(4) 120.2(4) 119.9(5) 60.7(4) 60.5(4) 108.1(5) 109.3(5) 61.0(4) 106.3(5) 106.5(5) 105.9(5) 58.4(4) 57.9(4) 124.8(5) 125.4(5) 120.6(4) 120.1(5) 119.3(4) 106.2(5) 60.7(4) 107.6(5) 106.2(5) 60.6(4) 58.5(4) 59.9(4) 59.9(4) 109.9(5) 108.9(5) 119.7(5) 125.0(5) 120.0(5) 124.7(6)

209


B(2)-B(6)-Br(6) B(8)-B(7)-B(12) B(8)-B(7)-B(3) B(12)-B(7)-B(3) B(8)-B(7)-B(2) B(12)-B(7)-B(2) B(3)-B(7)-B(2) B(8)-B(7)-B(l 1) B(12)-B(7)-B(ll) B(3)-B(7)-B(l 1) B(2)-B(7)-B(l 1) B(8)-B(7)-C1(7) B(12)-B(7)-CI(7) B(3)-B(7)-CI(7) B(2)-B(7)-CI(7) B(11)-B(7)-C1(7) B(12)-B(8)-B(4) B(12)-B(8)-B(7) B(4)-B(8)-B(7) B(12)-B(8)-B(3) B(4)-B(8)-B(3) B(7)-B(8)-B(3) B(12)-B(8)-B(9) B(4)-B(8)-B(9) B(7)-B(8)-B(9) B(3)-B(8)-B(9) B(12)-B(8)-CI(8) B(4)-B(8)-C!(8) B(7)-B(8)-C1(8) B(3)-B(8)-C1(8) B(9)-B(8)-C1(8) B(5)-B(9)-B(4) B(5)-B(9)-B(12) B(4)-B(9)-B(12) B(5)-B(9)-B(10) B(4)-B(9)-B(10) B(12)-B(9)-B(10) B(5)-B(9)-CI(9) B(4)-B(9)-CI(9) B(12)-B(9)-C1(9) B(10)-B(9)-C1(9) B(5)-B(9)-B(8) B(4)-B(9)-B(8) B(12)-B(9)-B(8) B(10)-B(9)-B(8) Cl(9)-B(9)-B(8) CI(10)-B(10)-B(5) CI(10)-B(10)-B(9) B(5)-B(10)-B(9) CI(10)-B(10)-B(12) B(5)-B(10)-B(12) B(9)-B(10)-B(12) Cl(10)-B(10)-B(6) B(5)-B(10)-B(6) B(9)-B(10)-B(6) B(12)-B(10)-B(6)

119.8(5) 58.1(4) 59.9(4) 105.8(5) 108.8(5) 108.6(5) 60.1(4) 107.5(5) 60.8(4) 107.2(5) 60.2(4) 121.2(5) 121.5(4) 123.1(5) 122.0(5) 122.0(4) 107.4(5) 61.1(4) 108.6(5) 108.3(5) 60.3(4) 60.0(4) 60.2(4) 59.1(4) 109.4(5) 107.9(5) 122.2(5) 120.7(4) 122.2(5) 122.0(5) 120.4(4) 60.7(4) 107.9(5) 105.2(5) 60.5(4) 108.1(5) 60.5(4) 121.1(5) 121.3(4) 123.8(5) 122.7(5) 107.7(5) 59.1(4) 57-5(4) 106.7(5) 122.3(5) 120.3(5) 120.7(5) 58.8(4) 124.2(5) 106.2(5) 59.9(4) 122.2(5) 60.5(4) 107.4(5) 106.2(6)

CI( 10)-B( 10)-B( 11) B(5)-B(10)-B(ll) B(9)-B( 10)-B( 11) B(12)-B(10)-B(l 1) B(6)-B( 10)-B( 11) C l(ll)-B (ll)-B (6) C l(ll)-B (ll)-B (7) B(6)-B(ll)-B(7) C l(ll)-B (ll)-B (2) B(6)-B(ll)-B(2) B(7)-B(ll)-B(2) Cl( 11)-B( 11)-B( 12) B(6)-B(ll)-B(12) B(7)-B( 11)-B( 12) B(2)-B(ll)-B(12) C l(ll)-B (ll)-B (10) B(6)-B( 11)-B( 10) B(7)-B(ll)-B(10) B(2)-B(ll)-B(10) B(12)-B(11>B(10) B(8)-B(12)-B(7) B(8)-B(12)-B(9) B(7)-B(12)-B(9) B(8)-B(12)-B(10) B(7)-B( 12)-B( 10) B(9)-B(12)-B(10) B(8)-B( 12)-C1(12) B(7)-B(12)-C1(12) B(9)-B(12)-C1(12) B(10)-B(12)-C1(12) B(8)-B( 12)-B( 11) B(7)-B(12)-B(ll) B(9)-B(12)-B(ll) B(10)-B(12)-B(ll) Cl( 12)-B( 12)-B(l 1)

122.9(5) 108.1(5) 109.0(5) 60.4(4) 59.1(4) 122.6(5) 121.9(5) 107.3(5) 121.2(5) 60.6(4) 59.7(4) 123.1(5) 106.1(5) 59.1(4) 106.8(5) 121.6(5) 60.3(4) 107.4(5) 109.3(5) 59.0(4) 60.9(4) 62.3(4) 110.9(5) 109.8(5) 109.5(5) 59.6(4) 121.8(5) 120.1(5) 121.6(5) 120.4(5) 109.1(5) 60.0(4) 109.0(5) 60.7(4) 119.7(4)

210


Compound IV-7 A tom ic coordinates and thermal parameters.

A g(l) C (ll) C(12) C(13) C(14) C(15) C(16) C(17) C{18) C(19) C(21) C(22) C(23) C(24) C(25) C(26) C(27) C(28) C(29) C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B(11) B(12) Cl(2) CI(3) Cl(4) Cl(5) Cl(6) Br(7) Br(8) Br(9) Br(10) B r(ll) Br(12)

X

y

10903(1) 12731(3) 12637(3) 11912(3) 11268(3) 11388(3) 12121(3) 12249(3) 13300(3) 10494(3) 15037(4) 14943(4) 15100(3) 15367(4) 15448(4) 15321(4) 15508(5) 14643(4) 15574(6) 12948(3) 12570(3) 12607(3) 12442(3) 12283(3) 12376(3) 11421(3) 11592(3) 11745(3) 11689(3) 11462(3) 11020(3) 13221(1) 13318(1) 12959(1) 12624(1) 12790(1) 10751(1) 11107(1) 11451(1) 11291(1) 10833(1) 9878(1)

16778(1) 17302(3) 16484(3) 16404(4) 17098(3) 17883(3) 17984(3) 18922(4) 15710(4) 16988(4) 13222(4) 12255(5) 12202(5) 13070(6) 14027(6) 14139(5) 15215(5) 11250(5) 12933(7) 13372(3) 13089(5) 14467(4) 14384(4) 13002(4) 12174(4) 12532(4) 12591(4) 14009(4) 14817(4) 13915(4) 13665(4) 12719(1) 15440(1) 15300(1) 12468(1) 10866(1) 11374(1) 11600(1) 14600(1) 16332(1) 14360(1) 13852(1)

z 3494(1) 4328(2) 4853(2) 5237(2) 5061(2) 4511(3) 4150(2) 3611(4) 5049(3) 5465(3) 937(4) 1300(4) 2043(4) 2428(5) 2092(4) 1339(4) 905(5) 865(4) 3245(5) 1903(2) 2783(3) 2426(3) 1447(3) 1206(3) 2037(2) 1679(3) 2648(3) 2879(3) 2043(3) 1319(3) 2203(3) 3504(1) 2776(1) 833(1) 358(1) 2023(1) 1250(1) 3340(1) 3838(1) 2053(1) 461(1) 2356(1)

U(eq) 76(1) 61(2) 58(2) 69(2) 56(2) 62(2) 56(2) 119(3) 99(2) 92(2) 114(3) 120(3) 129(3) 159(4) 154(3) 124(3) 228(6) 161(4) 251(5) 51(1) 61(2) 48(2) 50(2) 57(2) 46(2) 41(2) 45(2) 51(2) 48(2) 42(2) 45(2) 71(1) 75(1) 74(1) 72(1) 67(1) 62(1) 63(1) 58(1) 63(1) 67(1) 56(1)

Bond lengths Ag(l)-C(15) Ag(l)-Br(10) Ag(l)-Br(7)#l Ag(l)-Br(9)

C(ll)-C(16) C(ll)-C(12) C(12)-C(13) C(12)-C(18) C(13)-C(14)

2.421(5) 2.7498(19) 2.8457(13) 2.8729(14)

1.352(6) 1.387(6) 1.403(6) 1.497(7) 1.404(6)

211


C(14)-C(15) C(14)-C(19) C(15)-C(16) C(16)-C(17) C(21)-C(22) C(21)-C(26) C(22)-C(23) C(22)-C(28) C(23)-C(24) C(24)-C(25) C(24)-C(29) C(25)-C(26) C(26)-C(27) C(l)-B(4) C(l)-B(3) C(l)-B(5) C(l)-B(2) C(l)-B(6) B(2)-C1(2) B(2)-B(8) B(2)-B(6) B(2)-B(9) B(2)-B(3) B(3)-B(10) B(3)-B(9) B(3)-CI(3) B(3)-B(4) B(4)-B(10)

1.396(6) 1.495(6) 1.396(6) 1.519(7) 1.358(9) 1.415(9) 1.373(10) 1.539(9) 1.342(10) 1.322(10) 1.530(12) 1.389(10) 1.559(10) 1.706(6) 1.732(6) 1.740(7) 1.752(7) 1.760(6) 1.758(6) 1.760(7) 1.782(7) 1.785(7) 1.798(7) 1.735(7) 1.752(7) 1.791(5) 1.799(7) 1.742(7)

B (4)-B (ll) B(4)-B(5) B(4)-C1(4) B(5)-C1(5) B(5)-B(7) B(5)-B(ll) B(5)-B(6) B(6)-CI(6) B(6)-B(7) B(6)-B(8) B(7)-B(8) B(7)-B(12) B (7)-B (ll) B(7)-Br(7) B(8)-B(9) B(8)-B(12) B(8)-Br(8) B(9)-B(12) B(9)-B(10) B(9)-Br(9) B(10)-B (ll) B(10)-B(12) B(10)-Br(10) B (ll)-B (12) B (ll)-B r(ll) B(12)-Br(12) Br(7)-Ag(l)#2

1.748(7) 1.757(7) 1.799(5) 1.767(6) 1.772(7) 1.777(7) 1.819(7) 1.736(5) 1.775(7) 1.793(7) 1.783(7) 1.806(7) 1.807(6) 1.959(5) 1.794(7) 1.809(7) 1.920(5) 1.772(7) 1.809(7) 1.946(5) 1.752(7) 1.817(7) 1.960(5) 1.793(7) 1.953(5) 1.942(5) 2.8457(13)

139.01(11) 107.16(11) 110.65(4) 103.95(11) 87.04(3) 96.58(3) 121.1(4) 119.5(4) 122.0(4) 118.5(4) 120.4(4) 117.6(4) 122.5(4) 119.9(4) 121.5(4) 96.7(3) 89.0(3) 119.8(4) 120.4(4) 119.6(4) 118.2(7) 119.7(6) 118.5(6) 121.8(6) 122.4(7)

C(25)-C(24)-C(23) Q25)-C(24)-C(29) C(23)-C(24)-C(29) C(24)-C(25)-C(26) C(25)-C(26)-C(21) C(25)-C(26)-C(27) C(21)-C(26)-C(27) B(4)-C(l)-B(3) B(4)-C(l)-B(5) B(3)-C(l)-B(5) B(4)-C(l)-B(2) B(3)-C(l)-B(2) B(5)-C(l)-B(2) B(4)-C(l)-B(6) B(3)-C(l)-B(6) B(5)-C(l)-B(6) B(2)-C(l)-B(6) C(1)-B(2)-C1(2) C(l)-B(2)-B(8) Cl(2)-B(2)-B(8) C(l)-B(2)-B(6) Cl(2)-B(2)-B(6) B(8)-B(2)-B(6) C(l)-B(2)-B(9) Cl(2)-B(2)-B(9)

119.2(8) 121.3(7) 119.5(7) 121.6(7) 118.7(6) 123.3(6) 118.0(6) 63.1(3) 61.3(3) 112.7(3) 113.8(3) 62.1(3) 112.3(3) 113.3(3) 112.5(3) 62.6(3) 61.0(3) 120.3(3) 106.2(4) 126.0(4) 59.8(3) 121.1(3) 60.8(3) 104.3(4) 124.3(4)

Bond angles C( 15)-Ag( 1)-Br( 10) C(15)-Ag(l)-Br(7)#l Br(10)-Ag(l)-Br(7)#l C( 15)-Ag( 1)-Br(9) Br( 10)-Ag( 1)-Br(9) Br(7)#l-Ag(l)-Br(9) C( 16)-C( 11 )-C( 12) C(ll)-C(12)-C(13) C( 11 )-C( 12)-C( 18) C( 13)-C( 12)-C( 18) C( 14)-C( 13)-C( 12) C(15)-C(14)-C(13) C( 15)-C( 14)-C( 19) C( 13)-C( 14)-C( 19) C( 14)-C( 15)-C( 16) C( 14)-C( 15)-Ag( 1) C(16)-C(15)-Ag(l) C(ll)-C(16)-C(15) C(ll)-C(16)-C(17) C( 15)-C( 16)-C( 17) Q22)-C(21)-C(26) C(21)-C(22)-C(23) C(21)-C(22)-C(28) C(23)-C(22)-C(28) C(24)-C(23)-C(22)


B(8)-B(2)-B(9) B(6)-B(2)-B(9) C(l)-B(2)-B(3) Cl(2)-B(2)-B(3) B(8)-B(2)-B(3) B(6)-B(2)-B(3) B(9)-B(2)-B(3) C(l)-B(3)-B(10) ai)-B (3 )-B (9 ) B(10)-B(3)-B(9) C(1)-B(3)-CI(3) B( 10)-B(3)-C1(3) B(9)-B(3)-C1(3) C(l)-B(3)-B(2) B(10)-B(3)-B(2) B(9)-B(3)-B(2) CI(3)-B(3)-B(2) C(l)-B(3)-B(4) B(10)-B(3)-B(4) B(9)-B(3)-B(4) C!(3)-B(3)-B(4) B(2)-B(3)-B(4) C(l)-B(4)-B(10) C (l)-B(4)-B(l 1) B(10)-B(4)-B(ll) C(l)-B(4)-B(5) B(10)-B(4)-B(5) B(11)-B(4)-B(5) C(1)-B(4)-C1(4) B(10)-B(4)-C1(4) B(11)-B(4)-CI(4) B(5)-B(4)-CI(4) C(l)-B(4)-B(3) B(10)-B(4)-B(3) B(11)-B(4)-B(3) B(5)-B(4)-B(3) CI(4)-B(4)-B(3) C(l)-B(5)-B(4) C(l)-3(5)-CI(5) B(4)-B(5)-C1(5) C(l)-B(5)-B(7) B(4)-B(5)-B(7) Cl(5)-B(5)-B(7) C (l)-B (5)-B (ll) B(4)-B(5)-B(l 1) Cl(5)-B(5)-B(l 1) B(7)-B(5)-B(l 1) C(l)-B(5)-B(6) B(4)-B(5)-B(6) CI(5)-B(5)-B(6) B(7)-B(5)-B(6) B(11)-B(5)-B(6) CI(6)-B(6)-C(1) Cl(6)-B(6)-B(7) C(l)-B(6)-B(7) Cl(6)-B(6)-B(2)

C(1)-B(6>B(2) B(7)-B(6>B(2) CI(6)-B(6)-B(8) C(l)-B(6)-B(8) B(7)-B(6)-B(8) B(2)-B(6)-B(8) Cl(6)-B(6)-B(5) C(l)-B(6)-B(5) B(7)-B(6)-B(5) B(2)-B(6)-B(5) B(8)-B(6)-B(5) B(5)-B(7)-B(6) B(5)-B(7)-B(8) B(6)-B(7)-B(8) B(5)-B(7)-B(12) B(6)-B(7)-B(12) B(8)-B(7)-B(12) B(5)-B(7)-B(ll) B(6)-B(7)-B(ll) B(8)-B(7)-B(ll) B(12)-B(7)-B(ll) B(5)-B(7)-Br(7) B(6)-B(7)-Br(7) B(8)-B(7)-Br(7) B( 12)-B(7)-Br(7) B(ll)-B(7)-Br(7) B(2)-B(8)-B(7) B(2)-B(8)-B(6) B(7)-B(8)-B(6) B(2)-B(8)-B(9) B(7)-B(8)-B(9) B(6)-B(8)-B(9) B(2)-B(8)-B(12) B(7)-B(8)-B(12) B(6)-B(8)-B(12) B(9)-B(8)-B( 12) B(2)-B(8)-Br(8) B(7)-B(8)-Br(8) B(6)-B(8)-Br(8) B(9)-B(8)-Br(8) B( 12)-B(8)-Br(8) B(3)-B(9)-B(12) B(3)-B(9)-B(2) B(12)-B(9)-B(2) B(3)-B(9)-B(8) B(12)-B(9)-B(8) B(2)-B(9)-B(8) B(3)-B(9)-B(10) B(12)-B(9)-B(10) B(2)-B(9)-B( 10) B(8)-B(9)-B( 10) B(3)-B(9)-Br(9) B(12)-B(9)-Br(9) B(2)-B(9)-Br(9) B(8)-B(9)-Br(9) B(10)-B(9)-Br(9)

60.8(3) 109.1(4) 58.4(3) 119.0(3) 107.7(4) 108.4(4) 58.6(3) 105.2(3) 106.5(3) 62.5(3) 118.9(3) 124.3(3) 126.1(3) 59-5(3) 110.0(3) 60.3(3) 120.8(3) 57.8(3) 59.1(3) 108.7(3) 119.1(3) 107.3(3) 106.0(3) 107.0(3) 60.3(3) 60.3(3) 109.5(4) 60.9(3) 120.6(3) 123.1(3) 124.8(3) 120.8(3) 59.2(3) 58.6(3) 106.9(3) 108.8(3) 120.3(3) 58.4(3) 121.4(3) 121.3(3) 104.5(3) 108.1(4) 124.6(3) 104.2(3) 59.3(3) 125.6(3) 61.2(3) 59.2(3) 108.2(4) 119.4(3) 59.2(3) 108.4(4) 122.7(3) 125.3(3) 103.5(3) 120.8(3)

59.3(3) 106.6(3) 124.1(3) 104.4(3) 60.0(3) 59.0(3) 122.0(3) 58.1(3) 59.1(3) 107.3(4) 107.1(3) 61.7(3) 109.6(3) 60.5(3) 108.1(3) 109.2(3) 60.5(3) 59.5(3) 109.0(3) 108.2(3) 59.5(3) 120.3(3) 118.7(3) 120.6(3) 123.0(3) 123.3(3) 107.2(3) 60.2(3) 59.5(3) 60.3(3) 107.0(3) 108.2(3) 107.6(3) 60.4(3) 108.3(3) 58.9(3) 121.3(3) 123.5(3) 122.5(3) 120.8(3) 121.5(3) 108.2(4) 61.1(3) 108.1(3) 108.3(4) 61.0(3) 58.9(3) 58.3(3) 61.0(3) 107.2(4) 108.7(3) 120.8(3) 122.1(3) 121.1(3) 121.9(3) 122.4(3)

213


B(3)-B(10)-B(4) B(3)-B(10)-B(ll) B(4)-B(10)-B( 11) B(3)-B(10)-B(9) B(4)-B(10)-B(9) B(11)-B(10)-B(9) B(3)-B(10)-B(12) B(4)-B(10)-B(12) B(11)-B(10)-B(12) B(9)-B(10)-B(12) B(3)-B(10)-Br(10) B(4)-B(10)-Br(10) B(ll)-B(10)-Br(10) B(9)-B( lO)-Br(lO) B( 12)-B( 10)-Br( 10) B(4)-B(l 1)-B(10) B(4)-B(l 1)-B(5) B(10)-B(ll)-B(5) B(4)-B(ll)-B(12) B(10)-B(l 1)-B(12) B(5)-B(l 1)-B(12) B(4)-B(l 1)-B(7) B(10)-B(ll)-B(7) B(5)-B(l 1)-B(7) B(12)-B(ll)-B(7) B(4)-B(l 1)-Br(l 1) B( 10)-B( 11 )-Br( 11) B (5)-B (ll)-B r(ll) B( 12)-B( 11 )-Br( 11) B(7)-B(l 1)-Br(l 1) B(9)-B(12)-B(ll) B(9)-B(12)-B(7) B(11)-B(12)-B(7) B(9)-B(12)-B(8) B(11)-B(12)-B(8) B(7)-B(12)-B(8) B(9)-B(12)-B(10) B(11)-B(12)-B(10) B(7)-B(12)-B(10) B(8)-B(12)-B(10) B(9)-B(12)-Br(12) B(11)-B(12)-Br(12) B(7)-B( 12)-Br( 12) B(8)-B(12)-Br( 12) B(10)-B(12)-Br(12) B(7)-Br(7)-Ag(l)#2 B(9)-Br(9)-Ag(l) B( 10)-Br( 10)-Ag( 1)

62.3(3) 109.6(3) 60.0(3) 59.2(3) 108.7(3) 107.4(3) 106.9(3) 108.2(3) 60.3(3) 58.5(3) 121.8(3) 122.4(3) 121.5(3) 121.4(3) 120.9(3) 59.7(3) 59.8(3) 108.2(3) 109.0(3) 61.7(3) 108.5(3) 107.0(3) 108.7(3) 59.3(3) 60.2(3) 121.2(3) 122.7(3) 119.7(3) 122.5(3) 121.7(3) 107.2(3) 106.9(3) 60.3(3) 60.1(3) 107.6(3) 59.1(3) 60-5(3) 58.1(3) 106.0(3) 107.7(3) 122.9(3) 121.1(3) 122.1(3) 122.6(3) 122.6(3) 111.43(14) 103.17(14) 105.95(14)

214


Compound IV-8 A tom ic coordinates and thermal parameters. X

A g(l) Br(2) Br(3) Br(4) Br(5) Br(6) 1(7) 1(8) 1(9) 1(10) 1(11) 1(12) C(l) N(D C (ll) C(12) C(13) C(14) C(15) N(2) C(21) C(22) C(23) C(24) C(25) N(3) Q 31) C(32) C(33) C(34) C(35) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12)

-2728(1) 1973(1) 2410(1) -223(1) -2197(1) -892(1) 930(1) -567(1) -3686(1) -4145(1) -1250(1) -2970(1) 120(8) -1842(10) -616(14) -81(17) -860(30) -2106(19) -2544(15) -4720(9) -4990(14) -6176(19) -7195(16) -6978(13) -5746(11) 1973(15) 1895(16) 2820(30) 4050(20) 4241(13) 3229(14) 487(9) 681(9) -557(10) -1512(10) -893(10) -33(9) -697(10) -2084(8) -2270(9) -1036(9) -1760(9)

z 611(1) 4319(1) 3176(1) 3835(1) 5407(1) 5693(1) 1807(1) 1526(1) 2994(1) 4279(1) 3547(1) 1803(1) 4385(6) -692(7) -770(11) -1573(13) -2303(13) -2209(10) -1392(10) 463(7) -54(10) -236(11) 133(14) 658(11) 794(9) 5876(11) 6572(13) 7118(13) 7017(14) 6352(11) 5830(11) 3924(7) 3377(7) 3702(7) 4443(7) 4582(7) 2837(7) 2698(7) 3353(7) 3917(6) 3580(7) 2825(7)

y 1207(1) 2347(1) 1010(1) 36(1) 775(1) 2221(1) 2277(1) 688(1) 584(1) 2042(1) 3107(1) 2094(1) 1302(3) 1302(4) 1411(5) 1471(7) 1377(7) 1249(9) 1222(7) 820(4) 398(6) 203(7) 470(9) 916(7) 1080(5) 983(5) 653(7) 476(8) 672(8) 1025(7) 1142(7) 1916(4) 1279(4) 820(4) 1189(4) 1862(4) 1860(4) 1166(4) 1120(4) 1761(4) 2223(4) 1745(4)

U(eq) 79(1) 46(1) 49(1) 51(1) 52(1) 49(1) 52(1) 46(1) 49(1) 52(1) 52(1) 46(1) 31(2) 52(2) 69(4) 89(5) 102(7) 95(6) 75(4) 57(3) 76(4) 93(5) 108(7) 79(4) 57(3) 144(9) 93(6) 134(10) 118(9) 80(4) 90(5) 30(2) 30(2) 29(2) 31(2) 30(2) 32(2) 29(2) 27(2) 26(2) 29(2) 30(2)

Bond lengths A g (l)-N (l) Ag(l)-N(2) Ag(l)-I(12) Ag(l)-I(8)

Br(2)-B(2) Br(3)-B(3) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6)

2.258(11) 2.267(10) 2.8353(14) 2.8941(14)

1.936(10) 1.937(9) 1.919(9) 1.947(10) 1.928(10)

215


I(7)-B(7) I(8)-B(8) I(9)-B(9) I(10)-B(10) 1(11)-B(11) I(12)-B(12) C(l)-B(2) C(l)-B(3) C(l)-B(4) C(l)-B(5) C(l)-B(6) N (l)-C (ll) N(l)-C(15) C(ll)-C(12) C(12)-C(13) C(13)-C(14) C(14)-C(15) N(2)-C(21) N(2)-C(25) C(21)-C(22) C(22)-C(23) C(23)-C(24) C(24)-C(25) N(3)-C(35) N(3)-C(31) C(31)-C(32) C(32)-C(33) C(33)-C(34)

2.154(11) 2.159(10) 2.158(9) 2.146(9) 2.132(9) 2.161(10) 1.684(13) 1.688(14) 1.706(13) 1.717(13) 1.735(13) 1.305(17) 1.304(18) 1.39(2) 1.39(3) 1.34(3) 1.36(2) 1.316(16) 1.347(14) 1.336(19) 1.37(2) 1.36(2) 1.346(16) 1.359(17) 1.344(19) 1.33(2) 1.37(3) 1.35(2)

C(34)-C(35) B(2)-B(7) B(2)-B(3) B(2)-B(6) B (2)-B (ll) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(4)-B(8) B(4)-B(5) B(4)-B(9) B(5)-B(6) B(5)-B(10) B(5)-B(9) B(6)-B(10) B (6)-B (ll) B (7)-B (ll) B(7)-B(12) B(7)-B(8) B(8)-B(12) B(8)-B(9) B(9)-B(12) B(9)-B(10) B (10)-B (ll) B(10)-B(12) B(11)-B(12)

1.335(18) 1.763(16) 1.762(14) 1.786(14) 1.805(13) 1.769(15) 1.775(15) 1.775(14) 1.770(15) 1.776(15) 1.805(13) 1.747(14) 1.766(14) 1.784(15) 1.753(14) 1.782(15) 1.799(14) 1.809(14) 1.810(14) 1.785(13) 1.788(14) 1.745(13) 1.781(13) 1.781(13) 1.793(14) 1.788(15)

110.1(4) 123.8(2) 105.9(2) 98.9(2) 124.2(3) 94.76(4) 96.9(3) 97.4(3) 63.0(6) 115.0(7) 63.1(6) 113.3(7) 114.2(7) 62.5(6) 62.9(6) 114.6(7) 113.3(7) 60.8(6) 118.1(14) 121.7(10) 120.2(10) 121.3(16) 118.7(16) 119.0(17) 117.4(16)

N(l)-C(15)-C(14) C(21)-N(2)-C(25) C(21)-N(2)-Ag(l) C(25)-N(2)-Ag(l) N(2)-C(21)-C(22) C(21)-C(22)-C(23) C(24)-C(23)-C(22) C(25)-C(24)-C(23) N(2)-C(25)-C(24) C(35)-N(3)-C(31) C(32)-C(31)-N(3) C(33)-C(32)-C(31) C(32)-C(33)-C(34) C(35)-C(34)-C(33) C(34)-C(35)-N(3) C(l)-B(2)-B(7) C(l)-B(2)-B(3) B(7)-B(2)-B(3) C(l)-B(2)-B(6) B(7)-B(2)-B(6) B(3)-B(2)-B(6) C (l)-B (2)-B (ll) B(7)-B(2)-B( 11) B(3)-B(2)-B(l 1) B(6)-B(2)-B(l 1)

125.3(16) 115.7(11) 123.5(9) 119.8(8) 125.1(13) 117.4(13) 120.2(14) 117.6(14) 123.9(12) 106.8(16) 129.7(16) 118.3(15) 117.2(15) 117.8(15) 130.0(16) 105.9(7) 58.6(6) 60.5(6) 59.9(5) 108.4(7) 108.6(7) 105.9(6) 60.5(6) 108.7(7) 59.5(6)

Bond angles N(l)-Ag(l)-N(2) N(l)-Ag(l)-I(12) N(2)-Ag(l)-I(12) N(l)-Ag(l)-I(8) N(2)-Ag(l)-I(8) I(12)-Ag(l)-I(8) B(8)-I(8)-Ag(l) B(12)-I(12)-Ag(l) B(2)-C(l)-B(3) B(2)-C(l)-B(4) B(3)-C(l)-B(4) B(2)-C(l)-B(5) B(3)-C(l)-B(5) B(4)-C(l)-B(5) B(2)-C(l)-B(6) B(3)-C(l)-B(6) B(4)-C(l)-B(6) B(5)-C(l)-B(6) C(11)-N(1)-C(15) C(11)-N(l)-Ag(l) C(15)-N(l)-Ag(l) N(l)-C(ll)-C (12) C( 11)-C( 12)-C( 13) C( 14)-C( 13 )-C( 12) C(13)-C(14)-C(15)

216


C(l)-B(2)-Br(2) B(7)-B(2)-Br(2) B(3)-B(2)-Br(2) B(6)-B(2)-Br(2) B(11)-B(2)-Br(2) C(l)-B(3)-B(2) C(l)-B(3)-B(8) B(2)-B(3)-B(8) C(l)-B(3)-B(7) B(2)-B(3)-B(7) B(8)-B(3)-B(7) C(l)-B(3)-B(4) B(2)-B(3)-B(4) B(8)-B(3)-B(4) B(7)-B(3)-B(4) C(l)-B(3)-Br(3) B(2)-B(3)-Br(3) B(8)-B(3)-Br(3) B(7)-B(3)-Br(3) B(4)-B(3)-Br(3) C(l)-B(4)-B(8) C(l)-B(4)-B(5) B(8)-B(4)-B(5) C(l)-B(4)-B(3) B(8)-B(4)-B(3) B(5)-B(4)-B(3) C(l)-B(4)-B(9) B(8)-B(4)-B(9) B(5)-B(4)-B(9) B(3)-B(4)-B(9) C(l)-B(4)-Br(4) B(8)-B(4)-Br(4) B(5)-B(4)-Br(4) B(3)-B(4)-Br(4) B(9)-B(4)-Br(4) C(l)-B(5)-B(6) C(l)-B(5)-B(10) B(6)-B(5)-B(10) C(l)-B(5)-B(4) B(6)-B(5)-B(4) B(10)-B(5)-B(4) C(l)-B(5)-B(9) B(6)-B(5)-B(9) B(10)-B(5)-B(9) B(4)-B(5)-B(9) C(l)-B(5)-Br(5) B(6)-B(5)-Br(5) B(10)-B(5)-Br(5) B(4)-B(5)-Br(5) B(9)-B(5)-Br(5) C(l)-B(6)-B(5) C(l)-B(6)-B(10) B(5)-B(6)-B(10) C (l)-B (6)-B (ll) B(5)-B(6)-B(l 1) B(10)-B(6)-B(l 1)

121.2(6) 124.1(6) 120.9(6) 120.0(7) 123.8(6) 58.4(5) 105.3(7) 108.6(7) 105.3(7) 59.8(6) 61.4(6) 59.0(6) 107.8(7) 59.9(6) 109.1(7) 120.4(6) 119.1(6) 125.8(7) 124.0(6) 121.2(6) 104.5(7) 59.0(6) 107.8(7) 58.0(6) 59.9(6) 107.2(7) 104.9(7) 60.0(5) 59.8(6) 107.5(6) 121.8(6) 124.3(6) 121.4(6) 120.6(6) 125.1(6) 60.1(5) 106.1(7) 59.8(6) 58.5(5) 109.3(7) 109.6(7) 105.3(7) 108.3(7) 60.2(5) 60.9(6) 120.1(7) 121.0(7) 125.7(6) 117.8(6) 124.4(6) 59.1(5) 105.9(7) 60.6(6) 104.8(7) 108.6(7) 60.5(5)

C(l)-B(6)-B(2) B(5)-B(6)-B(2) B(10)-B(6)-B(2) B (ll)-B(6)-B(2) C(l)-B(6)-Br(6) B(5)-B(6)-Br(6) B(10)-B(6)-Br(6) B(11)-B(6)-Br(6) B(2)-B(6)-Br(6) B(2)-B(7)-B(3) B(2)-B(7)-B(ll) B(3)-B(7)-B(ll) B(2)-B(7)-B(12) B(3)-B(7)-B( 12) B(ll)-B(7)-B(12) B(2)-B(7)-B(8) B(3)-B(7)-B(8) B (ll)-B(7)-B(8) B(12)-B(7)-B(8) B(2)-B(7)-I(7) B(3)-B(7)-I(7) B(ll)-B(7)-I(7) B(12)-B(7)-I(7) B(8)-B(7M(7) B(3)-B(8)-B(4) B(3)-B(8)-B( 12) B(4)-B(8)-B(12) B(3)-B(8)-B(9) B(4)-B(8)-B(9) B(12)-B(8)-B(9) B(3)-B(8)-B(7) B(4)-B(8)-B(7) B( 12)-B(8)-B(7) B(9)-B(8)-B(7) B(3)-B(8)-I(8) B(4)-B(8)-I(8) B(12)-B(8)-I(8) B(9)-B(8)-I(8) B(7)-B(8)-I(8) B(12)-B(9)-B(10) B( 12)-B(9)-B(5) B(10)-B(9)-B(5) B(12)-B(9)-B(8) B(10)-B(9)-B(8) B(5)-B(9)-B(8) B(12)-B(9)-B(4) B(10)-B(9)-B(4) B(5)-B(9)-B(4) B(8)-B(9)-B(4) B(12)-B(9)-I(9) B(10)-B(9)-I(9) B(5)-B(9)-I(9) B(8)-B(9)-I(9) B(4)-B(9)-I(9) B(6)-B( 10)-B(5) B(6)-B( 10)-B( 11)

57.1(5) 107.0(7) 108.9(7) 60.8(6) 121.2(6) 120.8(6) 124.6(6) 124.4(6) 120.1(6) 59.7(6) 60.9(6) 108.4(8) 107.1(7) 106.4(7) 59.4(6) 106.7(7) 59.1(6) 107.2(7) 59.1(5) 122.8(6) 121.2(6) 122.8(6) 122.8(7) 121.3(6) 60.2(6) 107.7(7) 107.5(7) 108.5(7) 61.0(6) 58.5(5) 59.4(6) 107.8(7) 60.4(5) 107.3(6) 121.0(6) 119.3(6) 124.0(7) 121.2(6) 123.7(6) 61.1(5) 107.7(7) 59.4(6) 60.7(5) 109.1(6) 106.6(6) 107.7(6) 107.6(7) 59.3(6) 59.0(5) 123.1(6) 123.1(5) 122.1(6) 120.9(6) 120.0(5) 59.5(6) 60.6(6)

217


B(5)-B(10)-B(l 1) B(6)-B(10)-B(9) B(5)-B(10)-B(9) B(11)-B(10)-B(9) B(6)-B( 10)-B( 12) B(5)-B(10)-B(12) B(11)-B(10)-B(12) B(9)-B(10)-B(12) B(6)-B(10)-I(10) B(5)-B(10)-I(10) B( 11)-B( 10)-I(10) B(9)-B(10)-I(10) B(12)-B(10)-I(10) B (10)-B(ll)-B(6) B( 10)-B( 11 )-B( 12) B (6)-B(ll)-B(12) B(10)-B(l 1)-B(7) B(6)-B(ll)-B(7) B(12)-B(l 1)-B(7) B(10)-B(ll)-B(2) B (6)-B(ll)-B(2) B(12)-B(l 1)-B(2) B (7)-B(ll)-B(2) B (1 0 )-B (ll)-I(ll) B(6)-B(l 1)-I(11) B(12)-B(l l)-I (ll) B(7)-B(l l)-I (ll) B (2 )-B (ll)-I(ll) B(9)-B(12)-B(8) B(9)-B(12)-B(l 1) B(8)-B(12)-B(ll) B(9)-B(12)-B(10) B(8)-B(12)-B(10) B(11)-B(12)-B(10) B(9)-B(12)-B(7) B(8)-B(12)-B(7) B(11)-B(12)-B(7) B(10)-B(12)-B(7) B(9)-B(12)-I(12) B(8)-B(12)-I(12) B(11)-B(12)-I(12) B(10)-B(12)-I(12) B(7)-B(12)-I(12)

107.8(7) 108.2(6) 60.4(6) 107.6(6) 107.7(6) 106.4(7) 60.1(6) 58.4(5) 121.9(6) 121.0(6) 123.0(6) 120.8(5) 123.3(6) 58.9(5) 60.3(5) 106.6(7) 108.8(7) 107.0(7) 60.6(6) 106.8(7) 59.7(6) 106.2(7) 58.6(6) 123.4(6) 120.5(6) 125.4(6) 121.7(6) 120.0(6) 60.9(5) 108.9(7) 108.8(7) 60.5(6) 108.7(7) 59.7(6) 109.3(7) 60.5(6) 60.0(6) 107.8(7) 124.2(6) 124.4(7) 117.2(6) 120.4(6) 120.0(6)



A g(l) Ag(2) Ag(3) Br( 7) Br(8) Br(9) Br(10) B r(ll) Br( 12) C (i) C(l) C(2) C(3) C(4) C(5) N(3) C(6) 1(2) 1(3) 1(4) 1(5) 1(6) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B (ll) B(12) N (l) N(2)

X

y

-5000 -144(2) -5000 -3500(1) -243(1) -198(1) -3497(1) -5543(1) -1832(1) -3972(8) 923(11) 1598(11) 2967(11) 4191(12) -10128(13) -10128(13)

0

-1 0 0 0 0

-3075(1) -999(1) -3047(1) -6496(1) -6485(1) -3173(10) -2257(10) -3213(9) -4669(8) -4697(9) -3410(10) -1862(9) -1879(10) -3418(9) -4341(10) -2545(10) 2131(16) 384(12)

-2986(2) 5000 4741(1) 2204(1) -551(1) 228(1) 3543(1) 2880(1) 754(7) -5576(10) -6816(11) -3149(11) -2969(9) 5461(13) 5461(13) 5000 2527(1) -880(1) -2131(1) 514(1) 3369(1) 1934(10) 393(9) -171(9) 981(9) 2302(9) 2961(8) 1758(9) 484(8) 850(9) 2393(9) 2018(9) -3076(11) -4696(10)

z 5000 2451(2) 5000 2979(1) 2971(1) 1341(1) 428(1) 1449(1) 643(1) 3748(4) 970(9) 419(9) 1973(6) 1389(8) 4198(9) 4198(9) 5000 5301(1) 4266(1) 2648(1) 2678(1) 4313(1) 3831(6) 3430(6) 2709(6) 2725(7) 3434(6) 2879(6) 2848(6) 2145(6) 1704(6) 2135(6) 1799(6) 2392(7) 1439(8)

U(eq) 56(1) 217(1) 113(1) 63(1) 71(1) 63(1) 67(1) 71(1) 66(1) 47(2) 98(5) 104(4) 94(4) 105(5) 137(5) 137(5) 156(9) 68(1) 68(1) 66(1) 72(1) 76(1) 58(3) 53(3) 47(3) 49(3) 49(3) 49(3) 51(3) 48(3) 46(3) 52(3) 54(3) 181(7) 135(5)

Bond lengths A g (l)-C (l)# l A g (l)-C (l) Ag(2)-N(2) Ag(2)-N(l) Ag(2)-I(4) Ag(2)-Br(9) Ag(3)-Br(7)#2 Ag(3)-Br(7) Ag(3)-I(6)#2 Ag(3)-I(6) Ag(3)-I(2)#2

2.141(7) 2.141(7) 2.283(12) 2.393(18) 2.9532(19) 3.030(2) 2.9536(10) 2.9536(10) 2.9862(10) 2.9862(10) 3.0076(9)

Ag(3)-I(2) Br(7)-B(7) Br(8)-B(8) Br(9)-B(9) Br(10)-B(10) B r (ll)-B (ll) Br(12)-B(12) C O >B (5) C (l)-B (3) C (l)-B (4) C (l)-B (6) C(1>B(2)

3.0076(9) 1.944(9) 1.960(11) 2.008(8) 1.962(9) 1.914(9) 1.969(9) 1.713(12) 1.741(12) 1.743(10) 1.747(12) 1.753(15)


C(l)-N(2) C(l)-C(2) C(3)-N(l) C(3)-C(4) C(5)-C(6) C(6)-N(3)#3 C(6)-C(5)#3 I(2)-B(2) I(3)-B(3) I(4)-B(4) I(5)-B(5) I(6)-B(6) B(2)-B(7) B(2)-B(8) B(2)-B(6) B(2)-B(3) B(3)-B(9) B(3)-B(8) B(3)-B(4)

1.145(15) 1.525(15) 0.956(18) 1.462(16) 1.226(13) 1.226(13) 1.226(13) 2.211(9) 2.141(10) 2.120(9) 2.161(10) 2.138(8) 1.719(12) 1.741(12) 1.760(15) 1.770(13) 1.768(12) 1.788(14) 1.797(15)

B(4)-B(5) B(4)-B(10) B(4)-B(9) B(5)-B(10) B(5)-B(6) B(5)-B(ll) B(6)-B(7) B(6)-B(ll) B(7)-B(ll) B(7)-B(8) B(7)-B(12) B(8)-B(12) B(8)-B(9) B(9)-B(12) B(9)-B(10) B(10)-B(ll) B(10)-B(12) B(ll)-B(12)

1.721(12) 1.768(12) 1.801(14) 1.742(12) 1.784(14) 1.812(14) 1.760(14) 1.785(12) 1.802(15) 1.815(12) 1.816(11) 1.738(13) 1.753(14) 1.733(13) 1.804(14) 1.784(12) 1.801(16) 1.824(14)

Bond angles C(l')#l-A g(l)-C(l') N(2)-Ag(2)-N(l) N(2)-Ag(2)-I(4) N(l)-Ag(2)-I(4) N(2)-Ag(2)-Br(9) N( 1)-Ag(2)-Br(9) I(4)-Ag(2)-Br(9) Br(7)#2-Ag(3)-Br(7) Br(7)#2-Ag(3)-I(6)#2 Br(7)-Ag(3)-I(6)#2 Br(7)#2-Ag(3)-1(6) Br(7)-Ag(3)-I(6) I(6)#2-Ag(3)-I(6) Br(7)#2-Ag(3)-I(2)#2 Br(7)-Ag(3)-I(2)#2 I(6)#2-Ag(3)-I(2)#2 I(6)-Ag(3)-I(2)#2 Br(7)#2-Ag(3)-I(2) Br(7)-Ag(3)-I(2) 1(6)#2-Ag(3)-I(2) 1(6)-Ag(3)-I(2) I(2)#2-Ag(3)-I(2) B(7)-Br(7)-Ag(3) B(9)-Br(9)-Ag(2) B(5)-C(1>B(3) B(5)-C(1>B(4) B(3)-C(1>B(4) B(5)-C(1>B(6) B(3)-C(1>B(6) B(4)-C(1>B(6) B(5)-C(1>B(2) B(3)-C(1>B(2) B(4)-C(1>B(2) B(6)-C(1>B(2)

B(5)-C (l>A g(l) B(3)-C (l>A g(l) B (4)-C (l>A g(l) B(6)-C (l>A g(l) B(2)-C (l>A g(l) N(2)-C(l)-C(2) N(l)-C(3)-C(4) N(3)#3-C(6)-C(5)#3 N(3)#3-C(6)-C(5) C(5)#3-C(6)-C(5) B(2)-I(2)-Ag(3) B(4)-[(4)-Ag(2) B(6)-I(6)-Ag(3) B(7)-B(2)-B(8) B(7)-B(2)-C(l') B(8)-B(2)-C(l') B(7)-B(2)-B(6) B(8)-B(2)-B(6) C(1>B(2)-B(6) B(7)-B(2)-B(3) B(8)-B(2)-B(3) C(l')-B(2)-B(3) B(6)-B(2)-B(3) B(7)-B(2)-I(2) B(8)-B(2)-I(2) Q D-B(2)-I(2) B(6)-B(2)-I(2) B(3)-B(2)-I(2) C(l')-B(3)-B(9) C(l')-B(3)-B(2) B(9)-B(3)-B(2) ai-)-B(3)-B (8) B(9)-B(3)-B(8) B(2)-B(3)-B(8)

180.0 92.3(4) 102.1(3) 164.0(3) 112.4(3) 84.1(3) 84.13(5) 180.0 84.70(3) 95.30(3) 95.30(3) 84.70(3) 180.0 84.13(3) 95.87(3) 83.88(3) 96.12(3) 95.87(3) 84.13(3) 96.12(3) 83.88(3) 180.0 94.0(2) 96.4(3) 110.5(5) 59.7(5) 62.1(5) 62.1(5) 111.1(6) 110.8(5) 109.6(6) 60.9(5) 110.1(6) 60.4(5)

117.2(6) 123.6(5) 120.9(5) 116.7(4) 122.7(4) 175.1(13) 167.4(15) 0.0(14) 180.0(5) 180.0(5) 88.5(2) 96.7(2) 90.0(3) 63.3(5) 108.9(7) 108.3(7) 60.8(6) 111.1(6) 59.6(6) 112.4(6) 61.2(5) 59.2(6) 109.2(8) 123.5(6) 123.0(7) 117.9(5) 120.0(5) 117.8(6) 106.5(7) 59.9(5) 105.3(6) 106.7(6) 59.1(5) 58.6(5)

220


C(1>B(3)-B(4) B(9)-B(3)-B(4) B(2)-B(3)-B(4) B(8)-B(3)-B(4) C(1>B(3)-I(3) B(9)-B(3)-I(3) B(2)-B(3)-I(3) B(8)-B(3)-I(3) B(4)-B(3)-I(3) B(5)-B(4)-C( 1) B(5)-B(4)-B(10) C(1>B(4)-B(10) B(5)-B(4)-B(3) C(1>B(4)-B(3) B(10)-B(4)-B(3) B(5)-B(4)-B(9) C(1>B(4)-B(9) B(10)-B(4)-B(9) B(3)-B(4)-B(9) B(5)-B(4)-I(4) C(1>B(4)-I(4) B(10)-B(4)-I(4) B(3)-B(4)-I(4) B(9)-B(4)-I(4) C (n-B(5)-B(4) C(1>B(5)-B(10) B(4)-B(5)-B(10) C(1>B(5)-B(6) B(4)-B(5)-B(6) B(10)-B(5)-B(6) C(1>B(5)-B(11) B(4)-B(5)-B(l 1) B(10)-B(5)-B(ll) B(6)-B(5)-B(l 1) C(1>B(S)-I(5) B(4)-B(5)-I(5) B(10)-B(5)-I(5) B(6)-B(5)-I(5) B(11)-B(5)-I(5) C(1>B(6)-B(2) C(1>B(6)-B(7) B(2)-B(6)-B(7) C(1>B(6)-B(5) B(2)-B(6)-B(5) B(7)-B(6)-B(5) C(1>B(6)-B(11) B(2)-B(6)-B(l 1) B(7)-B(6)-B(l 1) B(5)-B(6)-B(l 1) C(1>B(6)-I(6) B(2)-B(6)-I(6) B(7)-B(6)-I(6) B(5)-B(6)-I(6) B(11)-B(6)-I(6) B(2)-B(7)-B(6) B(2)-B(7)-B(l 1)

59.0(5) 60.7(5) 107.0(7) 108.0(7) 121.9(5) 123.1(5) 123.3(6) 123.1(7) 120.9(6) 59.3(5) 59.9(5) 106.1(6) 107.5(7) 58.9(5) 107.8(7) 107.7(7) 104.9(6) 60.7(5) 58.9(5) 123.9(6) 123.2(5) 123.7(6) 119.6(5) 121.6(5) 61.0(5) 108.7(6) 61.4(5) 59.9(5) 110.1(7) 108.3(7) 107.5(7) 110.2(7) 60.2(5) 59.5(5) 122.0(6) 121.5(7) 122.2(6) 119.6(5) 120.3(6) 60.0(5) 107.3(6) 58.5(5) 58.0(5) 106.1(6) 109.0(6) 107.3(6) 106.9(6) 61.1(6) 61.0(5) 120.0(5) 122.1(5) 123.3(6) 121.3(6) 123.5(6) 60.8(6) 108.0(7)

B (6)-B(7)-B (ll) B(2)-B(7>B(8) B(6)-B(7)-B(8) B (ll)-B (7)-B(8) B(2)-B(7)-B( 12) B(6)-B(7)-B( 12) B(11)-B(7)-B(12) B(8)-B(7)-B(12) B(2)-B(7)-Br(7) B(6)-B(7)-Br(7) B(11)-B(7)-Br(7) B(8)-B(7)-Br(7) B( 12)-B(7)-Br(7) B(12)-B(8)-B(2) B(12)-B(8)-B(9) B(2)-B(8)-B(9) B(12)-B(8)-B(3) B(2)-B(8)-B(3) B(9)-B(8)-B(3) B(12)-B(8)-B(7) B(2)-B(8)-B(7) B(9)-B(8)-B(7) B(3)-B(8)-B(7) B(12)-B(8)-Br(8) B(2)-B(8)-Br(8) B(9)-B(8)-Br(8) B(3)-B(8)-Br(8) B(7)-B(8)-Br(8) B( 12)-B(9)-B(8) B(12)-B(9)-B(3) B(8)-B(9)-B(3) B( 12)-B(9)-B(4) B(8)-B(9)-B(4) B(3)-B(9)-B(4) B( 12)-B(9)-B( 10) B(8)-B(9)-B(10) B(3)-B(9)-B( 10) B(4)-B(9)-B(10) B(12)-B(9)-Br(9) B(8)-B(9)-Br(9) B(3)-B(9)-Br(9) B(4)-B(9)-Br(9) B(10)-B(9)-Br(9) B(5)-B( 10)-B(4) B (5)-B (10)-B (ll) B(4)-B( 10)-B( 11) B(5)-B(10)-B(12) B(4)-B(10)-B(12) B(11)-B( 10)-B( 12) B(5)-B(10)-B(9) B(4)-B( 10)-B(9) B(11)-B(10)-B(9) B( 12)-B( 10)-B(9) B(5)-B(10)-Br(10) B(4)-B(10)-Br(10) B(ll)-B(10)-Br(10)

60.1(5) 59.0(5) 107.7(6) 107.0(6) 104.4(6) 107.1(7) 60.5(5) 57.2(5) 122.6(6) 123.2(5) 122.4(6) 121.1(7) 122.6(6) 106.8(7) 59 j5(5) 107.3(8) 107.6(8) 60.2(5) 59.9(5) 61.4(5) 57.8(5) 108.4(7) 107.1(7) 123.4(6) 120.9(7) 123.5(6) 121.3(6) 121.1(7) 59.8(5) 108.7(6) 61.0(5) 108.5(7) 109.4(6) 60.4(5) 61.2(6) 108.7(6) 107.5(6) 58.7(5) 119.2(5) 120.4(7) 123.0(6) 123.0(6) 121.2(5) 58.7(5) 61.8(5) 109.4(6) 108.5(6) 107.0(6) 61.2(6) 106.7(6) 60.6(5) 107.6(7) 57.5(5) 124.0(7) 121.6(6) 121.6(6)

221


B( 12)-B( 10)-Br( 10) B(9)-B(10)-Br(10) B(10)-B(ll)-B(6) B(10)-B(l 1)-B(7) B(6)-B(ll)-B(7) B(10)-B(l 1)-B(5) B(6)-B(l 1)-B(5) B(7)-B(ll)-B(5) B( 10)-B( 11 )-B( 12) B(6)-B(ll)-B(12) B(7)-B(l 1)-B(12) B(5)-B(ll)-B(12) B(10)-B(ll)-Br(ll) B (6)-B (ll)-B r(ll) B (7)-B (ll)-B r(ll) B (5)-B (ll)-B r(ll) B( 12)-B( 11 )-Br( 11) B(9)-B(12)-B(8) B(9)-B(12)-B(10) B(8)-B(12)-B(10) B(9)-B(12)-B(7) B(8)-B(12)-B(7) B(10)-B(12)-B(7) B(9)-B(12)-B(ll) B(8)-B(12)-B(ll) B(10)-B(12)-B(ll) B(7)-B(12)-B(ll) B(9)-B( 12)-Br( 12) B(8)-B(12)-Br(12) B( 10)-B( 12)-Br( 12) B(7)-B(12)-Br(12) B(11)-B(12)-Br(12) C(3)-N(l)-Ag(2) C(l)-N(2)-Ag(2)

121.0(5) 120.8(5) 106.4(6) 108.2(6) 58.8(5) 57.9(5) 59.4(5) 105.9(6) 59.9(5) 105.7(6) 60.1(5) 104.6(6) 124.1(6) 120.7(5) 120.8(6) 123.6(7) 124.7(6) 60.6(5) 61.3(6) 109.5(7) 109.2(6) 61.4(5) 106.9(6) 109.0(7) 109.4(6) 59.0(5) 59.4(5) 126.1(5) 123.5(7) 121.7(5) 118.2(6) 116.2(5) 144.9(12) 164.8(12)

222



z 3523(1) 3512(4) 8318(4) 3534(7) 3397(10) 1927(5) 1628(5) 1068(5) 772(5) 1069(5) 1623(6) 1890(6) 1920(7) 253(6) 7570(5) 7140(6) 7559(6) 8218(5) 8231(5) 7240(5) 6841(5) 6174(6) 6196(6) 6851(5) 6012(6) 8082(1) 7157(1) 8080(1) 9445(1) 9442(1) 7345(1) 6460(1) 5039(1) 5038(1) 6459(1) 4599(1)

y -2913(1) -1867(2) -3584(2) -1349(3) -644(4) -3591(3) -3322(3) -2760(3) -2463(3) -2756(3) -3307(3) -3614(3) -3611(3) -1840(3) -3575(3) -3129(2) -3569(3) -4273(3) -4270(3) -4726(3) -4301(3) -3595(3) -3598(3) -4283(3) -4308(3) -3140(1) -2243(1) -3140(1) -4594(1) -4593(1) -5625(1) -4695(1) -3217(1) -3218(1) -4693(1) -4736(1)

X

A g(l) N (l) C(l) C( 2) C(3) C (ll) C( 12) C(13) C(14) C(15) C(16) C(17) C(18) C(19) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12) Br(2) Br(3) Br(4) Br(5) Br(6) Br(7) Br(8) Br(9) Br(10) B r(ll) Br(12)

7500(1) 7516(4) 7510(4) 7489(5) 7454(9) 7489(5) 8421(6) 8395(5) 7475(5) 6583(5) 6568(5) 9479(5) 5536(6) 7503(8) 8611(5) 7513(5) 6368(5) 6809(5) 8163(5) 7501(5) 8630(5) 8186(5) 6809(5) 6351(4) 7487(6) 9836(1) 7500(1) 5166(1) 6050(1) 8952(1) 7502(1) 9920(1) 9024(1) 5978(1) 5080(1) 7499(1)

U(eq) 90(1) 76(2) 43(2) 92(3) 182(6) 77(2) 88(3) 78(2) 71(2) 70(2) 76(2) 105(3) 116(4) 135(4) 53(2) 47(2) 46(2) 47(2) 45(2) 48(2) 50(2) 55(2) 51(2) 42(2) 55(2) 81(1) 99(1) 81(1) 84(1) 84(1) 109(1) 87(1) 82(1) 83(1) 88(1) 84(1)

Bond lengths A g(l)-N (l) Ag(l)-C (l 1) Ag(l)-Br(10) Ag(l)-Br(9) N(l)-C(2) C(l)-B(6) C(l)-B(2) C(l)-B(5) C(l)-B(4) C(l)-B(3)

C(2)-C(3) C (ll)-C(12) C(ll)-C(16) C(12)-C(13) C(12)-C(17) C(13)-C(14) C(14)-C(15) C(14)-C(19) C(15)-C(16) C(16)-C(18) B(2)-B(6)

2.235(5) 2.430(7) 2.7718(10) 2.7761(9) 1.108(8) 1.694(8) 1.686(9) 1.731(8) 1.738(8) 1.738(8)

1.517(11) 1.378(10) 1.383(9) 1.382(9) 1.531(10) 1.391(9) 1.357(9) 1.474(9) 1.359(9) 1.521(10) 1.786(9)

223


B(2)-B(3) B(2)-B(8) B(2)-B(9) B(2)-Br(2) B(3)-B(9) B(3)-B(10) B(3)-B(4) B(3)-Br(3) B (4)-B (ll) B(4)-B(10) B(4)-B(5) B(4)-Br(4) B(5)-B(6) B(5)-B(l 1) B(5)-B(7) B(5)-Br(5) B(6)-B(7) B(6)-B(8)

1.784(9) 1.787(9) 1.794(10) 1.934(7) 1.770(10) 1.776(9) 1.819(9) 1.894(5) 1.755(9) 1.761(10) 1.799(8) 1.907(6) 1.741(9) 1.772(9) 1.777(9) 1.917(7) 1.774(9) 1.804(9)

B(6)-Br(6) B(7)-B(12) B(7)-B(8) B (7)-B (ll) B(7)-Br(7) B(8)-B(12) B(8)-B(9) B(8)-Br(8) B(9)-B(10) B(9)-B(12) B(9)-Br(9) B (10)-B (ll) B(10)-B(12) B(10)-Br(10) B (ll)-B (12) B (ll)-B r (ll) B(12)-Br(12)

1.923(6) 1.749(9) 1.781(10) 1.819(9) 1.923(6) 1.787(10) 1.808(10) 1.917(7) 1.771(9) 1.780(10) 1.933(7) 1.770(9) 1.764(9) 1.951(7) 1.786(9) 1.916(6) 1.956(7)

Bond angles N (l)-A g (l)-C (ll) N(l)-Ag(l)-Br(10) C(11)-Ag(l)-Br(10) N(l)-Ag(l)-Br(9) C(11)-Ag(l)-Br(9) Br(10)-Ag(l)-Br(9) C(2)-N(l)-Ag(l) B(6)-C(l)-B(2) B(6)-C(l)-B(5) B(2)-C(l)-B(5) B(6)-C(l)-B(4) B(2)-C(l)-B(4j B(5)-C(l)-B(4) B(6)-C(l)-B(3) B(2)-C(l)-B(3) B(5)-C(l)-B(3) B(4)-C(l)-B(3) N(l)-C(2)-C(3) C(12)-C(l 1)-C(16) C( 12)-C( 11)-Ag( 1) C( 16)-C( 11 )-Ag( 1) C( 13)-C( 12)-C( 11) C(13)-C(12)-Q17) C(ll)-C(12)-C(17) C( 12)-C( 13)-C(14) C(15)-C(14)-C(13) C(15)-C(14)-C(19) C( 13)-C( 14)-C( 19) C( 14)-C( 15)-C( 16) C(15)-C(16)-C(l 1) C( 15)-C( 16)-C( 18) C( 11 )-C( 16)-C( 18) C(l)-B(2)-B(6) C(l)-B(2)-B(3) B(6)-B(2)-B(3)

126.2(2) 104.17(14) 113.15(16) 103.38(13) 113.66(16) 89.82(3) 177.1(6) 63.8(4) 61.1(3) 114.0(4) 113.7(4) 114.8(4) 62.5(3) 115.5(4) 62.8(4) 114.7(4) 63.1(3) 172.2(9) 119.3(6) 87.7(4) 87.7(4) 118.3(7) 118.6(6) 123.1(6) 123.1(6) 116.0(6) 123.5(7) 120.3(7) 123.0(6) 120.2(6) 120.1(6) 119.7(6) 58.3(3) 60.0(4) 108.8(5)

C(l)-B(2)-B(8) B(6)-B(2)-B(8) B(3)-B(2)-B(8) C(l)-B(2)-B(9) B(6)-B(2)-B(9) B(3)-B(2)-B(9) B(8)-B(2)-B(9) C(l)-B(2)-Br(2) B(6)-B(2)-Br(2) B(3)-B(2)-Br(2) B(8)-B(2)-Br(2) B(9)-B(2)-Br(2) C(l)-B(3)-B(9) C(l)-B(3)-B(10) B(9)-B(3)-B( 10) C(l)-B(3)-B(2) B(9)-B(3)-B(2) B(10)-B(3)-B(2) C(l)-B(3)-B(4) B(9)-B(3)-B(4) B(10)-B(3)-B(4) B(2)-B(3)-B(4) C(l)-B(3)-Br(3) B(9)-B(3)-Br(3) B(10)-B(3)-Br(3) B(2)-B(3)-Br(3) B(4)-B(3)-Br(3) C (l)-B (4)-B (ll) C( 1)-B(4)-B(10) B( 11)-B(4)-B( 10) C(l)-B(4)-B(5) B( 11)-B(4)-B(5) B(10)-B(4)-B(5) C(l)-B(4)-B(3) B(11)-B(4)-B(3)

105.8(4) 60.6(4) 109.1(4) 105.1(5) 108.3(4) 59.3(4) 60.6(4) 120.9(4) 121.0(4) 119.0(4) 124.6(4) 124.6(4) 103.9(4) 102.9(4) 59.9(4) 57.2(3) 60.6(4) 107.2(4) 58.4(3) 107.1(4) 58.7(4) 106.4(4) 123.3(4) 125.0(4) 124.5(4) 122.5(4) 120.4(4) 105.0(4) 103.5(4) 60.5(4) 58.6(3) 59.8(3) 107.1(4) 58.4(3) 108.7(4)

224


B(10)-B(4)-B(3) B(5)-B(4)-B(3) C(l)-B(4)-Br(4) B(ll)-B(4)-Br(4) B(10)-B(4)-Br(4) B(5)-B(4)-Br(4) B(3)-B(4)-Br(4) C(l)-B(5)-B(6) C(l)-B(5)-B(l 1) B(6)-B(5)-B(l 1) C(1)-B(5)-B(T) B(6)-B(5)-B(7) B(ll)-B(5)-B(7) C(l)-B(5)-B(4) B(6)-B(5)-B(4) B(11)-B(5)-B(4) B(7)-B(5)-B(4) C(l)-B(5)-Br(5) B(6)-B(5)-Br(5) B(11)-B(5)-Br(5) B(7)-B(5)-Br(5) B(4)-B(5)-Br(5) C(l)-B(6)-B(5) C(l)-B(6)-B(2) B(5)-B(6)-B(2) C(l)-B(6)-B(7) B(5)-B(6)-B(7) B(2)-B(6)-B(7) C(l)-B(6)-B(8) B(5)-B(6)-B(8) B(2)-B(6)-B(8) B(7)-B(6)-B(8) C(l)-B(6)-Br(6) B(5)-B(6)-Br(6) B(2)-B(6)-Br(6) B(7)-B(6)-Br(6) B(8)-B(6)-Br(6) B(12)-B(7)-B(8) B(12)-B(7)-B(6) B(8)-B(7)-B(6) B(12)-B(7)-B(5) B(8)-B(7)-B(5) B(6)-B(7)-B(5) B(12)-B(7)-B(ll) B(8)-B(7)-B(ll) B(6)-B(7)-B(ll) B(5)-B(7)-B(l 1) B(12)-B(7)-Br(7) B(8)-B(7)-Br(7) B(6)-B(7)-Br(7) B(5)-B(7)-Br(7) B(11)-B(7)-Br(7) B(7)-B(8)-B(12) B(7)-B(8)-B(2) B(12)-B(8)-B(2) B(7)-B(8)-B(6)

59.4(4) 107.6(4) 121.0(4) 124.9(4) 126.4(4) 120.6(4) 120.1(4) 58.4(3) 104.5(4) 110.0(5) 104.5(4) 60>5(4) 61.6(4) 58.9(3) 108.5(4) 58.9(4) 108.2(5) 120.9(4) 120.2(4) 124.4(4) 125.9(4) 119.3(4) 60.5(3) 57.9(3) 108.8(4) 106.3(4) 60.7(4) 107.6(4) 104.8(4) 108.9(5) 59.7(4) 59.7(4) 121.6(4) 122.2(4) 118.5(4) 125.7(4) 122.5(4) 60.8(4) 108.1(4) 61.0(4) 107.1(4) 108.3(4) 58.7(3) 60.0(4) 109.0(4) 106.5(4) 59.0(4) 124.6(4) 121.8(4) 120.1(4) 119.9(4) 122.5(4) 58.7(4) 107.2(5) 106.2(5) 59.3(3)

B(12)-B(8)-B(6) B(2)-B(8)-B(6) B(7)-B(8)-B(9) B(12)-B(8)-B(9) B(2)-B(8)-B(9) B(6)-B(8)-B(9) B(7)-B(8)-Br(8) B(12)-B(8)-Br(8) B(2)-B(8)-Br(8) B(6)-B(8)-Br(8) B(9)-B(8)-Br(8) B(3)-B(9)-B(10) B(3)-B(9)-B(12) B(10)-B(9)-B(12) B(3)-B(9)-B(2) B(10)-B(9)-B(2) B(12)-B(9)-B(2) B(3)-B(9)-B(8) B(10)-B(9)-B(8) B(12)-B(9)-B(8) B(2)-B(9)-B(8) B(3)-B(9>-Br(9) B( 10)-B(9)-Br(9) B(12)-B(9)-Br(9) B(2)-B(9)-Br(9) B(8)-B(9)-Br(9) B(4)-B( 10)-B( 11) B(4)-B( 10)-B( 12) B(ll)-B(10)-B(12) B(4)-B(10)-B(9) B(11)-B(10)-B(9) B(12)-B(10)-B(9) B(4)-B(10)-B(3) B(ll)-B(10)-B(3) B(12)-B( 10)-B(3) B(9)-B(10)-B(3) B(4)-B( 10)-Br( 10) B(11)-B(10)-Br(10) B(12)-B(10)-Br(10) B(9)-B(10)-Br(i0) B(3)-B(10)-Br(10) B(4)-B(ll)-B(10) B(4)-B(ll)-B(5) B(10)-B(ll)-B(5) B (4)-B (ll)-B (i2) B(10)-B(l 1)-B(12) B(5)-B(ll)-B(12) B(4)-B(ll)-B(7) B(10)-B(ll)-B(7) B(5)-B(ll)-B(7) B(12)-B(ll)-B(7) B (4)-B (ll)-B r(ll) B (10)-B (ll)-B r(ll) B(5)-B( 11)-Br(l 1) B (12)-B (ll)-B r(ll) B (7)-B (ll)-B r(ll)

105.2(5) 59.6(4) 106.9(5) 59.3(4) 59.9(4) 106.9(5) 123.2(4) 124.8(4) 120.9(4) 122.2(4) 122.0(4) 60.2(4) 107.9(5) 59.6(4) 60.1(4) 106.9(5) 106.2(5) 108.8(5) 107.8(5) 59.7(4) 59.5(4) 121.2(4) 124.7(5) 123.9(5) 120.3(4) 119.7(4) 59.6(4) 108.1(5) 60.7(4) 109.6(5) 110.0(5) 60.4(4) 61.9(4) 110.0(5) 108.4(5) 59.9(4) 119.8(4) 119.4(4) 122.4(4) 122.3(5) 121.1(4) 60.0(4) 61.3(3) 107.9(4) 107.4(4) 59.5(4) 105.7(4) 108.3(4) 106.2(4) 59.3(3) 58.0(4) 122.1(4) 123.2(4) 121.7(4) 122.7(4) 121.4(4)

225


B(7)-B( 12)-B( 10) B(7)-B(12)-B(9) B(10)-B(12)-B(9) B(7)-B(12)-B(ll) B(10)-B(12)-B(l 1) B(9)-B(12)-B(ll) B(7)-B(12)-B(8) B(10)-B(12)-B(8) B(9)-B(12)-B(8) B(ll)-B(12)-B(8) B(7)-B( 12)-Br( 12) B( 10)-B( 12)-Br( 12) B(9)-B(12)-Br(12) B(U)-B(12)-Br(12) B(8)-B(12)-Br(12) B(9)-Br(9)-Ag(l) B( 10)-Br(l0)-Ag( 1)

109.6(5) 109.7(5) 60.0(4) 61.9(4) 59.8(4) 108.9(5) 60.5(4) 109.1(5) 60.9(4) 110.2(5) 121.3(4) 121.3(4) 119.7(4) 121.9(4) 120.0(4) 100.6(2) 101.3(2)

226



A g(l) Ci(2) Cl(3) CI(4) Cl(5) CI(6) Cl(7) Cl(8) CI(9) Cl(10) C I(ll) CI( 12) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B(11) B(12) C(l) C (ll) C(12) C(13) C(14) C(15) C(16) C(17) C(18) C(21) C(22) C(23) C(24) C(25) C(26) C(27) C(28) C(31) C(3 2) C(33) C(34)

X

y

1796(1) 8827(1) 6571(1) 5088(1) 6458(1) 8772(1) 4958(1) 2584(1) 2521(1) 4846(1) 6335(1) 2488(1) 7152(3) 6023(3) 5291(3) 5983(3) 7125(3) 5296(3) 4135(3) 4118(3) 5252(3) 5977(3) 4110(3) 7034(3) 3007(4) 2819(4) 1434(4) 183(3) 354(4) 1754(5) 4518(6) -1348(5) 1238(3) 1127(3) -153(3) -1381(3) -1271(3) 7(3) 2634(4) -2765(4) 611(4) 889(4) -296(4) 1257(6)

9062(1) 14282(1) 15917(1) 14266(1) 11607(1) 11640(1) 14155(1) 14142(1) 11378(1) 9709(1) 11383(1) 11336(1) 13520(2) 14336(2) 13518(3) 12184(3) 12183(2) 13471(2) 13468(2) 12128(2) 11309(2) 12126(2) 1 2 1 0 1 (2 )

13488(2) 8273(3) 9186(3) 9438(3) 8806(3) 7901(3) 7629(3) 7966(6) 9053(4) 6987(2) 8163(2) 8539(2) 7752(3) 6586(3) 6211(2) 6585(4) 8156(4) 3986(3) 4849(3) 4149(3) 2891(4)

z 2160(1) 2023(1) 2886(1) 4159(1) 4053(1) 2700(1) 848(1) 2230(1) 2954(1) 2060(1) 741(1) 925(1) 2185(2) 2630(2) 3266(2) 3214(2) 2540(2) 1654(2) 2331(2) 2686(2) 2246(2) 1603(2) 1694(2) 3122(2) 3647(2) 4188(2) 4139(2) 3553(2) 3005(2) 3053(2) 3726(4) 3533(3) 754(2) 748(2) 850(2) 950(2) 932(2) 842(2) 656(3) 1062(2) 4916(2) 4502(2) 5413(2) 4828(3)

U(eq) 6 8 (1 )

65(1) 75(1) 87(1) 70(1) 6 8 (1 )

63(1) 78(1) 56(1) 51(1) 6 6 (1 )

61(1) 41(1) 45(1) 47(1) 41(1) 40(1) 40(1) 44(1) 39(1) 35(1) 38(1) 36(1) 44(1) 73(1) 67(1) 60(1) 55(1) 62(1) 71(1) 132(2) 8 6 (1 )

50(1) 50(1) 51(1) 51(1) 54(1) 54(1) 79(1) 76(1) 64(1) 69(1) 70(1) 96(1)

Bond lengths Ag(l)-C(22) Ag(l)-C(16)

Ag(l)-C(23) Ag(l)-C(15) Ag(l)-CI(9)

2.468(3) 2.521(3)

2.541(3) 2.633(3) 2.7079(8)

227


Ag(l)-CI(10) Cl(2)-B(2) Cl(3)-B(3) Cl(4)-B(4) CI(5)-B(5) CI(6)-B(6) CI(7)-B(7) Cl(8)-B(8) Cl(9)-B(9) CI(10)-B(10) CI(11)-B(11) Cl(12)-B(12) B(2)-C(l) B(2)-B(7) B(2)-B(3) B(2)-B(l 1) B(2)-B(6) B(3)-C(l) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(4)-C(l) B(4)-B(9) B(4)-B(8) B(4)-B(5) B(5)-C(l) B(5)-B(10) B(5)-B(9) B(5)-B(6) B(6)-C(l) B(6)-B(10) B(6)-B(l 1)

2.8708(7) 1.763(3) 1.767(3) 1.760(3) 1.766(3) 1.765(3) 1.776(3) 1.772(3) 1.793(3) 1.790(3) 1.774(3) 1.775(3) 1.723(4) 1.777(4) 1.778(4) 1.781(4) 1.786(4) 1.721(4) 1.776(4) 1.778(4) 1.786(4) 1.718(4) 1.776(4) 1.777(5) 1.793(4) 1.706(4) 1.772(4) 1.780(4) 1.789(4) 1.719(4) 1.767(4) 1.775(4)

B(7)-B(12) B(7)-B(ll) B(7)-B(8) B(8)-B(12) B(8)-B(9) B(9)-B( 10) B(9)-B(12) B(10)-B(ll) B(10)-B(12) B(11)-B(12) C(ll)-C(12) C(ll)-C(16) C(ll)-C(17) C(12)-C(13) C(13)-C(14) C(I4)-C(15) C(14)-C(18) C(15)-C(16) C(21)-C(26) C(21)-C(22) C(21)-C(27) C(22)-C(23) C(23)-C(24) C(24)-C(25) C(24)-C(28) C(25)-C(26) C(31)-C(32) C(31)-C(33) C(31)-C(34) C(32)-C(33)#l C(33)-C(32)#l

1.789(4) 1.800(4) 1.806(4) 1.787(4) 1.792(4) 1.780(4) 1.781(4) 1.792(4) 1.795(4) 1.790(4) 1.378(5) 1.386(6) 1.509(6) 1.373(5) 1.373(4) 1.373(4) 1.512(5) 1.397(5) 1.384(4) 1.399(4) 1.508(4) 1.392(4) 1.397(4) 1.381(4) 1.504(4) 1.384(4) 1.376(5) 1.380(5) 1.515(5) 1.387(5) 1.387(5)

116.55(10) 32.23(10) 119.89(11) 116.71(9) 31.34(12) 102.28(10) 131.13(7) 112.30(8) 116.27(7) 103.97(7) 86.57(7) 106.38(10) 113.87(7) 136.68(8) 81.265(19) 107.01(9) 103.39(8) 120.28(18) 105.11(18) 125.64(19) 58.85(16)

Cl(2)-B(2)-B(3) B(7)-B(2)-B(3) Q l)-B (2 )-B (ll) Cl(2)-B(2)-B(l 1) B(7)-B(2)-B(l 1) B(3)-B(2)-B(ll) C(l)-B(2)-B(6) Cl(2)-B(2)-B(6) B(7)-B(2)-B(6) B(3)-B(2)-B(6) B(ll)-B(2)-B(6) C(l)-B(3)-Cl(3) C(l)-B(3)-B(8) Cl(3)-B(3)-B(8) C(l)-B(3)-B(2) CI(3)-B(3)-B(2) B(8)-B(3)-B(2) C(l)-B(3)-B(7) Cl(3)-B(3)-B(7) B(8)-B(3)-B(7) B(2)-B(3)-B(7)

120.20(18) 60.01(16) 104.56(18) 125.56(19) 60.78(15) 108.39(18) 58.64(15) 119.54(17) 108.58(18) 108.17(19) 59.67(15) 121.16(19) 104.8(2) 125.22(19) 58.97(16) 119.43(18) 108.74(19) 105.15(18) 124.2(2) 61.06(16) 59.95(16)

Bond angles C(22)-Ag( 1)-C( 16) C(22)-Ag(l)-C(23) C( 16)-Ag( 1)-C(23) C(22)-Ag( 1)-C( 15) C( 16)-Ag( 1)-C( 15) C(23)-Ag(l)-C(15) C(22)-Ag( 1)-C1(9) C(16)-Ag(l)-Cl(9) C(23)-Ag(l)-Cl(9) C(15)-Ag(l)-Cl(9) C(22)-Ag( 1)-C1( 10) C( 16)-Ag( 1)-Cl( 10) C(23)-Ag( 1)-C1(10) C( 15)-Ag( 1)-CI( 10) Cl(9)-Ag(l)-Cl(10) B(9)-CI(9)-Ag(l) B( 10)-CI( 10)-Ag( 1) C(1)-B(2)-C1(2) C(l)-B(2)-B(7) Cl(2)-B(2)-B(7) C(l)-B(2)-B(3)

228


C(l)-B(3)-B(4) Cl(3)-B(3)-B(4) B(8)-B(3)-B(4) B(2)-B(3)-B(4) B(7)-B(3)-B(4) C(1)-B(4)-C1(4) C(l)-B(4)-B(9) Cl(4)-B(4)-B(9) C(l)-B(4)-B(8) CI(4)-B(4)-B(8) B(9)-B(4)-B(8) C(l)-B(4)-B(3) Cl(4)-B(4)-B(3) B(9)-B(4)-B(3) B(8)-B(4)-B(3) C(l)-B(4)-B(5) Cl(4)-B(4)-B(5) B(9)-B(4)-B(5) B(8)-B(4)-B(5) B(3)-B(4)-B(5) C(1)-B(5)-CI(5) C(l)-B(5)-B(10) CI(5)-B(5)-B(10) C(l)-B(5)-B(9) CI(5)-B(5)-B(9) B(10)-B(5)-B(9) C(l)-B(5)-B(6) CI(5)-B(5)-B(6) B(10)-B(5)-B(6) B(9)-B(5)-B(6) C(l)-B(5)-B(4) Cl(5)-B(5)-B(4) B(10)-B(5)-B(4) B(9)-B(5)-B(4) B(6)-B(5)-B(4) C(1)-B(6)-C1(6) C(l)-B(6)-B(10) Cl(6)-B(6)-B(10) C (l)-B (6)-B (ll) CI(6)-B(6)-B(11) B(10)-B(6)-B(l 1) C(l)-B(6)-B(2) Cl(6)-B(6)-B(2) B(10)-B(6)-B(2) B(11)-B(6)-B(2) C(l)-B(6)-B(5) CI(6)-B(6)-B(5) B(10)-B(6)-B(5) B(11)-B(6)-B(5) B(2)-B(6)-B(5) Cl(7)-B(7)-B(2) CI(7)-B(7)-B(3) B(2)-B(7)-B(3) Cl(7)-B(7)-B(12) B(2)-B(7)-B(12) B(3)-B(7)-B(12)

58.62(17) 120.65(19) 59.85(17) 108.4(2) 108.88(19) 121.5(2) 103.99(18) 125.23(19) 104.9(2) 125.0(2) 60.56(16) 58.80(16) 120.86(19) 107.7(2) 59.81(17) 58.10(15) 120.0(2) 59.82(15) 108.51(19) 107.60(19) 121.66(18) 104.51(18) 124.99(19) 104.32(19) 125.19(18) 60.14(15) 58.88(15) 120.58(18) 59.51(15) 107.56(18) 58.73(16) 120.50(19) 107.87(19) 59.62(16) 108.02(19) 121.12(18) 104.14(18) 126.27(18) 104.98(18) 124.14(18) 60.78(15) 58.84(15) 118.93(17) 108.23(18) 60.01(15) 58.15(15) 121.43(18) 59.76(15) 108.59(18) 107.82(19) 121.61(17) 121.61(18) 60.03(16) 122.98(18) 107.21(18) 106.85(19)

Cl(7)-B(7)-B(ll) B(2)-B(7)-B(ll) B(3)-B(7)-B(ll) B(12)-B(7)-B(ll) CI(7)-B(7)-B(8) B(2)-B(7)-B(8) B(3)-B(7)-B(8) B(12)-B(7)-B(8) B(li)-B(7)-B(8) Q(8)-B(8)-B(3) Cl(8)-B(8)-B(4) B(3)-B(8)-B(4) Cl(8)-B(8)-B( 12) B(3)-B(8)-B(12) B(4)-B(8)-B(12) Cl(8)-B(8)-B(9) B(3)-B(8)-B(9) B(4)-B(8)-B(9) B(12)-B(8)-B(9) CI(8)-B(8)-B(7) B(3)-B(8)-B(7) B(4)-B(8)-B(7) B(12)-B(8)-B(7) B(9)-B(8)-B(7) B(4)-B(9)-B( 10) B(4)-B(9)-B(5) B(10)-B(9)-B(5) B(4)-B(9)-B(12) B(10)-B(9)-B( 12) B(5)-B(9)-B(12) B(4)-B(9)-B(8) B(10)-B(9)-B(8) B(5)-B(9)-B(8) B(12)-B(9)-B(8) B(4)-B(9)-Cl(9) B(10)-B(9)-C1(9) B(5)-B(9)-C1(9) B( 12)-B(9)-CI(9) B(8)-B(9)-C1(9) B(6)-B(10)-B(5) B(6)-B( 10)-B(9) B(5)-B(10)-B(9) B(6)-B(10)-a(10) B(5)-B( 10)-C1( 10) B(9)-B( 10)-C1( 10) B(6)-B( 10)-B( 11) B(5)-B(10)-B(l 1) B(9)-B(10)-B( 11) Cl(10)-B(10)-B(l 1) B(6)-B(10)-B(12) B(5)-B(10)-B(12) B(9)-B( 10)-B(12) Cl(10)-B(10)-B(12) B(11)-B(10)-B(12) Cl(l 1)-B(11)-B(6) Q (ll)-B (ll)-B (2 )

122.22(19) 59.72(15) 107.56(19) 59.85(14) 122.04(18) 107.5(2) 59.43(16) 59.62(15) 107.67(18) 121.80(18) 121.16(19) 60.34(17) 12278(19) 106.99(18) 107.51(19) 122.15(17) 107.5(2) 59.70(16) 59.70(15) 122.1(2) 59.51(16) 108.04(19) 59.73(15) 107.55(18) 108.27(18) 60.56(16) 59.70(15) 107.80(19) 60.54(14) 108.17(18) 59.75(17) 108.65(18) 108.46(18) 60.02(16) 121.52(18) 121.19(17) 120.85(18) 122.20(17) 122.02(17) 60.73(15) 108.54(18) 60.16(15) 121.38(17) 120.39(17) 121.18(16) 59.82(15) 108.60(18) 108.14(18) 122.38(17) 107.64(17) 107.92(18) 59.77(15) 122.76(17) 59.88(14) 121.17(17) 122.37(17)

229


B(6)-B(l 1)-B(2) CI( 11 )-B( 11 )-B( 12) B(6)-B(l 1)-B(12) B(2)-B(l 1)-B(12) C l(ll)-B (ll)-B (10) B(6)-B(l 1)-B(10) B(2)-B(l 1)-B(10) B( 12)-B( 11 )-B( 10) Cl( 11)-B(11)-B(7) B(6)-B(ll)-B(7) B(2)-B(ll)-B(7) B(12)-B(ll)-B(7) B(10)-B(ll)-B(7) Cl( 12)-B( 12)-B(9) C! (12)-B( 12)-B(8) B(9)-B(12)-B(8) CI( 12)-B( 12)-B(7) B(9)-B(12)-B(7) B(8)-B(12)-B(7) Cl (12)-B( 12)-B( 11) B (9)-B(12)-B(ll) B(8)-B(12)-B(ll) B (7)-B(12)-B(ll) CI( 12)-B( 12)-B( 10) B(9)-B(12)-B(10) B(8)-B(12)-B(10) B(7)-B(12)-B(10) B(11)-B(12)-B(10) B(5)-C(l)-B(4) B(5)-C(l)-B(6) B(4)-C(l)-B(6) B(5)-C(l)-B(3) B(4)-C(l)-B(3) B(6)-C(l)-B(3) B(5)-C(l)-B(2) B(4)-C(l)-B(2) B(6)-C(l)-B(2) B(3)-C(l)-B(2) C(12)-C(ll)-C(16) C(12)-C(l 1)-C(17) C( 16)-C( 11 )-C(l 7) C( 13)-C( 12)-C( 11) C( 14)-C( 13)-C( 12) C(15)-C(14)-C(13) C(15)-C(14)-C(18) C(13)-C(14)-C(18) C(14)-C(15)-C(16) C( 14)-C( 15)-Ag( 1) C(16)-C(15)-Ag(l) C(ll)-C(16)-C(15) C (ll)-C (16)-A g(l) C( 15)-C( 16)-Ag( 1) C(26)-C(21)-C(22) C(26)-C(21)-C(27) C(22)-C(21)-C(27) C(23)-C(22)-C(21)

60.31(16) 122.44(18) 107.52(18) 106.97(18) 121.43(17) 59.40(14) 107.38(19) 60.14(14) 122.40(18) 108.07(19) 59.50(15) 59.77(14) 107.99(18) 120.72(16) 120.80(17) 60.28(16) 121.82(17) 108.75(18) 60.65(15) 122.18(18) 108.15(18) 108.91(18) 60.38(14) 121.69(16) 59.69(15) 108.19(19) 108.33(17) 59.97(14) 63.17(17) 62.97(15) 114.99(18) 114.89(19) 62.59(17) 114.10(19) 114.83(19) 114.3(2) 62.52(16) 62.18(16) 117.6(3) 120.6(4) 121.7(4) 120.9(3) 122.1(3) 117.8(3) 120.9(3) 121.2(3) 120.7(3) 103.13(19) 69.87(18) 120.9(3) 98.1(2) 78.8(2) 117.1(3) 121.8(3) 121.1(3) 121.1(2)

C(23)-C(22)-Ag(l) C(21)-C(22)-Ag( 1) C(22)-C(23)-C(24) C(22)-C(23)-Ag( 1) C(24)-C(23)-Ag( 1) C(25)-C(24)-C(23) C(25)-C(24)-C(28) C(23)-C(24)-C(28) C(24)-C(25)-C(26) C(21)-C(26)-C(25) C(32)-C(31)-C(33) C(32)-C(31)-C(34) C(33)-C(31)-C(34) C(31)-C(32)-C(33)#l C(31)-C(33)-C(32)#l

76.79(16) 100.85(17) 121.3(3) 70.98(15) 104.61(17) 116.9(3) 121.7(3) 121.4(3) 122.1(3) 121.5(3) 117.4(3) 121.8(4) 120.8(4) 121.4(3) 121.2(3)

230


Compound IV-12 Atomic coordinates and thermal parameters.

A g(l) CI(2) CI(3) B(2) B(3)

X

y

6311(1) 5504(1) 6291(1) 5261(2) 5631(2)

8689(1) 10625(1) 8057(1) 10324(2) 9068(2)

z 1311(1) 2334(1) 3502(1) 3705(2) 4261(2)

U(eq) 83(1) 57(1) 62(1) 39(1) 35(1)

Bond lengths Ag( 1)-Cl(3)#l Ag(l)-Cl(3)#2 Ag(l)-Cl(3) Ag(l)-C!(2)#2 Ag(l)-Cl(2) A g(l)-C l(2)#l Cl(2)-B(2) Cl(3)-B(3) B(2)-B(2)#3

2.8478(12) 2.8478(12) 2.8478(12) 2.9146(10) 2.9147(10) 2.9147(10) 1.779(3) 1.782(3) 1.774(4)

B(2)-B(2)#4 B(2)-B(3) B(2)-B(3)#3 B(2)-B(3)#5 B(3)-B(3)#6 B(3)-B(3)#5 B(3)-B(2)*4 B(3)-B(2)#6

1.774(4) 1.777(4) 1.782(4) 1.785(4) 1.768(3) 1.768(3) 1.782(4) 1.785(4)

75.17(4) 75.17(4) 75.17(4) 153.72(4) 78.81(2) 101.73(2) 101.73(2) 153.72(4) 78.81(2) 103.21(3) 78.81(2) 101.73(2) 153.72(4) 103.21(3) 103.21(3) 107.80(9) 108.60(9) 60.0 107.88(15) 60.24(17) 123.29(13) 122.87(13) 121.23(17) 59.99(17) 107.68(15) 107.0(2) 121.99(17) 107.65(13)

B(2)#4-B(2)-B(3)#5 B(3)-B(2)-B(3)#5 Cl(2)-B(2)-B(3)#5 B(3)#3-B(2)-B(3)#5 B(3)#6-B(3)-B(3)#5 B(3)#6-B(3)-B(2) B(3)#5-B(3)-B(2) B(3)#6-B(3)-B(2)#4 B(3)#5-B(3)-B(2)#4 B(2)-B(3)-B(2)#4 B(3)#6-B(3)-C1(3) B(3)#5-B(3)-C1(3) B(2)-B(3)*C1(3) B(2)#4-B(3)-C1(3) B(3)#6-B(3)-B(2)#6 B(3)#5-B(3)-B(2)#6 B(2)-B(3)-B(2)#6 B(2)#4-B(3)-B(2)#6 Cl(3)-B(3)-B(2)#6

107.80(13) 59^0(11) 120.34(17) 59.42(11) 108.02(16) 108.23(13) 60.45(13) 60.36(13) 108.19(13) 59.77(19) 120.90(16) 121.73(16) 122.53(16) 122.10(16) 60.05(17) 60.22(16) 108.9(2) 108.7(2) 120.12(17)

Bond angles C l(3)#l-Ag(l)-Cl(3)#2 Cl(3)#l-Ag(l)-C l(3) Cl(3)#2-Ag( 1)-CI(3) Cl(3)# 1-Ag( 1)-Cl(2)#2 Cl(3)#2-Ag(l)-CI(2)#2 Cl(3)-Ag( 1)-Cl(2)#2 Cl(3)# 1-Ag( 1)-Cl(2) CI(3)#2-Ag( 1)-Cl(2) CI(3)-Ag(l)-CI(2) Cl(2)#2-Ag(l)-Cl(2) Cl(3)#l-A g(l)-C l(2)#l Cl(3)#2-Ag(l)-CI(2)#l Cl(3)-Ag(l)-Cl(2)#l Cl(2)#2-Ag(l)-Cl(2)#l Cl(2)-Ag(l)-Cl(2)#l B(2)-CI(2)-Ag(l) B(3)-CI(3)-Ag(l) B(2)#3-B(2)-B(2)#4 B(2)#3-B(2)-B(3) B(2)#4-B(2)-B(3) B(2)#3-B(2)-CI(2) B(2)#4-B(2)-C1(2) B(3)-B(2)-C1(2) B(2)#3-B(2)-B(3)#3 B(2)#4-B(2)-B(3)#3 B(3)-B(2)-B(3)#3 Cl(2)-B(2)-B(3)#3 B(2)#3-B(2)-B(3)#5


Compound IV-13 Atom ic coordinates and thermal parameters.

Cs(l) C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(S) B(9) B(10) B( 11) B(12) Br(2) Br(3) Br(4) Br(5) Br(6) 1(7) 1(8) 1(9) 1(10) 1(H) 1(12) 0(1) 0(2) 0(3) 0(4) 0(5)

X

y

3275(1) 3605(2) 4449(3) 4173(3) 3401(3) 3233(3) 3891(3) 4834(3) 4197(3) 3593(3) 3898(3) 4664(3) 4484(3) 4841(1) 4261(1) 2657(1) 2309(1) 3662(1) 5847(1) 4385(1) 3031(1) 3705(1) 5451(1) 5056(1) 2480(2) 1935(2) 1880(2) 2944(2) 2628(2)

9191(1) 8846(4) 8873(7) 8818(6) 7960(5) 7519(5) 8063(5) 7866(6) 7356(6) 6509(6) 6543(6) 7422(6) 6444(7) 10322(1) 10187(1) 8412(1) 7458(1) 8614(1) 8198(1) 6873(1) 5070(1) 5144(1) 7067(1) 4849(1) 6185(4) 6995(5) 6790(5) 5913(5) 6445(5)

z 3776(1) -515(4) -760(5) 452(4) 479(4) -753(4) -1528(4) 50(5) 850(4) 109(5) -1136(5) -1139(5) -133(5) -1264(1) 1304(1) 1327(1) -1196(1) -2775(1) 611(1) 2346(1) 731(1) -2128(1) -2178(1) 1 1 2 (1 )

3470(3) 4861(2) 3759(2) 4228(2) 5164(3)

U(eq) 77(1) 29(1) 45(1) 37(1) 32(1) 34(1) 35(1) 38(2) 37(2) 38(2) 41(2) 42(2) 39(2) 58(1) 51(1) 51(1) 57(1) 65(1) 59(1) 48(1) 57(1) 59(1) 56(1) 61(1) 175(3) 124(3) 106(3) 129(5) 186(4)

Bond lengths Cs(l)-Br(4) Cs(l)-Br(2)#l C s(l)-0(1) Cs(l)-I(9)#2 Cs(l)-Br(5)#2 Cs(l)-I(8) Cs(l)-Br(3) Cs(l)-I(10)#2 Cs(l)-I(7)#l C(l)-B(2) C(l)-B(5) C(l)-B(3) C(l)-B(6) C(l)-B(4) B(2)-B(3) B(2)-B(7) B (2)-B (ll)

B(2)-B(6) B(2)-Br(2) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(3)-Br(3) B(4)-B(9) B(4)-B(8) B(4)-B(5) B(4)-Br(4) B(5)-B(6) B(5)-B(10) B(5)-B(9) B(5)-Br(5) B (6)-B (ll) B(6)-B(10) B(6)-Br(6) B (7)-B(ll)

3.7010(14) 3.760(3) 3.770(5) 3.8618(17) 3.8734(15) 3.9478(13) 4.0876(15) 4.241(3) 4.2603(13) 1.699(8) 1.704(8) 1.743(8) 1.748(8) 1.747(8) 1.761(9) 1.769(10) 1.775(10)

1.783(9) 1.941(8) 1.744(9) 1.781(9) 1.807(9) 1.953(7) 1.760(9) 1.788(8) 1.802(8) 1.946(6) 1.792(9) 1.797(9) 1.797(9) 1.924(6) 1.774(9) 1.804(9) 1 .8 8 6 ( 6 )

1.749(10)

232


B(7)-B(12) B(7)-B(8) B(7)-I(7) B(8)-B(12) B(8)-B(9) B(8)-I(8) B(9)-B(12) B(9)-B(10) B(9)-I(9) B(10)-B(12) B(10)-B(ll) B(10)-I( 10) B(11)-B(12)

1.769(10) 1.770(9) 2.177(6) 1.797(9) 1.839(9) 2.168(6) 1.791(8) 1.821(9) 2.150(7) 1.806(9) 1.810(9) 2.128(7) 1.811(10)

B (ll)-I (ll) B(12)-I(12) Br(2)-Cs(l)#3 Br(5)-Cs(l)#4 I(7)-Cs(1)#3 I(9)-Cs(l)#4 I(10)-Cs(l)#4 0(1)-C(4) 0(1)-C(3) C(2)-C(3) C(2)-C(5) C(4)-C(5)

2.151(7) 2.157(7) 3.760(3) 3.8734(15) 4.2603(12) 3.8618(17) 4.241(3) 1.424(5) 1.425(5) 1^543(5) 1.559(5) 1.557(5)

Bond.angles Br(4)-Cs(l)-Br(2)#l Br(4)-Cs(l)-0(1) Br(2)#l-Cs(l)-0(1) Br(4)-Cs(l)-C(4) Br(2)#l-Cs(l)-C(4) 0(1)-Cs(l)-C(4) Br(4)-Cs(l)-I(9)#2 Br(2)#l-Cs(l)-I(9)#2 0(1)-Cs(l)-I(9)#2 C(4)-Cs(l)-I(9)#2 Br(4)-Cs(l)-C(5) Br(2)#l-Cs(l)-C(5) 0(1)-Cs(l)-C(5) C(4)-Cs(l)-C(5) I(9)#2-Cs(l)-C(5) Br(4)-Cs(l)-C(3) Br(2)#l-Cs(l)-C(3) 0(1)-Cs(l)-C(3) C(4)-Cs(l)-C(3) I(9)#2-Cs( 1)-C(3) C(5)-Cs(l)-C(3) Br(4)-Cs( 1)-Br(5)#2 Br(2)# 1-Cs( 1)-Br(5)#2 0 ( 1)-Cs( 1)-Br(5)#2 C(4)-Cs(l)-Br(5)#2 I(9)#2-Cs(l)-Br(5)#2 C(5)-Cs(l)-Br(5)#2 C(3)-Cs(l)-Br(5)#2 Br(4)-Cs(l)-I(8) Br(2)#l-Cs(l)-I(8) 0(1)-Cs(l)-I(8) C(4)-Cs(l)-I(8) I(9)#2-Cs(l)-I(8) C(5)-Cs(l)-I(8) C(3)-Cs(l)-I(8) Br(5)#2-Cs( 1)-I(8) Br(4)-Cs(l)-Br(3) Br(2># 1-Cs( 1)-Br(3) 0(1)-Cs(l)-Br(3) C(4)-Cs(l)-Br(3)

I(9)#2-Cs(l)-Br(3) C(5)-Cs( 1)-Br(3) C(3)-Cs( 1)-Br(3) Br(5)#2-Cs(l)-Br(3) I(8)-Cs(l)-Br(3) Br(4)-Cs( 1)-!(10)#2 Br(2)#l -Cs( 1)-!(10)#2 O(l)-Cs(l)-I(10)#2 C(4)-Cs( 1)-I( 10)#2 I(9)#2-Cs( 1)-!(10)#2 C(5)-Cs( 1)-I( 10)#2 C(3)-Cs( 1)-I( 10)#2 Br(5)#2-Cs( 1)-!(10)#2 I(8)-Cs( 1)-I(10)#2 Br(3)-Cs(l)-I(10)#2 Br(4)-Cs( 1)-I(7)# 1 Br(2)#l-Cs(l)-I(7)#l 0(1)-C s(l)-I(7)#l C(4)-Cs( 1)-I( 7)# 1 I(9)#2-Cs( 1)-1(7)# 1

110.33(2) 62.97(6) 122.85(6) 82.03(5) 108.30(6) 21.62(8) 118.67(4) 129.24(3) 91.89(6) 91.27(6) 98.75(7) 116.87(6) 36.19(9) 23.36(8) 68.93(7) 65.95(5) 143.80(8) 21.45(8) 36-58(9) 73.16(7) 37.21(8) 97.95(2) 98.89(3) 137.61(6) 151.05(7) 63.156(17) 131.59(7) 117.30(8) 64.36(3) 62.70(3) 64.86(7) 62.01(6) 153.02(2) 84.09(7) 85.70(8) 143.57(2) 57.29(4) 58.43(2) 110.71(6) 119.06(6)

C(3)-Cs(l)-I(7)#l Br(5)#2-Cs(l)-I(7)#l I(8)-Cs(l)-I(7)#l Br(3)-Cs( 1)-I(7)#l I(10)#2-Cs(l)-I(7)#l B(2)-C(l)-B(5) B(2)-C(l)-B(3) B(5)-C(l)-B(3) B(2)-C(l)-B(6) B(5)-C(l)-B(6) B(3)-C(l)-B(6) B(2)-C(l)-B(4) B(5)-C( 1)-B(4) B(3)-C(l)-B(4) B(6)-C(l)-B(4) C(l)-B(2)-B(3) C(l)-B(2)-B(7) B(3)-B(2)-B(7) C (l)-B (2)-B (ll)

146.10(2) 142.42(7) 121.83(6) 83.48(2) 60.10(2) 59.221(15) 150.42(3) 79.22(6) 97.90(7) 61.65(4) 92.61(7) 61.37(8) 59.068(14) 122.21(3) 97.05(4) 147.39(2) 60.305(19) 149.52(6) 130.28(5) 71.18(4) 113.41(7) 141.30(6) 56.84(3) 122.19(4) 96.39(3) 111.92(3) 113.6(4) 61-5(3) 114.1(4) 62.3(4) 62-5(3) 113.4(4) 113.1(4) 62.9(3) 62.4(3) 114.3(4) 60.5(3) 106.4(5) 60.6(4) 106.1(5)

233


B (3)-B (2)-B (l 1) B(7)-B (2)-B (l 1) C (l)-B (2)-B (6) B(3)-B(2)-B(6) B(7)-B(2)-B(6) B(11)-B(2)-B(6) C (l)-B (2)-B r(2) B(3)-B(2)-Br(2) B(7)-B(2)-Br(2) B(11)-B(2)-Br(2) B(6)-B(2)-Br(2) C (l)-B (3)-B (8) C (l)-B (3)-B (2) B(8)-B(3)-B(2) C (l)-B (3)-B (7) B(8)-B(3)-B(7) B(2)-B(3)-B(7) C (l)-B (3)-B (4) B(8)-B(3)-B(4) B(2)-B(3)-B(4) B(7)-B(3)-B(4) C (l)-B (3)-B r(3) B(8)-B(3)-Br(3) B(2)-B(3)-Br(3) B(7)-B(3)-Br(3) B(4)-B(3)-Br(3) C (l)-B (4)-B (9) C (l)-B (4)-B (8) B(9)-B(4)-B(8) C (l)-B (4)-B (5) B(9)-B(4)-B(5) B(8)-B(4)-B(5) C (l)-B (4)-B (3) B(9)-B(4)-B(3) B(8)-B(4)-B(3) B(5)-B(4)-B(3) C (l)-B (4)-B r(4) B(9)-B(4)-Br(4) B(S)-B(4)-Br(4) B(5)-B(4)-Br(4) B(3)-B(4)-Br(4) C (l)-B (5)-B (6) C (l)-B (5)-B (10) B(6)-B(5)-B(10) C (l)-B (5)-B (9) B(6)-B(5)-B(9) B(10)-B(5)-B(9) C (l)-B (5)-B (4) B(6)-B(5)-B(4) B(10)-B(5)-B(4) B(9)-B(5)-B(4) C (l)-B (5)-B r(5) B(6)-B(5)-Br(5) B (l0)-B (5)-B r(5) B(9)-B(5)-Br(5) B(4)-B(5)-Br(5)

108.7(5) 59.1(4) 60.2(3) 110.8(5) 108.0(5) 59.8(4) 118.5(4) 119.6(5) 126.9(4) 125.5(4) 117.9(4) 106.0(4) 58.0(3) 108.9(5) 104.1(4) 60.3(4) 59.9(4) 58.9(3) 60.4(3) 107.4(4) 107.3(4) 120.3(4) 124.1(4) 121.1(4) 127.1(4) 119.3(4) 104.9(4) 104.0(4) 62.4(3) 57.4(3) 60.6(3) 109.1(4) 58.7(3) 108.3(4) 58.0(3) 106.5(4) 119.7(4) 125.6(4) 126.2(4) 120.1(4) 120.4(4) 60.0(3) 106.5(4) 60.4(4) 105.2(4) 109.1(4) 60.9(3) 59.7(3) 109.6(4) 108.3(4) 58.6(3) 120.1(4) 120.6(4) 125.2(4) 124.3(4) 119.0(4)

C(l)-B(6)-B(l 1) C(1)-B(6>B(2) B(ll)-B(6)-B(2) C(l)-B(6)-B(5) B(ll)-B(6)-BB(5) C( l)-B(6)-B( 10) B(ll)-B(6)-B(10) B(2)-B(6)-B(10) B(5)-B(6)-B(10) C(l)-B(6)-Br(6) B(11)-B(6)-Br(6) B(2)-B(6)-Br(6) B(5)-B(6)-Br(6) B(10)-B(6)-Br(6) B(11)-B(7)-B(2) B( 11)-B(7)-B( 12) B(2)-B(7)-B(12) B(ll)-B(7)-B(8) B(2)-B(7)-B(8) B(12)-B(7)-B(8) B(ll)-B(7)-B(3) B(2)-B(7)-B(3) B( 12)-B(7)-B(3) B(8)-B(7)-B(3) B(1 l)-B(7)-I(7) B(2)-B(7)-I(7) B(12)-B(7)-l(7) B(8)-B(7)-I(7) B(3)-B(7)-I(7) B(3)-B(8)-B(7) B(3)-B(8)-B(4) B(7)-B(8)-B(4) B(3)-B(8)-B(12) B(7)-B(8)-B( 12) B(4)-B(8)-B( 12) B(3)-B(8)-B(9) B(7)-B(8)-B(9) B(4)-B(8)-B(9) B(12)-B(8)-B(9) B(3)-B(8)-I(8) B(7)-B(8)-I(8) B(4)-B(8)-I(8) B(12)-B(8)-I(8) B(9)-B(8)-I(8) B(4)-B(9)-B( 12) B(4)-B(9)-B(5) B(12)-B(9)-B(5) B(4)-B(9)-B( 10) B( 12)-B(9)-B( 10) B(5)-B(9)-B(10) B(4)-B(9)-B(8) B(12)-B(9)-B(8) B(5)-B(9)-B(8) B(10)-B(9)-B(8) B(4)-B(9)-I(9)

104.0(4) 57.5(3) 59.9(4) 575(3) 107.6(4) 105.6(4) 104.3(4) 60.8(3) 107.9(4) 60.0(3) 119.0(4) 128.2(4) 121.3(4) 119.0(4) 126.3(4) 60.6(4) 62.0(4) 109.2(5) 110.9(4) 107.4(4) 61.0(4) 109.0(4) 59.5(4) 108.0(4) 58.8(3) 124.0(4) 120.5(4) 124.5(4) 119.2(4) 117.2(4) 60.9(4) 61-5(3) 108.7(4) 108.4(4) 595(4) 106.3(4) 107.6(4) 106.4(4) 58.1(3) 59.0(3) 123.0(4) 123.7(4) 121.3(4) 121.3(4) 120.6(4) 107.7(5) 60.9(3) 106.9(4) 109.0(5) 60.0(3) 59.5(4) 59.5(3) 59.3(3) 107.0(4) 107.5(4) 118.6(4)

234


B(12)-B(9)-I(9) B(5)-B(9)-I(9) B(10)-B(9)-I(9) B(8)-B(9)-I(9) B(5)-B(10)-B(6) B(5)-B(10)-B(12) B(6)-B(10)-B(12) B(5)-B(10)-B(ll) B(6)-B(10)-B(ll) B(12)-B(10)-B(l 1) B(5)-B(10)-B(9) B(6)-B(10)-B(9) B(12)-B(10)-B(9) B(11)-B(10)-B(9) B(5)-B(10)-l(10) B(6)-B(10)-I(10) B(12)-B(10)-I(10) B(11)-B(10)-I(10) B(9)-B(10)-I(10) B(7)-B(ll)-B(2) B(7)-B(l 1)-B(6) B(2)-B(ll)-B(6) B(7)-B(ll)-B(12) B(2)-B(ll)-B(12) B(6)-B(ll)-B(12) B(7)-B(l 1)-B(10) B(2)-B(l 1)-B(10) B(6)-B(l 1)-B(10) B( 12)-B( 11 )-B( 10) B(7)-B(l 1)-I(11) B (2 )-B (ll)-I(ll) B (6 )-B (ll)-I(ll) B( 12)-B( 11 )-I( 11) B( 10)-B( 11)-!(11) B(7)-B(12)-B(9) B(7)-B(12)-B(8) B(9)-B(12)-B(8) B(7)-B(12)-B(10) B(9)-B(12)-3(10) B(8)-B(12)-B(10) B(7)-B(12)-B(ll) B(9)-B(12)-B(ll) B(8)-B(12)-B(ll) B(10)-B(12)-B(l 1) B(7)-B(12)-I(12) B(9)-B(12)-I(12) B(8)-B(12)-I(12) B(10)-B(12)-I(12) B( 11)-B( 12)-I( 12) B(2)-Br(2)-Cs(l)#3 B(3)-Br(3)-Cs(l) B(4)-Br(4)-Cs( 1) B(5)-Br(5)-Cs(l)#4 B(7)-I(7)-Cs(l)#3 B(8)-I(8)-Cs(l) B(9)-I(9)-Cs(l)#4

B(10)-I(10)-Cs(l)#4 C(4)-0(l)-C(3) C(4)-0(1)-Cs(l) C(3)-0(1)-Cs(l) Q3)-C(2)-C(5) 0(1)-C(3)-C(2) 0(1)-C(3)-Cs(l) C(2)-C(3)-Cs(l) 0(1)-C(4)-C(5) 0 ( l)-C(4)-Cs( 1) C(5)-C(4)-Cs( 1) C(4)-C(5)-C(2) Q4)-C(5)-Cs(l) C(2)-C(5)-Cs(l)

123.4(4) 122.8(4) 124.3(4) 120.5(4) 59.7(4) 106.3(4) 107.1(5) 105.8(5) 58.8(4) 60.1(4) 59.5(3) 107.5(5) 59.2(3) 106.8(4) 121.1(4) 121.0(4) 124.2(4) 123.9(4) 122.2(4) 60.3(4) 109.4(5) 60.3(4) 59.6(4) 107.0(5) 108.2(4) 108.4(5) 107.9(4) 60.4(4) 59.8(3) 122.8(4) 122.8(4) 119.7(4) 122.6(4) 120.1(4) 108.6(5) 59.5(4) 61.7(3) 107.7(5) 60.8(3) 110.0(4) 58.5(4) 108.1(4) 106.9(5) 60.1(4) 122.3(3) 121.2(4) 121.8(4) 120.4(4) 122.0(4) 120.8(2) 103.96(18) 111.34(18) 108.64(18) 106.40(18) 102.32(17) 105.13(17)

99-52(17) 115.7(4) 81.1(3) 83.2(3) 105.5(3) 106.8(3) 75.4(3) 80.7(3) 105.5(4) 77.3(3) 80.1(3) 106.5(3) 76.6(3) 80.6(3)

235


Compound IY-14 A tom ic coordinates and thermal parameters. X

C(l) B(2) B(3) B(4) B(5)

B(6) B(7) B(8) B(9) B(10) B( 11) B(12) Cl(2) CI(3) Cl(4) Cl(5) Cl(6) Br(7) Br(8) Br(9) Br(10) B r(ll) Br(12) C(21) B(22) B(23) B(24) B(25) B(26) B(27) B(28) B(29) B(30) B(31) B(32) CI(22) Ci(23) Cl(24) Cl(25) Cl(26) Br(27) Br(28) Br(29) Br(30) Br(31) Br(32) Cl( 13) CI( 14) C(1Q C( IB) C(1A)

15742(3) 16923(4) 16407(4) 14940(4) 14511(5) 15722(4) 16779(4) 15552(4) 14403(4) 14868(4) 16350(4) 15545(4) 18172(1) 17176(1) 14234(1) 13421(1) 15843(1) 18096(1) 15436(1) 12947(1) 13984(1) 17169(1) 15384(1) 9651(3) 10895(4) 10773(4) 9414(4) 8732(4) 9627(4) 11499(3) 10573(4) 9280(4) 9469(4) 10798(4) 10616(4) 11613(1) 11359(1) 8647(1) 7273(1) 9111(1) 13095(1) 11128(1) 8342(1) 8700(1) 11619(1) 11184(1) 14363(1) 11119(1) 15574(4) 14342(5) 13614(5)

y 5494(2) 5621(3) 4545(3) 4713(3) 5887(3) 6453(3) 4910(3) 4357(3) 5172(3) 6261(3) 6091(3) 5302(3) 5865(1) 3714(1) 4039(1) 6387(1) 7496(1) 4365(1) 3148(1) 4921(1) 7235(1) 6894(1) 5182(1) 436(3) 848(3) -335(3) -479(3) 628(3) 1429(3) 177(3) -627(3) -45(3) 1125(3) 1250(3) 350(3) 1284(1) -1057(1) -1325(1) 856(1) 2454(1) -87(1) -1816(1) -529(1) 1984(1) 2261(1) 288(1) 1023(1) 3971(1) 2530(3) 1490(3) 2811(3)

z -1483(2) -2177(3) -1546(2) -1393(3) -1913(3) -2392(3) -2628(3) -2154(3) -2374(3) -3002(3) -3161(3) -3157(2) -1998(1) -738(1) -420(1) -1454(1) -2429(1) -3033(1) -1982(1) -2487(1) -3811(1) -4160(1) -4147(1) 3596(2) 3143(3) 3620(3) 3455(3) 2892(3) 2705(3) 2629(3) 2833(2) 2372(3) 1893(3) 2060(3) 1857(3) 3636(1) 4573(1) 4260(1) 3107(1) 2722(1) 2489(1) 2915(1) 1962(1) 935(1) 1268(1) 824(1) -1563(1) -3401(1) -3813(3) -3757(3) -3557(3)

U(eq) 49(1) 49(2) 48(2) 48(2) 56(2) 48(2) 45(2) 45(2) 44(2) 46(2) 46(2) 39(1) 76(1) 6 8 (1 ) 6 8 (1 )

81(1) 79(1) 71(1) 73(1) 77(1) 63(1) 64(1) 62(1) 54(1) 57(2) 51(2) 49(2) 47(2) 49(2) 40(1) 44(2) 50(2) 45(2) 49(2) 45(2) 87(1) 73(1) 74(1) 73(1) 77(1) 80(1) 69(1) 6 6 (1 )

59(1) 72(1) 70(1) 62(1) 62(1) 85(2) 8 8 (2 )

98(2)


C(2C) C(2B) C(2A) C(3C) C(3B) C(3A) C(4C) C(4B) C(4A) N (l) N(2) N(3) N(4) 0(1) 0(2)

16466(4) 14403(4) 15636(4) 9455(5) 9874(4) 7942(4) 9583(4) 8110(4) 10016(4) 14534(3) 15490(3) 9049(3) 9185(3) 15827(3) 8999(3)

1122(3) 1397(3) 1362(3) 3571(3) 3853(3) 3806(4) 6360(3) 7507(3) 7646(3) 2124(2) 1010(2) 4025(2) 7028(2) -80(3) 4830(3)

-17(3) 256(3) 1241(3) 3896(3) 5036(3) 4859(3) 1195(3) 1239(3) 1334(3) -3442(2) 643(2) 4434(2) 1518(2) -4547(2) 355(2)

82(2) 80(2) 85(2) 95(2) 72(2) 97(2) 86(2) 101(3) 81(2) 61(1) 56(1) 53(1) 61(1) 156(2) 162(2)

Bond lengths C(l)-B(5) C(l)-B(4) C(l)-B(6) C(l)-B(3) C(l)-B(2) B(2)-C1(2) B(2)-B(7) B (2)-B (ll) B(2)-B(3) B(2)-B(6) B(3)-C1(3) B(3)-B(7) B(3)-B(4) B(3)-B(8) B(4)-B(9) B(4)-B(8) B(4)-Cl(4) B(4)-B(5) B(5)-CI(5) B(5)-B(9) B(5)-B(10) B(5)-B(6) B(6)-C1(6) B(6)-B(10) B (6)-B (ll) B(7)-B(12) B(7)-B(8) B(7)-B(l 1) B(7)-Br(7) B(8)-B(9) B(8)-B(12) B(8)-Br(8) B(9)-B(10) B(9)-B(12) B(9)-Br(9) B(10)-B(l 1) B(10)-B(12) B(10)-Br(10)

1.696(7) 1.699(7) 1.701(5) 1.719(6) 1.737(6) 1.755(5) 1.767(8) 1.787(6) 1.804(6) 1.817(6) 1.764(4) 1.771(6) 1.773(7) 1.779(8) 1.764(6) 1.765(7) 1.780(4) 1.788(6) 1.770(5) 1.776(8) 1.777(6) 1.779(7) 1.757(5) 1.783(8) 1.787(7) 1.781(6) 1.785(6) 1.801(6) 1.941(5) 1.755(6) 1.788(5) 1.941(5) 1.796(6) 1.797(6) 1.954(5) 1.791(6) 1.815(7) 1.931(4)

B(11)-B(12) B (ll)-B r (ll) B(12)-Br(12) C(21)-B(22) C(21)-B(25) C(21)-B(26) C(21)-B(23) C(21)-B(24) B(22)-C1(22) B(22)-B(31) B(22)-B(27) B(22)-B(26) B(22)-B(23) B(23)-B(27) B(23)-B(28) B(23)-C1(23) B(23)-B(24) B(24)-B(28) B(24)-B(29) B(24)-CI(24) B(24)-B(25) B(25)-B(26) B(25)-B(30) B(25)-B(29) B(25)-C1(25) B(26)-C1(26) B(26)-B(31) B(26)-B(30) B(27)-B(31) B(27)-B(28) B(27)-B(32) B(27)-Br(27) B(28)-B(32) B(28)-B(29) B(28)-Br(28) B(29)-B(30) B(29)-B(32) B(29)-Br(29)

1.772(7) 1.940(4) 1.929(5) 1.708(7) 1.711(6) 1.716(5) 1.726(6) 1.744(7) 1.770(6) 1.772(7) 1.781(8) 1.782(7) 1.798(7) 1.762(6) 1.761(8) 1.774(4) 1.803(7) 1.733(6) 1.774(6) 1.779(4) 1.802(6) 1.754(7) 1.775(6) 1.777(7) 1.789(5) 1.754(5) 1.784(7) 1.802(8) 1.773(6) 1.779(7) 1.784(7) 1.938(4) 1.785(5) 1.822(6) 1.955(5) 1.795(6) 1.819(7) 1.905(6)

237


B(30)-B(31) B(30)-B(32) B(30)-Br(30) B(31)-B(32) B(31)-Br(31) B(32)-Br(32) C(1Q-N(1) C(1B)-N(1) C(1A)-N(1) C(2C)-N(2)

1.757(7) 1.774(6) 1.938(4) 1.766(8) 1.963(4) 1.934(5) 1.463(6) 1.480(7) 1.445(6) 1.525(6)

C(2B)-N(2) C(2A)-N(2) C(3C)-N(3) C(3B)-N(3) C(3A)-N(3) C(4Q-N(4) C(4B)-N(4) C(4A)-N(4)

1.507(6) 1.490(7) 1.479(7) 1.495(6) 1.467(5) 1.477(7) 1.458(6) 1.466(6)

Bond angles B(5)-C(l)-B(4) B(5)-C(l)-B(6) B(4)-C(l)-B(6) B(5)-C(l)-B(3) B(4)-C(l)-B(3) B(6)-C(l)-B(3) B(5)-C(l)-B(2) B(4)-C(l)-B(2) B(6)-C(l)-B(2) B(3)-C(l)-B(2) C(1)-B(2)-CI(2) C(l)-B(2)-B(7) Cl(2)-B(2)-B(7) C(l)-B(2)-B(l 1) Cl(2)-B(2)-B(l 1) B(7)-B(2)-B(l 1) C(l)-B(2)-B(3) Cl(2)-B(2)-B(3) B(7)-B(2)-B(3) B(11)-B(2)-B(3) C(l)-B(2)-B(6) Cl(2)-B(2)-B(6) B(7)-B(2)-B(6) B(ll)-B(2)-B(6) B(3)-B(2)-B(6) C(1)-B(3)-C1(3) C(l)-B(3)-B(7) Cl(3)-B(3)-B(7) C(l)-B(3)-B(4) Cl(3)-B(3)-B(4) B(7)-B(3)-B(4) C(l)-B(3)-B(8) Cl(3)-B(3)-B(8) B(T)-B(3)-B(8) B(4)-B(3)-B(8) C(l)-B(3)-B(2) Cl(3)-B(3)-B(2) B(7)-B(3)-B(2) B(4)-B(3)-B(2) B(8)-B(3)-B(2) C(l)-B(4)-B(9) C(l)-B(4)-B(8) B(9)-B(4)-B(8)

63.6(3) 63.2(3) 116.2(3) 115.8(4) 62.5(3) 116.2(3) 116.2(3) 115.2(4) 63.8(2) 62.9(3) 122.1(3) 103.0(3) 126.6(3) 102.4(3) 125.7(3) 60.9(3) 58.1(2) 121.4(3) 59.4(3) 107.6(4) 57.1(2) 119.7(3) 107.8(3) 59.5(3) 106.7(3) 121.6(3) 103.6(3) 125.6(3) 58.2(3) 120.4(2) 108.0(3) 103.3(3) 126.2(3) 60.4(3) 59.6(3) 59.0(2) 119.6(3) 59.3(3) 108.4(3) 107.8(3) 103.8(3) 104.7(3) 59.6(3)

C(l)-B(4)-B(3) B(9)-B(4)-B(3) B(8)-B(4)-B(3) C( 1)-B(4)-Cl(4) B(9)-B(4)-C1(4) B(8)-B(4)-C1(4) B (3)-B(4)-a(4) C(l)-B(4)-B(5) B(9)-B(4)-B(5) B(8)-B(4)-B(5) B(3)-B(4)-B(5) Cl(4)-B(4)-B(5) C(1)-B(5)-C1(5) C(l)-B(5)-B(9) Cl(5)-B(5)-B(9) C(l)-B(5)-B(10) CI(5)-B(5>B(10) B(9)-B(5)-B( 10) C(l)-B(5)-B(6) Cl(5)-B(5)-B(6) B(9)-B(5)-B(6) B(10)-B(5)-B(6) C(l)-B(5)-B(4) Cl(5)-B(5)-B(4) B(9)-B(5)-B(4) B(10)-B(5)-B(4) B(6)-B(5)-B(4) C( 1)-B(6)-Cl(6) C(l)-B(6)-B(5) Cl(6)-B(6)-B(5) C(l)-B(6)-B(10) CI(6)-B(6)-B( 10) B(5)-B(6)-B( 10) C (l)-B (6)-B (ll) Cl(6)-B(6)-B( 11) B(5)-B(6)-B(ll) B(10)-B(6)-B(ll) C(l)-B(6)-B(2) CI(6)-B(6)-B(2) B(5)-B(6)-B(2) B(10)-B(6)-B(2) B(11)-B(6)-B(2) B(2)-B(7)-B(3)

59.3(3) 108.1(3) 60.4(3) 121.3(3) 125.6(3) 125.7(3) 120.0(3) 58.1(3) 60.0(3) 108.1(3) 108.7(3) 119.6(3) 120.0(4) 103.4(3) 127.6(4) 104.6(3) 125.6(3) 60.7(3) 58.5(3) 118.6(3) 108.1(3) 60.2(3) 58.3(3) 120.5(3) 59.3(3) 108.5(4) 108.0(3) 121.9(4) 58.3(2) 121.5(3) 104.1(3) 125.7(3) 59.8(3) 103.8(3) 124.8(3) 107.6(4) 60.2(3) 59.1(2) 119.1(3) 108.3(3) 108.2(4) 59.4(3) 61.3(3)

238


B(2)-B(7)-B(12) B(3)-B(7)-B(12) B(2)-B(7)-B(8) B(3)-B(7)-B(8) B(12)-B(7)-B(8) B(2)-B(7)-B(l 1) B(3)-B(7)-B(l 1) B(12)-B(7)-B(l 1) B(8)-B(7)-B(ll) B(2)-B(7)-Br(7) B(3)-B(7)-Br(7) B(12)-B(7)-Br(7) B(8)-B(7)-Br(7) B(ll)-B(7)-Br(7) B(9)-B(8)-B(4) B(9)-B(8)-B(3) B(4)-B(8)-B(3) B(9)-B(8)-B(7) B(4)-B(8)-B(7) B(3)-B(8)-B(7) B(9)-B(8)-B(12) B(4)-B(8)-B(12) B(3)-B(8)-B(12) B(7)-B(8)-B(12) B(9)-B(8)-Br(8) B(4)-B(8)-Br(8) B(3)-B(8)-Br(8) B(7)-B(8)-Br(8) B(12)-B(8)-Br(8) B(8)-B(9)-B(4) B(8)-B(9)-B(5) B(4)-B(9)-B(5) B(8)-B(9)-B(10) B(4)-B(9)-B(10) B(5)-B(9)-B(10) B(8)-B(9)-B(12) B(4)-B(9)-B(12) B(5)-B(9)-B(12) B(10)-B(9)-B(12) B(8)-B(9)-Br(9) B(4)-B(9)-Br(9) B(5)-B(9)-Br(9) B(10)-B(9)-Br(9) B(12)-B(9)-Br(9) B(5)-B(10)-B(6) B(5)-B(10)-B(ll) B(6)-B(10)-B(ll) B(5)-B(10)-B(9) B(6)-B(10)-B(9) B(11)-B(10)-B(9) B(5)-B(10)-B(12) B(6)-B(10)-B(12) B(11)-B(10)-B(12) B(9)-B(10)-B(12) B(5)-B( 10)-Br( 10) B(6)-B(10)-Br(10)

108.6(3) 108.7(3) 109.1(3) 60.0(3) 60.2(2) 60.1(3) 108.5(3) 59.3(2) 107.3(3) 119.6(3) 121.2(3) 122.1(3) 123.0(3) 121.4(2) 60.1(3) 108.3(4) 60.0(3) 108.3(3) 107.7(4) 59.6(3) 60.9(2) 108.8(3) 108.0(3) 59.8(2) 121.8(3) 120.0(2) 120.3(2) 122.7(3) 123.2(3) 60.2(3) 109.1(4) 60.7(3) 109.5(3) 108.8(4) 59.7(3) 60.4(2) 108.5(3) 108.3(3) 60.7(2) 121.9(3) 121.3(3) 120.4(3) 120.5(3) 122.1(3) 60.0(3) 107.6(3) 60.0(3) 59.6(3) 107.0(3) 106.4(3) 107.5(3) 107.0(3) 58.9(3) 59.7(2) 121.3(3) 121.4(3)

B( 11)-B( 10)-Br( 10) B(9)-B(10)-Br(10) B(12)-B(10)-Br(10) B(12)-B(ll)-B(6) B(12)-B(ll)-B(2) B (6)-B(ll)-B(2) B(12)-B(l 1)-B(10) B(6)-B( 11)-B( 10) B(2)-B(l 1)-B( 10) B (12)-B(ll)-B(7) B(6)-B(ll)-B(7) B (2)-B(ll)-B(7) B(10)-B(l 1)-B(7) B (12)-B (ll)-B r(ll) B(6)-B(l 1)-Br(l 1) B(2)-B(l 1)-Br(l 1) B (10)-B (ll)-B r(ll) B (7)-B (ll)-B r(ll) B(ll)-B(12)-B(7) B(11)-B(12)-B(8) B(7)-B(12)-B(8) B(11)-B(12)-B(9) B(7)-B(12)-B(9) B(8)-B( 12)-B(9) B(11)-B(12)-B(10) B(7)-B( 12)-B( 10) B(8)-B( 12)-B( 10) B(9)-B(12)-B( 10) B(ll)-B(12)-Br(12) B(7)-B(12)-Br(12) B(8)-B(12)-Br(12) B(9)-B(12)-Br(12) B(10)-B( 12)-Br( 12) B(22)-C(21)-B(25) B(22)-C(21)-B(26) B(25)-C(21)-B(26) B(22)-C(21)-B(23) B(25)-C(21)-B(23) B(26)-C(21)-B(23) B(22)-C(21)-B(24) B(25)-C(21)-B(24) B(26)-C(21)-B(24) B(23)-C(21)-B(24) C(21)-B(22)-C1(22) C(21)-B(22)-B(31) Cl(22)-B(22)-B(31) C(21)-B(22)-B(27) Cl(22)-B(22)-B(27) B(31)-B(22)-B(27) C(21)-B(22)-B(26) Cl(22)-B(22)-B(26) B(31)-B(22)-B(26) B(27)-B(22)-B(26) C(21)-B(22)-B(23) C1(22)-B(22)'B(23) B(31)-B(22)-B(23)

122.6(2) 122.8(3) 123.1(3) 108.8(3) 108.1(3) 61.1(3) 613(3) 59.8(3) 109.2(3) 59.8(3) 107.7(3) 59.0(3) 1083(3) 122.7(3) 120.4(3) 120.0(3) 121.6(2) 122.5(3) 60.9(3) 108.4(3) 60.0(2) 107.2(3) 106.7(3) 58.6(2) 59.9(3) 108.3(4) 107.1(3) 59.6(2) 123.1(2) 123.2(3) 121.4(3) 120.9(3) 121.2(2) 113.5(3) 62.7(2) 61.6(3) 63.2(3) 114.6(4) 115.2(3) 114.4(3) 62.9(3) 114.1(3) 62.6(3) 119.6(3) 104.2(4) 127.7(3) 104.0(4) 126.3(3) 59.9(3) 58.8(2) 119.9(4) 60.3(3) 108.5(4) 58.9(3) 119.1(3) 107.0(4)

239


B(27)-B(22)-B(23) B(26)-B(22)-B(23) C(21)-B(23)-B(27) C(21)-B(23)-B(28) B(27)-B(23)-B(28) C(21)-B(23)-C1(23) B(27)-B(23)-C1(23) B(28)-B(23)-C1(23) C(21)-B(23)-B(22) B(27)-B(23)-B(22) B(28)-B(23)-B(22) CI(23)-B(23)-B(22) C(21)-B(23)-B(24) B(27)-B(23)-B(24) B(28)-B(23)-B(24) CI(23)-B(23)-B(24) B(22)-B(23)-B(24) B(28)-B(24)-C(21) B(28)-B(24)-B(29) C(21)-B(24)-B(29) B(28)-B(24)-C1(24) C(21)-B(24)-C1(24) B(29)-B(24)-C1(24) B(28)-B(24)-B(25) C(21)-B(24)-B(25) B(29)-B(24)-B(25) Cl(24)-B(24)-B(25) B(28)-B(24)-B(23) C(21)-B(24)-B(23) B(29)-B(24)-B(23) CI(24)-B(24)-B(23) B(25)-B(24)-B(23) C(21)-B(25)-B(26) C(21)-B(25)-B(30) B(26)-B(25)-B(30) C(21)-B(25)-B(29) B(26)-B(25)-B(29) B(30)-B(25)-B(29) C(21)-B(25)-C1(25) B(26)-B(25)-C1(25) B(30)-B(25)-CI(25) B(29)-B(25)-CI(25) C(21)-B(25)-B(24) B(26)-B(25)-B(24) B(30)-B(25)-B(24) B(29)-B(25)-B(24) CI(25)-B(25)-B(24) C(21)-B(26)-B(25) C(21)-B(26)-Cl(26) B(25)-B(26)-CI(26) C(21)-B(26)-B(22) B(25)-B(26)-B(22) CI(26)-B(26)-B(22) C(21)-B(26)-B(31) B(25)-B(26)-B(31) Cl(26)-B(26)-B(31)

B(22)-B(26)-B(31) C(21)-B(26)-B(30) B(25)-B(26)-B(30) Cl(26)-B(26)-B(30) B(22)-B(26)-B(30) B(31)-B(26)-B(30) B(23)-B(27>B(31) B(23)-B(27)-B(28) B(31)-B(27)-B(28) B(23)-B(27)-B(22) B(31)-B(27)-B(22) B(28)-B(27)-B(22) B(23)-B(27)-B(32) B(31)-B(27)-B(32) B(28)-B(27)-B(32) B(22)-B(27)-B(32) B(23)-B(27)-Br(27) B(31)-B(27)-Br(27) B(28)-B(27)-Br(27) B(22)-B(27)-Br(27) B(32)-B(27)-Br(27) B(24)-B(28)-B(23) B(24)-B(28)-B(27) B(23)-B(28)-B(27) B(24)-B(28)-B(32) B(23)-B(28)-B(32) B(27)-B(28)-B(32) B(24)-B(28)-B(29) B(23)-B(28)-B(29) B(27)-B(28)-B(29) B(32)-B(28)-B(29) B(24)-B(28)-Br(28) B(23)-B(28)-Br(28) B(27)-B(28)-Br(28) B(32)-B(28)-Br(28) B(29)-B(28)-Br(28) B(24)-B(29)-B(25) B(24)-B(29)-B(30) B(25)-B(29)-B(30) B(24)-B(29)-B(32) B(25)-B(29)-B(32) B(30)-B(29)-B(32) B(24)-B(29)-B(28) B(25)-B(29)-B(28) B(30)-B(29)-B(28) B(32)-B(29)-B(28) B(24)-B(29)-Br(29) B(25)-B(29)-Br(29) B(30)-B(29)-Br(29) B(32)-B(29)-Br(29) B(28)-B(29)-Br(29) B(31)-B(30)-B(32) B(31)-B(30)-B(25) B(32)-B(30)-B(25) B(31)-B(30)-B(29) B(32)-B(30)-B(29)

59.0(3) 108-5(4) 104.1(3) 103.8(3) 60.7(3) 120.3(3) 126.7(3) 126.3(3) 57.9(3) 60.0(3) 107.9(3) 120.6(4) 59.2(3) 107.0(3) 58.2(3) 120.1(3) 107.4(3) 104.2(3) 62.6(3) 105.1(3) 127.2(3) 119.2(3) 125.1(4) 108.1(3) 57.7(3) 59.6(3) 119.7(3) 59.7(3) 58.2(3) 110.2(3) 119.9(3) 106.7(3) 59.4(3) 105.9(3) 61.4(3) 106.4(3) 111.0(3) 60.7(3) 121.2(3) 119.6(3) 124.7(3) 122.6(4) 59.5(3) 109.5(3) 107.6(3) 59.4(3) 120.0(3) 59.1(2) 121.9(3) 120.9(3) 58.4(2) 107.9(3) 120.4(4) 103.4(3) 106.3(4) 126.0(3)

59.6(3) 104.5(3) 59.9(3) 125.4(3) 107.2(3) 58.7(3) 108.5(3) 59.6(3) 107.2(3) 61.0(3) 59.8(3) 107.9(3) 108.6(3) 59.5(3) 60.1(2) 108.0(3) 120.2(3) 122.9(3) 121.7(3) 121.5(3) 122.1(3) 62.1(3) 109.4(4) 59.7(3) 108.7(3) 108.6(3) 60.1(3) 59.8(2) 109.9(3) 108.9(3) 60.6(2) 121.0(3) 120.4(2) 121.1(3) 121.5(3) 121.3(3) 61.0(3) 108.0(4) 59.6(3) 105.4(4) 105.6(4) 58.8(2) 57.6(3) 105.3(4) 105.5(4) 58.7(2) 121.4(3) 121.8(3) 122.5(3) 124.5(3) 124.3(3) 60.0(3) 106.6(3) 107.6(3) 109.1(3) 61.3(3)

240


B(25)-B(30)-B(29) B(31)-B(30)-B(26) B(32)-B(30)-B(26) B(25)-B(30)-B(26) B(29)-B(30)-B(26) B(3 !)-B(30)-Br(30) B(32)-B(30)-Br(30) B(25)-B(30)-Br(30) B(29)-B(30)-Br(30) B(26)-B(30)-Br(30) B(30)-B(31)-B(32) B(30)-B(31)-B(22) B(32)-B(31)-B(22) B(30)-B(31)-B(27) B(32)-B(31)-B(27) B(22)-B(31)-B(27) B(30)-B(31)-B(26) B(32)-B(31 )-B(26) B(22)-B(31)-B(26) B(27)-B(31)-B(26) B(30)-B(31)-Br(31) B(32)-B(31)-Br(31) B(22)-B(31)-Br(31) B(27)-B(31)-Br(31) B(26)-B(31)-Br(31) B(31)-B(32)-B(30) B(31)-B(32)-B(27) B(30)-B(32)-B(27) B(31)-B(32)-B(28) B(30)-B(32)-B(28) B(27)-B(32)-B(28) B(31)-B(32)-B(29) B(30)-B(32)-B(29) B(27)-B(32)-B(29) B(28)-B(32)-B(29) B(31)-B(32)-Br(32) B(30)-B(32)-Br(32) B(27)-B(32)-Br(32) B(28)-B(32)-Br(32) B(29)-B(32)-Br(32) C(1A)-N(1)-C(1C) C(1A)-N(1)-C(1B) C(1C)-N(1)-C(1B) C(2A)-N(2)-C(2B) C(2A)-N(2)-C(2C) C(2B)-N(2)-C(2C) C(3A)-N(3)-C(3C) C(3A)-N(3)-C(3B) C(3C)-N(3)-C(3B) C(4B)-N(4)-C(4A) C(4B)-N(4)-C(4C) C(4A)-N(4)-C(4Q

59.7(3) 60.2(3) 108.3(3) 58.7(3) 108.1(3) 122.6(2) 124.6(3) 120.4(3) 121.8(3) 119.2(3) 60.5(3) 109.6(3) 109.2(3) 109.3(3) 60.5(3) 60.3(3) 61.1(3) 109.4(3) 60.1(3) 108.7(3) 121.9(2) 122.9(3) 119.0(4) 121.1(3) 119.9(3) 59.5(3) 59.9(3) 108.0(4) 107.2(3) 107.9(3) 59.8(2) 107.6(3) 59.9(2) 108.8(3) 60.7(2) 122.8(3) 121.3(3) 122.3(3) 121.9(3) 120.4(3) 110.4(4) 112.0(4) 112.3(4) 111.3(4) 113.7(4) 111.7(3) 113.2(4) 111.7(3) 111.0(4) 111.6(4) 112.9(4) 111.7(4)


Chapter 5 Compound V-9 A tom ic coordinates and thermal parameters. X

Cs(l) Br(7) Br(9) Br(10) Br(2) Br(6) Br(5) Br(3) Br(8) Br{4) C(l) B(9) B(5) B(6) B(7) B(10) B(3) B(4) B(8) B(2) 0(1)

2755(1) 5223(1) 668(1) 4210(1) 3567(1) 3881(1) 386(1) 2218(1) 1970(1) -951(1) 1255(7) 1568(8) 1357(8) 2977(10) 3522(9) 3180(9) 2095(8) 798(10) 2136(9) 2648(8) 2759(11)

y 9345(1) 11377(1) 9384(1) 8923(1) 13797(1) 11612(1) 12432(1) 12129(1) 9129(1) 10747(1) 12383(5) 10402(7) 11825(6) 11352(7) 11238(7) 10131(6) 11677(6) 11108(8) 10255(7) 12437(6) 7082(10)

z

829(1) -2516(1) -945(1) -1369(1) -1791(1) -348(1) -663(1) -3695(1) -3111(1) -2570(1) -2209(3) -1499(5) -1399(4) -1268(4) -2162(4) -1664(4) -2699(4) -2256(5) -2416(4) -1893(4) 203(6)

U(eq) 96(1) 73(1) 77(1) 79(1) 76(1) 71(1) 76(1) 83(1) 93(1) 90(1) 53(2) 55(3) 47(2) 64(3) 60(3) 57(3) 54(2) 73(3) 54(2) 53(2) 96(4)

Bond lengths C s(l)-0(1) Cs(l)-Br(6) Cs(l)-Br(7)#l Cs(l)-Br(6)#l Cs(l)-Br(4)#2 Cs(l)-Br(9) Cs(l)-Br(10)#l Cs(l)-Br(9)#2 Cs( 1)-Br(5)#2 Br(7)-B(7) Br(T)-Cs(l)#l Br(9)-B(9) Br(9)-Cs(l)#2 Br(10)-B(10) Br(10)-Cs(l)#l Br(2)-B(2) Br(6)-B(6) Br(6)-Cs(l)#l Br(5)-B(5) Br(5)-Cs(l)#2 Br(3)-B(3) Br(8)-B(8) Br(4)-B(4) Br(4)-Cs(l)#2

3.019(12) 3.7827(13) 3.7980(12) 3.8583(15) 3.8621(14) 3.8640(13) 3.8978(14) 3.9158(15) 3.9356(14) 1.938(9) 3.7980(12) 1.908(8) 3.9158(15) 1.896(8) 3.8978(14) 1.931(8) 1.942(8) 3.8583(15) 1.911(8) 3.9356(14) 1.959(8) 1.901(7) 1.935(11) 3.8621(14)

C(l)-B(2) C(l)-B(3) C(l)-B(4) C(l)-B(5) B(9)-B(10) B(9)-B(5) B(9)-B(4) B(9)-B(8) B(9)-B(6) B(5)-B(6) B(5)-B(2) B(5)-B(4) B(6)-B(10) B(6)-B(2) B(6)-B(7) B(7)-B(10) B(7)-B(3) B(7)-B(2) B(7)-B(8) B(10)-B(8) B(3)-B(4) B(3)-B(8) B(3)-B(2) B(4)-B(8)

1.537(11) 1.568(10) 1.638(12) 1.661(9) 1.761(13) 1.774(11) 1.809(12) 1.858(11) 1.908(13) 1.790(13) 1.839(11) 1.892(11) 1.693(11) 1.794(11) 1.805(11) 1.699(11) 1.827(12) 1.819(12) 1.922(12) 1.735(11) 1.773(13) 1.826(11) 1.839(11) 1.786(14)


Bond angles

0(1)-Cs(l)-Br(6) 0 ( 1)-Cs( 1)-Br(7)#l Br(6)-Cs(l)-Br(7)#l 0 ( 1)-Cs( 1)-Br(6)#l Br(6)-Cs( 1)-Br(6)# 1 Br(7)# 1-Cs( 1)-Br(6)#l Of 1)-Cs( 1)-Br(4)#2 Br(6)-Cs(l)-Br(4)#2 Br(7)#l-Cs(l)-Br(4)#2 Br(6># 1-Cs( 1)-Br(4)#2 0(1)-Cs(l)-Br(9) Br(6)-Cs( 1)-Br(9) Br(7># 1-Cs( 1)-Br(9) Br(6)#l-Cs(l)-Br(9) Br(4)#2-Cs( 1)-Br(9) O(l)-Cs(l)-Br(10)#l Br(6)-Cs(l)-Br(10>#l Br(7)#l-Cs(l)-Br(10)#l Br(6)#l-Cs(l)-Br(10)#l Br(4)#2-Cs( 1)-Br( 10)# 1 Br(9)-Cs(l)-Br( 10)#1 0 ( 1)-Cs( 1)-Br(9)#2 Br(6)-Cs(l)-Br(9)#2 Br(7)#l-Cs(l)-Br(9)#2 Br(6)#l -Cs( 1)-Br(9)#2 Br(4)#2-Cs( 1)-Br(9)#2 Br(9)-Cs( 1)-Br(9)#2 Br( 10)#1 -Cs(l)-Br(9)#2 0 ( 1)-Cs( 1)-Br(5)#2 Br(6)-Cs( 1)-Br(5)#2 Br(7)#l-Cs(l)-Br(5)#2 Br(6)# 1-Cs( 1)-Br(5)#2 Br(4)#2-Cs( 1)-Br(5)#2 Br(9)-Cs(l)-Br(5)#2 Br(10)#l-Cs(l)-Br(5)#2 Br(9)#2-Cs( 1)-Br(5)#2 B(7)-Br(7)-Cs(l)#l B(9)-Br(9)-Cs(l) B(9)-Br(9)-Cs( 1)#2 Cs(l)-Br(9)-Cs(l)#2 B( 10)-Br( 10)-Cs( 1}# 1 B(6)-Br(6)-Cs(l) B(6)-Br(6)-Cs( 1)# 1 Cs( 1)-Br(6)-Cs( 1)#1 B(5)-Br(5)-Cs( 1)#2 B(4)-Br(4)-Cs(l)#2 B(2)-C(l)-B(3) B(2)-C(l)-B(4) B(3)-C(l)-B(4) B(2)-C(l)-B(5) B(3)-C(l)-B(5) B(4)-C(l)-B(5) B(10)-B(9)-B(5)

B(10)-B(9)-B(4) B(5)-B(9)-B(4) B(10)-B(9)-B(8) B(5)-B(9)-B(8) B(4)-B(9)-B(8) B( 10)-B(9)-Br(9) B(5)-B(9)-Br(9) B(4)-B(9)-Br(9) B(8)-B(9)-Br(9) B(10)-B(9)-B(6) B(5)-B(9)-B(6) B(4)-B(9)-B(6) B(8)-B(9)-B(6) Br(9)-B(9)-B(6) C(l)-B(5)-B(9) C(l)-B(5)-B(6) B(9)-B(5)-B(6) C(l)-B(5)-B(2) B(9)-B(5)-B(2) B(6)-B(5)-B(2) C(l)-B(5)-B(4) B(9)-B(5>B(4) B(6)-B(5)-B(4) B(2)-B(5)-B(4) C(l)-B(5)-Br(5) B(9)-B(5)-Br(5) B(6)-B(5)-Br(5) B(2)-B(5)-Br(5) B(4)-B(5)-Br(5) B(10)-B(6)-B(5) B(10)-B(6)-B(2) B(5)-B(6>B(2) B(10)-B(6)-B(7) B(5)-B(6)-B(7) B(2)-B(6)-B(7) B(10)-B(6)-B(9) B(5)-B(6)-B(9) B(2)-B(6)-B(9) B(7)-B(6)-B(9) B(10)-B(6)-Br(6) B(5)-B(6)-Br(6) B(2)-B(6)-Br(6) B(7)-B(6)-Br(6) B(9)-B(6)-Br(6) B(10)-B(7)-B(6) B( 10)-B(7)-B(3) B(6)-B(7)-B(3) B(10)-B(7)-B(2) B(6)-B(7)-B(2) B(3)-B(7)-B(2) B(10)-B(7)-B(8) B(6)-B(7)-B(8) B(3)-B(7)-B(8)

116.4(2) 95.4(2) 118.73(3) 66.8(2) 76.72(3) 69.83(3) 108.2(2) 134.21(3) 64.24(3) 133.15(3) 72.0(2) 70.62(2) 167.18(3) 106.06(3) 116.65(3) 125.8(2) 58.25(2) 60.62(2) 59.42(3) 103.05(3) 128.61(3) 114.3(2) 93.10(3) 120.69(3) 168.44(3) 58.20(2) 64.75(3) 119.80(3) 58.5(2) 130.43(3) 110.78(3) 125.23(3) 66.76(2) 60.96(2) 169.50(3) 57.86(3) 99.8(2) 101.9(3) 104.4(3) 115.25(3) 94.9(3) 104.2(3) 98.2(3) 103.28(3) 101.6(2) 104.4(3) 72.6(5) 109.2(6) 67.1(5) 70.1(5) 107.4(5) 70.0(5) 109.3(6)

109.7(6) 63.7(5) 57.2(5) 104.0(5) 58.3(5) 118.5(5) 121.4(5) 122.1(6) 129.3(5) 54.8(4) 58.1(5) 100.6(6) 89.1(5) 132.5(5) 108.2(5) 105.5(5) 64.7(5) 51.8(4) 104.6(5) 59.2(4) 54.4(4) 59.0(5) 101.9(6) 87.8(5) 119.3(5) 122.4(5) 124.4(4) 129.7(5) 130.1(6) 111.7(6) 113.4(5) 61.7(5) 58.0(5) 104.2(5) 60.7(5) 58.2(5) 57.2(5) 101.1(6) 91.3(5) 117.9(6) 118.2(5) 121.4(5) 132.3(6) 129.0(5) 57.7(5) 110.4(6) 101.4(6) 111.8(6) 59.3(5) 60.6(5) 56.8(5) 90.3(5) 58.2(4)

243


B(2)-B(7)-B(8) B( 10)-B(7)-Br(7) B(6)-B(7)-Br(7) B(3)-B(7)-Br(7) B(2)-B(7)-Br(7) B(8)-B(7)-Br(7) B(7)-B(10)-B(6) B(7)-B(10)-B(8) B(6)-B(10)-B(8) B(7)-B(10)-B(9) B(6)-B(10)-B(9) B(8)-B(10)-B(9) B(7)-B( 10)-Br( 10) B(6)-B( 10)-Br( 10) B(8)-B(10)-Br(10) B(9)-B(10)-Br(10) C(l)-B(3)-B(4) C(l)-B(3)-B(8) B(4)-B(3)-B(8) C(l)-B(3)-B(7) B(4)-B(3)-B(7) B(8)-B(3)-B(7) C(l)-B(3)-B(2) B(4)-B(3)-B(2) B(8)-B(3)-B(2) B(7)-B(3)-B(2) C(l)-B(3)-Br(3) B(4)-B(3)-Br(3) B(8)-B(3)-Br(3) B(7)-B(3)-Br(3) B(2)-B(3)-Br(3) C(l)-B(4)-B(3) C(l)-B(4)-B(8) B(3)-B(4)-B(8) C(l)-B(4)-B(9) B(3)-B(4)-B(9) B(8)-B(4)-B(9) C(l)-B(4)-B(5) B(3)-B(4)-B(5) B(8)-B(4)-B(5) B(9)-B(4)-B(5) C(l)-B(4)-Br(4) B(3)-B(4)-Br(4) B(8)-B(4)-Br(4) B(9)-B(4)-Br(4) B(5)-B(4)-Br(4) B(10)-B(8)-B(4) B(10)-B(8)-B(3) B(4)-B(8)-B(3) B(10)-B(8)-B(9) B(4)-B(8)-B(9) B(3)-B(8)-B(9) B(10)-B(8)-Br(8) B(4)-B(8)-Br(8) B(3)-B(8)-Br(8) B(9)-B(8)-Br(8)

101.3(6) 118.9(6) 130.9(6) 121.2(5) 120.5(5) 131.4(5) 64.3(5) 68.1(5) 100.9(6) 100.3(6) 67.0(5) 64.2(5) 130.8(6) 130.6(6) 128.5(5) 128.9(5) 58.3(5) 111.3(6) 59.5(5) 107.8(6) 104.2(6) 63.5(5) 52.9(4) 91-5(5) 104.3(5) 59.5(4) 118.2(5) 130.8(5) 123.1(5) 120.7(5) 127.1(5) 54.6(5) 110.0(7) 61.8(5) 107.6(6) 103.9(7) 62.2(5) 55.6(4) 90.5(6) 102.2(6) 57.2(4) 120.2(6) 132.9(6) 123.1(6) 119.6(6) 127.1(6) 112.0(6) 108.8(5) 58.8(5) 58.6(4) 59.5(5) 99.9(5) 121.3(5) 120.1(5) 119.9(4) 133.0(5)

B(10)-B(8)-B(7) B(4)-B(8)-B(7) B(3)-B(8)-B(7) B(9)-B(8)-B(7) Br(8)-B(8)-B(7) C(l)-B(2)-B(6) C(l)-B(2)-B(7) B(6)-B(2)-B(7) C(l)-B(2)-B(5) B(6)-B(2>B(5) B(7)-B(2)-B(5) C(l)-B(2)-B(3) B(6)-B(2)-B(3) B(7)-B(2)-B(3) B(5)-B(2)-B(3) C(l)-B(2)-Br(2) B(6)-B(2)-Br(2) B(7)-B(2)-Br(2) B(5)-B(2)-Br(2) B(3)-B(2)-Br(2)

55.1(4) 100.0(6) 58.3(4) 89.3(5) 131.6(5) 111.0(6) 109.6(6) 59.9(5) 58.1(4) 59.0(5) 101.6(5) 54.5(4) 101.3(5) 59.9(4) 90.1(5) 121.9(5) 120.3(5) 118.3(5) 132.7(5) 130.6(5)

244


Compound V-10 A tom ic coordinates and thermal parameters. X

A g(l) Ag(2) Ag(3) N(l) 0(1) 0(2) 0(3) 0(4) Br(12) Br(13) Br(14) Br(15) Br(16) Br(17) Br(18) Br(19) Br(20) Br(22) Br(23) Br(24) Br(25) Br(26) Br(27) Br(28) Br(29) Br(30) C(ll) 0(12) 0(13) 0(14) 0(15) 0(16) 0(21) C(22) 0(23) 0(24) 0(25) 0(26) 0(31) 0(32) 0(33) 0(34) 0(1) B(12) B(13) B(14) B(15) B(16) B(17) B(18) B(19)

22109(1) 18132(1) 16093(1) 17164(4) 17671(3) 17122(3) 16683(3) 17962(5) 24943(1) 22836(1) 23088(1) 25181(1) 24490(1) 23163(1) 24813(1) 26160(1) 25146(1) 19426(1) 20929(1) 19735(1) 18191(1) 21266(1) 21508(1) 19546(1) 19350(1) 21081(1) 22213(3) 21629(3) 21722(3) 22357(3) 22906(4) 22865(3) 16455(4) 16731(3) 17456(4) 17823(4) 17508(3) 16836(3) 17440(10) 16834(7) 16869(7) 17597(8) 23983(3) 24586(3) 23684(2) 23781(3) 24678(3) 24437(3) 23860(2) 24585(3) 25157(2)

•

y 1272(1) 865(1) 2249(1) 974(4) 497(4) 1444(4) 997(4) -241(7) 4704(1) 3679(1) 2313(1) 3438(1) 3089(1) 1343(1) 1140(1) 2871(1) 1084(1) 3489(1) 4441(1) 3378(1) 2451(1) 2650(1) 2550(1) 1104(1) 1179(1) 707(1) -208(5) 145(4) 491(4) 432(5) 79(5) -220(5) 3438(5) 3830(5) 3712(5) 3132(5) 2743(5) 2881(5) 130(8) 281(6) -280(8) -626(8) 3595(3) 3677(3) 3227(3) 2632(3) 3087(3) 2845(3) 2134(3) 2046(3) 2778(3)

z

2788(1) 4529(1) 5435(1) 5682(4) 5756(3) 5103(3) 6092(3) 3442(5) 3979(1) 3990(1) 1966(1) 1955(1) 5354(1) 3951(1) 2433(1) 3868(1) 4643(1) 2136(1) 3912(1) 5568(1) 3795(1) 2604(1) 5127(1) 5023(1) 2551(1) 3841(1) 2287(3) 1898(3) 1207(3) 920(3) 1321(3) 2016(3) 6282(3) 5715(4) 5669(4) 6106(4) 6619(4) 6740(4) 2863(5) 3313(5) 3957(4) 4015(5) 2931(2) 3628(2) 3665(2) 2782(2) 2777(2) 4290(2) 3686(3) 3064(3) 3663(2)

U(eq) 6 6 (1 ) 1 0 0 (1 )

75(1) 74(3) 83(2) 81(2) 81(2) 284(5) 51(1) 64(1) 51(1) 53(1) 62(1) 60(1) 56(1) 54(1) 62(1) 64(1) 62(1) 60(1) 70(1) 52(1) 54(1) 51(1) 61(1) 47(1) 80(4) 61(3) 67(3) 92(4) 79(3) 89(4) 107(4) 131(4) 117(5) 98(4) 95(4) 90(4) 367(9) 199(5) 206(6) 182(8) 32(2) 32(2) 30(2) 42(3) 26(2) 34(1) 35(2) 43(2) 27(1)

245


B(20) C(2) B(22) B(23) B(24) B(25) B(26) B(27) B(28) B(29) B(30)

24727(3) 19541(3) 19723(3) 20396(3) 19870(3) 19227(3) 20607(3) 20695(3) 19859(3) 19754(3) 20536(3)

1952(3) 3505(3) 3040(3) 3445(3) 2992(3) 2592(3) 2546(3) 2525(3) 1911(3) 1948(3) 1692(3)

3997(3) 3850(3) 3115(2) 3872(3) 4593(3) 3828(3) 3345(3) 4380(3) 4327(3) 3277(3) 3840(3)

35(1) 48(2) 35(3) 28(2) 38(3) 45(3) 35(3) 34(2) 36(3) 28(2) 28(2)

Bond lengths

Ag(l)-Br(17) Ag(l)-Br(26) Ag(l)-Br(30) Ag(l)-Br(14) A g (l)-C (ll) Ag( 1)-C( 12) Ag(2)-0(2) Ag(2)-0(1) Ag(2)-0(4) Ag(2)-Br(28) Ag(2)-Br(25) Ag(3)-0(2) Ag(3)-0(3) Ag(3)-C(21) Ag(3)-Br(20)#l Ag(3)-Br(19)#l N (l)-0(1) N (l)-0 (3 ) N (l)-0(2) 0(4)-C(34) 0(4)-C(31) Br(12)-B(12) Br(13)-B(13) Br(14)-B(14) Br(15)-B(15) Br(16)-B(16) Br(17)-B(17) Br(18)-B(18) Br(19)-B(19) Br(19)-Ag(3)#2 Br(20)-B(20) Br(20)-Ag(3)#2 Br(22)-B(22) Br(23)-B(23) Br(24)-B(24) Br(25)-B(25) Br(26)-B(26) Br(27)-B(27) Br(2S)-B(28) Br(29)-B(29) Br(30)-B(30) C(11)-C(12)

2.7123(10) 2.7516(11) 3.0032(11) 3.0167(11) 2.592(6) 2.533(6) 2.455(6) 2.531(6) 2.650(6) 2.7382(12) 2.9122(15) 2.473(6) 2.549(6) 2.510(6) 2.8697(11) 3.0070(10) 1.227(9) 1.232(9) 1.287(8) 1.447(16) 1.475(17) 1.888(5) 1.912(5) 1.918(5) 1.931(5) 1.942(4) 1.940(5) 1.941(5) 1.889(4) 3.0070(10) 1.940(5) 2.8697(11) 1.926(4) 1.907(5) 1.905(5) 1.961(5) 1.929(5) 1.915(5) 1.952(5) 1.903(5) 1.908(5) 1.360(8)

C (ll)-C (16) C(12)-C(13) C(13)-C(14) C(14)-C(15) C(15)-C(16) C(21)-C(22) C(21)-C(26) C(22)-C(23) C(23)-C(24) C(24)-C(25) C(25)-C(26) C(31)-C(32) C(32)-C(33) C(33)-C(34) C(l)-B(12) C(l)-B(15) C(l)-B(13) C(l)-B(14) B(12)-B(19) B(12)-B(15) B(12)-B(16) B(12)-B(13) B(13)-B(16) B(13)-B(17) B(13)-B(14) B(14)-B(17) B(14)-B(18) B(14)-B(15) B(15)-B(18) B(15)-B(19) B(16)-B(20) B(16)-B(17) B(16)-B(19) B(17)-B(20) B(17)-B(18) B(18)-B(20) B(18)-B(19) B(19)-B(20) C(2)-B(22) C(2)-B(25) C(2)-B(23) Q 2)-B(24)

1.374(8) 1392(8) 1.360(8) 1.322(8) 1.350(8) 1.357(9) 1.371(9) 1.392(9) 1.366(10) 1.315(9) 1.330(9) 1.49(2) 1.471(14) 1.476(19) 1.596(6) 1.602(7) 1.608(6) 1.633(7) 1.817(7) 1.831(6) ■ 1.847(7) 1.860(7) 1.814(6) 1.813(7) 1.885(6) 1.804(6) 1.814(7) 1.847(7) 1.790(7) 1.807(6) 1.663(7) 1.853(6) 1.864(7) 1.692(7) 1.867(7) 1.672(7) 1.865(6) 1.716(7) 1.593(7) 1.602(7) 1.611(7) 1.636(7)

246


B(22)-B(29) B(22)-B(25) B(22)-B(26) B(22)-B(23) B(23)-B(27) B(23)-B(26) B(23)-B(24) B(24)-B(27) B(24)-B(28) B(24)-B(25) B(25)-B(28)

1.806(7) 1.821(7) 1.855(7) 1.869(6) 1.813(7) 1.815(7) 1.871(7) 1.811(7) 1.827(7) 1.842(7) 1.792(7)

B(25)-B(29) B(26)-B(30) B(26)-B(27) B(26)-B(29) B(27)-B(30) B(27)-B(28) B(28)-B(30) B(28)-B(29) B(29)-B(30)

114.76(3) 89.85(3) 85.46(3) 85.22(3) 81.85(3) 162.96(3) 50.62(18) 125.60(13) 99.90(13) 85.44(14) 129.78(15) 86.14(3) 51.11(18) 89.35(14) 84.89(13) 80.49(12) 129.73(13) 81.45(3) 125.0(7) 116.1(7) 118.8(7) 95.6(4) 97.5(5) 95.7(4) 166.7(2) 93.6(4) 110.2(11) 100.41(15) 107.26(14) 90.31(14) 89.89(15) 100.48(16) 104.73(15) 104.15(15) 97.32(16) 121.9(6) 116.9(6) 121.0(6) 119.6(6) 122.3(6) 118.1(6) 122.9(7)

C(21)-C(22)-C(23) C(24)-C(23)-C(22) C(25)-C(24)-C(23) C(24)-C(25)-C(26) C(25)-C(26)-C(21) 0(4)-C(31)-C(32) C(33)-C(32)-C(31) C(32)-C(33)-C(34) 0(4)-C(34)-C(33) B(12)-C(l)-B(15) B(12)-C(l)-B(13) B(15)-C(l)-B(13) B(12)-C(l)-B(14) B(15)-C(l)-B(14) B(13)-C(l)-B(14) C(l)-B(12)-B(19) C(l)-B(12)-B(15) B(19)-B(12)-B(15) C(l)-B(12)-B(16) B(19)-B(12)-B(16) B(15)-B(12)-B(16) C( 1)-B(12)-B( 13) B(19)-B(12)-B(13) B(15)-B(12)-B(13) B(16)-B(12)-B(13) C( 1)-B( 12)-Br( 12) B(19)-B(12)-Br(12) B(15)-B(12)-Br(12) B(16)-B(12)-Br(12) B( 13)-B(12)-Br( 12) C(l)-B(13)-B(16) C(l)-B(13)-B(17) B(16)-B(13)-B(17) C(l)-B(13)-B(12) B(16)-B(13)-B(12) B(17)-B(13)-B(12) C(l)-B(13)-B(14) B(16)-B(13)-B(14) B(17)-B(13)-B(14) B(12)-B(13)-B(14) C(l)-B(13)-Br(13) B(16)-B(13)-Br(13)

1.816(7) 1.667(7) 1.846(6) 1.872(7) 1.677(7) 1.861(7) 1.667(7) 1.874(6) 1.739(7)

Bond angles Br( 17)-Ag( 1)-Br(26) Br(17)-Ag(l)-Br(30) Br(26)-Ag( 1)-Br(30) Br( 17)-Ae( 1)-Br(14) Br( 26)-Ag( 1)-Br( 14) Br(30)-Ag( 1)-Br( 14) 0(2)-A g(2)-0(l) Of 2)-Ag(2)-Br(28) Of 1)-Ag(2)-Br(28) 0(2)-Ag(2)-Br(25) 0 ( 1)-Ag(2)-Br(25) Br(28)-Ag(2)-Br(25) 0(2)-A g(3)-0(3) O(2)-Ag(3)-Br(20)#l O(3)-Ag(3)-Br(20)#l 0(2)-Ag(3)-Br( 19)#1 0(3)-Ag(3)-Br(19)#l Br(20)#l-Ag(3)-Br(19)#l 0 (l)-N (l)-0 (3 ) 0 (l)-N (l)-0 (2 ) 0 (3 )-N (l)-0 (2 ) N(l)-0(1)-A g(2) N (l)-0(2)-A g(2) N (l)-0(2)-A g(3) Ag(2)-0(2)-Ag(3) N (l)-0(3)-A g(3) C(34)-0(4)-C(31) B( 14)-Br( 14)-Ag( 1) B( 17)-Br( 17)-Ag( 1) B(19)-Br(19)-Ag(3)#2 B(20)-Br(20)-Ag(3>#2 B(25)-Br(25)-Ag(2) B(26)-Br(26)-Ag(l) B(28)-Br(28)-Ag(2) B(30)-Br(30)-Ag(l) C(12)-C(ll)-C(16) C(ll)-C(12)-C(13) C( 14)-C( 13)-C( 12) C(15)-C(14)-C(13) C( 14)-C( 15 )-C( 16) C(15)-C(16)-C(ll) C(22)-C(21)-C(26)

116.3(7) 119.8(7) 119.8(7) 123.3(7) 117.2(7) 100.2(8) 110.7(10) 104.5(10) 107.3(9) 69.9(3) 71.0(3) 108.5(3) 109.9(3) 69.6(3) 71.1(3) 109.0(3) 55.2(3) 59.4(2) 107.2(3) 61.1(3) 100.7(3) 54.8(3) 102.7(3) 89.8(3) 58.6(2) 122.0(3) 121.3(3) 132.9(3) 120.9(3) 129.1(3) 108.2(3) 107.8(3) 61.4(3) 54.2(2) 60.4(3) 103.0(3) 55.1(3) 101.4(3) 58.4(3) 89.8(3) 119.3(3) 124.5(3)

247


B(17)-B(13)-Br(13) B( 12)-B( 13)-Br( 13) B( 14)-B( 13)-Br( 13) C(l)-B(14)-B(17) C(l)-B(14)-B(18) B( 17)-B( 14)-B( 18) C(l)-B(14)-B(15) B( 17)-B( 14)-B( 15) B( 18)-B( 14)-B( 15) C(l)-B(14)-B(13) B( 17)-B( 14)-B( 13) B(18)-B(14)-B(13) B( 15)-B( 14)-B( 13) C( 1)-B( 14)-Br(l 4) B( 17)-B( 14)-Br( 14) B( 18)-B( 14)-Br( 14) B(15)-B(14)-Br(14) B( 13)-B( 14)-Br( 14) C(l)-B(15)-B(18) C(l)-B(15)-B(19) B( 18)-B( 15)-B( 19) C(l)-B(15)-B(12) B(18)-B(15)-B(12) B( 19)-B( 15)-B(12) Q l)-B(15)-B(14) B( 18)-B( 15)-B( 14) B( 19)-B( 15)-B( 14) B(12)~B(15)-B(14) C( 1)-B( 15)-Br( 15) B( 18)-B( 15)-Br( 15) B( 19)-B( 15)-Br( 15) B( 12)-B(15)-Br( 15) B(14)-B(15)-Br(15) B(20)-B(16)-B(13) B(20)-B(16)-B(12) B(13)-B(16)-B(12) B(20)-B( 16)-B( 17) B( 13)- B( 16)-B( 17) B( 12)-B( 16)-B( 17) B(20)-B( 16)-B( 19) B(13)-B(16)-B(19) B( 12)-B( 16)-B( 19) B( 17)-B(16)-B(19) B(20)-B(16)-Br(16) B( 13)-B( 16)-Br( 16) B(12)-B(16)-Br(16) B(17)-B(16)-Br(16) B( 19)-B( 16)-Br( 16) B(20)-B(17)-B(14) B(20)-B( 17)-B( 13) B( 14)-B( 17)-B( 13) B(20)-B(17)-B(16) B(14)-B(17)-B(16) B( 13)-B( 17)-B( 16) B(20)-B( 17)-B( 18) B(14)-B(17)-B(18)

B(13)-B(17)-B(18) B(16)-B(17)-B(18) B(20)-B( 17)-Br( 17) B(14)-B(17)-Br(17) B(13)-B(17)-Br(17) B(16)-B(17)-Br(17) B(18)-B(17)-Br(17) B(20)-B(18)-B(15) B(20)-B(18)-B(14) B(15)-B(18)-B(14) B(20)-B(18)-B(19) B(15)-B(18)-B(19) B(14)-B(18)-B(19) B(20)-B(18)-B(17) B(15)-B(18)-B(17) B(14)-B(18)-B(17) B(19)-B(18)-B(17) B(20)-B(18)-Br(18) B(15)-B(18)-Br(18) B(14)-B(18)-Br(18) B(19)-B(18)-Br(18) B(17)-B(18)-Br(18) B(20)-B(19)-B(15) B(20)-B(19)-B(12) B(15)-B(19)-B(12) B(20)-B(19)-B(16) B(15)-B(19)-B(16) B(12)-B(19)-B(16) B(20)-B( 19)-B( 18) B(15)-B(19)-B(18) B(12)-B(19)-B(18) B(16)-B(19)-B(18) B(20)-B(19)-Br(19) B(15)-B( 19)-Br( 19) B(12)-B(19)-Br(19) B(16)-B(19)-Br(19) B(18)-B(19)-Br(19) B( 16)-B(20)-B( 18) B(16)-B(20)-B(17) B(18)-B(20)-B(17) B(16)-B(20)-B(19) B(18)-B(20)-B(19) B(17)-B(20)-B(19) B(16)-B(20)-Br(20) B(18)-B(20)-Br(20) B(17)-B(20)-Br(20) B( 19)-B(20)-Br(20) B(22)-C(2)-B(25) B(22)-C(2)-B(23) B(25)-C(2)-B(23) B(22)-C(2)-B(24) B(25)-C(2)-B(24) B(23)-C(2)-B(24) C(2)-B(22)-B(29) C(2)-B(22)-B(25) B(29)-B(22)-B(25)

122.0(3) 131.1(3) 128.3(3) 107.1(3) 106.9(3) 62-1(3) 54.4(3) 101.9(3) 58.5(3) 53.8(3) 58.8(3) 101.3(3) 88.5(3) 120.8(3) 122.8(3) 122.9(3) 130.4(3) 131.2(3) 109.5(4) 109.2(3) 62.4(3) 54.9(3) 103.7(3) 59.9(2) 56.0(3) 59.8(3) 104.4(3) 91.9(3) 117.5(3) 125.1(3) 121.0(3) 125.7(3) 130.8(3) 111.6(3) 111.2(3) 61.0(3) 57.2(3) 59.3(3) 101.9(3) 57.9(3) 102.6(3) 58.6(3) 91.7(3) 120.6(3) 119.0(3) 119.1(3) 131.6(3) 130.4(3) 110.6(4) 110.3(3) 62.8(3) 55.7(3) 103.0(3) 59.3(3) 55.8(3) 59.2(3)

102.0(3) 88.7(3) 117.3(3) 122.2(3) 122.2(3) 130.0(3) 131.1(3) 111.4(3) 111.1(4) 61.7(3) 57.7(3) 59.2(2) 103.4(3) 56.8(3) 101.6(3) 58.7(3) 91.2(3) 119.6(3) 121.3(3) 118.2(3) 132.2(3) 129.4(3) 108.6(3) 110.2(3) 60.7(2) 55.2(3) 100.9(3) 60.2(3) 55.5(3) 58.3(2) 101.4(3) 88.4(3) 119.8(3) 122.4(3) 121.1(3) 131.3(3) 131.5(3) 102.5(3) 67.0(3) 67.4(3) 66.9(3) 66.8(3) 102.9(3) 125.3(3) 132.2(4) 129.5(3) 127.4(3) 69.5(3) 71.4(3) 108.0(4) 109.4(4) 69.3(3) 70.4(3) 110.1(3) 55.5(3) 60.1(3)

248


C(2)-B(22)-B(26) B(29)-B(22)-B(26) B(25)-B(22)-B(26) C(2)-B(22)-B(23) B(29)-B(22)-B(23) B(25)-B(22)-B(23) B(26)-B(22)-B(23) C(2)-B(22)-Br(22) B(29)-B(22)-Br(22) B(25)-B(22)-Br(22) B(26)-B(22)-Br(22) B(23)-B(22)-Br(22) C(2)-B(23)-B(27) C(2)-B(23)-B(26) B(27)-B(23)-B(26) C(2)-B(23)-B(22) B(27)-B(23)-B(22) B(26)-B(23)-B(22) C(2)-B(23)-B(24) B(27)-B(23)-B(24) B(26)-B(23)-B(24) B(22)-B(23)-B(24) C(2)-B(23)-Br(23) B(27)-B(23)-Br(23) B(26)-B(23)-Br(23) B(22)-B(23)-Br(23) B(24)-B(23)-Br(23) C(2)-B(24)-B(27) C(2)-B(24)-B(28) B(27)-B(24)-B(28) C(2)-B(24)-B(25) B(27)-B(24)-B(25) B(28)-B(24)-B(25) C(2)-B(24)-B(23) B(27)-B(24)-B(23) B(28)-B(24)-B(23) B(25)-B(24)-B(23) C(2)-B(24)-Br(24) B(27)-B(24)-Br(24) B(28)-B(24)-Br(24) B(25)-B(24)-Br(24) B(23)-B(24)-Br(24) C(2)-B(25)-B(28) C(2)-B(25)-B(29) B(28)-B(25)-B(29) C(2)-B(25)-B(22) B(28)-B(25)-B(22) B(29)-B(25)-B(22) C(2)-B(25)-B(24) B(28)-B(25)-B(24) B(29)-B(25)-B(24) B(22)-B(25)-B(24) C(2)-B(25)-Br(25) B(28)-B(25)-Br(25) B(29)-B(25)-Br(25) B(22)-B(25)-Br(25)

107.3(3) 61-5(3) 100.9(3) 54.8(3) 103.0(3) 89.5(3) 58.4(3) 120.4(3) 121.5(3) 132.5(3) 121.8(3) 129.0(3) 108.4(4) 108.4(3) 61.2(3) 53.9(3) 102.6(3) 60.4(3) 55.4(3) 58.9(3) 101.9(3) 89.6(3) 118.0(3) 123.7(3) 124.2(3) 129.7(3) 129.0(3) 107.3(4) 106.9(3) 61.5(3) 54.5(3) 101.6(3) 58.5(3) 54.2(3) 59.0(3) 101.1(3) 88.8(3) 120.1(3) 122.8(3) 124.1(3) 131.0(3) 129.9(3) 110.1(4) 109.2(4) 62.6(3) 55.0(3) 103.6(3) 59-5(3) 56.2(3) 60.3(3) 104.9(3) 92.0(3) 118.3(3) 122.9(3) 121.4(3) 128.0(3)

B(24)-B(25>Br(25) B(30)-B(26)-B(23) B(30)-B(26)-B(27) B(23)-B(26)-B(27) B(30)-B(26)-B(22) B(23)-B(26)-B(22) B(27)-B(26)-B(22) B(30)-B(26)-B(29) B(23)-B(26)-B(29) B(27)-B(26>B(29) B(22)-B(26)-B(29) B(30)-B(26)-Br(26) B(23)-B(26)-Br(26) B(27)-B(26)-Br(26) B(22)-B(26)-Br(26) B(29)-B(26)-Br(26) B(30)-B(27)-B(23) B(30)-B(27)-B(24) B(23)-B(27)-B(24) B(30)-B(27)-B(26) B(23)-B(27)-B(26) B(24)-B(27)-B(26) B(30)-B(27)-B(28) B(23)-B(27)-B(28) B(24)-B(27)-B(28) B(26)-B(27)-B(28) B(30)-B(27)-Br(27) B(23)-B(27)-Br(27) B(24)-B(27)-Br(27) B(26)-B(27)-Br(27) B(28)-B(27)-Br(27) B(30)-B(28)-B(25) B(30)-B(28)-B(24) B(25)-B(28)-B(24) B(30)-B(28)-B(27) B(25)-B(28)-B(27) B(24)-B(28)-B(27) B(30)-B(28)-B(29) B(25)-B(28)-B(29) B(24)-B(28)-B(29) B(27)-B(28)-B(29) B(30)-B(28)-Br(28) B(25)-B(28)-Br(28) B(24)-B(28)-Br(28) B(27)-B(28)-Br(28) B(29)-B(28)-Br(28) B(30)-B(29)-B(22) B(30)-B(29)-B(25) B(22)-B(29)-B(25) B(30)-B(29)-B(28) B(22)-B(29)-B(28) B(25)-B(29)-B(28) B(30)-B(29)-B(26) B(22)-B(29)-B(26) B(25)-B(29)-B(26) B(28)-B(29)-B(26)

129.1(3) 111.2(3) 56.7(3) 59.3(3) 110.9(4) 61.2(3) 101.9(3) 58.5(3) 102.6(3) 91.9(3) 58.0(3) 122.6(3) 119.0(3) 134.8(3) 116.2(3) 128.1(3) 110.9(3) 111.2(4) 62.2(3) 56.2(3) 59.5(3) 103.0(3) 55.9(3) 102.0(3) 59.6(3) 88.9(3) 119.8(3) 120.8(3) 118.7(3) 132.5(3) 130.6(3) 112.0(3) 110.9(4) 61.2(3) 56.4(3) 101.6(3) 58.8(3) 58.5(3) 59.3(3) 103.2(3) 91.4(3) 119.8(3) 120.4(3) 118.7(3) 130.4(3) 131.4(3) 109.9(3) 107.6(3) 60.4(3) 54.8(3) 101.0(3) 58.1(3) 54.8(3) 60.6(3) 100.5(3) 87.8(3)

249


B(30)-B(29)-Br(29) B(22)-B(29)-Br(29) B(25)-B(29)-Br(29) B(28)-B(29)-Br(29) B(26)-B(29)-Br(29) B(28)-B(30)-B(26) B(28)-B(30)-B(27) B(26)-B(30)-B(27) B(28)-B(30)-B(29) B(26)-B(30)-B(29) B(27)-B(30)-B(29) B(28)-B(30)-Br(30) B(26)-B(30)-Br(30) B(27)-B(30)-Br(30) B(29)-B(30)-Br(30)

119.0(3) 122.5(3) 123.6(3) 130.9(3) 131.4(3) 102.4(4) 67.7(3) 67.1(3) 66.7(3) 66.6(3) 102.9(4) 128.7(3) 128.9(3) 128.5(3) 128.5(3)

250


Compound V -ll A tom ic coordinates and thermal parameters.

A g(l) C(l) C(2) C( 3) C(4) C(5) C(6) C( 7) Br(2) Br(3) Br(4) Br(5) Br(6) Br(7) Br(8) Br(9) Br(10) B(2) B(3) B(4) B(5) B(6) B(7) B(8)

B(9) B(10)

X -4252(1) -5265(4) -5581(6) -5740(6) -5111(5) -4266(6) -4037(6) -4706(5) -3739(1) -6843(1) -6892(1) -3746(1) -6115(1) -8495(1) -6272(1) -3989(1) -6948(1) -4879(4) -6224(4) -6198(5) -4881(5) -6016(4) -6964(5) -6017(5) -5103(5) -6366(5)

y

6639(1) 10056(4) 4618(5) 5600(6) 5970(5) 5362(5) 4425(5) 4029(6) 8186(1) 8640(1) 11816(1) 11363(1) 6924(1) 9600(1) 11510(1) 8798(1) 8594(1) 9006(4) 9224(5) 10568(5) 10380(4) 8446(4) 9536(4) 10377(5) 9277(5) 9117(4)

z 12365(1) 9885(4) 12850(6) 13224(4) 13903(5) 14202(6) 13765(5) 13113(5) 10006(1) 8902(1) 9962(1) 11061(1) 11035(1) 10946(1) 12507(1) 12519(1) 13087(1) 10460(3) 9955(4) 10444(4) 10914(4) 11020(5) 11028(4) 11676(4) 11677(4) 11959(4)

U(eq) 79(1) 48(1) 132(4) 112(3) 115(3) 137(4) 129(3) 125(4) 65(1) 59(1) 70(1) 81(1) 57(1) 64(1) 80(1) 59(1) 68(1) 37(1) 44(2) 46(2) 47(2) 49(2) 51(2) 48(2) 47(2) 45(2)

Bond lengths Ag(l)-C(3) Ag(l)-C(4) Ag(l)-Br(9) Ag(l)-Br(7)#l C(l)-B(4) C(l)-B(3) C(l)-B(5) C(l)-B(2) C(2)-C(3) C(2)-C(7) C(3)-C(4) C(4)-C(5) C(5)-C(6) C(6)-C(7) Br(2)-B(2) Br(3)-B(3) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6) Br(7)-B(7) Br(7)-Ag(l)#2

Br(8)-B(8) Br(9)-B(9) Br(10)-B(10) B(2)-B(6) B(2)-B(9) B(2)-B(5) B(2)-B(3) B(3)-B(4) B(3)-B(6) B(3)-B(7) B(4)-B(5) B(4)-B(8) B(4)-B(7) B(5)-B(9) B(5)-B(8) B(6)-B(10) B(6)-B(7) B(6)-B(9) B(7)-B( 10) B(7)-B(8) B(8)-B(10) B(8)-B(9)

2.628(8) 2.643(7) 2.7774(9) 2.7790(9) 1.583(8) 1.618(8) 1.637(8) 1.654(7) 1.379(9) 1.396(9) 1.359(9) 1.396(9) 1.385(9) 1.374(9) 1.906(5) 1.883(6) 1.948(6) 1.922(6) 1.942(5) 1.952(6) 2.7790(9)

1.915(6) 1.975(6) 1.929(6) 1.808(8) 1.836(7) 1.871(8) 1.884(7) 1.855(8) 1.866(9) 1.874(9) 1.827(9) 1.834(8) 1.845(8) 1.815(8) 1.824(9) 1.678(9) 1.838(8) 1.841(9) 1.650(9) 1.870(9) 1.714(8) 1.819(9)

251


B(9)-B (10)

1.670(9)

Bond angles

C(3)-Ag(l)-C(4) C(3)-Ag(l)-Br(9) C(4)-Ag(l)-Br(9) C(3)-Ag( 1)-Br(7)# 1 C(4)-Ag(l)-Br(7)#l Br(9)-Ag(l)-Br(7)#l B(4)-C(l)-B(3) B(4)-C(l)-B(5) B(3)-C(l)-B(5) B(4)-C(l)-B(2) B(3)-C(l)-B(2) B(5)-C(l)-B(2) C(3)-C(2)-C(7) C(4)-C(3)-C(2) C(4)-C(3)-Ag(l) C(2)-C(3)-Ag(l) C(3)-C(4)-C(5) C(3)-C(4)-Ag(l) C(5)-C(4)-Ag(l) C(6)-C(5)-C(4) C(7)-C(6)-C(5) C(6)-C(7)-C(2) B(7)-Br(7)-Ag(l)#2 B(9)-Br(9)-Ag(l) C(l)-B(2)-B(6) C(l)-B(2)-B(9) B(6)-B(2)-B(9) C(l)-B(2)-B(5) B(6)-B(2)-B(5) B(9)-B(2)-B(5) C(l)-B(2)-B(3) B(6)-B(2)-B(3) B(9)-B(2)-B(3) B(5)-B(2)-B(3) C(l)-B(2)-Br(2) B(6)-B(2)-Br(2) B(9)-B(2)-Br(2) B(5)-B(2)-Br(2) B(3)-B(2)-Br(2) C(l)-B(3)-B(4) C(l)-B(3)-B(6) B(4)-B(3)-B(6) C(l)-B(3)-B(7) B(4)-B(3)-B(7) B(6)-B(3)-B(7) C(l)-B(3)-B(2) B(4)-B(3)-B(2) B(6)-B(3)-B(2) B(7)-B(3)-B(2) C(l)-B(3)-Br(3) B(4)-B(3)-Br(3) B(6)-B(3)-Br(3)

B(7)-B(3)-Br(3) B(2)-B(3)-Br(3) C(l)-B(4)-B(5) C(l)-B(4)-B(8) B(5)-B(4)-B(8) C(l)-B(4)-B(7) B(5)-B(4)-B(7) B(8)-B(4)-B(7) C(l)-B(4)-B(3) B(5)-B(4)-B(3) B(8)-B(4)-B(3) B(7)-B(4)-B(3) C(l)-B(4)-Br(4) B(5)-B(4)-Br(4) B(8)-B(4)-Br(4) B(7)-B(4)-Br(4) B(3)-B(4)-Br(4) C(l)-B(5)-B(9) C(l)-B(5)-B(4) B(9)-B(5)-B(4) C(l)-B(5)-B(8) B(9)-B(5)-B(8) B(4)-B(5)-B(8) C(l)-B(5)-B(2) B(9)-B(5)-B(2) B(4)-B(5)-B(2) B(8)-B(5)-B(2) C(l)-B(5)-Br(5) B(9)-B(5)-Br(5) B(4)-B(5)-Br(5) B(8)-B(S)-Br(5) B(2)-B(5)-Br(5) B(10)-B(6)-B(2) B(10)-B(6)-B(7) B(2)-B(6)-B(7) B(10)-B(6)-B(9) B(2)-B(6)-B(9) B(7)-B(6)-B(9) B(10)-B(6)-B(3) B(2)-B(6)-BO) B(7)-B(6)-B(3) B(9)-B(6)-B(3) B(10)-B(6)-Br(6) B(2)-B(6)-Br(6) B(7)-B(6)-Br(6) B(9)-B(6)-Br(6) B(3)-B(6)-Br(6) B(10)-B(7)-B(6) B(10)-B(7)-B(4) B(6)-B(7)-B(4) B(10)-B(7)-B(3) B(6)-B(7)-B(3)

29.87(19) 123.06(16) 107.40(15) 108.76(15) 126.65(15) 125.47(3) 70.8(4) 69.1(4) 109.3(4) 107.0(4) 70.3(3) 69.3(3) 119.5(7) 121.2(7) 75.7(4) 99.2(5) 119.4(7) 74.5(4) 97.3(5) 119.6(7) 120.5(7) 119.3(7) 106.04(18) 99.67(17) 108.2(4) 107.2(4) 60.7(3) 54.9(3) 101.9(4) 58.6(3) 54.0(3) 60.7(3) 102.2(4) 90.0(4) 119.4(3) 123.4(3) 124.0(3) 129.6(3) 129.3(3) 53.7(3) 107.0(4) 99.4(4) 107.0(4) 59.3(3) 58.9(3) 55.7(3) 88.2(4) 57.7(3) 99.1(4) 121.4(4) 133.4(4) 122.3(4)

124.0(3) 130.0(4) 56.9(3) 111.1(4) 59.8(3) 110.0(4) 102.5(4) 61.1(3) 55.5(3) 92.3(4) 105.0(4) 60.9(3) 119.2(4) 131.2(4) 121.4(4) 120.6(4) 127.1(4) 108.9(4) 54.0(3) 101.0(4) 109.0(4) 60.0(3) 60.3(3) 55.8(3) 59.7(3) 89.4(4) 102.5(4) 119.4(4) 123.5(4) 130.2(4) 121.9(4) 130.3(4) 112.5(4) 55.7(3) 103.3(4) 56.4(4) 60.4(3) 88.7(4) 112.1(4) 61.7(3) 60.8(3) 102.8(4) 118.8(4) 116.7(3) 135.3(3) 127.5(4) 122.0(4) 57.2(4) 111.7(4) 100.8(4) 113.1(4) 60.3(3)

252


B(4)-B(7)-B(3) B(10)-B(7)-B(8) B(6)-B(7)-B(8) B(4)-B(7)-B(8) B(3)-B(7)-B(8) B(10)-B(7)-Br(7) B(6)-B(7)-Br(7) B(4)-B(7)-Br(7) B(3)-B(7)-Br(7) B(8)-B(7)-Br(7) B(10)-B(8)-B(9) B(10)-B(8)-B(5) B(9)-B(8)-B(5) B(10)-B(8)-B(4) B(9)-B(8)-B(4) B(5)-B(8)-B(4) B(10)-B(8)-B(7) B(9)-B(8)-B(7) B(5)-B(8)-B(7) B(4)-B(8)-B(7) B(10)-B(8)-Br(8) B(9)-B(8)-Br(8) B(5)-B(8)-Br(8) B(4)-B(8)-Br(8) B(7)-B(8)-Br(8) B(10)-B(9)-B(5) B(10)-B(9)-B(8) B(5)-B(9)-B(8) B(10)-B(9)-B(2) B(5)-B(9)-B(2) B(8)-B(9)-B(2) B(10)-B(9)-B(6) B(5)-B(9)-B(6) B(8)-B(9)-B(6) B(2)-B(9)-B(6) B(10)-B(9)-Br(9) B(5)-B(9)-Br(9) B(8)-B(9)-Br(9) B(2)-B(9)-Br(9) B(6)-B(9)-Br(9) B(7)-B(10)-B(9) B(7)-B(10)-B(6) B(9)-B(10)-B(6) B(7)-B(10)-B(8) B(9)-B(10)-B(8) B(6)-B(10)-B(8) B(7)-B(10)-Br(10) B(9)-B(10)-Br(10) B(6)-B( 10)-Br( 10) B(8)-B(10)-Br(10)

59.8(3) 57.9(3) 90.7(4) 59.2(3) 102.9(4) 121.6(4) 133.2(3) 117.9(4) 117.3(4) 130.5(4) 56.3(3) 110.8(4) 59.8(3) 109.2(4) 100.6(4) 59.9(3) 54.6(3) 88.4(4) 101.6(4) 59.7(3) 120.4(4) 133.4(4) 121.4(4) 120.2(4) 130.1(4) 113.3(4) 58.7(3) 60.2(3) 111.5(4) 61.6(3) 104.1(4) 56.9(3) 102.8(4) 92.2(4) 58.9(3) 119.8(4) 120.7(4) 134.1(4) 115.9(4) 126.9(4) 101.5(4) 67.0(4) 66.7(3) 67.5(4) 65.0(4) 102.1(4) 129.9(4) 128.5(4) 128.8(4) 129.0(4)


Compound V-12 A tom ic coordinates and thermal parameters. X

N (l) C!(2) Cl(3) Cl(4) Cl(5) CI(6) Cl (7) Cl(8) Cl(9) CI(10) C (l) C(2) C(3) C(4) C( 5) C(6) C(7) C(8) C(9) C(10) QH) C(12) C(13) C(14) C(15) C(16) C( 17) C(18) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10)

y 12575(2) 4884(1) 7046(1) 9506(1) 7346(1) 5457(1) 8805(1) 9064(1) 5718(1) 7285(1) 7200(3) 7185(3) 7058(3) 6076(4) 5960(4) 6823(5) 7806(4) 7933(3) 13464(3) 11564(3) 12755(3) 12556(3) 11638(3) 10733(3) 9887(3) 9934(3) 10813(4) 11670(3) 6189(3) 7147(3) 8244(3) 7284(3) 6455(3) 7926(3) 8034(3) 6571(3) 7264(3)

2066(3) 1629(1) 4591(1) 776(1) -2072(1) 4399(1) 3843(1) -896(1) -438(1) 2185(1) 1181(4) 679(4) 1887(4) 2607(5) 3636(6) 3947(7) 3241(6) 2205(5) 2030(6) 2147(5) 617(4) 3470(4) 3786(4) 4851(4) 5126(5) 4359(5) 3353(5) 3081(4) 1534(5) 2835(4) 1177(5) -121(5) 2789(5) 2540(5) 459(5) 694(5) 1823(5)

z

U(eq)

6250(2) 8682(1) 8091(1) 8211(1) 8741(1) 6284(1) 5898(1) 6301(1) 6734(1) 4618(1) 8620(2) 9783(2) 10343(3) 10674(3) 11258(4) 11517(4) 11202(4) 10620(3) 5397(3) 5867(3) 7097(3) 6617(3) 7412(3) 7120(3) 7839(3) 8850(3) 9159(3) 8447(3) 8017(3) 7787(3) 7794(3) 8035(3) 6761(3) 6591(3) 6757(3) 6929(3) 5959(3)

55(1) 65(1) 60(1) 63(1) 6 6 (1 )

69(1) 65(1) 77(1) 74(1) 78(1) 43(1) 53(1) 53(1) 78(1) 104(2) 102(2) 91(2) 6 8 (1 )

92(2) 76(1) 76(1) 61(1) 53(1) 63(1) 69(1) 69(1) 6 6 (1 )

62(1) 49(1) 44(1) 45(1) 47(1) 49(1) 47(1) 50(1) 53(1) 54(1)

Bond lengths

N(l)-C(10) N(l)-C(9) N (l)-C (l 1) N(l)-C(12) CI(2)-B(2) Cl(3)-B(3) Cl(4)-B(4) CI(5)-B(5) Cl(6)-B(6) Cl(7)-B(7)

Cl(8)-B(8) Cl(9)-B(9) Cl(10)-B(10) C(l)-C(2) C(l)-B(4) C(l)-B(3) C(l)-B(5) C(l)-B(2) C(2)-C(3) C(3)-C(4) C(3)-C(8)

1.489(5) 1.493(4) 1.497(5) 1.519(4) 1.773(4) 1.763(4) 1.770(4) 1.765(4) 1.791(4) 1.787(4)

1.779(4) 1.789(4) 1.778(4) 1.531(4) 1.605(5) 1.610(5) 1.610(5) 1.611(5) 1.501(5) 1.368(5) 1.384(5)

254


C(4)-C(5) C(5)-C(6) C(6)-C(7) C(7)-C(8) C(12)-C(13) C(13)-C(18) C(13)-C(14) C(14)-C(15) C(15)-C(16) C(16)-C(17) C(17)-C(18) B(2)-B(6) B(2)-B(9) B(2)-B(5) B(2)-B(3) B(3)-B(7)

1.386(6) 1.355(7) 1.357(7) 1.388(6) 1.506(5) 1.387(5) 1.394(5) 1.372(5) 1.370(5) 1.352(5) 1.374(5) 1.795(6) 1.830(6) 1.839(6) 1.844(5) 1.831(6)

B(3)-B(6) B(3)-B(4) B(4)-B(7) B(4)-B(8) B(4)-B(5) B(5)-B(9) B(5)-B(8) B(6)-B(10) B(6)-B(9) B(6)-B(7) B(7)-B(10) B(7)-B(8) B(8)-B(10) B(8)-B(9) B(9)-B(10)

1.833(6) 1.845(6) 1.815(6) 1.833(6) 1.841(6) 1.817(6) 1.839(6) 1.693(6) 1.852(6) 1.859(5) 1.682(6) 1.839(6) 1.682(6) 1.849(6) 1.682(6)

Bond angles C(10)-N(l)-C(9) C (10)-N(l)-C(ll) C (9)-N (l)-C (ll) C(10)-N(l)-C(12) C(9)-N(l)-C(12) C (ll)-N(l)-C (12) C(2)-C(l)-B(4) C(2)-C(l)-B(3) B(4)-C(l)-B(3) C(2)-C(l)-B(5) B(4)-C(l)-B(5) B(3)-C(l)-B(5) C(2)-C(l)-B(2) B(4)-C(l)-B(2) B(3)-C(l)-B(2) B(5)-C(l)-B(2) C(3)-C(2)-C(l) C(4)-C(3)-C(8) C(4)-C(3)-C(2) C(8)-C(3)-C(2) C(3)-C(4)-C(5) C(6)-C(5)-C(4) C(5)-C(6)-C(7) C(6)-C(7)-C(8) C(3)-C(8)-C(7) C(13)-C(12)-N(l) C(18)-C(13)-C(14) C( 18)-C( 13)-C( 12) C(14)-C(13)-C(12) C(15)-C(14)-C(13) C(16)-C(15)-C(14) C(17)-C(16)-C(15) C(16)-C(17)-C(18) C(17)-C(18)-C(13) C(1)-B(2)-C1(2) C(l)-B(2)-B(6) Cl(2)-B(2)-B(6)

C(l)-B(2)-B(9) Cl(2)-B(2)-B(9) B(6)-B(2)-B(9) C(l)-B(2)-B(5) CI(2)-B(2)-B(5) B(6)-B(2)-B(5) B(9)-B(2)-B(5) C(1)-B(2>B(3) CI(2)-B(2)-B(3) B(6)-B(2)-B(3) B(9)-B(2)-B(3) B(5)-B(2)-B(3) C(1)-B(3)-C1(3) C(l)-B(3)-B(7) Cl(3)-B(3)-B(7) C(l)-B(3)-B(6) Cl(3)-B(3)-B(6) B(7)-B(3)-B(6) C(l)-B(3)-B(2) Cl(3)-B(3)-B(2) B(7)-B(3)-B(2) B(6)-B(3)-B(2) C(l)-B(3)-B(4) Cl(3)-B(3)-B(4) B(7)-B(3)-B(4) B(6)-B(3)-B(4) B(2)-B(3)-B(4) C(1)-B(4)-C1(4) C(l)-B(4)-B(7) Cl(4)-B(4)-B(7) C(l)-B(4)-B(8) CI(4)-B(4)-B(8) B(7)-B(4)-B(8) C(l)-B(4)-B(5) Cl(4)-B(4)-B(5) B(7)-B(4)-B(5) B(8)-B(4)-B(5)

109.0(3) 108.5(3) 109.6(3) 111.8(3) 107.3(3) 110.6(3) 125.5(3) 132.9(3) 70.1(2) 118.5(3) 69.9(2) 108.5(3) 126.1(3) 107.7(3) 69.9(2) 69.6(2) 119.1(3) 117.8(4) 121.3(4) 120.6(4) 121.2(4) 120.4(5) 119.5(5) 120.6(5) 120.4(4) 115.0(3) 117.9(4) 122.1(4) 120.0(3) 120.3(4) 119.8(4) 121.2(4) 119.5(4) 121.2(4) 120.8(3) 109.5(3) 120.8(3)

108.8(3) 121.1(3) 61.4(2) 55.2(2) 130.4(3) 102.8(3) 59.4(2) 55.0(2) 130.2(3) 60.5(2) 103.1(3) 90.4(3) 124.0(3) 108.0(3) 119.8(2) 107.8(3) 119.6(3) 61.0(2) 55.1(2) 131.9(3) 101.0(3) 58.4(2) 54.8(2) 131.9(3) 59.2(2) 101.6(3) 89.5(2) 119.3(3) 109.0(3) 123.4(3) 109.5(3) 121.2(3) 60.6(2) 55.2(2) 128.7(3) 102.0(3) 60.1(2)

255


C(l)-B(4)-B(3) Cl(4)-B(4)-B(3) B(7)-B(4)-B(3) B(8)-B(4)-B(3) B(5)-B(4)-B(3) C(1)-B(5)-CI(5) C(l)-B(5)-B(9) Cl(5)-B(5)-B(9) C(l)-B(5)-B(8) Cl(5)-B(5)-B(8) B(9)-B(5)-Bf8) C(l)-B(5)-B(2) Cl(5)-B(5)-B(2) B(9)-B(5)-B(2) B(8)-B(5)-B(2) C(l)-B(5)-B{4) Cl(5)-B(5)-B(4) B(9)-B(5)-B(4) B(8)-B(5)-B(4) B(2)-B(5)-B(4) B(10)-B(6)-C1(6) B(10)-B(6)-B(2) CI(6)-B(6)-B(2) B(10)-B(6)-B(3) Cl(6)-B(6)-B(3) B(2)-B(6)-B(3) B(10)-B(6)-B(9) Cl(6)-B(6)-B(9) B(2)-B(6)-B(9) B(3)-B(6)-B(9) B(10)-B(6)-B(7) Cl(6)-B(6)-B(7) B(2)-B(6)-B(7) B(3)-B(6)-B(7) B(9)-B(6)-B(7) B(10)-B(7)-C1(7) B(10)-B(7)-B(4) Cl(7)-B(7)-B(4) B(10)-B(7)-B(3) Ci(7)-B(7)-B(3) B(4)-B(7)-B(3) B(10)-B(7)-B(8) Cl(7)-B(7)-B(8) B(4)-B(7)-B(8) B(3)-B(7)-B(8) B(10)-B(7)-B(6) Cl(7)-B(7)-B(6) B(4)-B(7)-B(6) B(3)-B(7)-B(6) B(8)-B(7)-B(6) B(10)-B(8)-CI(8) B(10)-B(8)-B(4) CI(8)-B(8)-B(4) B(10)-B(8)-B(5) Cl(8)-B(8)-B(5) B(4)-B(8)-B(5)

55.1(2) 130.9(3) 60.0(2) 102.9(3) 90.3(2) 119.8(3) 109.5(3) 121.6(3) 108.9(3) 122.3(3) 60.8(2) 55.2(2) 130.0(3) 60.1(2) 102.1(3) 54.9(2) 130.5(3) 102.4(3) 59.8(2) 89.8(2) 120.3(3) 111.7(3) 119.3(3) 111.3(3) 119.1(3) 61.1(2) 56.5(2) 131.5(3) 60.2(2) 102.7(3) 56.3(2) 137.8(3) 101.8(3) 59-5(2) 89.4(3) 120.2(3) 111.8(3) 119.5(3) 111.9(3) 118.6(3) 60.8(2) 56.9(2) 131.2(3) 60.2(2) 103.2(3) 56.9(2) 131.3(3) 101.8(3) 59.6(2) 90.4(3) 121.2(3) 110.9(3) 118.8(3) 110.5(3) 120.1(3) 60.2(2)

B(10)-B(8)-B(7) C!(8)-B(8)-B(7) B(4)-B(8)-B(7) B(5)-B(8)-B(7) B(10)-B(8)-B(9) Cl(8)-B(8)-B(9) B(4)-B(8)-B(9) B(5)-B(8>B(9) B(7)-B(8)-B(9) B(10)-B(9)-C1(9) B(10)-B(9)-B(5) Cl(9)-B(9)-B(5) B(10)-B(9)-B(2) Cl(9)-B(9)-B(2) B(5)-B(9)-B(2) B(10)-B(9)-B(8) CI(9)-B(9)-B(8) B(5)-B(9)-B(8) B(2)-B(9)-B(8) B(10)-B(9)-B(6) Cl(9)-B(9)-B(6) B(5)-B(9)-B(6) B(2)-B(9)-B(6) B(8)-B(9)-B(6) B(7)-B( 10)-B(8) B(7)-B(10)-B(9) B(8)-B(10)-B(9) B(7)-B(10)-B(6) B(8)-B( 10)-B(6) B(9)-B(10)-B(6) B(7)-B(10)-C1(10) B(8)-B( 10)-CI( 10) B(9)-B( 10)-C1( 10) B(6)-B( 10)-C1( 10)

56.8(2) 130.9(3) 59.2(2) 101.2(3) 56.7(2) 132.6(3) 101.5(3) 59.0(2) 90.0(3) 122.9(3) 111.6(3) 117.0(3) 110.5(3) 118.4(3) 60.6(2) 56.6(2) 131.3(3) 60.2(2) 102.1(3) 57.0(2) 133.1(3) 101.4(3) 58.4(2) 90.3(3) 66.3(3) 101.7(3) 66.7(3) 66.8(3) 102.0(3) 66.5(3) 128.9(3) 129.6(3) 129.4(3) 128.4(3)


Chapter 6 Compound VI-4 A tom ic coordinates and thermal parameters.

X

1(8) 1(9) 1(10) 1(11) 1(12) C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12) C(2) C(3) C(4) C(5) C(6) C(7) C(10) N (l) C(8) C(9) C( ll )

5842(1) 4503(1) 3987(3) 4834(1) 6356(1) 3117(8) 3817(9) 4052(9) 3659(8) 3109(8) 3227(9) 4937(8) 4834(7) 4249(8) 3987(9) 4388(9) 5027(9) 3545(11) 4070(12) 3239(9) 2229(9) 2378(9) 5914(6) 3890(30) 7078(8) 7682(14) 7388(13) 6661(18)

y -3727(1) -4504(1) -2669(4) -594(1) -2645(1) -2358(6) -1561(8) -2393(8) -3270(7) -2961(7) -1885(8) -1934(7) -2992(6) -3350(7) -2514(7) -1647(7) -2538(7) -709(8) -2341(8) -3986(8) -3382(10) -1371(9) -1395(5) -2400(20) -4855(7) -4658(12) -4760(12) -5695(14)

z

U(eq)

5175(1) 6641(1) 7644(2) 6800(1) 6751(1) 5650(5) 5655(6) 5221(5) 5594(6) 6265(6) 6298(7) 5663(5) 5629(5) 6256(5) 6704(6) 6324(6) 6295(6) 5363(7) 4452(8) 5221(6) 6484(6) 6562(7) 5316(4) 7420(20) 6606(4) 6190(8) 7190(8) 6498(10)

92(1) 102(1)

97(2) 98(1) 86(1)

62(3) 65(3) 57(3) 57(3) 60(3) 70(3) 55(3) 50(3) 56(3) 59(3) 60(3) 59(3) 93(4) 106(6) 79(3) 88(4) 89(4) 38(2) 103(14) 77(3) 118(5) 114(5) 140(7)

Bond lengths

I(8)-B(8) I(9)-B(9) I(10)-B(10) K l l ) - B (l l) I(12)-B(12) C(l)-B(2) C(l)-B(4) C(l)-B(5) B(2)-C(2) B (2)-B (ll) B(2)-B(3) B(2)-B(7) B(2)-B(6) B(3)-B(8) B(3)-C(3) B(3)-B(4) B(3)-B(7) B(4)-C(4) B(4)-B(9) B(4)-B(8) B(4)-B(5)

2.183(10) 2.160(12) 2.180(14) 2.176(12) 2.207(13) 1.680(17) 1.725(15) 1.740(17) 1.627(18) 1.756(19) 1.750(18) 1.746(17) 1.80(2) 1.785(16) 1.77(2) 1.797(18) 1.812(16) 1.597(16) 1.755(18) 1.773(15) 1.816(18)

B(5)-C(5) B(S)-B(9) B(5)-B(10) B(5)-B(6) B(6)-C(6) B (6)-B(ll) B(6)-B(10) B(7)-B(12) B(7)-B(8) B (7)-B(ll) B(7)-C(7) B(8)-B(12) B(8)-B(9) B(9)-B(12) B(9)-B(10) B(10)-C(10) B(10)-B(12) B(10)-B(ll) B(11)-B(12) N(l)-C(8) N(l)-C(9)

1.547(18) 1.782(16) 1.792(17) 1.815(19) 1.623(17) 1.738(18) 1.79(2) 1.779(18) 1.782(17) 1.786(17) 1.863(14) 1.735(16) 1.779(16) 1.773(17) 1.782(18) 1.67(5) 1.783(19) 1.795(17) 1.762(17) 1.34(2) 1.43(2)


N ( l) - C ( ll)

1.55(3)

Bond angles B(2)-C(l)-B(4) B(2)-C(l)-B(5) B(4)-C(l)-B(5) C(2)-B(2)-C(l) C(2)-B(2)-B(l 1) C(l)-B(2)-B(l 1) C(2)-B(2)-B(3) C(l)-B(2)-B(3) B(11)-B(2)-B(3) C(2)-B(2)-B(7) C(l)-B(2)-B(7) B(ll)-B(2)-B(7) B(3)-B(2)-B(7) C(2)-B(2)-B(6) C(l)-B(2)-B(6) B(11)-B(2)-B(6) B(3)-B(2)-B(6) B(7)-B(2)-B(6) B(2)-B(3)-B(8) B(2)-B(3)-C(3) B(8)-B(3)-C(3) B(2)-B(3)-B(4) B(8)-B(3)-B(4) C(3)-B(3)-B(4) B(2)-B(3)-B(7) B(8)-B(3)-B(7) C(3)-B(3)-B(7) B(4)-B(3)-B(7) C(4)-B(4)-C(l) C(4)-B(4)-B(9) C(l)-B(4)-B(9) C(4)-B(4)-B(8) C(l)-B(4)-B(8) B(9)-B(4)-B(8) C(4)-B(4)-B(3) C(l)-B(4)-B(3) B(9)-B(4)-B(3) B(8)-B(4)-B(3) C(4)-B(4)-B(5) C(l)-B(4)-B(5) B(9)-B(4)-B(5) B(8)-B(4)-B(5) B(3)-B(4)-B(5) C(5)-B(5)-C(l) C(5)-B(5)-B(9) C(l)-B(5)-B(9) C(5)-B(5)-B(10) C(l)-B(5)-B(10) B(9)-B(5)-B(10) C(5)-B(5)-B(6) C(l)-B(5)-B(6) B(9)-B(5)-B(6) B(10)-B(5)-B(6) C(5)-B(5)-B(4) C(l)-B(5)-B(4) B(9)-B(5)-B(4)

115.4(9) 117.5(8) 63.2(7) 123.2(11) 123.3(11) 103.1(9) 120.8(11) 58.7(7) 110.1(9) 123.1(11) 106.3(9) 61.3(7) 62.5(7) 119.3(11) 58.4(8) 58.5(8) 108.9(9) 109.3(9) 105.8(8) 122.3(9) 123.0(10) 108.5(9) 59.3(6) 121.5(9) 58.7(7) 59.4(7) 121.9(9) 107.8(8) 122.1(9) 126.6(10) 103.1(8) 126.2(10) 101.8(8) 60.6(6) 118.7(10) 57.0(7) 108.8(8) 60.0(7) 120.2(10) 58.8(7) 59.9(7) 108.1(8) 108.3(9) 122.4(10) 127.4(11) 101.3(8) 126.7(11) 102.2(8) 59.8(7) 121.2(10) 57.0(7) 106.1(8) 59.6(7) 120.8(10) 58.0(7) 58.4(7)

B(10)-B(5)-B(4) B(6)-B(5)-B(4) C(6)-B(6)-B(ll) C(6)-B(6)-B( 10) B( 11)-B(6)-B(10) C(6)-B(6)-B(2) B( 11)-B(6)-B(2) B(10)-B(6)-B(2) C(6)-B(6)-B(5) B(ll)-B(6)-B(5) B(10)-B(6)-B(5) B(2)-B(6>B(5) B(2)-B(7)-B( 12) B(2)-B(7)-B(8) B(12)-B(7)-B(8) B(2)-B(7)-B(ll) B(12)-B(7)-B(ll) B(8)-B(7)-B(ll) B(2)-B(7)-B(3) B(12)-B(7)-B(3) B(8)-B(7)-B(3) B(ll)-B(7)-B(3) B(2)-B(7)-C(7) B(12)-B(7)-C(7) B(8)-B(7)-C(7) B(ll)-B(7)-C(7) B(3)-B(7)-C(7) B(12)-B(8)-B(3) B(12)-B(8)-B(7) B(3)*B(8)-B(7) B(12)-B(8)-B(4) B(3)-B(8)-B(4) B(7)-B(8)-B(4) B( 12)-B(8)-B(9) B(3)-B(8)-B(9) B(7)-B(8)-B(9) B(4)-B(8)-B(9) B(12)-B(8)-I(8) B(3)-B(8)-I(8) B(7)-B(8)-I(8) B(4)-B(8)-I(8) B(9)-B(8)-I(8) B(4)-B(9)-B(12) B(4)-B(9)-B(8) B(12)-B(9)-B(8) B(4)-B(9)-B(5) B(12)-B(9)-B(5) B(8)-B(9)-B(5) B(4)-B(9)-B(10) B(12)-B(9)-B(10) B(8)-B(9)-B( 10) B(5)-B(9)-B(10) B(4)-B(9)-I(9) B(12)-B(9)-I(9) B(8)-B(9)-I(9) B(5)-B(9)-I(9)

106.6(8) 106.1(9) 127.2(10) 126.0(12) 61.1(7) 120.8(12) 59.6(8) 108.2(9) 118.2(10) 108.7(9) 59.6(7) 108.1(9) 106.3(9) 106.1(8) 58.3(6) 59.6(7) 59.2(7) 105.5(8) 58.9(7) 105.7(8) 59.5(6) 106.0(8) 122.2(9) 124.8(8) 122.0(8) 125.1(8) 120.5(8) 108.8(8) 60.8(7) 61.1(6) 108.2(8) 60.7(7) 110.2(7) 60.6(7) 108.2(8) 110.0(8) 59.2(7) 124.2(7) 119.6(7) 121.7(6) 118.5(7) 121.3(7) 107.3(9) 60.2(7) 58.5(7) 61.8(7) 108.2(8) 109.3(9) 109.7(9) 60.2(7) 107.8(8) 60.4(7) 120.6(8) 123.9(7) 123.6(7) 118.8(7)

258


B(10)-B(9)-I(9) C( 10)-B( 10)-B( 12) C( 10)-B( 10)-B( 11) B(12)-B(10)-B(l 1) C(10)-B(10)-B(9) B(12)-B(10)-B(9) B(ll)-B(10)-B(9) C(10)-B(10)-B(6) B(12)-B(10)-B(6) B(11)-B(10)-B(6) B(9)-B(10)-B(6) C(10)-B(10)-B(5) B(12)-B(10)-B(5) B(11)-B(10)-B(5) B(9)-B(10)-B(5) B(6)-B(10)-B(5) B(12)-B(10)-I(10) B(11)-B( 10)-I(10) B(9)-B(10)-I(10) B(6)-B(10)-I(10) B(5)-B(10)-I(10) B(6)-B(ll)-B(12) B(6)-B(l 1)-B(2) B(12)-B(ll)-B(2) B(6)-B(l l)-B(lO) B( 12)-B( 11 )-B( 10) B(2)-B(l 1)-B(10) B(6)-B(ll)-B(7)

120.3(8) 126.9(17) 114.8(14) 59.0(7) 132.9(15) 59.7(7) 106.6(9) 113.3(17) 105.2(9) 57.9(7) 107.1(9) 122.8(16) 107.3(9) 107.2(9) 59.8(7) 60.9(8) 121.4(8) 125.5(8) 118.7(8) 126.0(9) 120.7(8) 108.5(9) 61.9(8) 106.6(9) 60.9(7) 60.1(8) 109.8(9) 110.1(9)

B(12)-B(ll)-B(7) B(2)-B(l 1)-B(7) B(10)-B(ll)-B(7) B (6 )-B (ll)-I(ll) B (1 2 )-B (ll)-I(ll) B (2 )-B (ll)-I(ll) B (1 0 )-B (ll)-I(ll) B(7)-B(l 1)-I( 11) B(8)-B(12)-B(ll) B(8)-B( 12)-B(9) B(11)-B(12)-B(9) B(8)-B(12)-B(10) B(ll)-B(12)-B(10) B(9)-B( 12)-B( 10) B(8)-B(12)-B(7) B( 11)-B( 12)-B(7) B(9)-B( 12)-B(7) B(10)-B(12)-B(7) B(8)-B(12)-I(12) B(ll)-B(12)-I(12) B(9)-B(12)-I(12) B(10)-B(12)-I(12) B(7)-B(12)-I(12) I( 10)-C(10)-B( 10) C(8)-N(l)-C(9) C (8)-N (l)-C (ll) a 9 )-N (i)-a ii)

60.2(7) 59.1(7) 110.0(9) 119.6(8) 123.4(8) 121.1(8) 120.6(8) 121.0(7) 108.7(9) 60.9(7) 108.5(9) 109.8(9) 60.9(7) 60.1(7) 60.9(7) 60.6(7) 110.4(9) 110.9(9) 121.8(7) 120.9(7) 121.4(7) 119.7(8) 120.0(8) 130(5) 115.9(15) 111.5(15) 112.0(13)

259


Compound VI-7 A tom ic coordinates and thermal parameters.

C!(l) C(5) C(l) B(6) B(2) B(3) B(4) C(2) C(3) C(4)

X 4227(2) 4227(2) 4642(8) 4642(8) 5265(14) 3460(12) 3517(9) 5536(12) 2086(12) 2177(8)

z 1121(2) 1121(2) 3294(10) 3294(10) 5000 5000 3912(11) 5000 5000 2681(10)

V 1317(1) 1317(1) 559(5) 559(5) 1238(9) 760(9) -411(6) 2395(8) 1448(8) -782(6)

U(eq) 77(1) 77(1) 84(3) 84(3) 86(4) 85(4) 87(3) 122(5) 113(4) 104(3)

Bond lengths Cl(l)-C(5)#l C1(1)-C1(1)#1 CI(1)-C(1) C(l)-B(6)#2 C (l)-C (l)#2 C(l)-B(2) C(l)-B(4) C(l)-B(3) C(l)-B(4)#2 B(2)-C(2) B(2)-B(6)#3 B(2)-C(l)#3 B(2)-B(3)

1.772(4) 1.772(4) 2.040(8) 1.658(14) 1.658(14) 1.731(10) 1.745(10) 1.751(10) 1.768(11) 1.594(15) 1.731(10) 1.731(10) 1.778(18)

B(2)-B(4)#4 B(2)-B(4)#2 B(3)-C(3) B(3)-B(6)#3 B(3)-C(l)#3 B(3)-B(4) B(3)-B(4)#3 B(4)-C(4) B(4)-B(4)#3 B(4)-B(6)#2 B(4)-C(l)#2 B(4)-B(2)#4

1.805(14) 1.805(14) 1.569(14) 1.751(10) 1.751(10) 1.812(13) 1.812(13) 1.646(10) 1.720(17) 1.768(11) 1.768(11) 1.805(14)

0.00(13) 147.4(2) 147.4(2) 0.0(6) 111.1(6) 111.1(6) 62.6(5) 62.6(5) 112.4(6) 112.9(5) 112.9(5) 61.4(6) 62.4(5) 61.1(5) 61.1(5) 62.1(6) 113.6(5) 113.3(6) 122.6(2) 122.6(2) 116.5(5) 120.5(5) 117.0(5) 117.9(5) 125.4(5) 125.4(5)

C(l)-B(2)-B(6)#3 C(2)-B(2)-C( 1)#3 C( 1)-B(2)-C( 1)#3 B(6)#3-B(2)-C(l)#3 C(2)-B(2)-B(3) C(l)-B(2)-B(3) B(6)#3-B(2)-B(3) C(l)#3-B(2)-B(3) C(2)-B(2)-B(4)#4 C(l)-B(2)-B(4)#4 B(6)#3-B(2)-B(4)#4 C( 1)#3-B(2)-B(4)#4 B(3)-B(2)-B(4)#4 C(2)-B(2)-B(4)#2 C(l)-B(2)-B(4)#2 B(6)#3-B(2)-B(4)#2 C( 1)#3-B(2)-B(4)#2 B(3)-B(2)-B(4)#2 B(4)#4-B(2)-B(4)#2 C(3)-B(3)-B(6)#3 C(3)-B(3)-C( 1)#3 B(6)#3-B(3)-C(l)#3 C(3)-B(3)-C(l) B(6)#3-B(3)-C( 1) C( 1)#3-B(3)-C( 1) C(3)-B(3)-B(2)

102.2(8) 125.4(5) 102.2(8) 0.0(6) 120.5(10) 59.8(5) 59.8(5) 59.8(5) 121.3(8) 104.0(7) 60.0(5) 60.0(5) 110.3(7) 121.3(8) 60.0(5) 104.0(7) 104.0(7) 110.3(7) 56.9(7) 126.1(5) 126.1(5) 0.0(6) 126.1(5) 100.7(8) 100.7(8) 121.9(9)

Bond angles C(5)# 1-Cl( 1)-Cl( 1)# 1 C(5)#1-C1(1)-C(1) C1(1)#1-C1(1)-C(1) B(6)#2-C( 1)-C( 1)#2 B(6)#2-C( 1)-B(2) C( 1)#2-C( 1)-B(2) B(6)#2-C( 1)-B(4) C(l)#2-C(l)-B(4) B(2)-C(l)-B(4) B(6)#2-C( 1)-B(3) C(l)#2-C(l)-B(3) B(2)-C(l)-B(3) B(4)-C(l)-B(3) B(6)#2-C( 1)-B(4)#2 C( 1)#2-C( 1)-B(4)#2 B(2)-C( 1)-B(4)#2 B(4)-C( 1)-B(4)#2 B(3)-C( 1)-B(4)#2 B(6)#2-C( 1)-Cl( 1) C(1)#2-C(1)-C1(1) B(2)-C(1)-C1(1) B(4)-C(1)-CI(1) B(3)-C(1)-C1(1) B(4)#2-C(1)-C1(1) a 2 )-B (2)-C (l) C(2)-B(2)-B(6)#3

260


B(6)#3-B(3)-B(2) C(l)#3-B(3)-B(2) C(l)-B(3)-B(2) C(3)-B(3)-B(4) B(6)#3-B(3)-B(4) C( 1)#3-B(3)-B(4) C(l)-B(3)-B(4) B(2)-B(3)-B(4) C(3)-B(3)-B(4)#3 B(6)#3-B(3)-B(4)#3 C(l)#3-B(3)-B(4)#3 C( 1)-B(3)-B(4)#3 B(2)-B(3)-B(4)#3 B(4)-B(3)-B(4)#3 C(4)-B(4)-B(4)#3 C(4)-B(4)-C(l) B(4)#3-B(4)-C(l) C(4)-B(4)-B(6)#2

58.8(5) 58.8(5) 58.8(5) 123.2(8) 102.1(7) 102.1(7) 58.6(4) 107.2(7) 123.2(8) 58.6(4) 58.6(4) 102.1(7) 107.2(7) 56.7(7) 126.2(4) 120.5(6) 106.2(4) 120.9(6)

B(4)#3-B(4)-B(6)#2 C( 1 )-B(4)-B(6)#2 C(4)-B(4)-C(l)#2 B(4)#3-B(4)-C( 1)#2 C(l)-B(4)-C(l)#2 B(6)#2-B(4)-C( 1)#2 C(4)-B(4>B(2)#4 B(4)#3-B(4)-B(2)#4 C( 1)-B(4)-B(2)#4 B(6)#2-B(4)-B(2)#4 C(l)#2-B(4)-B(2)#4 C(4)-B(4)-B(3) B(4)#3-B(4)-B(3) C(l)-B(4)-B(3) B(6)#2-B(4)-B(3) C(l)#2-B(4)-B(3) B(2)#4-B(4)-B(3)

106.0(4) 56.3(5) 120.9(6) 106.0(4) 56.3(5) 0.0(6) 123.5(7) 61.5(3) 103.9(6) 58.0(5) 58.0(5) 121.9(6) 61.7(3) 58.9(5) 105.0(6) 105.0(6) 109.9(6)

261


Chapter 7 Compound V1I-1 A tom ic coordinates and thermal param eters X

B rfl) Br(2) Br(3) Br(4) Br(5) Br(6) B (l) B(2) B(3) B(4) B(5) B(6) 0(1)

-13110(1) -9076(1) -12584(1) -14464(1) -12049(1) -8805(1) -11420(8) -9529(10) -11156(10) -12056(10) -10955(9) -9409(9) -14410(10)

y 7950(1) 5537(1) 9077(1) 12579(1) 11195(1) 6893(1) 9067(8) 7977(8) 9542(10) 11222(8) 10620(10) 8538(8) 5627(9)

z

U(eq)

16202(1) 17581(1) 19468(1) 15926(1) 11894(1) 12957(1) 15547(8) 16161(8) 17031(10) 15449(9) 13539(9) 14090(10) 20624(9)

72(1) 55(1) 55(1) 56(1) 71(1) 71(1) 42(2) 51(2) 57(3) 49(2) 49(3) 49(3) 41(3)

Bond lengths B ifl)-B (l) Br(2)-B(2) Br(3)-B(3) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6) B (l)-B (6) B (l)-B (3) B (l)-B (5) B (l)-B (4) B(l)-B (2) B(2)-B (4)#l B(2)-B(6)

1.974(9) 1.988(6) 1.988(8) 1.943(7) 1.942(10) 1.958(10) 1.732(9) 1.749(15) 1.769(9) 1.770(11) 1.777(11) 1.710(10) 1.704(11)

B(2)-B(5)#l B(2)-B(3) B(3)-B(5)#l B(3)-B(4) B(3)-B(6)#l B(4)-B(2)#l B(4)-B(6)#l B(4)-B(5) B(5)-B(2)#l B(5)-B(3)#l B(5)-B(6) B(6)-B(4)#l B(6)-B(3)#l

1.704(15) 1.722(10) 1.721(12) 1.765(10) 1.785(11) 1.710(10) 1.709(14) 1.788(11) 1.704(15) 1.721(12) 1.810(9) 1.709(14) 1.785(11)

106.4(6) 62.2(4) 108.5(6) 109.7(5) 60.2(5) 60.7(4) 58.1(4) 58.5(4) 107.7(5) 106.8(7) 121.3(6) 122.1(4) 121.3(6) 121.7(4)

B(2)-B(l)-Br(l) B(4)#l-B(2)-B(6) B(4)#l-B(2)-B(5)#l B(6)-B(2)-B(5)#l B(4)#l-B(2)-B(3) B(6)-B(2)-B(3) B(5)#l-B(2)-B(3) B(4)#l-B(2)-B(l) B(6)-B(2)-B(l) B(5)#l-B(2)-B(l) B(3)-B(2)-B(l) B(4)#l-B(2)-Br(2) B(6)-B(2)-Br(2) B(5)#l-B(2)-Br(2)

122.6(4) 60.1(5) 63.1(5) 111.2(5) 110.3(6) 108.9(5) 60.3(5) 108.0(5) 59.6(4) 109.0(5) 59.9(5) 122.7(4) 120.1(5) 121.7(5)

Bond angles B (6)-B (l)-B (3) B (6)-B (l)-B (5) B (3)-B(l)-B (5) B (6)-B (l)-B (4) B (3)-B (l)-B (4) B (5)-B (l)-B (4)

B(6)-B(l)-B(2) B (3)-B (l)-B (2) B (5)-B (l)-B (2) B (4)-B (l)-B (2) B (6)-B (l)-B r(l) B (3)-B (l)-B r(l) B (5)-B (l)-B r(l) B (4)-B (l)-B r(l)

262


B(3)-B(2)-Br(2) B(l)-B(2)-Br(2) B(5># 1-B(3)-B(2) B(5)#l-B(3)-B(l) B(2)-B(3)-B(l) B(5)#l-B(3)-B(4) B(2)-B(3)-B(4) B(l)-B(3)-B(4) B(5)#l-B(3)-B(6)#l B(2)-B(3)-B(6)#l B(l)-B(3)-B(6)#l B(4)-B(3)-B(6)#l B(5)#l-B(3)-Br(3) B(2)-B(3)-Br(3) B(l)-B(3)-Br(3) B(4)-B(3)-Br(3) B(6># 1-B(3)-Br(3) B(2># 1-B(4)-B(6)#l B(2)#l-B(4)-B(3) B(6)#l-B(4)-B(3) B(2)#l -B(4)-B( 1) B(6)#l-B(4)-B(l) B(3)-B(4)-B(l) B(2)#l-B(4)-B(5) B(6)#l-B(4)-B(5) B(3)-B(4)-B(5) B(l)-B(4)-B(5) B(2)#l-B(4)-Br(4) B(6)#l-B(4)-Br(4) B(3)-B(4)-Br(4) B(l)-B(4)-Br(4) B(5)-B(4)-Br(4) B(2)#l -B(5)-B(3)#l B(2># 1-B(5)-B( 1) B(3)#l-B(5)-B(l) B(2># 1-B(5)-B(4) B(3)#l-B(5)-B(4) B(l)-B(5)-B(4) B(2)#l-B(5)-B(6) B(3)#l -B(5)-B(6) B(l)-B(5)-B(6) B(4)-B(5)-B(6) B(2)#l-B(5)-Br(5) B(3)#1-B(5)-Br(5) B(l)-B(5)-Br(5) B(4)-B(5)-Br(5) B(6)-B(5)-Br(5) B(2)-B(6)-B(4)#l B(2)-B(6)-B(l) B(4)#l-B(6)-B(l) B(2)-B(6)-B(3)#l B(4)#l-B(6)-B(3)#l B(l)-B(6)-B(3)#l B(2)-B(6)-B(5) B(4)#l-B(6)-B(5) B(l)-B(6)-B(5)

120.1(4) 119.5(6) 59.3(5) 109.5(6) 61.6(5) 109.3(5) 109.5(6) 60^(5) 62.1(5) 107.8(5) 106.3(6) 57.6(5) 120.4(6) 123.5(4) 122.6(6) 119.9(4) 120.6(6) 59.8(5) 108.0(6) 61.8(5) 106.3(5) 108.7(5) 59.3(5) 58.3(5) 107.1(5) 107.0(5) 59.6(4) 122.7(4) 124.1(5) 123.4(4) 120.2(6) 119.7(6) 60.4(5) 106.6(6) 106.9(5) 58.6(5) 106.8(7) 59.7(4) 107.5(6) 60.7(4) 57.9(3) 105.5(5) 125.3(4) 122.9(5) 120.1(6) 123.6(5) 120.5(6) 60.1(5) 62.3(4) 110.1(7) 107.3(7) 60.7(5) 105.8(5) 109.1(5) 107.8(6) 59.9(3)

B(3)#l-B(6)-B(5) B(2)-B(6)-Br(6) B(4)#l-B(6)-Br(6) B(l)-B(6)-Br(6) B(3)#l-B(6)-Br(6) B(5VB(6)-Br(6)

57.2(4) 123.7(4) 123.0(4) 120.3(6) 122.1(5) 119.1(6)


Compound VI1-2 A tom ic coordinates and thermal parameters.

X

Brfl) Cl(l) Br(2) CI(2) C(l) B(2) B(3) 0(1)

6248(3) 6248(3) 5840(4) 5840(4) 4550(20) 4550(20) 4720(30) 10000

y 792(3) 792(3) -2618(4) -2618(4) -2990(20) -2990(20) -1360(30) 0

z

1345(1) 1345(1) 355(2) 355(2) 1038(9) 1038(9) 1516(9) 628(16)

U(eq) 65(2) 65(2) 68(2) 68(2) 48(7) 48(7) 54(8) 112(13)

Bond lengths

Br(l)-B(3) C(l)-B(3)#l C(l)-B(2)#l C (l)-C (l)#l C(l)-C(l)#2 C(l)-B(2)#2 C(l)-B(3) C(l)-B(3)#3

1.86(2) 1.78(3) 1.79(3) 1.79(3) 1.79(3) 1.79(3) 1.80(3) 1.80(3)

B(3)-B(2)#2 B(3)-C(l)#2 B(3)-B(3)#3 B(3)-B(3)#4 B(3)-C(l)#4 B(3)-B(2)#4 0(1)....0(1)#5

1.78(3) 1.78(3) 1.79(2) 1.79(2) 1.80(3) 1.80(3) 2.71

Bond angles B(3)#l-C(l)-B(2)#l B(3)# 1-C( 1)-C( 1)# 1 B(2)#l-C (l)-C (l)#l B(3)#l -C( 1)-C( 1)#2 B(2)#l -C( 1)-C( 1)#2 C (l)#l-C (l)-C (l)#2 B(3># 1-C( 1)-B(2)#2 B(2)#l-C(l)-B(2)#2 C(l)#l-C(l)-B(2)#2 C(l)#2-C(l)-B(2)#2 B(3)#l-C(l)-B(3) B(2)#l-C(l)-B(3) C (l)#l-C (l)-B(3) C(l)#2-C(l)-B(3) B(2)#2-C( 1)-B(3) B(3)#l-C(l)-B(3)#3 B(2># 1-C( 1)-B(3)#3 C(l)#l-C(l)-B(3)#3 C(l)#2-C(l)-B(3)#3 B(2)#2-C( 1)-B(3)#3 B(3)-C(l)-B(3)#3 B(2)#2-B(3)-C(l)#2 B(2)#2-B(3)-B(3)#3 C( 1)#2-B(3 )-B(3)#3 B(2)#2-B(3)-B(3)#4 C( 1)#2-B(3)-B(3)#4

60.4(13) 60.4(13) 0.0(13) 108.3(12) 60.000(1) 60.000(1) 108.3(12) 60.000(1) 60.000(1) 0.0(3) 107.9(16) 107.5(11) 107.5(11) 59.4(13) 59.4(13) 60.1(9) 108.1(10) 108.1(10) 107.4(10) 107.4(10) 59.7(8) 0(2) 108.4(10) 108.4(10) 60.5(10) 60.5(10)

B(3)#3-B(3)-B(3)#4 B(2)#2-B(3)-C( 1) C(l)#2-B(3)-C(l) B(3)#3-B(3)-C( 1) B(3)#4-B(3)-C( 1) B(2)#2-B(3)-C(l)#4 C(l)#2-B(3)-C(l)#4 B(3)#3-B(3)-C(l)#4 B(3)#4-B(3)-C(l)#4 C(l)-B(3)-C(l)#4 B(2)#2-B(3)-B(2)#4 C( 1)#2-B(3)-B(2)#4 B(3)#3-B(3)-B(2)#4 B(3)#4-B(3)-B(2)#4 C(l)-B(3)-B(2)#4 C(l)#4-B(3)-B(2)#4 B(2)#2-B(3)-Br( 1) C(l)#2-B(3)-Br(l) B(3)#3-B(3)-Br(l) B(3)#4-B(3)-Br( 1) C(l)-B(3)-Br(l) C(l)#4-B(3)-Br(l) B(2)#4-B(3)-Br(l)

107.6(13) 60.2(14) 60.2(14) 60.2(10) 108.2(10) 108.7(15) 108.7(15) 59.4(13) 60.1(12) 107.9(16) 108.7(15) 108.7(15) 59.4(13) 60.1(12) 107.9(16) 0(2) 121.1(14) 121.1(14) 121.7(15) 122.1(15) 121.2(12) 122.0(13) 122.0(13)


Compound VII-3 A tom ic coordinates and thermal parameters. X

1(2) 1(3) 1(4) 1(5) K6) Br(7) Br(8) Br(9) Br(10) BrCll) Br(12) 1(22) 1(23) 1(24) 1(25) 1(26) Br(27) Br(28) Br(29) Br(30) Br(31) Br(32) C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B(11) B(12) C(2) B(22) B(23) B(24) B(25) B(26) B(27) B(28) B(29) B(30) B(31) B(32) 0(8W ) 0(7W ) 0(1W ) 0(2W ) 0(3W )

-12412(1) -11237(1) -11874(1) -13430(1) -13775(1) -10163(1) -9821(1) -11125(1) -12273(1) -11676(1) -10133(1) -17641(1) -16302(1) -16315(1) -17718(1) -18505(1) -18553(1) -17707(1) -18599(1) -19886(1) -19874(1) -19855(1) -12421(3) -12035(3) -11450(3) -11732(3) -12471(3) -12657(3) -10991(3) -10843(3) -11404(3) -12000(3) -11724(3) -10999(3) -17403(2) -17964(3) -17328(3) -17330(3) -17994(3) -18347(3) -18334(3) -17938(3) -18372(3) -18933(3) -18962(3) -18922(3) -16707(10) -15741(8) -11931(13) -14776(14) -18151(11)

y -3889(1) -2185(1) -1365(1) -2604(1) -4179(1) -3953(1) -2420(1) -2674(1) -4366(1) -5129(1) -4202(1) 1208(1) -340(1) -1732(1) -1064(1) 779(1) -189(1) -1953(1) -2358(1) -853(1) 487(1) -1432(1) -2900(2) -3620(3) -2811(3) -2415(2) -2999(3) -3712(2) -3609(2) -2869(3) -3019(3) -3768(3) -4168(2) -3709(3) -257(2) 236(3) -501(3) -1136(2) -797(3) 44(3) -431(2) -1250(3) -1415(2) -688(3) -88(3) -966(3) 1071(10) 2616(6) -5977(12) -4501(10) 973(9)

z -5319(1) -5003(1) -7068(1) -8646(1) -7548(1) -4955(1) -5979(1) -8158(1) -8462(1) -6506(1) -6885(1) -7746(1) -7764(1) -6307(1) -5454(1) -6343(1) -9435(1) -8550(1) -7186(1) -7215(1) -8595(1) -9076(1) -6709(2) -6112(3) -5942(2) -6876(2) -7623(2) -7133(3) -5932(3) -6412(3) -7373(3) -7527(3) -6647(3) -6800(3) -6832(2) -7662(3) -7657(2) -6974(3) -6590(3) -7000(3) -8402(2) -7960(3) -7391(3) -7361(3) -8019(3) -8211(3) -4374(9) -4341(7) -4929(11) -10091(12) -10747(9)

U(eq) 150(1) 143(1) 131(1) 153(1) 158(1) 104(1) 108(1) 118(1) 116(1) 106(1) 102(1) 262(1) 218(1) 206(1) 191(1) 186(1) 180(1) 120(1) 146(1) 124(1) 159(1) 156(1) 86(4) 86(5) 72(5) 81(6) 79(5) 81(5) 76(5) 70(5) 93(6) 58(4) 66(4) 81(6) 207(6) 120(7) 152(8) 109(6) 156(8) 154(8) 121(7) 97(6) 105(7) 85(5) 109(8) 99(6) 121(8) 84(5) 205(11) 199(11) 137(8)


0(4W ) -15381(18) -735(16) -4159(16) 262(16) 0(6W ) -14961(14) 2460(12) -2696(13) 242(11) Q(5W)______________-15816(9)______________ 1931(12)_____________ -3422(10)___________ 206(8) Bond lengths I(2)-B(2) I(3)-B(3) I(4)-B(4) I(5)-B(5) I(6)-B(6) Br(7)-B(7) Br(8)-B(8) Br(9)-B(9) Br(10)-B(10) Br(l 1)-B(11) Br(12)-B(12) I(22)-B(22) I(23)-B(23) I(24)-B(24) I(25)-B(25) I(26)-B(26) Br(27)-B(27) Br(28)-B(28) Br(29)-B(29) Br(30)-B(30) Br(31)-B(31) Br(32)-B(32) C(l)-B(6) C(l)-B(3) C(l)-B(2) C(l)-B(4) C(l)-B(5) B (2)-B (ll) B(2)-B(6) B(2)-B(7) B(2)-B(3) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(4)-B(8) B(4)-B(9) B(4)-B(5) B(5)-B(10) B(5)-B(6) B(5)-B(9) B(6)-B(10)

2.068(6) 2.095(5) 2.093(5) 2.129(4) 2.094(5) 1.948(4) 1.927(5) 1.974(6) 2.035(5) 1.905(5) 1.981(6) 2.037(6) 2.079(6) 2.106(4) 2.110(5) 2.053(6) 1.935(5) 1.981(6) 1.988(5) 1.987(6) 1.927(5) 2.010(5) 1.759(6) 1.759(5) 1.764(6) 1.767(7) 1.766(6) 1.790(8) 1.801(6) 1.841(8) 1.876(7) 1.789(8) 1.790(7) 1.830(6) 1.742(6) 1.824(7) 1.873(6) 1.722(7) 1.828(7) 1.845(7) 1.752(8)

B (6)-B (ll) B(7)-B(12) B (7)-B (ll) B(7)-B(8) B(8)-B(9) B(8)-B(12) B(9)-B(12) B(9)-B(10) B (10)-B (ll) B(10)-B(12) B (ll)-B (12) C(2)-B(23) C(2)-B(25) Q 2)-B(26) C(2)-B(22) C(2)-B(24) B(22)-B(31) B(22)-B(26) B(22)-B(27) B(22)-B(23) B(23)-B(27) B(23)-B(28) B(23)-B(24) B(24)-B(28) B(24)-B(29) B(24)-B(25) B(25)-B(30) B(25)-B(26) B(25)-B(29) B(26)-B(30) B(26)-B(31) B(27)-B(32) B(27)-B(31) B(27)-B(28) B(28)-B(29) B(28)-B(32) B(29)-B(32) B(29)-B(30) B(30)-B(31) B(30)-B(32) B(31)-B(32)

1.806(6) 1.711(8) 1.813(6) 1.825(7) 1.706(6) 1.784(7) 1.700(7) 1.794(7) 1.744(7) 1.766(6) 1.784(8) 1.761(7) 1.764(7) 1.764(6) 1.764(6) 1.765(6) 1.800(7) 1.804(9) 1.836(7) 1.882(8) 1.785(6) 1.793(7) 1.835(7) 1.747(6) 1.833(6) 1.869(8) 1.728(6) 1.823(6) 1.848(7) 1.751(7) 1.804(7) 1.698(8) 1.811(8) 1.817(6) 1.704(9) 1.782(8) 1.702(7) 1.797(8) 1.734(8) 1.769(8) 1.777(8)

Bond angles


B(6)-C(l)-B(3) B(6)-C(l)-B(2) B(3)-C(l)-B(2) B(6)-C(l)-B(4) B(3)-C(l)-B(4) B(2)-C(l)-B(4) B(6)-C(l)-B(5) B(3)-C(l)-B(5) B(2)-C(l)-B(5) B(4)-C(l)-B(5) C(l)-B(2)-B(l 1) C(l)-B(2)-B(6) B(11)-B(2)-B(6) C(l)-B(2)-B(7) B(11)-B(2)-B(7) B(6)-B(2)-B(7) C(l)-B(2)-B(3) B(11)-B(2)-B(3) B(6)-B(2)-B(3) B(7)-B(2)-B(3) C(l)-B(2)-I(2) B(11)-B(2)-I(2) B(6)-B(2)-I(2) B(7)-B(2)-I(2) B(3)-B(2)-I(2) C(l)-B(3)-B(8) C(l)-B(3)-B(7) B(8)-B(3)-B(7) C(l)-B(3)-B(4) B(8)-B(3)-B(4) B(7)-B(3)-B(4) C(l)-B(3)-B(2) B(8)-B(3)-B(2) B(7)-B(3)-B(2) B(4)-B(3)-B(2) C(l)-B(3)-I(3) B(8)-B(3)-I(3) B(7)-B(3)-I(3) B(4)-B(3)-I(3) B(2)-B(3)-I(3) B(8)-B(4)-C(l) B(8)-B(4)-B(9) C(l)-B(4)-B(9) B(8)-B(4)-B(3) C(l)-B(4)-B(3) B(9)-B(4)-B(3) B(8)-B(4)-B(5) C(l)-B(4)-B(5) B(9)-B(4)-B(5) B(3)-B(4)-B(5) B(8)-B(4)-I(4) C(l)-B(4)-I(4) B(9)-B(4)-I(4) B(3)-B(4)-I(4) B(5)-B(4)-I(4) B(10)-B(5)-C(l)

B(10)-B(5)-B(6) C(l)-B(5)-B(6) B(10)-B(5)-B(9) C(l)-B(5)-B(9) B(6)-B(5)-B(9) B( 10)-B(5)-B(4) C(l)-B(5)-B(4) B(6)-B(5)-B(4) B(9)-B(5)-B(4) B(10)-B(5)-I(5) C(l)-B(5)-I(5) B(6)-B(5)-I(5) B(9)-B(5)-I(5) B(4)-B(5)-I(5) B(10)-B(6)-C(l) B(10)-B(6)-B(2) C(l)-B(6)-B(2) B(10)-B(6)-B(ll) C (l)-B (6)-B (ll) B(2)-B(6)-B(ll) B(10)-B(6)-B(5) C(l)-B(6)-B(5) B(2)-B(6)-B(5) B(11)-B(6)-B(5) B(10)-B(6)-I(6) C(l)-B(6)-I(6) B(2)-B(6)-I(6) B(ll)-B(6)-I(6) B(5)-B(6)-I(6) B(12)-B(7)-B(3) B(12)-B(7)-B(ll) B(3)-B(7)-B(ll) B(12)-B(7)-B(8) B(3)-B(7)-B(8) B(ll)-B(7)-B(8) B(12)-B(7)-B(2) B(3)-B(7)-B(2) B(ll)-B(7)-B(2) B(8)-B(7)-B(2) B(12)-B(7)-Br(7) B(3)-B(7)-Br(7) B(ll)-B(7)-Br(7) B(8)-B(7)-Br(7) B(2)-B(7)-Br(7) B(9)-B(8)-B(4) B(9)-B(8)-B(12) B(4)-B(8)-B(12) B(9)-B(8)-B(3) B(4)-B(8)-B(3) B(12)-B(8)-B(3) B(9)-B(8)-B(7) B(4)-B(8)-B(7) B( 12)-B(8)-B(7) B(3)-B(8)-B(7) B(9)-B(8)-Br(8) B(4)-B(8)-Br(8)

115.4(3) 61.5(2) 64.3(3) 116.6(4) 62.5(3) 116.4(3) 62.5(3) 114.9(4) 113.5(3) 64.0(3) 103.8(4) 59.1(2) 60.4(3) 101.1(3) 59.9(3) 107.4(4) 57.7(2) 106.6(4) 107.9(3) 57.6(3) 121.7(4) 128.0(3) 122.6(3) 125.5(3) 117.8(3) 102.6(3) 103.3(3) 61.3(3) 59.0(2) 57.5(3) 107.1(4) 57.9(2) 108.9(4) 60.2(3) 108.1(3) 120.5(3) 126.1(3) 127.9(3) 118.7(3) 120.6(3) 104.2(3) 57.1(3) 102.5(3) 60.0(3) 58.5(2) 104.5(3) 106.4(3) 58.0(2) 59.9(3) 106.7(3) 127.6(3) 121.5(3) 126.3(3) 123.6(3) 118.5(2) 101.9(3)

59.1(3) 58.6(3) 60.3(3) 101.7(3) 107.5(3) 107.1(3) 58.0(2) 108.3(3) 58.7(3) 126.4(3) 122.5(3) 119.2(3) 127.2(3) 120.8(3) 101.0(4) 105.7(3) 59.4(2) 58.7(3) 103.4(3) 59.5(3) 57.4(3) 59.0(3) 108.9(3) 106.1(4) 126.9(3) 124.7(3) 119.6(4) 123.4(3) 122.8(3) 108.3(3) 60.8(3) 109.3(3) 60.5(3) 59.3(3) 109.3(3) 107.5(3) 62.2(3) 58.6(3) 108.8(3) 124.8(3) 118.5(3) 121.7(3) 122.6(3) 118.8(3) 63.9(3) 58.2(3) 108.9(3) 111.5(3) 62.4(3) 105.2(4) 105.6(3) 109.4(4) 56.6(3) 59.4(3) 123.0(4) 121.6(3)

267


B(12)-B(8)-Br(8) B(3)-B(8)-Br(8) B(7)-B(8)-Br(8) B(12)-B(9)-B(8) B(12)-B(9)-B(10) B(8)-B(9)-B( 10) B(12)-B(9)-B(4) B(8)-B(9)-B(4) B(10)-B(9)-B(4) B(12)-B(9)-B(5) B(8)-B(9)-B(5) B(10)-B(9)-B(5) B(4)-B(9)-B(5) B(12)-B(9)-Br(9) B(8)-B(9)-Br(9) B(10)-B(9)-Br(9) B(4)-B(9)-Br(9) B(5)-B(9)-Br(9) B(5)-B(10)-B(l 1) B(5)-B(10)-B(6) B(11)-B(10)-B(6) B(5)-B( 10)-B( 12) B(11)-B(10)-B(12) B(6)-B(10)-B(12) B(5)-B(10)-B(9) B(11)-B(10)-B(9) B(6)-B(10)-B(9) B( 12)-B( 10)-B(9) B(5)-B( 10)-Br( 10) B (ll)-B (10)-B r(10) B(6)-B( 10)-Br( 10) B( 12)-B( 10)-Br( 10) B(9)-B(10)-Br(10) B (10)-B(l 1)-B(12) B (10)-B (ll)-B (2) B (12)-B (ll)-B (2) B (10)-B (ll)-B (7) B (12)-B (ll)-B (7) B (2)-B (l 1)-B(7) B (10)-B (ll)-B (6) B (12)-B (ll)-B (6) B (2)-B (ll)-B (6) B (7)-B (ll)-B (6) B( 10)-B( U ) -B r(ll) B (1 2 )-B (ll)-B r(ll) B (2 )-B (ll)-B r(l 1) B (7 )-B (ll)-B r(ll) B (6 )-B (ll)-B r(ll) B(9)-B(12)-B(7) B(9)-B(12)-B(10) B(7)-B(12)-B(10) B (9)-B (12)-B (ll) B (7)-B (12)-B (ll) B(10)-B(12)-B(l 1) B(9)-B(12)-B(8) B(7)-B(12)-B(8)

122.9(4) 120.0(3) 120.2(3) 63.2(3) 60.7(3) 110.2(4) 109.0(4) 59.0(3) 106.2(4) 107.0(4) 109.2(4) 56.5(3) 61.4(3) 126.2(4) 123.5(3) 122.0(3) 118.7(3) 116.5(3) 113.9(4) 63.5(3) 62.2(3) 109.7(4) 61.1(3) 110.8(4) 63.3(3) 109.3(3) 113.3(4) 57.0(3) 120.6(3) 117.9(3) 120.2(3) 119.5(4) 120.0(4) 60.1(3) 106.5(3) 106.7(4) 105.1(3) 56.8(3) 61.5(3) 59.1(3) 107.5(3) 60.1(3) 108.3(3) 124.3(3) 122.6(4) 121.2(4) 121.4(3) 122.5(3) 111.1(4) 62.3(3) 108.6(4) 111.8(4) 62.4(3) 58.8(3) 58.6(3) 62.9(3)

B(10)-B(12)-B(8) B( 11)-B(12)-B(8) B(9)-B(12)-Br(12) B(7)-B( 12)-Br( 12) B(10)-B(12)-Br(12) B(ll)-B(12)-Br(12) B(8)-B(12)-Br(12) B(23)-C(2)-B(25) B(23)-C(2)-B(26) B(25)-C(2)-B(26) B(23)-C(2)-B(22) B(25)-C(2)-B(22) B(26)-C(2)-B(22) B(23)-Q2)-B(24) B(25)-C(2)-B(24) B(26)-C(2)-B(24) B(22)-C(2)-B(24) C(2)-B(22)-B(31) C(2)-B(22)-B(26) B(31)-B(22)-B(26) C(2)-B(22)-B(27) B(31)-B(22)-B(27) B(26)-B(22)-B(27) C(2)-B(22)-B(23) B(31)-B(22)-B(23) B(26)-B(22)-B(23) B(27)-B(22)-B(23) C(2)-B(22)-I(22) B(31)-B(22)-I(22) B(26)-B(22)-I(22) B(27)-B(22)-I(22) B(23)-B(22)-I(22) C(2)-B(23)-B(27) C(2)-B(23)-B(28) B(27)-B(23)-B(28) C(2)-B(23)-B(24) B(27)-B(23)-B(24) B(28)-B(23)-B(24) C(2)-B(23)-B(22) B(27)-B(23)-B(22) B(28)-B(23)-B(22) B(24)-B(23)-B(22) C(2)-B(23)-I(23) B(27)-B(23)-I(23) B(28)-B(23)-l(23) B(24)-B(23)-I(23) B(22)-B(23)-I(23) B(28)-B(24)-C(2) B(28)-B(24)-B(29) C(2)-B(24)-B(29) B(28)-B(24)-B(23) C(2)-B(24)-B(23) B(29)-B(24)-B(23) B(28)-B(24)-B(25) C(2)-B(24)-B(25) B(29)-B(24)-B(25)

107.9(4) 112-5(4) 118.0(4) 121.4(3) 121.2(4) 120.1(3) 120.7(3) 114.9(3) 115.5(3) 62.2(3) 64.5(3) 113.4(3) 61-5(3) 62.7(3) 64.0(3) 116.5(3) 116.7(3) 103.6(4) 59.3(3) 60.1(3) 100.5(3) 59.8(3) 106.8(4) 57.7(3) 106.5(4) 108.0(4) 57.4(3) 121.1(3) 126.9(3) 119.5(4) 128.6(4) 120.5(4) 102.7(4) 102.3(4) 61.0(3) 58.8(3) 106.6(3) 57.5(3) 57.8(3) 60.0(3) 108.6(4) 107.8(4) 122.4(3) 126.6(3) 125.5(4) 120.1(3) 120.7(3) 104.0(3) 56.8(3) 102.5(3) 60.0(3) 58-5(3) 104.3(3) 106.1(3) 58.0(3) 59.9(3)

268


B(23)-B(24)-B(25) B(28)-B(24)-I(24) C(2)-B(24)-I(24) B(29)-B(24)-I(24) B(23)-B(24)-I(24) B(25)-B(24)-I(24) B(30)-B(25)-C(2) B(30)-B(25)-B(26) C(2)-B(25)-B(26) B(30)-B(25)-B(29) C(2)-B(25)-B(29) B(26)-B(25)-B(29) B(30)-B(25)-B(24) C(2)-B(25)-B(24) B(26)-B(25)-B(24) B(29)-B(25)-B( 24) B(30)-B(25)-I(25) Q2)-B(25)-I(25) B(26)-B(25)-I(25) B(29)-B(25)-l(25) B(24)-B(25)-I(25) B(30)-B(26)-C(2) B(30)-B(26)-B(31) C(2)-B(26)-B(31) B(30)-B(26)-B(22) C(2)-B(26)-B(22) B(31)-B(26)-B(22) B(30)-B(26)-B(25) C(2)-B(26)-B(25) B(31)-B(26)-B(25) B(22)-B(26)-B(25) B(30)-B(26)-[(26) C(2)-B(26)-I(26) B(31)-B(26)-I(26) B(22)-B(26)-I(26) B(25)-B(26)-I(26) B(32)-B(27)-B(23) B(32)-B(27)-B(31) B(23)-B(27)-B(31) B(32)-B(27)-B(28) B(23)-B(27)-B(28) B(31)-B(27)-B(28) B(32)-B(27)-B(22) B(23)-B(27)-B(22) B(31)-B(27)-B(22) B(28)-B(27)-B(22) B(32)-B(27)-Br(27) B(23)-B(27)-Br(27) B(31)-B(27)-Br(27) B(28)-B(27)-Br(27) B(22)-B(27)-Br(27) B(29)-B(28)-B(24) B(29)-B(28)-B(32) B(24)-B(28)-B(32) B(29)-B(28)-B(23) B(24)-B(28)-B(23)

106.7(3) 123.7(3) 124.2(2) 126.3(3) 121.3(3) 122.6(3) 102.3(3) 59.0(3) 58.9(3) 60.2(3) 101.9(4) 107.6(3) 107.5(3) 58.1(3) 108.7(4) 59.1(3) 127.1(4) 124.2(3) 123.6(3) 123.0(3) 117.4(3) 101.3(3) 58.3(3) 103.4(4) 105.9(4) 59.2(3) 59.8(3) 57.8(3) 58.9(3) 106.0(3) 108.7(4) 125.6(4) 123.5(3) 126.3(3) 122.3(3) 119.3(3) 109.3(3) 60.7(3) 110.2(3) 60.8(3) 59.7(3) 109.7(4) 108.3(4) 62.6(3) 59.1(3) 109.6(3) 123.0(3) 120.2(4) 119.1(3) 123.9(3) 118.1(3) 64.1(3) 58.4(3) 109.1(4) 111.8(4) 62.4(3)

B(32)-B(28)-B(23) B(29)-B(28)-B(27) B(24)-B(28)-B(27) B(32)-B(28)-B(27) B(23)-B(28)-B(27) B(29)-B(28)-Br(28) B(24)-B(28)-Br(28) B(32)-B(28)-Br(28) B(23)-B(28)-Br(28) B(27)-B(28)-Br(28) B(32)-B(29)-B(28) B(32)-B(29)-B(30) B(28)-B(29)*B(30) B(32)-B(29)-B(24) B(28)-B(29)-B(24) B(30)-B(29)-B(24) B(32)-B(29)-B(25) B(28)-B(29)-B(25) B(30)-B(29)-B(25) B(24)-B(29)-B(25) B(32)-B(29)-Br(29) B(28)-B(29)-Br(29) B(30)-B(29)-Br(29) B(24)-B(29)-Br(29) B(25)-B(29)-Br(29) B(25)-B(30)-B(31) B(25)-B(30)-B(26) B(31)-B(30)-B(26) B(25)-B(30)-B(32) B(31)-B(30)-B(32) B(26)-B(30)-B(32) B(25)-B(30)-B(29) B(31)-B(30)-B(29) B(26)-B(30)-B(29) B(32)-B(30)-B(29) B(25)-B(30)-Br(30) B(31)-B(30)-Br(30) B(26)-B(30)-Br(30) B(32)-B(30)-Br(30) B(29)-B(30)-Br(30) B(30)-B(31)-B(32) B(30)-B(31)-B(22) B(32)-B(31)-B(22) B(30)-B(31)-B(26) B(32)-B(31)-B(26) B(22)-B(31)-B(26) B(30)-B(31)-B(27) B(32)-B(31)-B(27) B(22)-B(31)-B(27) B(26)-B(31)-B(27) B(30)-B(31)-Br(31) B(32)-B(31)-Br(31) B(22)-B(31)-Br(31) B(26)-B(31)-Br(31) B(27)-B(31)-Br(31) B(27)-B(32)-B(29)

105.3(4) 105.3(4) 109.1(3) 5623(3) 59.3(3) 124.1(3) 121.9(3) 123.2(3) 118.8(4) 119.6(3) 63.1(3) 60.7(3) 110.3(4) 108.8(4) 59.1(3) 106.2(3) 106.8(4) 108.8(4) 56.6(3) 61.0(3) 125.5(3) 121.8(4) 123.2(4) 118.6(3) 118.3(3) 113.6(4) 63.2(3) 62.4(3) 109.2(4) 60.9(3) 110.5(4) 63.2(3) 109.2(4) 113.1(3) 57.0(3) 119.1(4) 120.4(3) 121.5(4) 120.1(3) 117.9(4) 60.5(3) 106.8(3) 106.5(4) 59.3(3) 107.8(3) 60.1(3) 105.0(4) 56.5(3) 61.1(3) 107.8(3) 123.0(4) 124.1(3) 120.8(4) 120.3(4) 123.9(3) 110.9(4)


B(27)-B(32)-B(30) B(29)-B(32)-B(30) B(27)-B(32)-B(31) B(29)-B(32)-B(31) B(30)-B(32)-B(31) B(27)-B(32)-B(28) B(29)-B(32)-B(28) B(30)-B(32)-B(28)

108.5(4) 62.3(3) 62.8(3) 111.7(4) 58.5(3) 62.9(3) 58.5(3) 108.0(3)

B(31)-B(32)-B(28) B(27)-B(32)-Br(32) B(29)-B(32)-Br(32) B(30)-B(32)-Br(32) B(31)-B(32)-Br(32) B(28)-B(32)-Br(32)

112.9(4) 120.3(4) 118.2(4) 123.0(4) 120.9(3) 119.0(4)

270


Compound VII-4 A tom ic coordinates and thermal parameters.

Br(2) Br(3) Br(4) Br(5) Br(6) Br(7) Br(8) Br(9) Br(10) B rfll) Br(12) C( 1) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B(11) B(12) 0(1) 0(2) 0(3) 0(4)

X

V

z

2227(1) 2195(1) 4750(1) 6402(1) 4850(1) -305(1) 1348(1) 4013(1) 4021(1) 1375(1) 857(1) 3991(6) 2613(7) 2568(7) 3858(6) 4604(6) 3834(7) 1466(6) 2184(7) 3469(6) 3503(8) 2275(8) 2072(7) 1741(6) 7029(7) 8945(8) 6400(12)

1599(1) 3443(1) 4511(1) 3283(1) 1518(1) 2952(1) 4790(1) 4679(1) 2771(1) 1706(1) 3690(1) 2896(3) 2415(3) 3294(3) 3795(3) 3237(3) 2372(3) 3055(3) 3918(3) 3854(3) 2972(3) 2469(3) 3412(3) 5413(3) 142(3) 1005(5) -595(6)

3693(1) 4793(1) 3842(1) 2216(1) 2072(1) 2351(1) 2498(1) 867(1) -253(1) 700(1) -42(1) 3199(5) 2876(5) 3428(5) 2971(5) 2195(6) 2121(5) 2305(7) 2334(6) 1596(5) 1028(6) 1533(5) 1148(6) -1059(5) 2217(6) 2465(7) 587(9)

U(eq) 59(1) 68(1) 64(1) 71(1) 55(1) 61(1) 63(1) 62(1) 68(1) 61(1) 60(1) 46(2) 42(2) 39(2) 38(2) 53(2) 38(2) 46(2) 50(2) 36(2) 50(2) 49(2) 47(2) 105(2) 108(3) 61(3) 101(4)

Bond lengths Br(2)-B(2) Br(3)-B(3) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6) Br(7)-B(7) Br(8)-B(8) Br(9)-B(9) Br(10)-B(10) Br(l 1)-B(11) Br(12)-B(12) C(l)-B(5) C(l)-B(6) C(l)-B(4) C(l)-B(2) C(l)-B(3) B(2)-B(ll) B(2)-B(6) B(2)-B(7)

B(2)-B(3) B(3)-B(7) B(3)-B(8) B(3)-B(4) B(4)-B(5) B(4)-B(9) B(4)-B(8) B(5)-B(9) B(5)-B(6) B(5)-B(10) B (6)-B (ll) B(6)-B(10) B(7)-B(8) B (7)-B (ll) B(7)-B(12) B(8)-B(12) B(8)-B(9) B(9)-B(12) B(9)-B(10) B(10)-B(12)

1.950(7) 1.914(7) 1.908(6) 1.938(7) 1.946(6) 1.932(7) 1.896(7) 1.957(6) 1.890(8) 1.951(6) 1.923(7) 1.692(11) 1.701(9) 1.711(7) 1.729(9) 1.779(10) 1.730(10) 1.779(11) 1.791(9)

1.801(9) 1.777(10) 1.836(10) 1.861(10) 1.745(10) 1.774(9) 1.869(10) 1.765(9) 1.816(9) 1.830(10) 1.735(11) 1.803(9) 1.790(9) 1.813(11) 1.870(12) 1.801(11) 1.825(11) 1.731(9) 1.813(9) 1.780(11)

271


B(10)-B(ll)

1.839(11)

B (ll)-B (12)

1.839(8)

Bond angles B(5)-C(l)-B(6) B(5)-C(l)-B(4) B(6)-C(l)-B(4) B(5)-C(l)-B(2) B(6)-C(l)-B(2) B(4)-C(l)-B(2) B(5)-C(l)-B(3) B(6)-C(l)-B(3) B(4)-C(l)-B(3) B(2)-C(l)-B(3) C (l)-B (2)-B (ll) C(l)-B(2)-B(6) B(ll)-B(2)-B(6) C(l)-B(2)-B(7) B(11)-B(2)-B(7) B(6)-B(2)-B(7) C(l)-B(2)-B(3) B(11)-B(2)-B(3) B(6)-B(2)-B(3) B(7)-B(2)-B(3) C(l)-B(2)-Br(2) B(11)-B(2)-Br(2) B(6)-B(2)-Br(2) B(7)-B(2)-Br(2) B(3)-B(2)-Br(2) B(7)-B(3)-C(l) B(7)-B(3)-B(2) C(l)-B(3)-B(2) B(7)-B(3)-B(8) C(l)-B(3)-B(8) B(2)-B(3)-B(8) B(7)-B(3)-B(4) C(l)-B(3)-B(4) B(2)-B(3)-B(4) B(8)-B(3)-B(4) B(7)-B(3)-Br(3) C(l)-B(3)-Br(3) B(2)-B(3)-Br(3) B(8)-B(3)-Br(3) B(4)-B(3)-Br(3) C(l)-B(4)-B(5) Ql)-B(4)-B(9) B(5)-B(4)-B(9) C(l)-B(4)-B(3) B(5)-B(4)-B(3) B(9)-B(4)-B(3) C(l)-B(4)-B(8) B(5)-B(4)-B(8) B(9)-B(4)-B(8) B(3)-B(4)-B(8) C(l)-B(4)-Br(4) B(5)-B(4)-Br(4)

64.7(4) 61.7(4) 115.5(5) 116.3(5) 62.5(4) 115.3(4) 115.9(4) 114.5(5) 64.4(4) 61.8(4) 103.8(5) 58.0(4) 59.2(4) 104.9(4) 62.0(4) 109.0(5) 60.5(4) 109.6(4) 109.7(5) 59.3(4) 122.1(4) 124.9(4) 121.1(4) 123.7(5) 118.3(5) 103.4(5) 60.0(4) 57.7(4) 59.4(4) 102.8(5) 106.8(5) 107.1(5) 56.0(3) 105.0(5) 60.7(4) 125.8(5) 123.0(4) 122.0(4) 125.1(4) 121.0(4) 58.6(4) 103.7(4) 60.2(4) 59.6(4) 109.3(4) 107.2(4) 104.2(4) 108.9(5) 60.1(4) 59.0(4) 124.7(4) 122.1(4)

B(9)-B(4)-Br(4) B(3)-B(4)-Br(4) B(8)-B(4)-Br(4) C(l)-B(5)-B(4) C(l)-B(5)-B(9) B(4)-B(5)-B(9) C(l)-B(5)-B(6) B(4)-B(5)-B(6) B(9)-B(5)-B(6) C(l)-B(5)-B(10) B(4)-B(5)-B( 10) B(9)-B(5)-B( 10) B(6)-B(5)-B( 10) C(l)-B(5)-Br(5) B(4)-B(5>Br(5) B(9)-B(5)-Br(5) B(6)-B(5)-Br(5) B( 10)-B(5)-Br(5) C (l)-B (6)-B (ll) C(l)-B(6)-B(2) B(ll)-B(6)-B(2) C(l)-B(6)-B(10) B( 11)-B(6)-B( 10) B(2)-B(6)-B( 10) C(l)-B(6)-B(5) B(11)-B(6)-B(5) B(2)-B(6)-B(5) B(10)-B(6)-B(5) C(l)-B(6)-Br(6) B(11)-B(6)-Br(6) B(2)-B(6)-Br(6) B( 10)-B(6)-Br(6) B(5)-B(6)-Br(6) B(3)-B(7)-B(8) B(3)-B(7)-B(2) B(8)-B(7)-B(2) B(3)-B(7)-B(ll) B(8)-B(7)-B(ll) B(2)-B(7)-B(ll) B(3)-B(7)-B( 12) B(8)-B(7)-B(12) B(2)-B(7)-B( 12) B(11)-B(7)-B(12) B(3)-B(7)-Br(7) B(8)-B(7)-Br(7) B(2)-B(7)-Br(7) B(11)-B(7)-Br(7) B(12)-B(7)-Br(7) B(7)-B(8)-B( 12) B(7)-B(8)-B(9) B(12)-B(8)-B(9) B(7)-B(8)-B(3)

124.4(4) 119.5(4) 121.8(4) 59.7(4) 104.9(5) 60.7(4) 57.9(4) 108.2(5) 106.6(4) 104.9(5) 110.3(5) 60.5(4) 59.3(3) 122.0(4) 121.7(4) 126.4(5) 119.2(4) 121.9(5) 104.8(5) 59.5(4) 59.0(4) 105.8(4) 62.6(4) 110.1(5) 57.4(4) 109.2(4) 107.8(5) 60.8(4) 121.7(4) 125.5(4) 122.1(4) 121.5(5) 118.7(5) 62.0(4) 60.6(4) 109.3(5) 107.0(5) 108.0(5) 57.4(4) 107.3(5) 58.9(4) 105.2(5) 59.9(4) 121.6(5) 121.1(4) 122.5(5) 122.1(4) 123.2(4) 62.8(4) 107.2(5) 57.0(4) 58.7(4)


B(12)-B(8)-B(3) B(9)-B(8)-B(3) B(7)-B(8)-B(4) B(12)-B(8)-B(4) B(9)-B(8)-B(4) B(3)-B(8)-B(4) B(7)-B(8)-Br(8) B(12)-B(8)-Br(8) B(9)-B(8)-Br(8) B(3)-B(8)-Br(8) B(4)-B(8)-Br(8) B(12)-B(9)-B(5) B(12)-B(9)-B(4) B(5)-B(9)-B(4) B(12)-B(9)-B(10) B(5)-B(9)-B(10) B(4)-B(9)-B(10) B(12)-B(9)-B(8) B(5)-B(9)-B(8) B(4)-B(9)-B(8) B(10)-B(9)-B(8) B(12)-B(9)-Br(9) B(5)-B(9)-Br(9) B(4)-B(9)-Br(9) B(10)-B(9)-Br(9) B(8)-B(9)-Br(9) B(12)-B(10)-B(6) B(12)-B(10)-B(9) B(6)-B(10)-B(9) B(12)-B(10)-B(5) B(6)-B(10)-B(5) B(9)-B(10)-B(5) B(12)-B(10)-B(l 1) B(6)-B(10)-B(ll) B(9)-B(10)-B(ll) B(5)-B(10)-B(ll)

107.8(4) 106.2(5) 106.2(4) 103.4(5) 57.4(4) 60.3(4) 124.6(5) 126.1(5) 122.4(4) 120.6(5) 119.9(4) 109.4(4) 110.6(5) 59.1(4) 60.2(4) 61.5(4) 109.8(4) 60.8(4) 110.0(5) 62.6(4) 110.2(5) 122.1(4) 119.3(4) 120.2(4) 119.5(4) 121.6(4) 106.0(6) 57.6(4) 105.1(5) 104.5(5) 60.0(4) 57.9(3) 61.0(4) 56.9(4) 104.7(5) 104.2(5)

B(12)-B(10)-Br(10) B(6)-B( 10)-Br( 10) B(9)-B( 10)-Br( 10) B(5)-B( 10)-Br( 10) B(11)-B(10)-Br(10) B(2)-B(ll)-B(6) B(2)-B(ll)-B(7) B(6)-B( 11)-B(7) B(2)-B(ll)-B(10) B(6)-B( 11)-B( 10) B(7)-B( 11)-B( 10) B(2)-B(ll)-B(12) B(6)-B(ll)-B(12) B(7)-B(ll)-B(12) B(10)-B(ll)-B(12) B (2)-B (ll)-B r(ll) B(6)-B( 11)-Br( 11) B (7)-B (ll)-B r(ll) B (10)-B(ll)-Br(ll) B (12)-B(ll)-Br(ll) B(9)-B(12)-B(10) B(9)-B(12)-B(8) B(10)-B(12)-B(8) B(9)-B(12)-B(ll) B(10)-B(12)-B(l 1) B(8)-B(12)-B( 11) B(9)-B(12)-B(7) B(10)-B(12)-B(7) B(8)-B(12)-B(7) B(11)-B(12)-B(7) B(9)-B(12)-Br(12) B(10)-B(12)-Br(12) B(8)-B(12)-Br(12) B(ll)-B(12)-Br(12) B(7)-B( 12)-Br( 12)

124.3(5) 121.7(4) 125.0(4) 122.7(5) 123.8(4) 61.8(4) 60.7(4) 110.0(5) 110.8(5) 60.5(4) 109.6(4) 109.1(4) 106.4(5) 61.6(4) 57.9(4) 121.2(4) 121.4(4) 120.8(5) 119.8(4) 121.9(4) 62.2(4) 62.2(4) 112.9(5) 108.2(5) 61.0(4) 106.5(5) 107.7(5) 109.6(4) 58.3(4) 58.5(4) 125.1(4) 122.4(5) 119.1(4) 120.9(4) 117.6(4)

273



Br(2) Br(3) Br(4) Br(5) Br(6) Br(7) Br(8) Br(9) Br(10) Br(31) Br(51) Br(71) Br(81)

C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) O (IW ) 0(2W ) 0 (3W ) 0(4W ) 0 (5 W)

11398(1) 13449(1) 15585(1) 13455(1) 10733(1) 13802(1) 13806(1) 10732(1) 11372(1) 13818(1) 13803(1) 13459(1) 13431(1) 13522(2) 12220(2) 13148(2) 14058(2) 13173(2) 11904(2) 13175(2) 13171(2) 11898(2) 12143(2) 15833(2) 11289(2) 8716(2) 7749(3) 7735(3)

y 4539(1) 6044(1) 7516(1) 6032(1) 7469(1) 9560(1) 9554(1) 7457(1) 10439(1) 5446(1) 5406(1) 8973(1) 8928(1) 5905(2) 6079(2) 6696(2) 7389(2) 6694(2) 7517(2) 8398(2) 8391(2) 7507(2) 8836(2) 7502(2) 555(2) 5535(2) 7530(4) 7478(4)

z

U(eq)

6604(1) 8855(1) 7646(1) 5377(1) 7690(1) 8450(1) 5947(1) 5177(1) 6590(1) 8465(1) 5971(1) 8845(1) 5353(1) 7120(1) 6799(1) 7742(2) 7270(1) 6338(1) 7250(1) 7600(2) 6493(2) 6197(1) 6783(2) 5220(2) 4210(2) 6067(2) 6098(3) 5263(3)

70(1) 60(1) 52(1) 65(1) 72(1) 53(1) 55(1) 72(1) 70(1) 41(1) 22(1) 51(1) 46(1) 53(1) 42(1) 43(1) 43(1) 40(1) 40(1) 44(1) 45(1) 38(1) 44(1) 171(1) 144(1) 145(1) 120(2) 113(2)

Bond lengths Br(2)-B(2) Br(3)-B(3) Br(4)-B(4) Br(5)-B(5) Br(6)-B(6) Br(7)-B(7) Br(8)-B(8) Br(9)-B(9) Br(10)-B(10) Br(31)-B(3) Br(51)-B(5) C (l)-B (5) C (l)-B (3) C (l)-B (2) C (l)-B (4) B(2)-B(9) B(2)-B(6) B(2)-B(3)

B(2)-B(5) B(3)-B(7) B(3)-B(6) B(3)-B(4) B(4)-B(7) B(4)-B(8) B(4)-B(5) B(5)-B(8) B(5)-B(9) B(6)-B(10) B(6)-B(7) B(6)-B(9) B(7)-B(10) B(7)-B(8) B(8)-B(10) B(8)-B(9) B(9)-B(10)

1.916(2) 1.987(3) 1.915(3) 1.974(3) 1.949(3) 1.897(2) 1.911(3) 1.945(2) 1.940(2) 1.841(3) 1.816(3) 1.541(3) 1.578(4) 1.639(3) 1.697(3) 1.805(3) 1.817(4) 1.827(3)

1.828(4) 1.807(4) 1.807(3) 1.826(4) 1.810(4) 1.817(3) 1.824(3) 1.803(3) 1.834(3) 1.692(4) 1.840(3) 1.849(3) 1.688(3) 1.946(4) 1.670(4) 1.843(3) 1.702(3)

274


Bond angles

B(5)-C(l)-B(3) B(5)-C(l)-B(2) B(3)-C(l)-B(2) B(5)-C(l)-B(4) B(3)-C(l)-B(4) B(2)-C(l)-B(4) C(l)-B(2)-B(9) C(l)-B(2)-B(6) B(9)-B(2)-B(6) C(l)-B(2)-B(3) B(9)-B(2)-B(3) B(6)-B(2)-B(3) C(l)-B(2)-B(5) B(9)-B(2)-B(5) B(6)-B(2)-B(5) B(3)-B(2)-B(5) C(l)-B(2)-Br(2) B(9)-B(2)-Br(2) B(6)-B(2)-Br(2) B(3)-B(2)-Br(2) B(5)-B(2)-Br(2) C(l)-B(3)-B(7) C(l)-B(3)-B(6) B(7)-B(3)-B(6) C(l)-B(3)-B(2) B(7)-B(3)-B(2) B(6)-B(3)-B(2) C(l)-B(3)-B(4) B(7)-B(3)-B(4) B(6)-B(3)-B(4) B(2)-B(3)-B(4) C(l)-B(3)-Br(3) B(7)-B(3)-Br(3) B(6)-B(3)-Br(3) B(2)-B(3)-Br(3) B(4)-B(3)-Br(3) C(l)-B(4)-B(7) C(l)-B(4)-B(8) B(7)-B(4)-B(8) C( 1)-B(4)-B(5) B(7)-B(4)-B(5) B(8)-B(4)-B(5) C(l)-B(4)-B(3) B(7)-B(4)-B(3) B(8)-B(4)-B(3) B(5)-B(4)-B(3) C(l)-B(4)-Br(4) B(7)-B(4)-Br(4) B(8)-B(4)-Br(4) B(5)-B(4)-Br(4) B(3)-B(4)-Br(4) C(l)-B(5)-B(8) C(l)-B(5)-B(4) B(8)-B(5)-B(4)

105.39(19) 70.11(16) 69.21(16) 68.40(15) 67.66(16) 106.87(17) 108.24(18) 108.02(16) 61.42(13) 53.82(14) 101.32(16) 59.46(13) 52.44(13) 60.64(14) 101.03(16) 85.48(15) 116.07(16) 125.86(14) 125.49(17) 129.39(16) 130.80(16) 113.6(2) 111.33(17) 61.21(13) 56.98(14) 105.27(16) 59.98(13) 59.27(15) 59.77(15) 103.06(17) 94.35(17) 119.65(16) 118.08(15) 119.50(17) 128.99(16) 129.59(14) 107.83(18) 106.36(15) 64.90(14) 51.76(12) 103.32(15) 59.36(13) 53.07(14) 59.61(15) 102.30(16) 85.64(15) 117.24(15) 124.69(15) 124.61(17) 129.19(17) 130.62(15) 114.31(18) 59.84(14) 60.10(13)

Br(51)-B(5)-B(4) C(l)-B(5)-B(2) B(8)-B(5)-B(2) B(4)-B(5)-B(2) C(l)-B(5)-B(9) B(8)-B(5>B(9) B(4)-B(5)-B(9) B(2)-B(5>B(9) C(l)-B(5)-Br(5) B(8)-B(5>Br(5) B(4)-B(5>Br(5) B(2)-B(5)-Br(5) B(9)-B(5)-Br(5) B(10)-B(6)-B(3) B(10)-B(6)-B(2) B(3)-B(6>B(2) B(10)-B(6)-B(7) B(3)-B(6)-B(7) B(2)-B(6)-B(7) B(10)-B(6)-B(9) B(3)-B(6)-B(9) B(2)-B(6)-B(9) B(7)-B(6)-B(9) B(10)-B(6)-Br(6) B(3)-B(6>BK6) B(2)-B(6)-Br(6) B(7)-B(6)-Br(6) B(9)-B(6)-Br(6) B(10)-B(7)-B(3) B(10)-B(7)-B(4) B(3)-B(7)-B(4) B(10)-B(7)-B(6) B(3)-B(7)-B(6) B(4)-B(7)-B(6) B(10)-B(7)-Br(7) B(3)-B(7)-Br(7) B(4)-B(7>Br(7) B(6)-B(7)-Br(7) B(10)-B(7)-B(8) B(3)-B(7>B(8) B(4)-B(7)-B(8) B(6)-B(7)-B(8) Br(7)-B(7)-B(8) B(10)-B(8)-B(5) B(10)-B(8)-B(4) B(5)-B(8)-B(4) B(10)-B(8)-B(9) B(5)-B(8)-B(9) B(4)-B(8)-B(9) B(10)-B(8)-Br(8) B(5)-B(8)-Br(8) B(4)-B(8)-Br(8) B(9)-B(8)-Br(8) B(10)-B(8)-B(7)

112.50(15) 57.46(15) 104.30(18) 94.37(17) 111.3(2) 60.88(13) 103.06(17) 59.04(14) 119.29(17) 119.18(16) 131.55(16) 127.48(15) 118.27(14) 109.65(17) 111.24(18) 60.56(13) 56.90(13) 59.39(13) 104.35(16) 57.23(14) 100.37(17) 58.96(13) 92.28(16) 120.93(16) 121.10(16) 118.65(15) 129.77(16) 130.99(13) 109.86(16) 108.30(18) 60.62(15) 57.13(14) 59.40(13) 102.38(16) 121.19(16) 123.41(15) 117.89(14) 134.64(18) 54.17(14) 98.11(16) 57.71(13) 87.83(15) 130.38(16) 111.36(19) 108.78(19) 60.54(13) 57.70(14) 60.39(13) 103.03(17) 120.89(16) 122.20(18) 117.73(15) 133.89(15) 55.00(14)


B(5)-B(8)-B(7) B(4)-B(8)-B(7) B(9)-B(8)-B(7) Br(8)-B(8)-B(7) B(10)-B(9)-B(2) B(10)-B(9)-B(5) B(2)-B(9)-B(5) B(10)-B(9)-B(8) B(2)-B(9)-B(8) B(5)-B(9)-B(8) B(10)-B(9)-B(6) B(2)-B(9)-B(6) B(5)-B(9)-B(6) B(8)-B(9)-B(6) B(10)-B(9)-Br(9)

98.93(16) 57.39(14) 89.16(16) 130.07(15) 111.39(16) 108.44(15) 60.32(14) 56.06(14) 103.65(15) 58.73(13) 56.73(14) 59.63(14) 99.60(15) 90.73(15) 121.10(15)

B(2)-B(9)-Br(9) B(5)-B(9)-Br(9) B(8)-B(9)-Br(9) B(6)-B(9)-Br(9) B(8)-B( 10)-B(6) B(8)-B( 10)-B(7) B(6)-B( 10)-B(7) B(8)-B(10)-B(9) B(6)-B( 10)-B(9) B(7)-B(10)-B(9) B(8)-B(10)-Br(10) B(6)-B(10)-Br(10) B(7)-B(10)*Br(10) B(9)-B( 10)-Br( 10)

118.77(14) 121.88(15) 130.45(16) 131.62(15) 102.77(18) 70.83(16) 65.97(14) 66.24(15) 66.04(15) 103.42(17) 128.59(18) 128.59(18) 128.12(16) 128.37(15)

276



C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B (ll) B(12) Cl(2) Cl(3) Cl(4) Cl(5) Cl(6) Cl(7) Cl(8) CI(9) Cl(10) C I(ll) Cl(12) C(2) B(22) B(23) B(24) B(25) B(26) B(27) B(28) B(29) B(30) B(31) B(32) Cl(22) Cl(23) CI(24) Cl(25) CI(26) Cl(27) Cl(28) CI(29) 0 (3 0 ) 0 (3 1 ) Cl(32) O(IW) 0(2W ) 0(3) N (l) C(3)

3380(3) 3515(4) 1946(4) 1980(4) 3580(4) 4534(4) 2129(4) 1165(4) 2182(4) 3771(4) 3728(4) 2284(4) 4246(1) 1092(1) 1152(1) 4337(1) 6264(1) 1331(1) -599(1) 1479(1) 4746(1) 4678(1) 1669(1) -999(4) -1116(4) -2433(4) -2468(4) -1159(4) -320(4) -2763(4) -3607(4) -2815(4) -1496(4) -1448(4) -3010(4) -161(1) -2806(1) -2846(1) -250(1) 1426(1) -3629(1) -5339(1) -3732(1) -989(1) -902(1) -4131(1) -2286(4) -6220(4) -2013(3) -1936(3) -1505(5)

y -228(1) 177(1) 17(1) -486(1) -642(1) -229(1) 164(1) -250(1) -657(1) -493(1) 13(1) -253(1) 590(1) 272(1) -740(1) -1042(1) -215(1) 581(1) -252(1) -1096(1) -763(1) 276(1) -266(1) -2355(1) -1875(1) -2136(1) -2601(1) -2625(1) -2179(1) -1803(1) -2251(1) -2551(1) -2291(1) -1829(1) -2057(1) -1549(1) -2078(1) -3000(1) -3050(1) -2169(1) -1373(1) -2285(1) -2901(1) -2372(1) -1424(1) -1898(1) -778(1) -1635(1) -1277(1) -1380(1) -1770(1)

z 3884(3) 3204(3) 3477(3) 3504(4) 3254(3) 3064(3) 2261(3) 2451(3) 2313(3) 2043(3) 2008(3) 1531(3) 3781(1) 4315(1) 4376(1) 3880(1) 3500(1) 1753(1) 2171(1) 1862(1) 1303(1) 1230(1) 243(1) -1066(3) -1264(3) -842(3) -1387(3) -2148(4) -2066(4) -1814(3) -1888(3) -2687(3) -3112(3) -2570(3) -2967(3) -479(1) 377(1) -692(1) -2200(1) -2045(1) -1648(1) -1794(1) -3447(1) -4299(1) -3183(1) -4011(1) 386(2) 353(3) 1686(2) 3305(3) 3215(4)

U(eq) 37(1) 36(1) 39(1) 44(1) 39(1) 40(1) 38(1) 39(1) 43(1) 41(1) 42(1) 42(1) 56(1) 55(1) 64(1) 61(1) 53(1) 53(1) 59(1) 71(1) 69(1) 64(1) 67(1) 44(1) 43(1) 41(1) 44(1) 46(1) 46(1) 39(1) 38(1) 42(1) 44(1) 39(1) 40(1) 63(1) 74(1) 68(1) 75(1) 81(1) 57(1) 60(1) 62(1) 75(1) 58(1) 62(1) 104(1) 119(1) 81(1) 58(1) 112(2)

277


C(4) C(5) 0(4) N(2) C(6) C(7) C(8)

-2095(5) -2142(4) -7033(3) -7323(3) -7877(5) -7202(5) -6960(4)

-1245(1) -1163(1) -1134(1) -1118(1) -734(1) -1313(1) -1291(1)

4292(4) 2545(4) -933(3) -2587(3) -2628(4) -3521(4) -1761(4)

93(2) 59(1) 85(1) 61(1) 89(2) 88(2) 64(1)

Bond lengths C(l)-B(4) C(l)-B(3) C(l)-B(2) C(l)-B(5) C(l)-B(6) B (2)-B (ll) B(2)-B(7) B(2)-C1(2) B(2)-B(3) B(2)-B(6) B(3)-B(7) B(3)-CI(3) B(3)-B(8) B(3)-B(4) B(4)-B(8) B(4)-B(9) B(4)-C1(4) B(4)-B(5) B(5)-B(10) B(5)-C1(5) B(5)-B(9) B(5)-B(6) B(6)-B(10) B (6)-B (ll) B(6)-C1(6) B(7)-C1(7) B (7)-B (ll) B(7)-B(8) B(7)-B(12) B(8)-C1(8) B(8)-B(9) B(8)-B(12) B(9)-C1(9) B(9)-B(12) B(9)-B(10) B(10)-B(12) B(10)-CI(10) B (10)-B (ll) B(11)-B(12) B(1 l)-C l(ll) B(12)-C1(12) C(2)-B(23) C(2)-B(22) C(2)-B(26) C(2)-B(24) C(2)-B(25)

1.706(5) 1.716(5) 1.718(5) 1.722(5) 1.722(5) 1.767(6) 1.767(6) 1.771(4) 1.773(5) 1.791(5) 1.766(6) 1.769(4) 1.777(6) 1.778(5) 1.761(6) 1.768(6) 1.784(4) 1.789(6) 1.765(6) 1.769(4) 1.774(6) 1.790(6) 1.761(6) 1.770(6) 1.773(4) 1.776(4) 1.784(6) 1.797(5) 1.796(6) 1.776(4) 1.795(6) 1.801(6) 1.779(4) 1.791(6) 1.796(6) 1.784(6) 1.783(4) 1.787(6) 1.784(6) 1.787(4) 1.776(4) 1.711(5) 1.721(5) 1.723(5) 1.725(5) 1.741(6)

B(22)-B(27) B(22)-B(31) B(22)-C1(22) B(22)-B(23) B(22)-B(26) B(23)-C1(23) B(23)-B(27) B(23)-B(28) B(23)-B(24) B(24)-B(29) B(24)-B(28) B(24)-Q(24) B(24)-B(25) B(25)-B(29) B(25)-B(30) B(25)-CI(25) B(25)-B(26) B(26)-B(31) B(26)-C1(26) B(26)-B(30) B(27)-Q(27) B(27)-B(31) B(27)-B(32) B(27)-B(28) B(28)-CI(28) B(28)-B(29) B(28)-B(32) B(29)-B(30) B(29)-C1(29) B(29)-B(32) B(30)-B(32) B(30)-C1(30) B(30)-B(31) B(31)-Cl(3l) B(31)-B(32) B(32)-CI(32) 0(3)-C(5) N(l)-C(5) N(l)-C(3) N(l)-C(4) 0(4)-C(8) N(2)-C(8) N(2)-C(6) N(2)-C(7) 0(1W )...0(3) 0(2W )...0(4)

1.751(6) 1.767(6) 1.766(4) 1.782(6) 1.798(6) 1.761(4) 1.767(6) 1.771(6) 1.800(6) 1.763(6) 1.763(6) 1.768(4) 1.793(6) 1.756(6) 1.764(6) 1.766(4) 1.788(6) 1.756(6) 1.765(4) 1.770(7) 1.786(4) 1.794(5) 1.794(6) 1.795(5) 1.782(4) 1.785(6) 1.798(6) 1.782(6) 1.789(4) 1.790(5) 1.777(6) 1.782(4) 1.787(5) 1.783(4) 1.792(6) 1.783(4) 1.259(5) 1.281(5) 1.454(5) 1.455(5) 1.265(5) 1.287(5) 1.465(5) 1.465(5) 2.487(5) 2.545(5)


Bond angles

B(4)-C(l)-B(3) B(4)-C(l)-B(2) B(3)-C(l)-B(2) B(4)-C(l)-B(5) B(3)-C(l)-B(5) B(2)-C(l)-B(5) B(4)-C(l)-B(6) B(3)-C(l)-B(6) B(2)-C(l)-B(6) B(5)-C(l)-B(6) C (l)-B(2)-B(ll) C(l)-B(2)-B(7) B(11)-B(2)-B(7) C (l)-B (2)-a(2) B(11)-B(2)-C1(2) B(7)-B(2)-CI(2) C(l)-B(2)-B(3) B(11)-B(2)-B(3) B(7)-B(2)-B(3) CI(2)-B(2)-B(3) C(l)-B(2)-B(6) B(11)-B(2)-B(6) B(7)-B(2)-B(6) Cl(2)-B(2)-B(6) B(3)-B(2)-B(6) C(l)-B(3)-B(7) C(1)-B(3)-CI(3) B(7)-B(3)-C1(3) C(l)-B(3)-B(2) B(7)-B(3)-B(2) CI(3)-B(3)-B(2) C(l)-B(3)-B(8) B(7)-B(3)-B(8) Cl(3)-B(3)-B(8) B(2)-B(3)-B(8) C(l)-B(3)-B(4) B(7)-B(3)-B(4) CI(3)-B(3)-B(4) B(2)-B(3)-B(4) B(8)-B(3)-B(4) C(l)-B(4)-B(8) C(l)-B(4)-B(9) B(8)-B(4)-B(9) C(l)-B(4)-B(3) B(8)-B(4)-B(3) B(9)-B(4)-B(3) C(1)-B(4)-CI(4) B(8)-B(4)-C1(4) B(9)-B(4)-CI(4) B(3)-B(4)-C1(4) C(l)-B(4)-B(5) B(8)-B(4)-B(5) B(9)-B(4)-B(5) B(3)-B(4)-B(5)

62.6(2) 114.0(3) 62.2(2) 62.9(2) 114.9(3) 114.6(3) 114.4(3) 114.3(3) 62.8(2) 62.6(2) 104.5(3) 104.8(3) 60.6(2) 120.5(3) 125.5(3) 125.8(3) 58.9(2) 108.3(3) 59.9(2) 120.2(2) 58.7(2) 59.7(2) 108.3(3) 119.6(3) 108.3(3) 104.9(3) 121.1(3) 125.2(3) 59.0(2) 59.9(2) 120.3(3) 104.6(3) 61.0(2) 124.8(3) 108.7(3) 58.4(2) 108.0(3) 120.4(3) 107.9(3) 59.4(2) 105.7(3) 105.3(3) 61.1(3) 59.0(2) 60.3(2) 109.1(3) 121.0(3) 124.6(3) 124.2(3) 120.4(3) 59.0(2) 109.1(3) 59.8(2) 108.7(3)

Cl(4)-B(4)-B(5) C(l)-B(5)-B(10) C(1)*B(5)-C1(5) B(10)-B(5)-C1(5) C(l)-B(5)-B(9) B(10)-B(5)-B(9) Cl(5)-B(5)-B(9) C(1)-B(5>B(4) B(10)-B(5)-B(4) Cl(5)-B(5)-B(4) B(9)-B(5>B(4) C(l)-B(5)-B(6) B(10)-B(5)-B(6) a(5)-B(5)-B(6) B(9)-B(5)-B(6) B(4)-B(5)-B(6) C(l)-B(6)-B(10) C (l)-B (6)-B (ll) B(10)-B(6)-B(ll) C(1)-B(6)-C1(6) B(10)-B(6)-CI(6) B(11)-B(6)-C1(6) C(l)-B(6)-B(2) B(10)-B(6)-B(2) B(ll)-B(6)-B(2) Cl(6)-B(6)-B(2) C(l)-B(6)-B(5) B(10)-B(6)-B(5) B(ll)-B(6)-B(5) CI(6)-B(6)-B(5) B(2)-B(6)-B(5) B(3)-B(7)-B(2) B(3)-B(7)-C1(7) B(2)-B(7)-CI(7) B(3)-B(7)-B(ll) B(2)-B(7)-B(ll) Cl(7)-B(7)-B(ll) B(3)-B(7)-B(8) B(2)-B(7)-B(8) Cl(7)-B(7)-B(8) B(ll)-B(7)-B(8) B(3)-B(7)-B(12) B(2)-B(7)-B(12) Cl(7)-B(7)-B(12) B(11)-B(7)-B(12) B(8)-B(7)-B(12) B(4)-B(8)-B(3) B(4)-B(8)-C1(8) B(3)-B(8)-C1(8) B(4)-B(8)-B(9) B(3)-B(8)-B(9) Cl(8)-B(8)-B(9) B(4)-B(8)-B(7) B(3)-B(8)-B(7)

119.5(3) 104.1(3) 120.8(3) 126.3(3) 104.3(3) 61.0(2) 125.1(3) 58.1(2) 107.7(3) 120.0(3) 59.5(2) 58.7(2) 59.4(2) 120.9(3) 108.3(3) 107.2(3) 104.4(3) 104.2(3) 60.8(2) 120.8(3) 125.8(3) 125.6(3) 58.5(2) 108.1(3) 59.5(2) 120.0(3) 58.7(2) 59.6(2) 108.2(3) 120.3(3) 107.9(3) 60.2(2) 120.5(3) 122.3(3) 107.9(3) 59.7(2) 123.4(3) 59.8(2) 108.0(3) 120.3(3) 108.1(3) 107.7(3) 107.5(3) 122.4(3) 59.8(2) 60.2(2) 60.3(2) 121.2(3) 119.8(3) 59.6(2) 107.9(3) 123.4(3) 107.4(3) 59.2(2)

279


CI(8)-B(8)-B(7) B(9)-B(8)-B(7) B(4)-B(8)-B(12) B(3)-B(8)-B(12) Cl(8)-B(8)-B(12) B(9)-B(8)-B(12) B(7)-B(8)-B(12) B(4)-B(9)-B(5) B(4)-B(9)-C1(9) B(5)-B(9)-C1(9) B(4)-B(9)-B(12) B(5)-B(9)-B(12) CI(9)-B(9)-B(12) B(4)-B(9)-B(8) B(5)-B(9)-B(8) Cl(9)-B(9)-B(8) B(12)-B(9)-B(8) B(4)-B(9)-B(10) B(5)-B(9)-B(10) Cl(9)-B(9)-B(10) B(12)-B(9)-B(10) B(8)-B(9)-B(10) B(6)-B( 10)-B(5) B(6)-B(10)-B(12) B(5)-B( 10)-B( 12) B(6)-B( 10)-C1( 10) B(5)-B( 10)-C1( 10) B( 12)-B( 10)-C1( 10) B(6)-B(10)-B(ll) B(5)-B(10)-B(ll) B(12)-B(10)-B(l 1) CI( 10)-B( 10)-B( 11) B(6)-B(10)-B(9) B(5)-B(10)-B(9) B(12)-B(10)-B(9) Cl( 10)-B( 10)-B(9) B(11)-B(10)-B(9) B(2)-B(ll)-B(6) B(2)-B(ll)-B(12) B(6)-B(ll)-B(12) B(2)-B(ll)-B(7) B(6)-B(ll)-B(7) B(12)-B(ll)-B(7) B(2)-B(ll)-B(10) B(6)-B(ll)-B(10) B(12)-B(ll)-B(10) B(7)-B(ll)-B(10) B(2)-B(l l)-C l(ll) B(6)-B(11)-C1(11) B(12)-B(11)-CI(11) B(7)-B(11)-C1(11) B(10)-B(11)-C1(11) Cl(12)-B(12)-B(10) CI(12)-B(12)-B(11) B(10)-B(12)-B(l 1) Cl( 12)-B( 12)-B(9)

121.5(3) 107.8(3) 107.0(3) 107.1(3) 124.2(3) 59.8(2) 59.9(2) 60.7(2) 121.5(3) 121.1(3) 107.1(3) 107.4(3) 122.9(3) 59.3(2) 108.3(3) 121.7(3) 60.3(2) 107.3(3) 59.3(2) 122.7(3) 59.6(2) 107.8(3) 61.0(2) 108.2(3) 108.1(3) 120.8(3) 120.4(3) 122.5(3) 59.9(2) 108.6(3) 60.0(2) 122.3(3) 108.6(3) 59.7(2) 60.1(2) 121.6(3) 108.0(3) 60.9(2) 108.0(3) 107.7(3) 59.7(2) 108.5(3) 60.4(2) 108.0(3) 59.3(2) 59.9(2) 108.3(3) 121.2(3) 120.4(3) 122.7(3) 122.4(3) 121.6(3) 122.4(3) 122.1(3) 60.1(2) 121.5(3)

B(10)-B(12)-B(9) B(11)-B(12)-B(9) Cl(12)-B(12)-B(7) B(10)-B(12)-B(7) B(11)-B(12)-B(7) B(9)-B(12)-B(7) C!( 12)-B( 12)-B(8) B(10)-B(12)-B(8) B(ll)-B(12)-B(8) B(9)-B(12)-B(8) B(7)-B(12)-B(8) B(23)-C(2)-B(22) B(23)-C(2)-B(26) B(22)-C(2)-B(26) B(23)-C(2)-B(24) B(22)-C(2)-B(24) B(26)-C(2)-B(24) B(23)-C(2)-B(25) B(22)-C(2)-B(25) B(26)-C(2)-B(25) B(24)-C(2)-B(25) C(2)-B(22)-B(27) C(2)-B(22)-B(31) B(27)-B(22)-B(31) C(2)-B(22)-C1(22) B(27)-B(22)-C1(22) B(31)-B(22)-CI(22) C(2)-B(22)-B(23) B(27)-B(22)-B(23) B(31)-B(22)-B(23) Cl(22)-B(22)-B(23) C(2)-B(22)-B(26) B(27)-B(22)-B(26) B(31)-B(22)-B(26) Cl(22)-B(22)-B(26) B(23)-B(22)-B(26) C(2)-B(23)-C1(23) C(2)-B(23)-B(27) Cl(23)-B(23)-B(27) C(2)-B(23)-B(28) C!(23)-B(23)-B(28) B(27)-B(23)-B(28) C(2)-B(23)-B(22) Cl(23)-B(23)-B(22) B(27)-B(23)-B(22) B(28)-B(23)-B(22) C(2)-B(23)-B(24) Cl(23)-B(23)-B(24) B(27)-B(23)-B(24) B(28)-B(23)-B(24) B(22)-B(23)-B(24) C(2)-B(24)-B(29) C(2)-B(24)-B(28) B(29)-B(24)-B(28) C(2)-B(24)-CI(24) B(29)-B(24)-C1(24)

60.3(2) 108.4(3) 121.4(3) 107.9(3) 59.8(2) 108.0(3) 121.0(3) 108.1(3) 107.9(3) 59.9(2) 59.9(2) 62.5(2) 114.7(3) 63.0(2) 63.2(2) 114.7(3) 114.0(3) 114.6(3) 114.3(3) 62.2(2) 62.3(2) 104.5(3) 104.3(3) 61.3(2) 121.9(3) 125.1(3) 124.1(3) 58.4(2) 60.0(2) 108.9(3) 121.0(3) 58.6(2) 108.0(3) 59.0(2) 120.1(3) 107.7(3) 121.2(3) 104.3(3) 125.7(3) 104.2(3) 125.1(3) 61.0(2) 59.0(2) 120.7(3) 59.1(2) 108.1(3) 58.8(2) 119.9(3) 108.0(3) 59.2(2) 108.3(3) 104.4(3) 104.0(3) 60.8(2) 120.5(3) 126.0(3)


B(28)-B(24)-C1(24) C(2)-B(24)-B(25) B(29)-B(24)-B(25) B(28)-B(24)-B(25) Cl(24)-B(24)-B(25) C(2)-B(24)-B(23) B(29)-B(24)-B(23) B(28)-B(24)-B(23) Cl(24)-B(24)-B(23) B(25)-B(24)-B(23) C(2)-B(25)-B(29) C(2)-B(25)-B(30) B(29)-B(25)-B(30) C(2)-B(25)-CI(25) B(29)-B(25)-C1(25) B(30)-B(25)-C1(25) C(2)-B(25)-B(26) B(29)-B(25)-B(26) B(30)-B(25)-B(26) Cl(25)-B(25)-B(26) C(2)-B(25)-B(24) B(29)-B(25)-B(24) B(30)-B(25)-B(24) Cl(25)-B(25)-B(24) B(26)-B(25)-B(24) C(2)-B(26)-B(31) C(2)-B(26)-CI(26) B(31)-B(26)-C1(26) C(2)-B(26)-B(30) B(31)-B(26)-B(30) Cl(26)-B(26)-B(30) C(2)-B(26)-B(25) B (31)-B(26)-B(25) CI(26)-B(26)-B(25) B(30)-B(26)-B(25) C(2)-B(26)-B(22) B(31)-B(26)-B(22) CI(26)-B(26)-B(22) B(30)-B(26)-B(22) B(25)-B(26)-B(22) B(22)-B(27)-B(23) B(22)-B(27)-C1(27) B(23)-B(27)-CI(27) B(22)-B(27)-B(31) B(23)-B(27)-B(31) CI(27)-B(27)-B(31) B(22)-B(27)-B(32) B(23)-B(27)-B(32) CI(27)-B(27)-B(32) B(31)-B(27)-B(32) B(22)-B(27)-B(28) B(23)-B(27)-B(28) Cl(27)-B(27)-B(28) B(31)-B(27)-B(28) B(32)-B(27)-B(28) B(24)-B(28)-B(23)

126.0(3) 59.3(2) 59.2(2) 107.9(3) 120.1(3) 58.0(2) 108.1(3) 59.6(2) 120.1(3) 107.9(3) 104.0(3) 104.3(3) 60.8(2) 120.7(3) 125.7(3) 126.0(3) 58.4(2) 108.2(3) 59.8(2) 120.4(3) 58.4(2) 59.6(2) 108.3(3) 119.7(3) 107.7(3) 104.7(3) 120.2(3) 126.1(3) 104.8(3) 60.9(3) 125.5(3) 59.4(2) 108.5(3) 119.0(3) 59.4(2) 58.5(2) 59.6(2) 120.6(3) 108.2(3) 108.4(3) 60.9(2) 121.7(3) 121.2(3) 59.8(2) 108.3(3) 122.2(3) 108.1(3) 108.0(3) 121.7(3) 59.9(2) 108.4(3) 59.6(2) 121.3(3) 107.9(3) 60.1(2) 61.2(2)

B(24)-B(28)-CI(28) B(23)-B(28)-C1(28) B(24)-B(28)-B(29) B(23)-B(28)-B(29) Cl(28)-B(28)-B(29) B(24)-B(28)-B(27) B(23)-B(28)-B(27) CI(28)-B(28)-B(27) B(29)-B(28)-B(27) B(24)-B(28)-B(32) B(23)-B(28)-B(32) Cl(28)-B(28)-B(32) B(29)-B(28)-B(32) B(27)-B(28)-B(32) B(25)-B(29)-B(24) B(25>B(29)-B(30) B(24)-B(29)-B(30) B(25)-B(29)-B(28) B(24)-B(29)-B(28) B(30)-B(29)-B(28) B(25)-B(29)-C1(29) B(24)-B(29)-C1(29) B(30)-B(29)-C1(29) B(28)-B(29)-C1(29) B(25)-B(29)-B(32) B(24)-B(29)-B(32) B(30)-B(29)-B(32) B(28)-B(29)-B(32) CI(29)-B(29)-B(32) B(25)-B(30)-B(26) B(25)-B(30)-B(32) B(26)-B(30)-B(32) B(25)-B(30)-C1(30) B(26)-B(30)-C1(30) B(32)-B(30)-C1(30) B(25)-B(30)-B(29) B(26)-B(30)-B(29) B(32)-B(30)-B(29) Cl(30)-B(30)-B(29) B(25)-B(30)-B(31) B(26)-B(30)-B(31) B(32)-B(30)-B(31) Cl(30)-B(30)-B(31) B(29)-B(30)-B(31) B(26)-B(31)-B(22) B(26)-B(31)-CI(31) B(22)-B(31)-Cl(31) B(26)-B(31)-B(30) B(22)-B(31)-B(30) Cl(31)-B (31)-B(30) B(26)-B(31)-B(27) B(22)-B(31)-B(27) Cl(31)-B(31)-B(27) B(30)-B(31)-B(27) B(26)-B(31)-B(32) B(22)-B(31)-B(32)

121.6(3) 121.2(3) 59.6(2) 108.4(3) 122.2(3) 108.4(3) 59.4(2) 121.5(3) 107.9(3) 107.9(3) 107.7(3) 122.0(3) 59.9(2) 59.9(2) 61.3(3) 59.8(2) 108.8(3) 108.6(3) 59.6(2) 108.1(3) 121.9(3) 121.7(3) 121.5(3) 121.4(3) 107.9(3) 108.2(3) 59.7(2) 60.4(2) 121.2(3) 60.8(2) 108.1(3) 107.7(3) 121.0(3) 121.2(3) 122.4(3) 59.4(2) 107.9(3) 60.4(2) 122.2(3) 108.2(3) 59.2(2) 60.4(2) 121.7(3) 108.4(3) 61.4(3) 121.3(3) 120.9(3) 59.9(2) 108.8(3) 122.2(3) 108.0(3) 58.9(2) 121.9(3) 107.7(3) 107.6(3) 107.5(3)


CI(31)-B(31)-B(32) B(30)-B(31)-B(32) B(27)-B(31)-B(32) B(30)-B(32)-C1(32) B(30)-B(32)-B(29) Cl(32)-B(32)-B(29) B(30)-B(32)-B(27) Cl(32)-B(32)-B(27) B(29)-B(32)-B(27) B(30)-B(32)-B(31) CI(32)-B(32)-B(31) B(29)-B(32)-B(31) B(27)-B(32)-B(31) B(30)-B(32)-B(28)

Cl(32)-B(32)-B(28) B(29)-B(32)-B(28) B(27)-B(32)-B(28) B(31)-B(32)-B(28) C(5)-N(l)-C(3) C(5)-N(l)-C(4) C(3)-N(l)-C(4) 0(3)-C(5)-N(l) C(8)-N(2)-C(6) C(8)-N(2)-C(7) C(6)-N(2)-C(7) CX4VQ8)-N(2)

122.5(3) 59.5(2) 60.0(2) 121.6(3) 60.0(2) 121.1(3) 108.1(3) 122.3(3) 107.7(3) 60.1(2) 122.5(3) 107.8(3) 60.0(2) 107.8(3)

121.4(3) 59.7(2) 60.0(2) 107.9(3) 121.2(4) 121.3(4) 117.5(4) 121.9(4) 122.3(4) 119.0(4) 118.7(4) 121.6(4)

282


Compound V1I-7 A tom ic coordinates and thermal parameters.

X

C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B( 10) B( 11) B(12) CI(2) Cl(3) Cl(4) Cl(5) Ct(6) Br(7) Br(8) Br(9) Br(10) Br(l 1) Br(12)

ccn

B(13) B(14) B(15) B(16) B(17) B(18) B(19) B(20) B(21) B(22) B(23) CI( 13) Cl( 14) Cl( 15) Cl(16) 0 (1 7 ) Br(18) Br(19) Br(20) Br(21) Br(22) Br(23) C(l") B(24) B(25) B(26)

-6123(13) -6237(15) -5392(19) -6266(10) -7618(17) -7688(14) -6517(16) -6462(9) -7736(7) -8729(17) -7946(14) -8060(20) -5466(4) -3696(4) -5247(5) -8000(5) -8155(5) -5871(2) -5712(2) -8628(2) -10554(2) -8855(2) -9100(2) -1642(13) -1551(14) -528(14) -1440(11) -2986(11) -3040(15) -1320(8) -1141(13) -2801(12) -3862(13) -2845(9) -2800(20) -753(4) 1225(4) -688(5) -3782(4) -3835(5) -292(2) -249(2) -3577(2) -5698(2) -3706(2) -3405(2) -1022(14) -2477(14) -1250(19) -432(16)

y 6241(12) 6407(12) 7173(18) 7302(7) 6599(13) 6099(15) 7742(13) 8231(7) 8029(9) 7261(13) 7071(14) 8245(16) 5631(3) 6994(4) 7285(4) 6005(4) 4960(4) 8333(2) 9442(2) 8777(2) 7249(2) 6955(2) 9395(2) 1114(11) 1705(14) 1927(8) 1811(10) 1444(8) 1459(8) 2870(8) 2938(10) 2663(9) 2448(8) 2634(15) 3455(14) 1148(3) 1482(3) 1132(4) 616(3) 636(3) 3746(1) 3722(2) 3131(2) 2780(2) 3188(1) 4778(2) 1429(7) 1696(6) 2464(8) 2486(14)

z

-3088(5) -2494(5) -2888(6) -3447(4) -3408(5) -2801(4) -2464(5) -3050(4) -3392(4) -2984(5) -2379(5) -2771(6) -2040(1) -2858(2) -3996(1) -3923(1) -2713(2) -1886(1) -3172(1) -3901(1) -3049(1) -1793(1) -2549(1) -301(4) 210(7) -320(4) -858(6) -649(5) 9(4) 0(5) -696(5) -855(5) -304(5) 153(5) -356(8) 739(1) -314(2) -1372(1) -951(2) 350(1) 333(1) -1070(1) -1492(1) -325(1) 771(1) -392(1) -3489(4) -3192(5) -3166(4) -3740(6)

U(eq) 57(5) 49(5) 72(7) 63(6) 54(5) 65(5) 49(5) 62(5) 43(5) 60(5) 51(5) 76(7) 67(1) 91(2) 89(2) 81(2) 84(2) 77(1) 97(1) 81(1) 77(1) 71(1) 83(1) 47(4) 56(6) 58(6) 79(8) 66(6) 54(5) 77(6) 120(11) 59(6) 46(5) 76(7) 104(8) 66(1) 66(1) 75(2) 81(1) 74(1) 82(1) 84(1) 91(1) 75(1) 69(1) 86(1) 64(6) 49(5) 77(7) 78(5)


B(27) B(28) B(29) B(30) B(31) B(32) B(33) B(34) Cl(24) Cl(25) Cl(26) Cl(27) CI(28) Br(29) Br(30) Br(31) Br(32) Br(33) Br(34) 0(1) N (l) C (ll)

0(12) 0(13) 0(2) N(2) 0(21) C(22) 0(23) 0(3) N(3) 0(31) 0(32) 0(33) 0(4) 0 (5 ) 0 (6 )

-1070(20) -2290(18) -2907(15) -1671(14) -1669(10) -2742(14) -3704(16) -3105(10) -2797(5) -434(5) 1285(4) -28(5) -2530(6) -3997(2) -1256(2) -997(2) -3528(2) -5396(2) -4381(2) 7082(17) 7008(13) 6580(20) 7080(30) 7074(14) 2341(17) 2379(11) 2910(20) 2080(20) 2190(18) 6963(12) 7565(13) 7335(15) 8136(17) 6955(17) 5848(16) 1692(15) 7287(16)

1692(13) 1192(11) 2937(7) 3481(11) 3086(18) 2228(17) 2175(13) 3318(17) 952(3) 2572(4) 2592(5) 986(4) -26(4) 3710(1) 4779(2) 3673(2) 1941(2) 1962(2) 4337(1) 6467(10) 8117(12) 8111(18) 9163(17) 7369(11) 3817(6) 2175(5) 2194(16) 1228(13) 3013(7) 8783(5) 7145(4) 6226(6) 7392(9) 7876(5) 10054(8) 5012(7) 5275(7)

-4141(8) -3786(5) -3246(7) -3587(5) -4199(5) -4249(6) -3653(5) -3883(5) -2683(1) -2605(1) -3749(2) -4537(2) -3857(2) -2783(1) -3485(1) -4759(1) -4836(1) -3612(1) -4140(1) 1725(5) 1795(5) 2322(7) 1561(10) 1546(5) 1511(4) 1482(3) 966(6) 1711(7) 1694(4) -4937(4) -4811(4) -4956(5) -4360(5) -5068(4) -5574(4) 2147(3) 1081(4)

73(6) 51(5) 71(6) 37(4) 98(7) 66(6) 49(5) 74(7) 82(2) 91(2) 103(2) 89(2) 91(2) 75(1) 95(1) 91(1) 90(1) 76(1) 76(1) 113(6) 83(5) 121(9) 181(14) 59(5) 122(7) 54(4) 146(8) 121(7) 101(8) 107(6) 113(7) 136(11) 161(9) 162(8) 141(7) 116(6) 115(6)

Bond lengths

C(l)-B(4) C(l)-B(5) C(l)-B(6) B(2)-C1(2) B(2)-B(3) B(2)-B(7) B(2)-B(6) B (2)-B (ll) B(3)-CI(3) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(4)-B(8) B(4)-B(9) B(4)-B(5)

B(4)-CI(4) B(5)-CI(5) B(5)-B(6) * B(5)-B(10) B(5)-B(9) B(6)-C1(6) B (6)-B (ll) B(6)-B(10) B(7)-B(8) B(7)-B(12) B (7)-B (ll) B(7)-BB(17) C(1>B(16) C(1>B(15) B(13)-B(22) B(13)-B(17) B(13)-B(18) B(13)-C1(13) B(13)-B(14) B(14)-B(18) B(14)-B(19) B(14)-B(15) B(14)-C1(14) B(15)-B(20) B(15)-B(19) B(15)-C1(15) B(15)-B(16) B(16)-C1(16) B(16)-B(20) B(16)-B(17) B(16)-B(21) B(17)-B(21) B(17)-B(22) B(17)-C1(1T) B(18)-B(22) B(18)-B(23) B(18)-B(19) B(18)-Br(18) B(19)-Br(19) B(19)-B(20) B(19)-B(23) B(20)-B(23) B(20)-B(21) B(20)-Br(20) B(21)-B(22) B(21)-B(23) B(21)-Br(21) B(22)-B(23) B(22)-Br(22) B(23)-Br(23) C(l")-B(28) C(l")-B(26)

1.755(19) 1.870(10) 1.89(2) 1.72(3) 1.847(19) 1.898(18) 1.858(15) 1.89(3) 1.89(2) 1.678(19) 1.693(17) 1.794(19) 1-71(2) 1-72(2) 1-72(2) 1.769(17) 1.82(2) 1.689(13) 1.741(17) 1.783(19) 1.824(14) 1.692(13) 1.69(2) 1.817(15) 1.819(18) 1.733(12) 1.778(17) 1.800(18) 1.818(16) 1.700(13) 1.71(2) 1.726(14) 1.696(12) 1.88(2) 1.910(19) 1.970(11) 1.795(12) 1.869(19) 1.99(3) 1.78(3) 1.890(19) 1.974(14) 1.697(19) 1.88(3) 1.885(13) 1.76(3) 2.018(14) 1.827(18) 1.63(2) 1.76(2)

C(l")-B(27) B(24)-B(29) B(24)-C1(24) B(24)-B(25) B(24)-B(28) B(24)-B(33) B(25)-B(29) B(25)-B(26) B(25)-CI(25) B(25)-B(30) B(26)-B(27) B(26)-B(30) B(26)-C1(26) B(26)-B(31) B(27)-C1(27) B(27)-B(28) B(27)-B(32) B(27)-B(31) B(28)-C1(28) B(28)-B(33) B(28)-B(32) B(29)-B(30) B(29)-B(34) B(29)-B(33) B(29)-Br(29) B(30)-B(34) B(30)-B(31) B(30)-Br(30) B(3l)-B(34) B(31)-B(32) B(31)-Br(31) B(32)-B(34) B(32)-Br(32) B(32)-B(33) B(33)-Br(33) B(33)-B(34) B(34)-Br(34) O d)-Q 13) N ( i) - a i3 ) N(1)-Q11) N(l)-C(12) 0(2)-C(23) N(2)-C(23) N(2)-C(22) N(2)-C(21) 0(3)-C(33) N(3)-C(33) N(3)-C(31) N(3)-Q32)

1.81(2) 1.693(11) 1.752(13) 1.76(2) 1.787(19) 1.84(2) 1.75(2) 1.77(2) 1.786(14) 1.780(18) 1.77(3) 1.79(2) 1.800(17) 1.88(2) 1.73(2) 1.78(3) 1.80(2) 1.92(3) 1.739(16) 1.88(2) 1.88(2) 1.80(2) 1.81(2) 1.84(2) 1.923(15) 1.745(19) 1.78(2) 1.919(16) 1.700(13) 1.74(3) 1.872(16) 1.82(3) 1.891(17) 1.90(2) 1.813(17) 1.85(3) 1.896(16) 1.31(2) 1.24(2) 1.50(2) 1.56(3) 1.221(15) 1.292(11) 1.49(2) 1.51(2) 1.306(10) 1.293(12) 1.388(11) 1.448(16)

Bond angles

B(5)-C(l)-B(6) Cl(2)-B(2)-B(3)

62.2(8) 110.3(9)

59.1(8) 122.9(11)

285


Cl(2)-B(2)-B(7) B(3)-B(2)-B(7) Cl(2)-B(2)-B(6) B(3)-B(2)-B(6) B(7)-B(2)-B(6) Cl(2)-B(2)-B(l 1) B(3)-B(2)-B(l 1) B(7)-B(2)-B(ll) B(6)-B(2)-B(ll) Cl(3)-B(3)-B(8) CI(3)-B(3)-B(7) B(8)-B(3)-B(7) Cl(3)-B(3)-B(4) B(8)-B(3)-B(4) B(7)-B(3)-B(4) CI(3)-B(3)-B(2) B(8)-B(3)-B(2) B(7)-B(3)-B(2) B(4)-B(3)-B(2) B(8)-B(4)-B(9) B(8)-B(4)-C(l) B(9)-B(4)-C(l) B(8)-B(4)-B(3) B(9)-B(4)-B(3) C(l)-B(4)-B(3) B(8)-B(4)-B(5) B(9)-B(4)-B(5) C(l)-B(4)-B(5) B(3)-B(4)-B(5) B(8)-B(4)-C1(4) B(9)-B(4)-C1(4) C(1)-B(4)-C1(4) B(3)-B(4)-CI(4) B(5)-B(4)-C1(4) CI(5)-B(5)-B(6) CI(5)-B(5)-C(1) B(6)-B(5)-C(l) CI(5)-B(5)-B(10) B(6)-B(5)-B(10) C(l)-B(5)-B(10) Cl(5)-B(5)-B(4) B(6)-B(5)-B(4) C(l)-B(5)-B(4) B(10)-B(5)-B(4) Cl(5)-B(5)-B(9) B(6)-B(5)-B(9) C(l)-B(5)-B(9) B(10)-B(5)-B(9) B(4)-B(5)-B(9) Cl(6)-B(6)-B(5) Cl(6)-B(6)-B(l 1) B(5)-B(6)-B(l 1) Cl(6)-B(6)-C(l) B(5)-B(6)-C(l) B(11)-B(6)-C(1) CI(6)-B(6)-B(2)

123.6(10) 58.3(10) 120.9(11) 110.1(10) 104.7(11) 119.4(9) 108.5(12) 60.1(9) 57.1(9) 129.6(15) 128.0(13) 59.0(9) 123.4(10) 57-5(7) 103.9(11) 117.0(12) 108.5(12) 61.7(10) 105.8(13) 59.8(5) 105.1(8) 113.9(8) 60.0(9) 111.9(9) 57.7(10) 111.4(8) 67.3(8) 60.9(8) 110.2(10) 124.2(7) 123.5(7) 117.0(7) 114.9(8) 120.3(8) 124.2(13) 122.1(11) 61.4(8) 127.7(12) 62.1(9) 106.2(10) 118.3(10) 107.8(11) 56.9(8) 103.6(11) 122.4(9) 109.4(11) 99.9(11) 60.7(8) 53.7(6) 118.6(11) 125.5(9) 110.0(13) 120.9(11) 59.5(8) 103.8(12) 120.5(10)

B(5)-B(6)-B(2) B(ll)-B(6)-B(2) C(l)-B(6)-B(2) CI(6)-B(6)-B( 10) B(5)-B(6)-B(10) B(11)-B(6)-B(10) C(1)*B(6)-B(10) B(2)-B(6)-B(10) B(8)-B(7)-B(3) B(8)-B(7)-B(2) B(3)-B(7)-B(2) B(8)-B(7)-B(12) B(3)-B(7)-B(12) B(2)-B(7)-B(12) B(8)-B(7)-B(l 1) B(3)-B(7)-B(l 1) B(2)-B(7)-B(ll) B(12)-B(7)-B(ll) B(8)-B(7)-Br(7) B(3)-B(7>Br(7) B(2)-B(7)-Br(7) B(12)-B(7)-Br(7) B(11)-B(7)-Br(7) B(9)-B(8)-B(4) B(9)-B(8)-B(7) B(4)-B(8)-B(7) B(9)-B(8)-B(3) B(4)-B(8>B(3) B(7)-B(8)-B(3) B(9)-B(8)-B(12) B(4)-B(8)-B(12) B(7)-B(8)-B(12) B(3)-B(8)-B(12) B(9)-B(8)-Br(8) B(4)-B(8)-Br(8) B(7)-B(8)-Br(8) B(3)-B(8)-Br(8) B(12)-B(8)-Br(8) B(8)-B(9)-B(4) B(8)-B(9)-B(12) B(4)-B(9)-B( 12) B(8)-B(9)-Br(9) B(4)-B(9)-Br(9) B(12)-B(9)-Br(9) B(8)-B(9)-B( 10) B(4)-B(9)-B( 10) B(12)-B(9)-B(10) Br(9)-B(9)-B( 10) B(8)-B(9)-B(5) B(4)-B(9)-B(5) B(12)-B(9)-B(5) Br(9)-B(9)-B(5) B(10)-B(9)-B(5) B(12)-B(10)-B(5) B(12)-B(10)-B(6) B(5)-B(10)-B(6)

105.9(11) 62.9(9) 53.7(8) 127.3(10) 59.4(8) 61.2(9) 102.8(11) 108.3(13) 60.1(9) 108.0(10) 60.0(11) 60.8(8) 110.0(11) 110.0(12) 110.6(10) 111.5(13) 62.0(9) 61.4(10) 124.3(11) 119.4(11) 117.7(9) 123.2(11) 117.8(9) 60.3(5) 113.1(9) 109.2(9) 114.5(10) 62.5(8) 60.9(8) 60.2(7) 106.9(9) 63.1(8) 112.5(11) 118.6(7) 122.1(7) 119.6(8) 117.2(9) 121.4(9) 59.9(5) 63.2(9) 108.9(9) 131.6(8) 125.3(7) 123.6(9) 105.5(8) 103.8(9) 56.2(9) 116.7(6) 105.2(8) 59.0(7) 102.1(10) 117.4(7) 55.7(8) 109.9(13) 109.3(12) 585(8)

286


B( 12)-B( 10)-B( 11) B(5)-B(10)-B(l 1) B(6)-B(10)-B(l 1) B( 12)-B( 10)-Br( 10) B(5)-B( 10)-Br( 10) B(6)-B(10)-Br(10) B(ll)-B(10)-Br(10) B(12)-B(10)-B(9) B(5)-B(10)-B(9) B(6)-B(10)-B(9) B(11)-B(10)-B(9) Br( 10)-B( 10)-B(9) B(6)-B(ll)-B(10) B(6)-B(ll)-B(7) B(10)-B(ll)-B(7) B(6)-B(l 1)-Br(l 1) B (10)-B (ll)-B r(ll) B(7)-B(l 1)-Br(l 1) B(6)-B(l 1)-B(12) B(10)-B(l 1)-B(12) B(7)-B(l 1)-B(12) B r(ll)-B (ll)-B (12) B(6)-B(ll)-B(2) B(10)-B(l 1)-B(2) B(7)-B(ll)-B(2) Br( 11)-B( 11)-B(2) B(12)-B(l 1)-B(2) B(10)-B(12)-B(9) B(10)-B(12)-B(8) B(9)-B(12)-B(8) B(10)-B(12)-B(7) B(9)-B(12)-B(7) B(8)-B(12)-B(7) B(10)-B(12)-B(l 1) B(9)-B(12)-B(ll) B(8)-B(12)-B(ll) B(7)-B(12)-B(U) B( 10)-B( 12)-Br( 12) B(9)-B(12)-Br(12) B(8)-B(12)-Br(12) B(7)-B( 12)-Br( 12) B(11)-B(12)-Br(12) B(17)-C(1>B(16) B(17)-C(1>B(15) B(16)-C(1>B(15) B(22)-B( 13)-B( 17) B(22)-B( 13)-B( 18) B( 17)-B( 13)-B(18) B(22)-B(13)-CI(13) B( 17)-B( 13)-C1( 13) B(18)-B(13)-CI(13) B(22)-B( 13)-B( 14) B(17)-B(13)-B(14) B( 18)-B( 13)-B( 14) CI(13)-B(13)-B(14) B(18)-B(14)-B(19)

63.7(10) 106.4(11) 57.7(8) 124.0(12) 119.1(10) 118.4(11) 120.8(10) 57.8(9) 63.6(9) 108.8(10) 108.6(11) 124.1(8) 61.0(9) 105.2(10) 102.1(11) 122.2(12) 124.1(10) 124.7(10) 104.9(10) 55.0(9) 59.0(10) 124.0(11) 60.0(8) 106.0(10) 57.9(9) 123.4(9) 104.9(11) 66.0(9) 107.9(12) 56.6(7) 107.6(14) 104.3(12) 56.2(9) 61.3(10) 113.0(13) 105.4(12) 59.6(9) 122.4(14) 123.1(11) 124.0(13) 120.7(11) 118.8(10) 64.6(8) 115.3(9) 62.8(7) 59.8(8) 59.2(8) 109.0(10) 130.3(12) 124.4(12) 121.4(11) 103.1(11) 108.7(11) 56.8(7) 117.3(9) 67.7(8)

B(18)-B(14)-B(15) B(19)-B(14)-B(15) B( 18)-B( 14)-B( 13) B(19)-B(14)-B(13) B(15)-B(14)-B(13) B( 18)-B( 14)-Ci( 14) B( 19)-B( 14)-CI( 14) B(15)-B(14)-C1(14) B( 13)-B( 14)-CI( 14) B(20)-B(15)-B(19) B(20)-B( 15)-B(14) B(19)-B(15)-B(14) B(20)-B( 15)-C( 1^ B(19)-B(15)-C(l') B(14)-B(15)-C(l') B(20)-B(15)-C1(15) B(19)-B(15)-a(15) B(14)-B(15)-a(15) C(1>B(15)-CI(15) B(20)-B( 15)-B( 16) B(19)-B(15)-B(16) B(14)-B(15)-B(16) C(1>B(15)-B(16) Cl(15)-B(15)-B(16) C (i> B (i6 )-c i(i6 ) CX1>B(16)-B(20) Q(16)-B(16)-B(20) C(1>B(16)-B(17) C1(16)-B(16>B(17) B(20)-B(16)-B(17) C(1>B(16)-B(15) Cl(16)-B(16)-B(15) B(20)-B(16)-B(15) B(17)-B(16)-B(15) C(1>B(16)-B(21) Cl(16)-B(16)-B(21) B(20)-B( 16)-B(21) B(17)-B(16)-B(21) B(15)-B(16)-B(21) C(n-B(17)-B(21) C(1>B(17)-B(22) B(21)-B(17)-B(22) C(1>B(17)-B(13) B(21)-B(17)-B(13) B(22)-B(17)-B(13) C(1>B(17)-CI(17) B(21)-B(17)-C1(17) B(22)-B( 17)-Cl( 17) B(13)-B(17)-C1(17) C(1>B(17)-B(16) B(21)-B(17)-B(16) B(22)-B(17)-B(16) B(13)-B(17)-B(16) Cl(17)-B(17)-B(16) B( 14)-B( 18)-B(22) B(14)-B(18)-B(13)

108.4(9) 57.4(8) 58.6(8) 115.0(9) 108.2(10) 126.5(9) 120.0(9) 119.5(7) 120.3(8) 67.1(8) 108.7(10) 60.1(8) 101.8(9) 106.7(10) 57.2(8) 128.0(10) 125.4(9) 120.8(7) 117.0(8) 60.7(7) 116.6(9) 106.1(10) 55.9(7) 114.5(9) 124.2(8) 102.4(9) 126.5(9) 57.3(7) 120.0(8) 106.1(8) 61.3(7) 123.4(9) 56.1(6) 108.3(9) 101.3(9) 122.4(8) 63.4(7) 56.0(6) 108.0(8) 107.0(9) 100.7(10) 59.7(7) 58.1(9) 111.5(10) 59.7(8) 122.8(8) 122.3(10) 127.4(9) 118.4(9) 58.1(7) 62.5(7) 105.8(8) 108.5(10) 121.1(8) 109.7(10) 64.6(8)


B(22)-B(18)-B(13) B(14)-B(18)-B(23) B(22)-B(18)-B(23) B( 13)-B( 18)-B(23) B( 14) -B( 18)-B( 19) B(22)-B(18)-B(19) B( 13)-B( 18)-B( 19) B(23)-B(18)-B(19) B( 14)-B( 18)-Br(18) B(22)-B( 18)-Br( 18) B(13)-B(18)-Br(18) B(23)-B( 18)-Br( 18) B( 19)-B( 18)-Br( 18) B( 15)-B( 19)-B( 14) B(15)-B(19)-Br(19) B(14)-B(19)-Br(19) B( 15)-B( 19)-B(20) B(14)-B(19)-B(20) Br( 19)-B( 19)-B(20) B(15)-B(19)-B(18) B(14)-B(19)-B(18) Br(19)-B(19)-B(18) B(20)-B(19)-B(18) B( 15)-B( 19)-B(23) B( 14)-B( 19)-B(23) Br(19)-B(19)-B(23) B(20)-B( 19)-B(23) B(18)-B(19)-B(23) B(1S)-B(20)-B(23) B( 15)-B(20)-B( 16) B(23)-B(20)-B(16) B( 15)-B(20)-B( 19) B(23)-B(20)-B( 19) B(16)-B(20)-B(19) B(15)-B(20)-B(21) B(23)-B(20)-B(21) B(16)-B(20)-B(21) B( 19)-B(20)-B(21) B(15)-B(20)-Br(20) B(23)-B(20)-Br(20) B( 16)-B(20)-Br(20) B( 19)-B(20)-Br(20) B(21)-B(20)-Br(20) B(22)-B(21 )-B( 17) B(22)-B(21 )-B( 16) B(17)-B(21)-B(16) B(22)-B(21)-B(23) B(17)-B(21)-B(23) B(16)-B(21)-B(23) B(22)-B(21)-Br(21) B(17)-B(21)-Br(21) B(16)-B(21)-Br(21) B(23)-B(21)-Br(21) B(22)-B(21)-B(20) B(17)-B(21)-B(20) B( 16)-B(21)-B(20)

B(23)-B(21)-B(20) Br(21)-B(21)-B(20) B(18)-B(22)-B(21) B(18)-B(22)-B(13) B(21)-B(22)-B(13) B(18)-B(22)-B(17) B(21)-B(22)-B(17) B(13)-B(22)-B(17) B( 18)-B(22)-B(23) B(21)-B(22)-B(23) B( 13)-B(22)-B(23) B( 17)-B(22)-B(23) B( 18)*B(22)-Br(22) B(21)-B(22)-Br(22) B( 13)-B(22)-Br(22) B( 17)-B(22)-Br(22) B(23)-B(22)-Br(22) B(22)-B(23)-B(20) B(22)-B(23)-Br(23) B(20)-B(23)-Br(23) B(22)-B(23)-B(21) B(20)-B(23)-B(21) Br(23)-B(23)-B(21) B(22)-B(23)-B(18) B(20)-B(23)-B(18) Br(23)-B(23)-B(18) B(21)-B(23)-B( 18) B(22)-B(23)-B(19) B(20)-B(23)-B( 19) Br(23)-B(23)-B(19) B(21)-B(23)-B(19) B(18)-B(23)-B(19) B(28)-C( 1")-B(26) B(28)-C(l")-B(27) B(26)-C( 1”)-B(27) B(29)-B(24)-C1(24) B(29)-B(24)-B(25) Cl(24)-B(24)-B(25) B(29)-B(24)-B(28) Cl(24)-B(24)-B(28) B(25)-B(24)-B(28) B(29)-B(24)-B(33) CI(24)-B(24)-B(33) B(25)-B(24)-B(33) B(28)-B(24)-B(33) B(29)-B(25)-B(24) B(29)-B(25)-B(26) B(24)-B(25)-B(26) B(29)-B(25)-C1(25) B(24)-B(25)-a(25) B(26)-B(25)-C1(25) B(29)-B(25)-B(30) B(24)-B(25)-B(30) B(26)-B(25)-B(30) CI(25>B(25)-B(30) C( 1”)-B(26)-B(27)

60.0(8) 108.7(10) 58.6(9) 109.5(10) 57-5(7) 109.5(9) 111.6(10) 63.1(9) 119.1(7) 126.9(9) 125.0(9) 118.0(8) 113.4(7) 62.6(8) 124.1(9) 128.4(9) 56-5(6) 102.9(9) 123.2(8) 102.7(9) 54.9(6) 128.8(9) 98.4(8) 101.7(10) 102.2(9) 122.0(9) 54.8(9) 57.8(8) 111.0(11) 63.2(7) 111.0(11) 56.5(7) 66.0(10) 110.0(8) 110.4(9) 61.7(10) 59.3(7) 113.6(9) 117.8(9) 122.3(9) 117.2(8) 120.0(8) 121.3(7) 60-5(9) 105.6(9) 61-5(7) 58.7(10) 108.9(10) 104.7(10) 127.9(8) 125.3(9) 122.4(8) 119.7(8) 100.4(9) 105.5(8) 57.3(7)

56.2(9) 121.3(7) 118.0(10) 60.7(8) 112.3(13) 110.9(10) 59.8(8) 60-5(10) 66.0(10) 66.0(10) 116.2(11) 114.3(11) 119.3(10) 116.4(6) 118.0(10) 118-3(9) 117.3(12) 102.5(12) 127.7(14) 123.7(12) 55.4(9) 62.1(9) 125.0(14) 55.3(7) 102.7(11) 124.9(13) 101.1(10) 103.5(11) 59.2(9) 119.7(13) 108.7(11) 59.1(9) 111.2(9) 62.0(9) 59.5(9) 125.5(10) 60.9(8) 120.1(9) 109.6(10) 120.4(7) 104.6(10) 62.5(9) 123.9(10) 110.9(9) 62.4(8) 57.6(8) 108.9(10) 109.3(10) 121.8(9) 120.2(8) 122.1(12) 61.2(8) 107.7(11) 60.3(8) 122.7(9) 61.6(10)

288


C(l")-B(26)-B(25) B(27)-B(26)-B(25) C(l")-B(26)-B(30) B(27)-B(26)-B(30) B(25)-B(26)-B(30) C(1")-B(26)-C1(26) B(27)-B(26)-CI(26) B(25)-B(26)-C1(26) B(30)-B(26)-C1(26) C( 1”)-B(26)-B(31) B(27)-B(26)-B(31) B(25)-B(26)-B(31) B(30)-B(26)-B(31) Cl(26)-B(26)-B(31) CI(27)-B(27)-B(26) CI(27)-B(27)-B(28) B(26)-B(27)-B(28) CI(27)-B(27)-B(32) B(26)-B(27)-B(32) B(28)-B(27)-B(32) CI(27)-B(27)-C( 1") B(26)-B(27)-C(l”) B(28)-B(27)-C( 1") B(32)-B(27)-C( 1") Cl(27)-B(27)-B(31) B(26)-B(27)-B(31) B(28)-B(27)-B(31) B(32)-B(27)-B(31) C( 1")-B(27)-B(31) C(1")-B(28)-C1(28) C( 1")-B(28)-B(27) Cl(28)-B(28)-B(27) C(l")-B(28)-B(24) Cl(28)-B(28)-B(24) B(27)-B(28)-B(24) C( 1”)-B(28)-B(33) CI(28)-B(28)-B(33) B(27)-B(28)-B(33) B(24)-B(28)-B(33) C(l")-B(28)-B(32) Cl(28)-B(28)-B(32) B(27)-B(28)-B(32) B(24)-B(28)-B(32) B(33)-B(28)-B(32) B(24)-B(29)-B(25) B(24)-B(29)-B(30) B(25)-B(29)-B(30) B(24)-B(29)-B(34) B(25)-B(29)-B(34) B(30)-B(29)-B(34) B(24)-B(29)-B(33) B(25)-B(29)-B(33) B(30)-B(29)-B(33) B(34)-B(29)-B(33) B(24)-B(29)-Br(29) B(25)-B(29)-Br(29)

56.8(7) 109.8(13) 103.9(11) 110.0(11) 60.0(8) 121.7(11) 120.7(12) 118.3(11) 122.9(12) 107.4(12) 63.2(10) 107.0(10) 58.0(8) 125.6(11) 119.9(13) 122.2(12) 104.2(13) 127.2(14) 106.1(13) 63.3(11) 121.0(11) 59.0(10) 54.1(9) 103.8(13) 127.3(13) 61.3(9) 105.3(11) 55.6(10) 104.1(11) 119.8(9) 63.9(10) 119.9(10) 59.3(8) 119.0(9) 112.0(12) 108.2(10) 120.9(12) 110.7(11) 60.1(7) ’07.9(11) 124.9(10) 58.9(9) 107.9(10) 60.8(8) 61.5(7) 110.0(10) 60.2(8) 110.1(12) 106.9(10) 57.9(8) 62.6(8) 111.4(9) 109.0(11) 61.0(10) 124.2(11) 125.5(10)

B(30)-B(29)-Br(29) B(34)-B(29)-Br(29) B(33)-B(29)-Br(29) B(34)-B(30)-B(31) B(34)-B(30)-B(26) B(31)-B(30)-B(26) B(34)-B(30)-B(25) B(31)-B(30)-B(25) B(26)-B(30)-B(25) B(34)-B(30)-B(29) B(31)-B(30)-B(29) B(26)-B(30)-B(29) B(25)-B(30)-B(29) B(34)-B(30)-Br(30) B(31)-B(30)-Br(30) B(26)*B(30)-Br(30) B(25)-B(30)-Br(30) B(29)-B(30)-Br(30) B(34)-B(31)-B(32) B(34)-B(31)-B(30) B(32)-B(31)-B(30) B(34)-B(31)-Br(31) B(32)-B(31)-Br(31) B(30)-B(31)-Br(31) B(34)-B(31>B(26) B(32)-B(31)-B(26) B(30)-B(31)-B(26) Br(31)-B(31)-B(26) B(34)-B(31)-B(27) B(32)-B(31)-B(27) B(30)-B(31)-B(27) Br(31)-B(31)-B(27) B(26)-B(31)-B(27) B(31)-B(32)-B(27) B(31)-B(32)-B(34) B(27)-B(32)-B(34) B(31)-B(32)-B(28) B(27)-B(32)-B(28) B(34)-B(32)-B(28) B(31)-B(32)-Br(32) B(27)-B(32)-Br(32) B(34)-B(32)-Br(32) B(28)-B(32)-Br(32) B(31)-B(32)-B(33) B(27)-B(32)-B(33) B(34)-B(32)-B(33) B(28)-B(32)-B(33) Br(32)-B(32)-B(33) Br(33)-B(33)-B(24) Br(33)-B(33)-B(29) B(24)-B(33)-B(29) Br(33)-B(33)-B(34) B(24)-B(33)-B(34) B(29)-B(33)-B(34) Br(33)-B(33)-B(28) B(24)-B(33)-B(28)

119.7(7) 116.6(8) 117.5(9) 57.6(6) 107.9(11) 63.8(9) 108.4(12) 111.4(11) 59.6(8) 61.3(9) 108.2(11) 106.4(10) 58.6(9) 120.9(11) 117.7(11) 121.3(10) 123.2(9) 124.1(9) 63.8(11) 60.1(8) 109.9(10) 133.3(12) 120.8(10) 127.7(14) 105.5(10) 103.9(14) 58.2(8) 116.3(8) 107.9(14) 58.7(11) 103.8(11) 112.4(10) 55.5(10) 65.7(10) 57.1(9) 108.1(12) 108.8(11) 57.8(10) 104.0(10) 125.0(11) 118.2(12) 128.8(11) 118.2(13) 108.5(12) 108.8(12) 59.6(9) 59.6(9) 118.9(10) 123.0(9) 125.9(10) 54.9(6) 126.6(10) 102.2(10) 58.7(8) 124.1(11) 57.5(7)


B(29)-B(33)-B(28) B(34)-B(33)-B(28) Br(33)-B(33)-B(32) B(24)-B(33)-B(32) B(29)-B(33)-B(32) B(34)-B(33)-B(32) B(28)-B(33)-B(32) B(31)-B(34)-B(30) B(31)-B(34)-B(29) B(30)-B(34)-B(29) B(31)-B(34)-B(32) B(30)-B(34)-B(32) B(29)-B(34)-B(32) B(31)-B(34)-B(33) B(30)-B(34)-B(33) B(29)-B(34)-B(33) B(32)-B(34)-B(33) B(31)-B(34)-Br(34)

99.9(10) 102.8(10) 124.2(9) 104.9(10) 103.7(12) 58.0(10) 59.6(9) 62.2(8) 111.5(9) 60.8(8) 59.1(10) 107.8(10) 108.3(13) 112.5(15) 110.8(11) 60.3(8) 62.4(10) 117.0(11)

B(30)-B(34)-Br(34) B(29)-B(34)-Br(34) B(32)-B(34)-Br(34) B(33)-B(34)-Br(34) C(13)-N(1)-Q11) C(13)-N(l)-C(12) C (ll)-N (l)-C (12) N(l)-C(13)-0(1) C(23)-N(2)-C(22) C(23)-N(2)-C(21) C(22)-N(2)-C(21) 0(2)-C(23)-N(2) C(33)-N(3)-C(31) C(33)-N(3)-C(32) C(31)-N(3)-C(32) N(3)-C(33)-0(3)

126.1(14) 126.0(9) 115.9(8) 116.5(8) 121.9(17) 122.3(15) 114.7(17) 124.8(14) 124.4(11) 116.0(12) 119.6(12) 126.8(12) 113.8(10) 116.3(9) 128.4(9) 120.2(11)

290


Compound V ll-8 A tom ic coordinates and thermal parameters.

C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12) 1(2) 1(3) 1(4) 1(5) 1(6) 1(7) 1(8) 1(9) 1(10) 1(11) 1(12) 0(1) 0(2) 0(3) C(2) C(3) C(4) C(5) a s-)

X -8970(30) -8730(30) -8440(30) -9600(30) -10570(30) -10080(30) -9440(30) -9880(30) -11160(30) -11560(20) -10440(30) -11110(30) -7145(15) -6452(14) -8940(15) -11249(15) -10109(15) -8578(15) -9701(14) -12778(14) -13500(14) -10958(15) -12516(15) -370(50) -8660(70) -11932(17) -13270(30) -12760(20) -10750(20) -11020(50) -10330(50)

y 1529(12) 996(12) 1992(13) 2410(12) 1735(14) 842(13) 1550(13) 2435(11) 2281(12) 1291(14) 857(11) 1762(13) 218(1) 2383(1) 3359(1) 1786(2) -156(1) 1441(1) 3469(1) 3082(1) 811(1) -176(1) 1866(1) 2860(20) 4880(30) 6146(11) 6140(30) 5690(14) 5746(15) 4898(13) 5280(40)

z -6395(16) -5610(20) -5560(20) -6251(16) -6692(14) -6320(20) -4870(20) -5232(17) -5974(17) -5991(17) -5287(17) -5124(18) -5466(10) -5371(10) -6913(10) -7914(10) -7022(10) -3656(10) -4605(10) -6196(10) -6205(10) -4698(10) -4158(10) 7490(20) -8270(50) -7844(12) -9061(13) -8341(19) -7638(17) -7670(60) -8340(30)

U(eq) 53(4) 55(5) 60(6) 49(5) 50(5) 63(7) 55(5) 48(5) 49(5) 47(4) 47(4) 49(5) 77(1) 75(1) 89(1) 94(1) 87(1) 78(1) 67(1) 68(1) 85(1) 88(1) 79(1) 132(12) 210(30) 220(30) 300(80) 650(70) 500(200) 110(30) 100(20)

Bond lengths C(l)-B(2) C(l)-B(6) C(l)-B(4) B(2)-B(7) B(2)-B(6) B(2)-B(3) B (2)-B (ll) B(2)-I(2) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(3)-I(3) B(4)-B(9) B(4)-B(5) B(4)-B(8) B(4)-[(4)

B(5)-B(9) B(5)-B(6) B(5)-B(10) B(5)-I(5) B(6)-B(10) B (6)-B (ll) B(6)-I(6) B (7)-B (ll) B(7)-B(8) B(7)-B(12) B(7)-I(7) B(8)-B(12) B(8)-B(9) B(8)-I(8) B(9)-B(12) B(9)-B(10) B(9)-I(9)

1.66(3) 1.67(4) 1.72(3) 1.78(4) 1.80(4) 1.80(3) 1.84(3) 2.12(2) 1.76(3) 1.77(4) 1.78(4) 2.13(2) 1.68(3) 1.70(3) 1.78(3) 2.16(2)

1.70(3) 1.78(4) 1.78(3) 2.170(17) 1.80(4) 1.83(4) 2.15(2) 1.73(3) 1.75(3) 1.76(4) 2.21(3) 1.75(3) 1.78(4) 2.14(2) 1.72(3) 1.81(3) 2.19(2)

291


B(10)-B(12) B(10)-B(l 1) B(10)-I(10) B(11)-B(12) B (ll)-I (tl) B(12)-I(12) 0(2)-C(5')

0(3)-C(4) 0(3)-C(3) C(2)-C(3) C(4)-C(5) Q 4 )-Q 5 ’)

1.74(3) 1.79(3) 2.15(2) 1.78(3) 2.18(2) 2.23(2) 1.82(7)

1.4200(11) 1.4200(11) 1.5400(11) 1.5400(11) 1.5400(11)

Bond angles B(2)-C(l)-B(6) B(2)-C(l)-B(4) B(6)-C(l)-B(4) C(l)-B(2)-B(7) C(l)-B(2)-B(6) B(7)-B(2)-B(6) C(l)-B(2)-B(3) B(7)-B(2)-B(3) B(6)-B(2)-B(3) C(l)-B(2)-B(l 1) B(7)-B(2)-B(l 1) B(6)-B(2)-B(l 1) B(3)-B(2)-B(l 1) C(l)-B(2)-I(2) B(7)-B(2)-l(2) B(6)-B(2)-I(2) B(3)-B(2)-I(2) B(11)-B(2)-I(2) B(8)-B(3)-B(7) B(8)-B(3)-B(4) B(7)-B(3)-B(4) B(8)-B(3)-B(2) B(7)-B(3)-B(2) B(4)-B(3)-B(2) B(8)-B(3)-I(3) B(7)-B(3)-I(3) B(4)-B(3)-I(3) B(2)-B(3)-I(3) B(9)-B(4)-B(5) B(9)-B(4)-C(l) B(5)-B(4)-C(l) B(9)-B(4)-B(8) B(5)-B(4)-B(8) C(l)-B(4)-B(8) B(9)-B(4)-B(3) B(5)-B(4)-B(3) C(l)-B(4)-B(3) B(8)-B(4)-B(3) B(9)-B(4)-I(4) B(5)-B(4)-I(4) C(l)-B(4)-I(4) B(8)-B(4)-I(4) B(3)-B(4)-I(4) B(9)-B(5)-B(4) B(9)-B(5)-B(6) B(4)-B(5)-B(6)

B(9)-B(5)-B( 10) B(4)-B(5>B(10) B(6)-B(5)-B(10) B(9)-B(5)-I(5) B(4)-B(5)-l(5) B(6)-B(5)-I(5) B(10)-B(5)-I(5) C(l)-B(6)-B(5) C(l)-B(6)-B(10) B(5)-B(6)-B( 10) C(l)-B(6)-B(2) B(5)-B(6)-B(2) B(10)-B(6)-B(2) C (l)-B (6)-B (ll) B(5)-B(6)-B(ll) B(10)-B(6)-B(ll) B(2)-B(6)-B(ll) C(l)-B(6)-I(6) B(5)-B(6)-I(6) B(10)-B(6)-I(6) B(2)-B(6)-I(6) B(ll)-B(6)-I(6) B(ll)-B(7)-B(8) B(ll)-B(7)-B(3) B(8)-B(7)-B(3) B(ll)-B(7)-B(12) B(8)-B(7)-B(12) B(3)-B(7)-B(12) B(ll)-B(7)-B(2) B(8)-B(7)-B(2) B(3)-B(7)-B(2) B(12)-B(7)-B(2) B(ll)-B(7)-I(7) B(8)-B(7)-I(7) B(3)-B(7)-I(7) B(12)-B(7)-I(7) B(2)-B(7)-I(7) B(12)-B(8)-B(7) B(12)-B(8)-B(3) B(7)-B(8)-B(3) B(12)-B(8)-B(4) B(7)-B(8)-B(4) B(3)-B(8)-B(4) B( 12)-B(8)-B(9) B(7)-B(8)-B(9) B(3)-B(8)-B(9)

65.7(17) 116.7(16) 114.3(17) 102.2(15) 57.3(16) 104.8(17) 59.2(15) 59.1(13) 107.1(18) 102.6(17) 57.0(13) 60.1(16) 105.5(15) 123.2(16) 127.4(18) 120.9(14) 121.7(15) 125.7(14) 59.5(13) 60.4(13) 105.2(16) 109.1(16) 59.7(14) 106.6(17) 125.8(14) 127(2) 122.6(17) 118.4(14) 60.4(15) 105.7(16) 59.7(13) 62.0(14) 109.7(15) 103.9(15) 109.9(16) 109.8(15) 58.7(13) 59.1(14) 124.9(14) 120.5(14) 121.3(13) 124.1(13) 118.1(16) 59.0(13) 111.0(16) 109.6(16)

62.7(12) 110.0(13) 61.0(15) 124.7(14) 122.9(15) 116.7(14) 120.6(15) 59.2(14) 105.1(15) 59.6(13) 57.0(14) 106.9(16) 108.7(18) 103.0(17) 105.5(15) 58.9(15) 60.9(16) 124.1(19) 123.4(18) 123.8(15) 119.7(14) 123.8(17) 111.5(19) 112.2(19) 59.9(14) 61.3(14) 59.6(14) 107.5(19) 63.3(14) 110.7(19) 61.1(14) 110.7(19) 121.1(16) 119.6(15) 117.3(16) 125.1(16) 117.8(15) 60.6(13) 108.8(14) 60.6(14) 103.5(17) 106.1(15) 60.5(15) 58.5(13) 106.0(15) 106.2(16)

292


B(4)-B(8)-B(9) B(12)-B(8)-I(8) B(7)-B(8)-I(8) B(3)-B(8)-I(8) B(4)-B(8)-I(8) B(9)-B(8)-I(8) B(4)-B(9)-B(5) B(4)-B(9)-B(12) B(5)-B(9)-B(12) B(4)-B(9)-B(8) B(5)-B(9)-B(8) B(12)-B(9)-B(8) B(4)-B(9)-B(10) B(5)-B(9)-B(10) B(12)-B(9)-B(10) B(8)-B(9)-B(10) B(4)-B(9)-I(9) B(5)-B(9)-I(9) B(12)-B(9)-I(9) B(8)-B(9)-I(9) B(10)-B(9)-I(9) B( 12)-B( 10)-B(5) B( 12)-B( 10)-B( 11) B(5)-B(10)-B(ll) B(12)-B(10)-B(6) B(5)-B(10)-B(6) B(ll)-B(10)-B(6) B(12)-B(10)-B(9) B(5)-B(10)-B(9) B(ll)-B(10)-B(9) B(6)-B(10)-B(9) B(12)-B(10)-I(10) B(5)-B(10)-I(10) B(11)-B(10)-I(10) B(6)-B(10)-I(10) B(9)-B(10)-I(10) B(7)-B(l 1)-B(12)

56.1(13) 125.7(13) 126.0(16) 119.9(15) 120.0(13) 122.0(14) 60.6(14) 109.2(16) 107.9(15) 61.9(14) 109.8(15) 59.7(13) 109.8(15) 60.8(14) 59.0(12) 108.3(14) 124.0(12) 122.2(15) 119.1(13) 121.9(15) 118.2(15) 103.4(14) 60.6(13) 107.1(15) 107.6(16) 59.4(14) 61.2(15) 57.9(13) 56.4(11) 106.3(15) 104.7(15) 121.9(13) 126.5(14) 118.7(14) 121.6(14) 126.2(14) 60.3(13)

B(7)-B(ll)-B(10) B(12)-B(ll)-B(10) B(7)-B( 11 )-B(6) B(12)-B(ll)-B(6) B( 10)-B( 11)-B(6) B(7)-B(ll)-B(2) B(12)-B(l 1)-B(2) B(10)-B(ll)-B(2) B(6)-B(ll)-B(2) B (7 )-B (ll)-I(ll) B (1 2 )-B (ll)-l(ll) B (10)-B (ll)-I(ll) B (6 )-B (ll)-I(ll) B (2 )-B (ll)-I(ll) B(9)-B(12)-B(10) B(9)-B(12)-B(8) B(10)-B(12)-B(8) B(9)-B(12)-B(7) B(10)-B(12)-B(7) B(8)-B(12)-B(7) B (9)-B(12)-B(ll) B(10)-B(12)-B(l 1) B(8)-B( 12)-B( 11) B(7)-B(12)-B(ll) B(9)-B(12)-I(12) B(10)-B(12)-I(12) B(8)-B(12)-I(12) B(7)-B(12)-I(12) B(ll)-B(12)-I(12) C(4)-0(3)-C(3) 0(3)-C(3)-C(2) 0(3)-C(4)-C(5) 0(3)-C(4)-C(5) C(5)-C(4)-C(5 ) Q 4 ) -a 5 ) -0 (2 )

107.7(16) 58.5(13) 106.0(17) 105.1(16) 59.9(14) 59.7(13) 107.1(14) 107.9(16) 58.9(15) 124.3(17) 126.4(14) 121.4(14) 120.0(13) 120.0(13) 63.0(15) 61.9(15) 113.2(15) 108.0(16) 108.0(16) 59.8(13) 110.5(16) 60.9(14) 109.1(14) 58.3(13) 126.1(14) 121.8(13) 120.0(14) 117.7(16) 116.9(13) 108.85(11) 109.62(11) 109.62(11) 109.62(11) 59(5) 116(4)


Compound VII-9 A tom ic coordinates and thermal parameters.

Cl(2) Cl(3) CI(4) Cl(5) Cl(6) Cl(7) Cl(8) CI(9) Cl(10) C l(ll) Cl(12) C(l) B(2) B(3) B(4) B(5) B(6) B(7) B(8) B(9) B(10) B( 11) B(12) C(2) C(3) C(4) C(5) 0(1) 0(2) 0(3) 0(4)

X

V

4171(1) 2670(1) 2935(1) 4549(1) 5346(1) 1584(1) 820(1) 2054(1) 3574(1) 3320(1) 1236(1) 3873(1) 3572(1) 2822(1) 2954(1) 3778(1) 4169(1) 2340(1) 1965(1) 2559(1) 3309(1) 3179(1) 2182(1) 2315(1) 301(1) 1529(2) 617(2) 3092(1) 2269(1) -528(1) 788(1)

-6402(1) -9180(1) -10619(1) -8722(1) -6124(1) -5908(1) -8594(1) -8278(1) -5373(1) -3919(1) -5343(1) -8131(2) -6786(2) -8180(2) -8897(2) -7941(2) -6637(2) -6588(2) -7897(2) -7749(2) -6331(2) -5622(2) -6320(2) -2979(2) -1669(2) -2989(4) -2654(3) -3601(2) -2420(2) -1121(2) -1351(1)

U(eq) 81(1) 73(1) 73(1) 71(1) 83(1) 75(1) 80(1) 73(1) 86(1) 87(1) 76(1) 50(1) 54(1) 52(1) 51(1) 52(1) 57(1) 54(1) 53(1) 52(1) 56(1) 57(1) 53(1) 75(1) 60(1) 151(1) 110(1) 147(1) 87(1) 94(1) 74(1)

z 1299(1) 944(1) 2839(1) 4360(1) 3405(1) 838(1) 1840(1) 4011(1) 4357(1) 2400(1) 2759(1) 2572(1) 1962(1) 1786(1) 2736(1) 3498(1) 3021(1) 1752(1) 2239(1) 3301(1) 3477(1) 2518(1) 2698(1) -131(1) 741(1) -887(2) 1389(2) -80(1) 481(1) 594(1) 337(1)

Bond lengths Cl(2)-B(2) Cl(3)-B(3) CI(4)-B(4) Cl(5)-B(5) Cl(6)-B(6) C!(7)-B(7) Cl(8)-B(8) Cl(9)-B(9) Cl(10)-B(10) CI( 11)-B( 11) Cl(12)-B(12) C(l)-B(6) C(l)-B(2) C(l)-B(4) C(l)-B(5) Q l)-B (3)

B (2)-B (ll) B(2)-B(3) B(2)-B(7) B(2)-B(6) B(3)-B(8) B(3)-B(7) B(3)-B(4) B(4)-B(8) B(4)-B(9) B(4)-B(5) B(5)-B(9) B(5)-B(10) B(5)-B(6) B(6)-B(10) B (6)-B (ll) B(7)-B(8) B(7)-B(12)

1.766(2) 1.7619(19) 1.7713(19) 1.7640(17) 1.7586(19) 1.7731(18) 1.7823(17) 1.774(2) 1.770(2) 1.775(2) 1.784(2) 1.710(2) 1.711(2) 1.712(2) 1.714(3) 1.719(2)

1.777(3) 1.782(3) 1.788(3) 1.791(3) 1.777(3) 1.777(3) 1.788(3) 1.778(2) 1.778(3) 1.783(2) 1.771(2) 1.789(3) 1.789(3) 1.787(3) 1.790(3) 1.792(3) 1.801(3)

294


B(7)-B(l 1) B(8)-B(12) B(8)-B(9) B(9)-B(12) B(9)-B(10) B(10)-B(12) B (10)-B(ll) B (ll)-B(12)

1.803(3) 1.785(3) 1.795(3) 1.785(2) 1.802(3) 1.790(2) 1.801(3) 1.800(3)

C(2)-0(2) C (2)-0(l) C(2)-C(4) C(3)-0(4) C(3)-0(3) C(3)-C(5)

1.252(3) 1.315(3) 1.457(3) 1.240(2) 1.319(2) 1.479(3)

Bond angles B(6)-C(l)-B(2) B(6)-C(l)-B(4) B(2)-C(l)-B(4) B(6)-C(l)-B(5) B(2)-C( 1)-B(5) B(4)-C(l)-B(5) B(6)-C(l)-B(3) B(2)-C(l)-B(3) B(4)-C(l)-B(3) B(5)-C(l)-B(3) C(1)-B(2)-C1(2) C(l)-B(2)-B(ll) Cl(2)-B(2)-B(ll) C(l)-B(2)-B(3) Cl(2)-B(2)-B(3) B(11)-B(2)-B(3) C(l)-B(2)-B(7) Cl(2)-B(2)-B(7) B(11)-B(2)-B(7) B(3)-B(2)-B(7) C(l)-B(2)-B(6) Cl(2)-B(2)-B(6) B(11)-B(2)-B(6) B(3)-B(2)-B(6) B(7)-B(2)-B(6) C(1)-B(3)-C1(3) C(l)-B(3)-B(8) Cl(3)-B(3)-B(8) C(l)-B(3)-B(7) CI(3)-B(3)-B(7) B(8)-B(3)-B(7) C(l)-B(3)-B(2) Cl(3)-B(3)-B(2) B(8)-B(3)-B(2) B(7)-B(3)-B(2) C(l)-B(3)-B(4) Cl(3)-B(3)-B(4) B(8)-B(3)-B(4) B(7)-B(3)-B(4) B(2)-B(3)-B(4) C(1)-B(4)-C1(4) C(l)-B(4)-B(8) CI(4)-B(4)-B(8) C(l)-B(4)-B(9) CI(4)-B(4)-B(9)

63.12(10) 115.20(13) 114.87(11) 62.98(11) 115.12(13) 62.72(10) 115.14(12) 62.59(10) 62.81(10) 114.83(12) 121.00(13) 104.70(13) 124.91(13) 58.92(10) 120.45(13) 108.39(14) 104.75(13) 125.40(12) 60.74(11) 59.70(10) 58.40(10) 119.53(12) 60-24(11) 108.22(13) 108.77(14) 121.23(12) 104.31(13) 125.43(11) 104.89(12) 124.84(12) 60-57(11) 58.49(9) 120.02(13) 108.35(13) 60.32(10) 58.40(9) 120.30(12) 59.83(10) 108.53(14) 107.83(12) 121.03(12) 104.55(12) 125.50(11) 104.46(12) 125.23(13)

B(8)-B(4)-B(9) C(l)-B(4)-B(5) Cl(4)-B(4)-B(5) B(8)-B(4)-B(5) B(9)-B(4)-B(5) C(l)-B(4)-B(3) Cl(4)-B(4)-B(3) B(8)-B(4)-B(3) B(9)-B(4)-B(3) B(5)-B(4)-B(3) C(l)-B(5)-Q(5) C(l)-B(5)-B(9) Cl(5)-B(5)-B(9) C(l)-B(5)-B(4) Cl(5)-B(5)-B(4) B(9)-B(5>B(4) C(l)-B(5)-B(10) Cl(5)-B(5)-B( 10) B(9)-B(5)-B( 10) B(4)-B(5)-B(10) C(1)*B(5)-B(6) CI(5)-B(5)-B(6) B(9)-B(5)-B(6) B(4)-B(5)-B(6) B(10)-B(5)-B(6) C( 1)-B(6)-Q(6) C(l)-B(6)-B(10) CI(6)-B(6)-B( 10) C(l)-B(6)-B(5) Cl(6)-B(6)-B(5) B(10)-B(6)-B(5) C (l)-B (6)-B (ll) CI(6)-B(6)-B( 11) B(10)-B(6)-B(ll) B(5)-B(6)-B(l 1) C(l)-B(6)-B(2) Cl(6)-B(6)-B(2) B(10)-B(6)-B(2) B(5)-B(6)-B(2) B(ll)-B(6)-B(2) Cl(7)-B(7)-B(3) CI(7)-B(7)-B(2) B(3)-B(7)-B(2) C!(7)-B(7)-B(8) B(3)-B(7)-B(8)

60.64(10) 58.70(10) 119.92(11) 108.21(13) 59.64(10) 58.79(10) 120.26(12) 59.77(10) 108.32(13) 108.21(13) 122.10(12) 104.68(11) 123.73(13) 58.58(10) 119.44(12) 60.04(10) 104.46(13) 125.06(12) 60.83(10) 108.58(12) 58.39(10) 121.32(11) 108.64(12) 107.98(13) 59.96(11) 120.93(13) 104.69(13) 125.22(13) 58.63(10) 119.88(11) 60.02(11) 104.19(12) 125.89(13) 60.43(11) 108.05(13) 58.48(10) 120.61(14) 107.99(13) 107.75(13) 59.51(11) 121.24(12) 122.29(13) 59.98(10) 121.50(11) 59.71(11)


B(2)-B(7)-B(8) CI(7)-B(7)-B(12) B(3)-B(7)-B(12) B(2)-B(7)-B(12) B(8)-B(7)-B(12) Cl(7)-B(7)-B(ll) B(3)-B(7)-B(l 1) B(2)-B(7)-B( 11) B(8)-B(7)-B(l 1) B(12)-B(7)-B(ll) B(3)-B(8)-B(4) B(3)-B(8)-C1(8) B(4)-B(8)-C1(8) B(3)-B(8)-B(12) B(4)-B(8)-B(12) Cl(8)-B(8)-B( 12) B(3)-B(8)-B(7) B(4)-B(8)-B(7) CI(8)-B(8)-B(7) B(12)-B(8)-B(7) B(3)-B(8)-B(9) B(4)-B(8)-B(9) Cl(8)-B(8)-B(9) B(12)-B(8)-B(9) B(7)-B(8)-B(9) B(5)-B(9)-CI(9) B(5)-B(9)-B(4) Cl(9)-B(9)-B(4) B(5)-B(9)-B(12) Cl(9)-B(9)-B(12) B(4)-B(9)-B(12) B(5)-B(9)-B(8) CI(9)-B(9)-B(8) B(4)-B(9)-B(8) B(12)-B(9)-B(8) B(5)-B(9)-B(10) Cl(9)-B(9)-B(10) B(4)-B(9)-B(10) B(12)-B(9)-B(10) B(8)-B(9)-B(10) Cl(10)-B(10)-B(6) CI(10)-B(10)-B(5) B(6)-B(10)-B(5) Cl( 10)-B( 10)-B( 12) B(6)-B(10)-B(12) B(5)-B(10)-B(12)

107.41(12) 122.87(12) 107.07(13) 106.87(12) 5938(11) 122.73(12) 107.50(12) 59.33(11) 107.67(13) 59.93(11) 60.40(10) 121.45(12) 120.53(12) 107.76(13) 107.52(11) 122.90(12) 59.72(11) 108.29(13) 122.39(11) 60.44(11) 108.07(11) 59.69(10) 121.20(13) 59.82(10) 108.51(12) 120.42(11) 60.32(10) 120.98(12) 107.75(13) 123.31(12) 107.50(13) 107.98(13) 122.58(11) 59.67(10) 59.81(10) 60.06(10) 121.68(12) 108.19(13) 59.85(10) 107.90(13) 121.31(12) 121.55(12) 60.02(11) 123.00(13) 107.62(13) 106.79(12)

CI( 10)-B( 10)-B( 11) B(6)-B( 10)-B( 11) B(5)-B( 10)-B( 11) B(12)-B(10)-B(l 1) Q(10)-B(10)-B(9) B(6)-B( 10)-B(9) B(5)-B( 10)-B(9) B(12)-B(10)-B(9) B( 11)-B( 10)-B(9) C l(ll)-B (ll)-B (2) a (ll)-B (ll)- B ( 6 ) B(2)-B(ll)-B(6) Q (ll)-B (ll)-B (1 2 ) B(2)-B( 11)-B( 12) B(6)-B(l 1)-B(12) C l(ll)-B (ll)-B (10) B(2)-B(l 1)-B(10) B(6)-B(ll)-B(10) B(12)-B(ll)-B(10) C l(ll)-B (ll)-B (7) B(2)-B(ll)-B(7) B(6)-B(l 1)-B(7) B(12)-B(ll)-B(7) B(10)-B(ll)-B(7) Cl(12)-B(12)-B(8) CI(12)-B(12)-B(9) B(8)-B( 12)-B(9) Cl(12)-B(12)-B( 10) B(8)-B(12)-B(10) B(9)-B(12)-B(10) Cl(12)-B(12)-B(l 1) B(8)-B(12)-B(ll) B(9)-B( 12)-B( 11) B(10)-B(12)-B(l 1) Cl(12)-B(12)-B(7) B(8)-B(12)-B(7) B(9)-B(12)-B(7) B(10)-B(12)-B(7) B(11)-B(12)-B(7) 0(2)-C (2)-0(l) 0(2)-C(2)-C(4) 0(1)-C(2)-C(4) 0(4)-C (3)-0(3) 0(4)-C(3)-C(5) 0(3)-C(3)-C(S)

122.14(12) 59.87(11) 107.61(14) 60.17(11) 122.31(14) 107.32(13) 59.10(10) 59.60(10) 107.72(12) 120.94(14) 120.81(13) 60.26(11) 123.59(13) 107.38(13) 107.06(13) 121.87(12) 108.02(13) 59.71(11) 59.62(11) 122.07(12) 59.93(10) 108.15(13) 59.99(11) 108.19(13) 120.52(11) 121.22(13) 60.37(10) 122.01(13) 108.90(12) 60.55(10) 122.27(12) 108.11(14) 108.50(12) 60.21(11) 120.88(11) 59.97(11) 108.58(13) 108.74(14) 60.08(11) 118.66(18) 122.1(2) 119.2(2) 119.62(16) 122.16(17) 118.21(19)


Chapter 8 Compound VIII-1 A tom ic coordinates and thermal parameters. X

A g(l) Ag(2) Co(l) Co(2) C (l) c c n

C(2) C(2') C(5) C(6) C( 7) C(8) C(9) C(10) C (ll) C(12) C(13) C(14) C(15) C(16) C(17) C(18) C(21) C(21r) C(22) C(22) C(23) C(24) C(25) C( 26) C( 27) C(28) C(29) C(30) C(31) C(32) C(33) C(34) C(35) C(36) C( 37) C(38) C(39) C(40) C(41) C(42) C(43) C(44)

362(2) 69(2) 2539(1) 2238(2) 3369(16) 3302(15) 3304(14) 3295(15) 411(12) 418(12) -428(12) -1292(13) -1289(12) -462(11) -258(16) -945(24) -1738(26) -1840(16) -1125(21) -293(17) -967(38) -1220(35) 3031(15) 3050(13) 2997(16) 2958(15) 112(15) 86(12) -722(11) -1583(14) -1583(11) -730(14) -443(23) -1280(27) -1966(27) -1862(21) -1004(34) -440(22) -1539(36) -906(46) 4565(17) 4188(20) 4380(16) 4990(19) 5356(18) 5187(19) 4308(27) 5172(21)

y 3944(1) 8970(1) 5366(2) 10318(2) 5961(15) 5733(15) 4963(13) 4735(16) 5327(14) 5478(11) 5541(13) 5549(13) 5450(16) 5320(13) 2616(14) 2882(16) 3202(19) 3191(19) 2871(17) 2621(14) 2855(24) 2865(34) 10819(15) 10719(12) 9786(15) 9734(14) 10426(12) 10439(12) 10521(12) 10632(14) 10624(13) 10507(16) 7658(17) 7945(20) 8126(19) 8010(18) 7740(16) 7526(15) 8143(25) 7497(28) 4106(17) 4417(20) 3970(18) 3332(17) 3083(19) 3445(18) 4518(26) 2884(19)

z 7567(2) 7503(2) 7372(1) 7626(1) 8206(11) 6386(13) 8372(13) 6521(11) 6962(8) 7812(10) 8194(11) 7775(10) 6971(13) 6574(10) 7930(18) 8310(18) 8004(25) 7201(25) 6716(20) 7098(16) 9197(18) 5820(19) 8472(11) 6710(11) 8607(11) 6755(10) 7180(10) 8029(9) 8408(11) 7961(13) 7164(12) 6790(11) 8072(20) 8307(15) 7810(20) 7008(20) 6697(15) 7171(27) 9204(17) 5806(21) 2042(14) 2742(15) 3437(14) 3487(15) 2782(15) 2138(16) 1258(21) 4223(17)

U(eq) 131(1) 150(1) 45(1) 45(1) 66(6) 66(6) 60(5) 69(7) 49(4) 48(4) 56(5) 57(5) 70(6) 51(4) 75(7) 87(8) 113(11) 109(12) 100(9) 72(6) 187(23) 199(23) 61(6) 51(5) 67(7) 55(5) 56(5) 46(4) 52(5) 69(6) 60(6) 66(6) 87(9) 92(10) 1 1 2 (1 1 )

104(10) 124(16) 112(13) 172(20) 233(32) 84(6) 1 0 1 (8 )

85(6) 90(7) 92(7) 93(7) 152(13) 110(9)


C(45) C(46) C(47) C(48) C(49) C(50) C(51) C(52) C(53) C(54) C(55) C(56) C(57) C(58) C(59) C(60) B(4) B(4') B(9) 8(5") B(5) B(6-) B(7) B(7-) BCS") B(8) B(90 B(12) B(10) B(IO') B(6) B(1F) 6(120 B(11) B(24) B(240 B(25) 8(250 B(26) B(260 B(27) B(270 B(280 B(28) B(29) B(290 B(212) B(210) B(210) B(211) B(211) B(212)

3939(13) 3917(14) 3995(14) 4054(13) 4108(14) 4043(14) 3882(18) 4116(14) 4958(17) 5674(15) 5553(16) 4730(17) 4044(20) 4116(18) 5078(20) 4605(24) 2255(18) 2235(20) 1662(18) 2790(20) 2887(19) 3586(17) 2219(17) 2165(17) 1403(16) 1456(16) 1604(18) 1648(18) 2518(18) 2468(18) 3583(16) 2859(23) 1604(20) 2841(16) 1948(15) 1980(16) 2607(21) 2661(22) 3284(18) 3295(16) 1847(18) 1838(17) 1153(15) 1113(14) 1366(16) 1395(19) 1286(21) 2166(17) 2224(14) 2497(21) 2486(17) 1310(19)

960(12) 1169(14) 572(13) -267(12) -469(14) 110(12) 1599(16) -909(14) -2432(16) -2283(14) -2555(15) -2938(17) -3084(18) -2841(17) -2131(19) -3231(22) 6389(16) 6100(26) 6171(17) 5961(21) 6505(16) 5142(19) 4578(16) 4348(17) 5278(15) 5514(16) 5677(18) 5081(16) 5735(18) 5035(20) 5577(20) 4282(23) 4597(18) 4727(18) 11246(16) 11226(15) 11290(22) 11089(22) 10318(24) 10164(20) 9467(15) 9418(14) 10349(16) 10415(15) 10970(16) 10861(20) 9755(18) 10431(20) 10219(20) 9482(22) 9368(17) 9879(16)

2068(11) 2821(12) 3441(12) 3245(11) 2457(12) 1904(12) 1414(13) 3897(11) 1316(14) 1871(12) 2627(13) 2898(14) 2348(15) 1585(14) 458(16) 3686(17) 8069(12) 6516(23) 9005(13) 5489(13) 8957(14) 5589(11) 8327(12) 6599(14) 6559(12) 8220(12) 5583(11) 9162(14) 9705(12) 5074(16) 9140(12) 5710(15) 5714(15) 9247(13) 8428(16) 6753(16) 9320(14) 5832(20) 9439(12) 5851(12) 8517(12) 6773(10) 6824(11) 8444(10) 9323(15) 5869(16) 5883(13) 9909(12) 5331(13) 9427(16) 5881(11) 9372(13)

54(5) 63(5) 67(5) 54(5) 64(5) 59(5) 87(7) 68(5) 81(6) 68(6) 72(6) 84(7) 93(7) 86(7) 102(8) 119(10) 57(6) 125(18) 63(6) 75(8) 65(7) 70(8) 56(6) 68(8) 53(5) 61(6) 69(8) 63(7) 69(7) 78(8) 73(8) 95(10) 69(7) 64(7) 61(7) 63(7) 78(9) 91(10) 79(8) 68(8) 58(7) 50(6) 58(6) 49(5) 66(7) 76(8) 68(7) 74(8) 68(7) 81(9) 57(6) 62(7)

Bond lengths A g(l)-C (l 1)

Ag(l)-C(5)

2.37(2)

2.43(2)

298


Ag(l)-C(6) Ag(l)-C(16) Ag(2)-C(23) Ag(2)-C(29) Ag(2)-C(34) Ag(2)-C(24) Co(l)-B(4') Co(l)-C(2') Co(l)-B(4) Co(l)-B(7) Co(l)-C(l) C o(l)-C (n Co(l)-B(8) Co(l)-C(2) Cofn-EfS1) Co(l)-B(7') Co(2)-C(21) Co(2)-C(21r) Co(2)-C(2T)

Co(2)-B(24) Co(2)-B(28') Co(2)-B(27') Co(2)-C(22) Co(2)-B(24') Co(2)-B(28) Co(2)-B(27) C(l)-C(2) C(l)-B(5) C(l)-B(6) C(l)-B(4) C(1>B(4') C(1>C(2') C (1>B (5) C (i> B (60 C(2)-B(6) C (2)-B (ll) C(2)-B(7) C(2>B(11') C(2>B(7') C(2>B(6’) C(5)-C(10) C(5)-C(6) Q sj- bcs-) C(6)-C(7) C(6)-B(8) C(7)-C(8) C(8)-C(9) C(9)-C(10) C(11)-C(12) C(11)-C(16) C(12)-C(13) C(12)-C(17) C(13)-C(14) C(14)-C(15) C(15)-C(16) C(15)-C(18)

2.48(2) 2.43(2) 2.38(2) 2.41(2) 2.47(3) 2.50(2) 1.91(5) 2.06(2) 2.05(2) 2.10(2) 2.06(2) 2.08(2) 2.12(2) 2.11(2) 2.12(2) 2.15(2) 1.98(2) 2.04(2) 2.02(2) 2.05(2) 2.05(2) 2.11(2) 2.15(2) 2.10(3) 2.12(2) 2.10(2) 1.61(3) 1.69(3) 1.72(3) 1.73(3) 1.63(4) 1.60(3) 1.72(3) 1.70(3) 1.67(3) 1.67(3) 1.65(3) 1.67(4) 1.72(3) 1.76(3) 1.40(2) 1.46(2) 1.56(3) 1.37(2) 1.62(3) 1.41(3) 1.37(3) 1.37(2) 1.24(4) 1.41(4) 1.33(4) 1.51(4) 1.37(4) 1.40(4) 1.40(4) 1.53(4)

C(21)-C(22) C(21)-B(24) C(21)-B(25) C(21)-B(26) C(21>C(220 C(21 > 8 (2 5 0 C(21')-B(24r) C(21')-B(26') C(22)-B(26) C(22)-B(211) C(22)-B(27) C(22')-B(27') C(22>B(211) C(22>B(26') C(23)-C(24) C(23)-C(28) C(23)-B(28,) C(24)-C(25) C(24)-B(28) C(25)-C(26) C(26)-C(27) C(27)-C(28) C(29)-C(30) C(29)-C(34) C(30)-C(31) C(30)-C(35) C(31)-C(32) C(32)-C(33) C(33)-C(34) C(33)-C(36) C(37)-C(42) C(37)-C(38) C(37)-C(43) C(38)-C(39) C(39)-C(40) C(40)-C(41) C(40)-C(44) C(41)-C(42) C(45)-C(46) C(45)-C(50) C(45)-C(51) C(46)-C(47) C(47)-C(48) C(48)-C(49) C(48)-C(52) C(49)-C(50) C(53)-C(58) C(53)-C(54) C(53)-C(59) C(54)-C(55) C(55)-C(56) C(56)-C(57) C(56)-C(60) C(57)-C(58) B(4)-B(5) B(4)-B(8)

1.66(3) 1.68(3) 1.73(3) 1.86(3) 1.57(3) 1.69(4) 1.72(3) 1.74(3) 1.69(3) 1.64(3) 1.71(4) 1.66(3) 1.72(3) 1.75(3) 1.44(2) 1.36(3) 1.60(3) 1.32(2) 1.61(3) 1.44(3) 1.35(3) 1.38(3) 1.33(4) 1.54(5) 1.31(4) 1.60(4) 1.38(4) 1.39(5) 1.18(5) 1.57(4) 1.38(3) 1.39(4) 1.53(4) 1.40(3) 1.33(3) 1.36(4) 1.46(4) 1.26(3) 1-32(3) 1.39(3) 1.51(3) 1.42(3) 1.38(3) 1.38(3) 1-51(3) 1.32(3) 1.43(3) 1.40(3) 1.54(4) 1.37(3) 1.39(3) 1.36(3) 1.43(3) 1.36(3) 1.76(3) 1.81(3)

299


B(4)-B(9) B(4>B(8') B (4>B (9r) B(4')-B(5') B(9)-B(8) B(9)-B(5) B(9)-B(12) B(9)-B(10) B(5>B(6') B(5')-B(10r) BfSO-B^1) B(5)-B(10) B(5)-B(6) B (6 > B (llr) B ^ -B O O 1) B(7)-B(8) B(7)-B(l 1) B(7)-B(12) B(7')-B(ll') B(7r)-B(12') B(7')-B(8') B(8>B(9') B(8')-B(12') B(8)-B(12) B(9>B(12') B(9')-B(10r) B(12)-B(l 1) B(12)-B(10) B (10)-B (ll) B(10)-B(6) B (10')-B (ll’) B(10>B(12') B(6)-B(l 1) B(11>B(12') B(24)-B(29) B(24)-B(28)

1.83(3) 1.76(4) 1.93(4) 1.93(4) 1.72(3) 1.81(4) 1.75(4) 1.83(3) 1.73(4) 1.69(4) 1.74(4) 1.84(3) 1.80(4) 1.72(4) 1.81(3) 1.85(4) 1.80(3) 1.82(3) 1.81(3) 1.74(4) 1.83(3) 1.80(3) 1.82(3) 1.76(3) 1.73(4) 1.81(3) 1.78(3) 1.85(4) 1.84(4) 1.81(3) 1.70(4) 1.78(4) 1.72(4) 1.84(4) 1.79(4) 1.77(3)

B(24)-B(25) B (24>B (28*) B(24')-B(29') B(24>B(25') B(25)-B(210) B(25)-B(26) B(25)-B(29) B(25')-B(26') B(25>B(210) B(25>B(29') B(26)-B(211) B(26)-B(210) B(26>B(211) B(26>B(210) B(27)-B(212) B(27)-B(211) B(27)-B(28) B(27>B(211) B(27>B(28') B(27’)*B(212) B(28,)-B(29') B(28>B(212) B(28)-B(29) B(28)-B(212) B(29)-B(210) B(29)-B(212) B(29r)-B(212) B(29')-B(210) B(212)-B(210) B(212)-B(211) B(210)-B(212) B(210)-B(211) B(210)-B(211) B(211)-B(212)

1.78(4) 1.82(3) 1.81(4) 1.85(3) 1.81(4) 1.83(5) 1.83(4) 1.72(4) 1.74(5) 1.83(4) 1.73(5) 1.78(3) 1.71(4) 1.75(3) 1.77(3) 1.79(4) 1.83(3) 1.77(3) 1.77(3) 1.78(3) 1.85(3) 1.87(3) 1.77(3) 1.81(3) 1.73(4) 1.74(3) 1.76(4) 1.80(4) 1.78(4) 1.80(4) 1.75(3) 1.78(4) 1.68(4) 1.79(4)

158.2(7) 147.8(8) 34.7(5) 34.2(9) 131.0(7) 156.8(7) 160.3(11) 149.2(12) 36.9(11) 34.3(6) 131.9(10) 162.1(7) 83.1(11) 84.8(11) 153.2(9) 154.6(10) 111.4(9)

B(4)-Co( 1)-B(7) B (4>C o(l)-C (l) C (2> C o(l)-C (l) B(4)-Co(l)-C(l) B(7)-Co(l)-C(l) B(4')-Co(l)-C(l') C(2')-Co(l)-C(l') B(4)-Co(l)-C(l') B (7)-C o(l)-C (l’) C (l)-C o(l)-C (l') B(4r)-Co( 1)-B(8) C(2')-Co(l)-B(8) B(4)-Co(l)-B(8) B(7)-Co(l)-B(8) C(l)-Co(l)-B(8) C (l> C o(l)-B (8) B(4’)-Co(l)-C(2)

89.1(10) 111.5(11) 114.1(9) 49.7(9) 82.4(8) 48.1(10) 45.6(9) 110.2(9) 154.6(9) 97.4(8) 106.7(11) 155.3(9) 51-5(9) 51.9(10) 83.9(8) 153.4(10) 155.6(10)

Bond angles C( 11)-Ag( 1)-C(5) C(11)-Ag(l)-C(6) C(5)-Ag(l)-C(6) C(11)-Ag(l)-C(16) C(5)-Ag( 1)-C( 16) C(6)-Ag( 1)-C( 16) C(23)-Ag(2)-C(29) C(23)-Ag(2)-C(34) C(29)-Ag(2)-C(34) C(23)-Ag(2)-C(24) C(29)-Ag(2)-C(24) C(34)-Ag(2)-C(24) B(4>Co(l)-C(2') B (4>Co(l)-B(4) C (2>Co(l)-B(4) B(4>Co(l)-B(7) C(2>Co(l)-B(7)

300


C(2>Co(l)-C(2) B(4)-Co(l)-C(2) B(7)-Co( 1)-C(2) C(l)-Co(l)-C(2) C (l>C o(l)-C (2) B(8)-Co(l)-C(2) B(4>C o(l)-B (8) C(2>Co(l)-B(8') B(4)-Co(l)-B(8') B(7)-Co(l)-B(8') C(l)-Co(l)-B(8') C (lr)-Co(l)-B(8') B(8)-Co(l)-B(8') C(2)-Co(l)-B(8') B(4>Co(l)-B(7') C(2>Co(l)-B(7') B(4)-Co(l)-B(7') B(7)-Co(l)-B(7r) C(l)-Co(l)-B(7') C(l>C o(l)-B (7') B(8)-Co(l)-B(7r) C(2)-Co(l)-B(7') B(8>C o(l)-B (7r) C(21)-Co(2)-C(21') C(21)-Co(2)-C(22’) C(21')-Co(2)-C(22') C(21)-Co(2)-B(24) C(21>Co(2)-B(24) C(22>Co(2)-B(24) C(21)-Co(2)-B(28’) C(21>Co(2)-B(28') C(22')-Co(2)-B(28’) B(24)-Co(2)-B(28r) C(21)-Co(2)-B(27') C(21>Co(2)-B(27’) C(22')-Co(2)-B(27r) B(24)-Co(2)-B(27r) B(28')-Co(2)-B(27') C(21)-Co(2)-C(22) C(21')-Co(2)-C(22) C(22>Co(2)-C(22) B(24)-Co(2)-C(22) B(28')-Co(2)-C(22) B(27’)-Co(2)-C(22) C(21)-Co(2)-B(24’) C(21r)-Co(2)-B(24r) C(22>Co(2)-B(24’) B(24)-Co(2)-B(24r) B(28>Co(2)-B(24') B(27')-Co(2)-B(24r) C(22)-Co(2)-B(24') C(21)-Co(2)-B(28) C(21>Co(2)-B(28) C(22>Co(2)-B(28) B(24)-Co(2)-B(28) B(28>Co(2)-B(28)

98.7(8) 83.0(8) 46.3(9) 45-5(8) 117.9(8) 81.8(8) 51-5(10) 84.5(9) 106.2(9) 107.4(9) 154.7(9) 83.6(9) 84.4(9) 152.9(9) 86.6(12) 48.1(9) 154.3(10) 88.2(10) 154.4(9) 81.2(10) 108.8(10) 112.8(10) 50.8(9) 96.2(8) 115.4(8) 45-5(8) 49.0(9) 113.3(9) 156.6(9) 153.0(9) 84.7(8) 84.4(8) 105.9(9) 156.5(9) 80.7(9) 47.3(9) 152.8(9) 50.3(9) 47.0(9) 115.6(8) 97.8(8) 82.5(10) 153.5(9) 113.4(9) 109.3(10) 49.0(8) 83.4(8) 86-5(11) 52.2(9) 86.3(8) 154.3(10) 85.4(8) 154.5(8) 153.2(9) 50.2(9) 82.7(7)

B(27f)-Co(2)-B(28) C(22)-Co(2)-B(28) B(24>Co(2)-B(28) C(21)-Co(2)-B(27) C(21>Co(2)-B(27) C(22>Co(2)-B(27) B(24)-Co(2)-B(27) B(28>Co(2)-B(27) B(27')-Co(2)-B(27) C(22)-C o(2)-B(27) B (24>C o(2)-B(27) B(28)-Co(2)-B(27) C(2)-C(l)-B(5) C(2)-C(l)-B(6) B(5)-C(l)-B(6) C(2)-C(l)-B(4) B(5)-C(l)-B(4) B(6)-C(l)-B(4) C(2)-C(l)-Co(l) B(5)-C(l)-C o(l) B(6)-C(l)-C o(l) B(4)-C( 1)-Co( 1) B(4’)-C( 1 r)-C(2T) B(4r)-C (l ')-B(5') C(2')-C(1>B(5') B (4>C (1>B (6') C(2')-C(l,)-B(6') B (5>C (1>B (6') B (4 > C (l> C o (l) C (2 > C (l> C o (l) B (5 > C (l> C o (l) B(6')-C(lr)-Co(l) C(l)-C(2)-B(6) C (l)-C (2)-B (l 1) B(6)-C(2)-B( 11) C(l)-C(2)-B(7) B(6)-C(2)-B(7) B(ll)-C (2)-B(7) C(l)*C(2)-Co(l) B(6)-C(2)-Co(l) B( 1 l)-C(2)-Co( 1) B(7)-C(2)-C o( 1) C (1>C(2>B(11') C( 1r)-C(2r)-B(7') B (11>C (2>B (7’) C d )-Q 2 )-B (6 ) B(11,)-C (2>B (6,) B(7')-C(2>B(6') C (l)-C (2 > C o (l) B (ll> C (2 > C o (l) B (7> C (2> C o(l) B (6> C (2> C o(l) C(10)-C(5)-C(6) Q io V ^ ^ s o C(6)-C(5)-B(8') C(10)-C(5)-Ag(l)

107.4(9) 84.0(8) 106.5(8) 83.5(9) 154.0(8) 111.4(8) 86.1(9) 107.2(10) 89.3(9) 47.4(10) 154.7(9) 51-5(9) 110(2) 60(2) 63.7(14) 111(2) 61.9(14) 115(2) 68.6(13) 122(2) 124(2) 64.8(11) 109(2) 70(2) 109(2) 122(2) 64.4(14) 61(2) 61(2) 66.6(11) 124(2) 128(2) 63(2) 114(2) 62(2) 114(2) 118(2) 65.8(13) 65.9(12) 125(2) 125.7(13) 66.6(11) 108(2) 112(2) 65(2) 60.4(14) 60(2) 115(2) 67.8(13) 127(2) 68.6(9) 125(2) 118(2) 125.8(14) 115.9(14) 995(13)

301


C(6)-C(5)-Ag(l) B(8>C(5)-Ag(l) C(7)-C(6)-C(5) C(7)-C(6)-B(8) C(5)-C(6)-B(8) C(7)-C(6)-Ag(l) C(5)-C(6)-Ag(l) B(8)-C(6)-Ag(l) C(6)-C(7)-C(8) C(9)-C(8)-C(7) C(10)-C(9)-C(8) C(9)-C(10)-C(5) C( 12)-C( 11 )-C( 16) C( 12)-C( 11 )-Ag( 1) C( 16)-C( 11)-Ag( 1) C( 11 )-C( 12)-C( 13) C( 11 )-C( 12)-C( 17) C(13)-C(12)-C(17) C( 12)-C( 13)-C( 14) C( 13)-C( 14)-C( 15) C( 16)-C( 15)-C( 14) C(16)-C(15)-C(18) C( 14)-C( 15)-C( 18) C(15)-C(16)-C(ll) C( 15)-C( 16)-Ag( 1) C( 11 )-C( 16)-Ag( 1) C(22)-C(21)-B(24) C(22)-C(21)-B(25) B(24)-C(21)-B(25) C(22)-C(21)-B(26) B(24)-C(21)-B(26) B(25)-C(21)-B(26) C(22)-C(21)-Co(2) B(24)-C(21)-Co(2) B(25)-C(21)-Co(2) B(26)-C(21)-Co(2) C(22')-C(21 r)-B(25") C(22>C(21>B(24') B(25>C(21>B(24') C(22>C(21>B(26') B(25')-C(21 ')-B(26') B(24r)-C(21f)-B(26') C(22>C(21>Co(2) B(25>C(21>Co(2) B(24>C(21>Co(2) B(26>C(21>Co(2) C(21)-C(22)-B(26) C(21)-C(22)-B(211) B(26)-C(22)-B(211) C(21)-C(22)-B(27) B(26)-C(22)-B(27) B(211 )-C(22)-B(27) C(21)-C(22)-Co(2) B(26)-C(22)-Co(2) B(21 l)-C(22)-Co(2) B(27)-C(22)-Co(2)

C (2 l')-C (2 2 y B (2 7 r)

74.4(10) 99.6(13) 119(2) 126(2) 115.5(14) 97.1(12) 70.9(11) 97.7(12) 121(2) 120(2) 121(2) 122(2) 120(3) 97(2) 75.3(12) 126(3) 122(3) 112(4) 118(3) 121(3) 116(3) 122(3) 122(3) 119(3) 103(2) 70.4(12) 112(2) 108(2) 63(2) 57(2) 113(2) 61(2) 71.7(12) 67.5(11) 125(2) 125(2) 111(2) 113(2) 65.8(14) 63.5(14) 60(2) 117(2) 66.7(11) 126.7(14) 67.4(10) 127(2) 67(2) 115(2) 63(2) 108(2) 117(2) 65(2) 61.2(9) 125(2) 124(2) 64.9(10)

C(21’)-C(22')'B(211) B(27>C(22>B(211) C(21>C(22>B(26') B(27>C(22>B(26') B(211)-C(22>B(26') C(21>C(22>Co(2) B(27>C(22>Co(2) B(211)-C(22')-Co(2) B(26>C(22>Co(2) C(24)-C(23)-C(28) C(24)-C(23)-B(28') C(28)-C(23)-B(28') C(24)-C(23)-Ag(2) C(28)-C(23)-Ag(2) B(28>C(23)-Ag(2) C(25)-C(24)-C(23) C(25)-C(24)-B(28) C(23)-C(24)-B(28) C(25)-C(24)-Ag(2) C(23)-C(24)-Ag(2) B(28)-C(24)-Ag(2) C(24)-C(25)-C(26) C(27)-C(26)-C(25) C(28)-C(27)-C(26) C(27)-C(28)-C(23) C(30)-C(29)-C(34) C(30)-C(29)-Ag(2) C(34)-C(29)-Ag(2) C(31)-C(30)-C(29) C(31)-C(30)-C(35) C(29)-C(30)-C(35) C(32)-C(31)-C(30) C(31)-C(32)-C(33) C(34)-C(33)-C(32) C(34)-C(33)-C(36) C(32)-C(33)-C(36) C(33)-C(34)-C(29) C(33)-C(34)-Ag(2) C(29)-C(34)-Ag(2) C(42)-C(37)-C(38) C(42)-C(37)-C(43) C(38)-C(37)-C(43) C(39)-C(38)-C(37) C(40)-C(39)-C(38) C(41)-C(40)-C(39) C(41)-C(40)-C(44) C(39)-C(40)-C(44) C(42)-C(41)-C(40) C(41)-C(42)-C(37) C(46)-C(45)-C(50) C(46)-C(45)-C(51) C(50)-C(45)-C(51) C(45)-C(46)-C(47) C(48)-C(47)-C(46) C(49)-C(48)-C(47)

112(2) 109(2) 63.1(12) 63.0(14) 113.4(14) 58.9(13) 67.7(11) 69.1(9) 126.1(14) 127(2) 117(2) 114(2) 129(2) 77.4(11) 100(2) 92.1(13) 121(2) 125(2) 114(2) 105.0(13) 68.3(10) 98.1(12) 119(2) 121(2) 118(2) 124(2) 110(2) 95(2) 73.6(13) 123(3) 113(4) 124(3) 121(3) 121(3) 115(3) 122(4) 122(4) 129(3) 95(2) 70(2) 115(2) 125(3) 120(3) 118(3) 124(3) 114(3) 123(3) 123(3) 124(3) 125(3) 116(2) 123(2) 121(2) 123(2) 118(2) 118(2)

302


C(49)-C(48)-C(52) C(47)-C(4S)-C(52) C(50)-C(49)-C(48) C(49)-C(50)-C(45) C(58)-C(53)-C(54) C(58)-C(53)-C(59) C(54)-C(53)-C(59) C(55)-C(54)-C(53) C(54)-C(55)-C(56) C(57)-C(56)-C(55) C(57)-C(56)-C(60) C(55)-C(56)-C(60) C(56)-C(57)-C(58) C(53)-C(58)-C(57) B(5)-B(4)-C(l) B(5)-B(4)-B(8) C(l)-B(4)-B(8) B(5)-B(4)-B(9) C(l)-B(4)-B(9) B(8)-B(4)-B(9) B(5)-B(4)-C o(1) C(l)-B(4)-Co(l) B(8)-B(4)-Co(l) B(9)-B(4)-Co(l) C(1')-B(4>B(8') C (l> B (4 > C o (l) B (8> B (4> C o(l) C (l> B (4 > B (9 r) B (8>B (4,)-B(9') Co( 1)-B(4')-B(9r) C(1>B(4>B (5') B(S>B(4>B(5') C o(l)-B (4>B (5’) B (9>B (4>B(5') B(8)-B(9)-B(5) B(8)-B(9)-B(12) B(5)-B(9)-B(12) B(8)-B(9)-B(4) B(5)-B(9)-B(4) B(12)-B(9)-B(4) B(8)-B(9)-B(10) B(5)-B(9)-B(10) B(12)-B(9)-B(10) B(4)-B(9)-B(10) C(1')-B(5>B(6') C(1’)-B(5>B(10') B (6>B(5>B(10') C (1>B(5>B(9') B(6')-B(5')-B(9') B (10>B (5’)-B(9') C(1')-B(5>B(4’) B(6r)-B(5’)-B(4r) B (10>B (5’)-B(4’) B(9’)-B(5')-B(4') C(l)-B(5)-B(4) C(l)-B(5)-B(9)

123(2) 119(2) 122(2) 123(2) 118(2) 123(2) 120(2) 119(2) 124(2) 116(2) 120(3) 124(2) 123(3) 120(2) 57.8(13) 106(2) 104(2) 60.6(13) 103(2) 56.2(13) 119(2) 65.5(11) 66.2(10) 116(2) 111(3) 71(2) 70(2) 101(2) 58.0(13) 121(2) 57.1(14) 103(2) 122(2) 53.7(14) 108(2) 61(2) 108(2) 61.3(13) 57.7(13) 109(2) 113(2) 60.7(14) 62(2) 109(2) 58.9(13) 107(2) 64(2) 105(2) 115(2) 64(2) 53(2) 105(2) 112(2) 63(2) 60.3(14) 106(2)

B(4)-B(5)-B(9) C(l)-B(5)-B(10) B(4)-B(5)-B(10) B(9)-B(5>B(10) C(l)-B(5)-B(6) B(4)-B(5)-B(6) B(9)-B(5)-B(6) B(10)-B(5)-B(6) B ( l l ,)-B(6')-C(l') B(11>B(6>C(2') C(1>B(6>C(2') B (ll> B (6 > B (5 ') C (l)-B (6)-B (5) C(2')-B(6>B(5') B(11>B(6>B(10') C(1’)-B(6>B(10') C(2')-B(6')-B( 101) B(5 ,)-B(6,)-B( 101) C(2)-B(7)-B(8) C (2)-B(7)-B(ll) B (8)-B(7)-B(ll) C(2)-B(7)-B( 12) B(8)-B(7)-B(12) B(11)-B(7)-B(12) C(2)-B(7)-Co( 1) B(8)-B(7)-C o(1) B(1 l)-B(7)-Co(l) B(12)-B(7)-C o(1) C(2>B(7>B(11') B(11>B(7>B(12') C(2>B (7> B (8') B (11>B (7> B (8’) B(12')-B(7')-B(8') C(2')-B(7>Co(l) B (ll> B (7 > C o (l) B (12> B (7> C o(l) B (8> B (7> C o(l) C(5)-B(8>B(4') B(9')-B(8>B(4') C(5)-B(8')-B(7') B(9,)-B(8')-B(7’) B(4')-B(8>B(7') C(5)-B(8>B(12') B(9>B(8>B(12') B (4> B (8> B (12,) B(7>B(8>B(12') C (5)-B(8>C o(l) B(9,)-B (8>C o(l) B (4)-B (8>C o(l) B (7> B (8> C o(l) B(12>B(8')-Co(l) C(6)-B(8)-B(9) C(6)-B(8)-B(7) B(9)-B(8)-B(7)

61.7(14) 107(2) 112(2) 60.1(13) 59.2(13) 110(2) 106(2) 59-5(13) 102(2) 57.3(14) 55.3(12) 103(2) 60(2) 102(2) 58(2) 103(2) 101(2) 57(2) 104(2) 57.5(13) 105(2) 103(2) 57.4(12) 58.9(13) 67.1(11) 64.6(10) 119(2) 116(2) 57(2) 106(2) 63(2) 105(2) 110(2) 61.2(14) 63.3(10) 115(2) 118(2) 63.7(9) 122(2) 126(2) 66(2) 124(2) 103(2) 102(2) 121(2) 57.1(14) 108(2) 57.0(13) 112.9(12) 117(2) 58(2) 65.4(9) 115.6(14) 120(2) 123(2) 108(2)

303


C(6)-B(8)-B(4) B(9)-B(8)-B(4) B(7)-B(S)-B(4) C(6)-B(8)-B(12) B(9)-B(8)-B(12) B(7)-B(8)-B(12) B(4)-B(8)-B(12) C(6)-B(8)-Co(l) B(9)-B(8)-Co(l) B(7)-B(8)-Co(l) B(4)-B(8)-Co(l) B( 12)-B(8)-Co( 1) B(12>B(9>B(8') B(12’)-B (9>B (5’) B ^ - B ^ - B C S 1) B (12>B (9r)-B(10') B (8> B (9> B (10r) B (5>B (9)-B (10r) B(12')-B(9')-B(4r) B(8>B(9')-B(4’) B(5')-B(9')-B(4') B(10>B(9>B(4') B (ll)-B(12)-B(9) B(11)-B(12)-B(8) B(9)-B(12)-B(8) B(11)-B(12)-B(10) B(9)-B(12)-B(10) B(8)-B(12)-B(10) B(11)-B(12)-B(7) B(9)-B(12)-B(7) B(8)-B(12)-B(7) B(10)-B(12)-B(7) B(11)-B( 10)-B( 12) B(11)-B(10)-B(6) B(12)-B(10)-B(6) B(11)-B(10)-B(9) B(12)-B(10)-B(9) B(6)-B(10)-B(9) B(11)-B(10)-B(5) B(12)-B(10)-B(5) B(6)-B(10)-B(5) B(9)-B(10)-B(5) B (11>B (10> B (5’) B(11>B(10>B(6') B(5>B(10>B(6') B(11>B(10>B(12') B(5>B(10')-B(12') B(6>B(10>B(12') B(11>B(10>B(9') B (5> B (10> B (9r) B(6>B(10>B(9') B (12)-B (10>B (9) C(2)-B(6)-B(l 1) C(2)-B(6)-C(l) B(11)-B(6)-C(1) C(2)-B(6)-B(10)

122(2) 62.6(14) 106(2) 121(2) 60.5(14) 603(13) 110(2) 111.2(12) 118(2) 633(9) 62.4(10) 118(2) 62.1(14) 106(2) 109(2) 60(2) 111(2) 57(2) 104(2) 56.1(14) 62.9(14) 106(2) 108(2) 110(2) 58.5(14) 61(2) 60.9(14) 109(2) 60.1(14) 108(2) 62.1(14) 110(2) 57.7(13) 56.3(14) 102(2) 103(2) 56.8(13) 105(2) 102.5(14) 103(2) 59(2) 59.2(14) 105(2) 59(2) 59(2) 64(2) 106(2) 110(2) 108(2) 60(2) 108(2) 58(2) 58.9(14) 56.7(12) 106(2) 108(2)

B( 11)-B(6)-B( 10) C(l)-B(6)-B(10) C(2)-B(6)-B(5) B (ll)-B(6)-B(5) C(l)-B(6)-B(5) B(10)-B(6)-B(5) C(2>B(11>B(6') C (2>B (11>B (10’) B(6>B(11>B(10') C(2>B(11>B(7') B ^ - B O O - B ^ 1) B (10>B(11>B(7') C(2>B(11>B(12') B ^ -B a O -B ^ ') B( 10,)-B( 11 ')-B( 121) B (7>B (11> B (12,) B(9 ,)-B( 12”)-B( lO') B(9’)-B(12')-B(7') B (10>B (12> B (7,) B(9')-B(12')-B(8,) B(10>B(12>B(8') B(7>B (12>B(8') B (9>B (12> B (11,) B (10>B (12>B (11,) B (7> B (12’)-B(11') B(8>B(12')-B(11') C(2)-B( 11 )-B( 12) C(2)-B(ll)-B(6) B(12)-B(11)-B(6) C(2)-B( 11)-B( 10) B(12)-B(l 1)-B(10) B(6)-B(ll)-B(10) C(2)-B(ll)-B(7) B(12)-B(ll)-B(7) B (6)-B(ll)-B(7) B(10)-B(ll)-B(7) C(21)-B(24)-B(29) C(21)-B(24)-B(28) B(29)-B(24)-B(28) C(21)-B(24)-B(25) B(29)-B(24)-B(25) B(28)-B(24)-B(25) C(21)-B(24)-Co(2) B(29)-B(24)-Co(2) B(28)-B(24)-Co(2) B(25)-B(24)-Co(2) C (21>B (24>B (28,) C(21f)-B(24')-B(29 ■) B(28’)-B(24,)-B(29') C(21>B(24>B(25') B(28,)-B(24>B(25,) B(29')-B(24>B(25') C(21')-B(24>Co(2) B(28')-B(24,)-Co(2) B(29')-B(24>Co(2) B(25>B(24>Co(2)

63(2) 107(2) 103(2) 109(2) 57.1(14) 61.4(14) 62(2) 110(2) 64(2) 59.0(13) 112(2) 108(2) 103(2) 111(2) 60(2) 57.0(14) 62(2) 110(2) 108(2) 60.7(13) 111(2) 61.8(13) 106(2) 56(2) 60.4(14) 109(2) 103.3(14) 59.2(13) 109(2) 106(2) 613(14) 61(2) 56.6(12) 60.9(12) 108(2) 111(2) 107(2) 108(2) 59.7(13) 60.1(14) 62(2) 111(2) 63.4(11) 119(2) 66.9(10) 119(2) 102(2) 102(2) 61.2(13) 57(2) 108(2) 60(2) 63.7(11) 62.4(10) 116(2) 115(2)

304


C(21)-B(25)-B(210) C(21)-B(25)-B(24) B(210)-B(25)-B(24) C(21)-B(25)-B(26) B(210)-B(25)-B(26) B(24)-B(25)-B(26) C(21)-B(25)-B(29) B(210)-B(25)-B(29) B(24)-B(25)-B(29) B(26)-B(25)-B(29) C(21>B(25>B(26-) C(21>B(25>B(210) B(26>B(25>B(210) C(21')-B(25')-B(24r) B(26>B(25>B(24') B(210)-B(25')-B(24') C(21>B(25>B(29') B(26>B(25>B(29') B(210)-B(25r)-B(29') B (24>B (25>B(29r) B(211)-B(26)-C(22) B(211)-B(26)-B(210) C(22)-B(26)-B(210) B(211)-B(26)-B(25) C(22)-B(26)-B(25) B(210)-B(26)-B(25) B(211)-B(26)-C(21) C(22)-B(26)-C(21) B(210)-B(26)-C(21) B(25)-B(26)-C(21) B(25>B(26>B(211) B(25VB(26>B(210) B(211)-B(26>B(210) B (25>B(26r)-C(22') B(211)-B(26>C(22') B(210)-B(26>C(22’) B (25>B (26>C (21’) B(211)-B(26’)-C(21r) B(210)-B(26')-C(21') C(22')-B(26>C(21’) B(212)-B(27)-C(22) B(212)-B(27)-B(211) C(22)-B(27)-B(211) B(212)-B(27)-B(28) C(22)-B(27)-B(28) B(211)-B(27)-B(28) B(212)-B(27)-Co(2) C(22)-B(27)-Co(2) B(211 )-B(27)-Co(2) B(28)-B(27)-Co(2) C (22>B(27>B (211) C(22')-B(27')-B(28') B(211)-B(27>B(28') C(22>B(27>B(212) B(211)-B(27')-B(212) B(28')-B(27>B(212)

105(2) 57.1(13) 105(2) 62.8(14) 59(2) 110(2) 103(2) 57(2) 59(2) 106(2) 61(2) 106(2) 61(2) 57.7(14) 111(2) 109(2) 103(2) 110(2) 61(2) 59(2) 57(2) 61(2) 102(2) 108(2) 102(2) 60(2) 101(2) 55.4(11) 101(2) 56.1(14) 107(2) 60(2) 58(2) 102(2) 59.9(13) 103(2) 59(2) 102(2) 103(2) 53.6(11) 103(2) 60.5(14) 55.6(13) 60.4(12) 107(2) 110(2) 118(2) 67.7(10) 118(2) 64.7(9) 60.2(12) 106(2) 111(2) 108(2) 61.0(13) 63.4(13)

C(22>B(27>Co(2) B(211)-B(27>Co(2) B(28>B(27>Co(2) B(212)-B(27>Co(2) C(23)-B(281)-B(24') C(23)-B(28>B(29') B(24>B(28>B(29') C(23)-B(28>B(27') B(24>B(28')-B(27') B(29')-B(28')-B(27') C(23)-B(28>B(212) B(24>B(28>B(212) B(29>B(28>B(212) B(27')-B(28')-B(212) C(23)-B(28>Co(2) B(24>B(28>Co(2) B(29')-B(28>Co(2) B(27>B(28>Co(2) B(212)-B(28')-Co(2) C(24)-B(28)-B(29) C(24)-B(28)-B(24) B(29)-B(28)-B(24) C(24)-B(28)-B(212) B(29)-B(28)'B(212) B(24)-B(28)-B(212) C(24)-B(28)-B(27) B(29)-B(28)-B(27) B(24)-B(28)-B(27) B(212)-B(28)-B(27) C(24)-B(28)-Co(2) B(29)-B(28)-Co(2) B(24)-B(28)-Co(2) B(212)-B(28)-Co(2) B(27)-B(28)-Co(2) B(210)-B(29)-B(212) B(210)-B(29)-B(28) B(212)-B(29)-B(28) B(210)-B(29)-B(24) B(212)-B(29)-B(24) B(28)-B(29)-B(24) B(210)-B(29)-B(25) B(212)-B(29)-B(25) B(28)-B(29)-B(25) B(24)-B(29)-B(25) B(212)-B(29’)-B(28') B(212)-B(29,)-B(24,) B(28>B(29>B(24') B(212)-B(29>B(210) B(28>B(29>B(210) B(24>B(29>B(210) B(212)-B(29>B(25,) B(28')-B(29,)-B(25') B(24')-B(29')-B(25') B(210)-B(29')-B(25') B(29>B(212)-B(210) B(29')-B(212)-B(27')

63.6(9) 119(2) 62.9(8) 120(2) 124(2) 118(2) 59(2) 126(2) 106.6(14) 102.8(14) 117(2) 105(2) 56.7(13) 58.5(12) 116.0(12) 65.4(11) 117.0(13) 66.7(11) 119(2) 122(2) 125(2) 60.6(14) 122(2) 58.1(12) 105(2) 124(2) 104(2) 103.8(14) 58.0(12) 113.1(11) 116.1(13) 62.8(10) 115.0(13) 63.8(9) 61(2) 112(2) 62.2(14) 108(2) 108(2) 59.7(12) 61(2) 109(2) 109(2) 58.9(13) 62.2(14) 110(2) 59.9(12) 60(2) 109(2) 108(2) 107(2) 108(2) 61(2) 57(2) 61(2) 106(2)

305


—“

m co J

r l —• r i r i ^ *-4 rl «-* *-*l rZZl r l ZZ sr-iy rS»y CQ

p 2 2 v o O vo r l H VO r i r- P P 2 P 2 r l r i r l r i n r l ri r l rl r i r i r i rl n r l r l do m m m u m m u m mm

ss

sss

AAo

Ov h H ri rl n

mmm


l a A rT rl

Compound VIII-2 Atomic coordinates and thermal parameters. X

Ag Ag' Br(8) Br(12) Br(9) Co N (l) N(2) N(2') C (l) C(2) C( 3) C(4) C(5) C(6) 0(6-)

B(7) B( 11) B(6) B(4) B(8) B(12) B(10) B(5) B(9)

-4715(30) -5397(30) 1 (1 )

-1832(1) 1834(1) 0 -5001(10) -6391(19) -8814(55) 761(5) -762(5) -4999(8) -5013(9) -6982(15) -7427(24) -7781(46) -1335(6) -1326(7) -2(7) 1331(6) 1(6) -827(7) 0(6) 1328(7) 823(6)

y 7329(8) 7235(11) 2212(1) 2442(1) 2442(1) 5000 6192(8) 8473(14) 8315(46) 5616(5) 5614(5) 5813(8) 5329(9) 8851(30) 10573(23) 9784(49) 4391(5) 4933(5) 5733(6) 4394(6) 3569(5) 3618(5) 4436(5) 4928(5) 3619(5)

z -2513(13) -2529(9) 76(1) 1249(1) 1249(1) 0 -3185(4) -2501(7) -2502(19) 623(2) 624(2) -3558(4) -4028(4) -2502(4) -2499(9) -2508(14) 499(3) 1113(3) 1184(3) 493(3) 430(3) 1008(3) 1436(3) 1113(3) 1010(3)

U(eq) 115(7) 144(7) 66(1) 68(1) 68(1) 35(1) 121(3) 120(8) 270(30) 42(1) 41(1) 77(2) 84(3) 301(22) 99(12) 213(21) 42(2) 46(2) 49(2) 41(2) 42(2) 45(2) 44(2) 47(2) 43(2)

Bond lengths Ag-N(2) A g-N (l) A g-N (l)#l Ag'-N(2) Ag'-N(l) Ag’-N (l)# l Ag'-N(2)#l Br(8)-B(8) Br(l2)-B(12) Br(9)-B(9) Co-C(l)#2 Co-C(l) Co-C(2)#2 Co-C(2) Co-B(4) Co-B(4)#2 Co-B(7)#2 Co-B(7) Co-B(8)#2 Co-B(8) N(l)-C(3) N (l)-A g#l

N (l)-A g’#l N(2)-C(5) N(2)-AgWl N (2> Q 5) C(l)-C(2) C(l)-B(5) Q D -B (4) C(l)-B(6) C (2)-B(ll) C(2)-B(7) C(2)-B(6) C(3)-C(4) C(5)-C(6') C(6)-C(6') B(7)-B(12) B(7)-B(8) B (7)-B(ll) B (ll)-B (6) B (ll)-B(12) B(ll)-B(10) B(6)-B(5) B(6)-B(10) B(4)-B(8)

2.31(3) 2.33(3) 2.38(3) 1.90(3) 2.24(2) 2.37(2) 2.48(3) 1.963(7) 1.953(7) 1.952(7) 2.018(6) 2.018(6) 2.023(6) 2.023(6) 2.094(7) 2.094(7) 2.113(7) 2.113(7) 2.148(7) 2.148(7) 1.111(12) 2.38(3)

2.37(2) 0.80(3) 2.48(3) 2.08(6) 1.640(8) 1.689(10) 1.700(9) 1.723(10) 1.687(9) 1.700(9) 1.717(10) 1.40(2) 1.46(5) 1.07(5) 1.767(10) 1.785(9) 1.788(10) 1.758(10) 1.772(9) 1.783(10) 1.768(10) 1.776(10) 1.780(9)

307


B(4)-B(9) B(4)-B(5) B(8)-B(9) B(8)-B(12) B(12)-B(9)

1.787(10) 1.796(10) 1.791(10) 1.792(10) 1.776(10)

B(12)-B(10) B(10)-B(9) B(10)-B(5) B(5)-B(9)

1.784(10) 1.781(10) 1.787(10) 1.765(10)

Bond angles Ag'#l-Ag-N(2)#l Ag#l-Ag-N(2)#l Ag’-Ag-N(2)#l Ag'#l-Ag-N(2) Ag#l-Ag-N(2) Ag'-Ag-N(2) N(2)#l-Ag-N(2) Ag'#l-Ag-N(l) A g#l-A g-N (l) Ag'-Ag-N(l) N(2)#l-Ag-N(l) N(2)-Ag-N(l) A g'#l-Ag-N(l)#l Ag# 1- Ag-N( 1)# 1 Ag'-Ag-N(l)#l N(2)#l-Ag-N (l)#l N(2)-Ag-N(l)#l N (l)-A g-N (l)#l Ag#l-Ag'-Ag Ag#l-Ag'-Ag'#l Ag-Ag'-Ag'#l Ag#l-Ag'-N(2) Ag-Ag’-N(2) Ag'#l-Ag'-N(2) Ag#l-Ag'-N(l) Ag-Ag'-N(l) Ag'#l-Ag’-N(l) N(2)-Ag'-N(l) Ag# 1- Ag’-N( 1)# 1 Ag-Ag'-N(l)#l Ag'#l-Ag'-N(l)#l N(2)-Ag'-N(l)#l N(l)-Ag'-N(l)#l Ag#l-Ag'-N(2)#l Ag-Ag'-N(2)#l Ag'#l-Ag'-N(2)#l N(2)-Ag'-N(2)#l N(l)-Ag'-N(2)#l N (l)# l-A g ’-N(2)#l C(l)#2-Co-C(l) C( 1)#2-Co-C(2)#2 C(l)-Co-C(2)#2 C(l)#2-Co-C(2) C(l)-Co-C(2) C(2)#2-Co-C(2) C(l)#2-Co-B(4) C(l)-Co-B(4) C(2)#2-Co-B(4)

94(10) 129.0(14) 139(2) 146(10) 39.0(8) 48(2) 90.7(11) 98(10) 88(5) 74(2) 125(2) 107.2(12) 45(10) 78(5) 80(3) 122(2) 105(2) 102.6(6) 45(10) 47(10) 11(3) 80(10) 115(2) 123.2(12) 132(10) 87(2) 87(3) 129(2) 77(10) 82(3) 71(3) 122.0(12) 105.8(8) 32(10) 30(2) 39.8(8) 85.1(12) 104.4(11) 100.8(13) 180.0 47.9(2) 132.1(2) 132.1(2) 47.9(2) 180.0 131.2(3) 48.8(3) 96.0(3)

C(2)-Co-B(4) C(l)#2-Co-B(4)#2 C(l)-Co-B(4)#2 C(2)#2-Co-B(4)#2 C(2)-Co-B(4)#2 B(4)-Co-B(4)#2 C( 1)#2-Co-B(7)#2 C(l)-Co-B(7)#2 C(2)#2-Co-B(7)#2 C(2)-Co-B(7)#2 B(4)-Co-B(7)#2 B(4)#2-Co-B(7)#2 C( 1)#2-Co-B(7) C(l)-Co-B(7) C(2)#2-Co-B(7) C(2)-Co-B(7) B(4)-Co-B(7) B(4)#2-Co-B(7) B(7)#2-Co-B(7) C(l)#2-Co-B(8)#2 C(l)-Co-B(8)#2 C(2)#2-Co-B(8)#2 C(2)-Co-B(8)#2 B(4)-Co-B(8)#2 B(4)#2-Co-B(8)#2 B(7)#2-Co-B(8)#2 B(7)-Co-B(8)#2 C(l)#2-Co-B(8) C(l)-Co-B(8) C(2)#2-Co-B(8) C(2)-Co-B(8) B(4)-Co-B(8) B(4)#2-Co-B(8) B(7)#2-Co-B(8) B(7)-Co-B(8) B(8)#2-Co-B(8) C(3)-N(l)-Ag' C(3)-N(l)-Ag Ag'-N(l)-Ag C(3)-N(l)-Ag#l Ag'-N(l)-Ag#l Ag-N(l)-Ag#l C(3)-N(l)-Ag’#l Ag'-N(l)-Ag'#l Ag-N(l)-Ag’#l Ag#l-N(l)-Ag'#l C(5)-N(2)-N(2) C(5)-N(2)-Ag#l

84.0(3) 48.8(3) 131.2(3) 84.0(3) 96.0(3) 180.0 83.7(3) 96.3(3) 48.5(3) 131.5(3) 94.0(3) 86.0(3) 96.2(2) 83.7(3) 131.5(3) 48.5(3) 86.0(3) 94.0(3) 180.0 83.1(3) 96.9(3) 83.0(3) 97.0(3) 130.4(3) 49.6(3) 49.5(3) 130.5(3) 96.9(3) 83.1(3) 97.0(3) 83.0(3) 49.6(3) 130.4(3) 130.5(3) 49.5(3) 180.0 164.4(12) 164.9(12) 18.6(5) 166.0(11) 4(2) 15(2) 166.1(11) 22(2) 4.8(11) 18.1(5) 41(3) 166(4)


N(2>N(2)-Ag#l C(5)-N(2)-A e ' N(2>N(2)-AgAg#l-N(2)-Ag' C(5)-N(2)-Ag N(2>N(2)-Ag Ag#l-N(2)-Ag Ag'-N(2)-Ag C(5)-N(2)-Ag'#l N(2>N(2)-Ag'#l Ag#l-N(2)-Ag’# l Ag'-N(2)-Ag'#l Ag'N(2)-Ag'#l C(5)-N(2>N(2) C(2)-C(l)-B(5) C(2)-C(l)-B(4) B(5)-C(l)-B(4) C(2)-C(l)-B(6) B(5)-C(l)-B(6) B(4)-C(l)-B(6) C(2)-C(l)-Co B(5)-C(l)-Co B(4)-C(l)-Co B(6)-C(l)-Co C(l)-C(2)-B(l 1) C(l)-C(2)-B(7) B(ll)-C(2)-B(7) C(l)-C(2)-B(6) B(11)-C(2)-B(6) B(7)-C(2)-B(6) C(l)-C(2)-Co B(1 l)-C(2)-Co B(7)-C(2)-C o B(6)-C(2)-Co N(l)-C(3)-C(4) N(2)-C(5)-C(6') N(2)-C(5)-N(2') C(6r)-C(5)-N(2r) C(6)-C(6')-C(5) C(2)-B(7)-B(12) C(2)-B(7)-B(8) B(12)-B(7)-B(8) C(2)-B(7)-B(l 1) B(12)-B(7)-B(l 1) B(8)-B(7)-B(l 1) C(2)-B(7)-Co B(12)-B(7)-Co B(8)-B(7)-Co B(ll)-B(7)-Co C(2)-B(ll)-B(6) C(2)-B(ll)-B(12) B(6)-B(l 1)-B(12) C(2)-B(ll)-B(10) B(6)-B(l I)-B(IO) B(12)-B(l 1)-B(10) C(2)-B(ll)-B(7)

125(2) 161(4) 120(2) 6(2) 178(3) 137(2) 12.0(14) 17.0(7) 177(3) 136(2) 11.5(6) 17.0(13) 2.6(12) 14.6(12) 111.0(5) 111.1(5) 64.0(4) 61.3(4) 62.4(4) 115.6(5) 66.2(3) 126.3(4) 67.9(3) 124.4(4) 111.3(5) 111.3(5) 63.7(4) 61.7(4) 62.2(4) 115.2(5) 65.9(3) 126.7(4) 68.5(3) 124.5(4) 179.2(12) 163(5) 124(4) 73(3) 123(5) 103.9(5) 105.0(5) 60.6(4) 57.8(4) 59.8(4) 108.4(5) 63.0(3) 118.8(4) 66.3(3) 116.3(4) 59.7(4) 104.2(5) 108.2(5) 105.7(5) 60.2(4) 60.3(4) 58.5(4)

B(6)-B(ll)-B(7) B(12)-B(ll)-B(7) B(10)-B(ll)-B(7) C(2)-B(6)-C(l) C(2)-B(6)-B(ll) C (l)-B (6)-B (ll) C(2)-B(6)-B(5) C(l)-B(6)-B(5) B(U)-B(6)-B(5) C(2)-B(6)-B(10) C(l)-B(6)-B(10) B( 11)-B(6)-B( 10) B(5)-B(6)-B(10) C(l)-B(4)-B(8) C(l)-B(4)-B(9) B(8)-B(4)-B(9) C(l)-B(4)-B(5) B(8)-B(4)-B(5) B(9)-B(4)-B(5) C(l)-B(4)-Co B(8)-B(4)-Co B(9)-B(4)-Co B(5)-B(4)-Co B(4)-B(8)-B(7) B(4)-B(8)-B(9) B(7)-B(8)-B(9) B(4)-B(8)-B(12) B(7)-B(8)-B(12) B(9)-B(8)-B(12) B(4)-B(8)-Br(8) B(7)-B(8)-Br(8) B(9)-B(8)-Br(8) B( 12)-B(8)-Br(8) B(4)-B(8)-Co B(7)-B(8)-Co B(9)-B(8)-Co B(12)-B(8)-Co Br(8)-B(8)-Co B(7)-B(12)-B(ll) B(7)-B(12)-B(9) B(11)-B(12)-B(9) B(7)-B(12)-B(10) B(11)-B(12)-B(10) B(9)-B(12)-B(10) B(7)-B(12)-B(8) B(11)-B(12)-B(8) B(9)-B(12)-B(8) B(10)-B(12)-B(8) B(7)-B(12)-Br(12) B( 11)-B(12)-Br( 12) B(9)-B(12)-Br(12) B(10)-B( 12)-Br( 12) B(8)-B(12)-Br(12) B(6)-B( 10)-B(9) B(6)-B(10)-B(ll) B(9)-B(10)-B(l 1)

108.8(5) 593(4) 108.4(5) 56.9(4) 58.1(4) 104.2(5) 103.8(5) 57.9(4) 108.2(5) 104.7(5) 104.7(5) 60.6(4) 60.5(4) 105.2(5) 103.2(5) 60.3(4) 57.7(4) 107.8(5) 59.0(4) 63.3(3) 66.8(3) 118.9(4) 116.4(4) 107.3(5) 60.1(4) 106.7(5) 107.4(5) 59.2(4) 59.4(4) 123.9(4) 124.1(4) 116.8(4) 116.8(4) 63.6(3) 64.2(3) 116.0(4) 115.9(4) 118.5(3) 60.7(4) 108.1(5) 107.6(5) 109.3(5) 60.2(4) 60.0(4) 60.2(4) 108.8(5) 60.2(4) 109.3(5) 120.5(4) 119.6(4) 123.7(4) 120.3(4) 122.6(4) 107.0(5) 59.2(4) 107.0(5)

309


106.9(5) 59.8(4) B(6)-B(10)-B(12) B(9)-B(10)-B(12)

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>»z n^ z s ^ z B(10>B(9') B(6')-B(10')-B(9r) B(5>B(10>B(11') B (6>B(10>B(11’) B(9')-B(10')-B(l l 1) B(5')-B(10')-B(12') B (6>B(10>B(12,) B(9>B(10>B(12') B(11>B(10>B(12') C(2’)-B(11>B(6') C(2')-B(l 1')-B(7') B(6>B(11>B(7') ^ - B d H - B d O 1) B(6>B(11>B(10') 8(70-8(11>B(10") C(20-B(110-B(120 B(60-B(11>B(120 B(70-B(110-B(120 B(lO0-B(110-B(120 B(70-B(120-B(80 B(70-B(120-B(90 B(80-B(120-B(90 B(70-B(120-B(lO0 B(80-B(120-B(lO0 B(90-B(120-B(lO0 B(70-B(120-B(110 B(80-B(120-B(110 B(90-B(12>B(110 B(lO0-B(120-B(110 Ag-C(5)-C(6) Ag-Q5)-C(10) C(6)-C(5)-C( 10) Ag-C(6)-C(5) Ag-C(6)-C(7) C(5)-C(6)-C(7) C(6)-C(7)-C(8) C(6)-C(7)-C( 12) C(8)-C(7)-C( 12) C(7)-C(8)-C(9) C(8)-C(9)-C(10) C(5)-C( 10)-C(9) C(5)-C(10)-C(ll)

124.7(3) 61.4(3) 67.0(2) 111.6(3) 115.2(4) 124.5(3) 110.8(4) 62.3(3) 63.3(3) 64.6(2) 117.8(3) 58.0(3) 65-3(2) 104.3(3) 107.3(4) 117.7(3) 102.9(4) 59.1(3) 59.7(3) 58.4(3) 59.2(3) 109.1(4) 104.2(3) 60.4(3) 108.7(4) 104.7(3) 108.7(3) 60.4(3) 60.0(3) 55.9(3) 58.7(3) 103.9(4) 104.3(3) 104.1(3) 60.3(3) 102.9(4) 58.0(3) 107.9(3) 60.1(3) 64.0(3) 65.1(3) 103.7(3) 116.5(3) 57.3(3) 107.0(3) 117.9(3) 103.0(3) 60.0(3) 59.5(3) 64.4(2) 64.5(2) 107.5(3) 117.0(3) 59.9(3) 107.3(3) 116.8(2)

107.6(3) 59.4(3) 59.9(3) 60.6(3) 60J(3) 109.1(4) 109.1(3) 60.2(3) 109.2(3) 108.3(4) 108.1(3) 60.3(3) 60.1(3) 59.2(3) 59.8(3) 107.6(5) 106.8(5) 59.9(3) 107.8(4) 108.0(4) 108.3(4) 60.5(3) 60.0(3) 59.7(4) 59.5(3) 109.9(5) 105.4(4) 60.1(3) 108.7(4) 105.0(4) 108.6(4) 59.8(3) 60.2(3) 60.6(3) 108.2(5) 59.8(3) 109.2(4) 108.3(4) 59.4(3) 60.7(3) 108.4(4) 106.8(4) 59.8(3) 67.7(3) 105.0(4) 121.4(7) 80.0(3) 99.1(3) 120.5(6) 117.6(6) 121.2(7) 121.2(9) 120.7(9) 122.5(7) 117.2(6) 121.0(7)

314


C(9)-C(10)-C(ll)

121.8(7)

315


Synthesis, Structure, and Weakly Coordinating

Synthesis, Structure, and Weakly Coordinating

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