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Structure Reports Online ISSN 1600-5368
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Hexa-µ2-acetato-κ12O :O -µ3-oxido-tris[aquachromium(III)] nitrate acetic acid solvate Mohd Jamil Maah, Che Ibrahim Abdullah, Seng Neon Gan, Aishah Mohd Jelan and Seik Weng Ng
Acta Cryst. (2008). E64, m1310
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ISSN 1600-5368
Volume 61 Part 11 November 2005
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Inorganic compounds
Metal-organic compounds
Organic compounds
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Crystallography Journals Online is available from journals.iucr.org Acta Cryst. (2008). E64, m1310
Maah et al. · [Cr3 (C2 H3 O2 )6 O(H2 O)3 ]NO3 ·C2 H4 O2
metal-organic compounds ˚ c = 15.0427 (2) A = 91.532 (1) ˚3 V = 2553.62 (5) A Z=4
Acta Crystallographica Section E
Structure Reports Online
Mo K radiation = 1.35 mm1 T = 100 (2) K 0.20 0.10 0.05 mm
ISSN 1600-5368
Data collection
Hexa-l2-acetato-j12O:O0 -l3-oxido-tris[aquachromium(III)] nitrate acetic acid solvate
Bruker SMART APEX diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996) Tmin = 0.774, Tmax = 0.936
22819 measured reflections 5836 independent reflections 5092 reflections with I > 2(I) Rint = 0.046
Refinement
Mohd Jamil Maah,a* Che Ibrahim Abdullah,a Seng Neon Gan,a Aishah Mohd Jelanb and Seik Weng Nga a
Department of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and bCentre for Foundation Studies in Science, University of Malaya, 50603 Kuala Lumpur, Malaysia Correspondence e-mail:
[email protected] Received 15 September 2008; accepted 16 September 2008 ˚; Key indicators: single-crystal X-ray study; T = 100 K; mean (C–C) = 0.008 A R factor = 0.068; wR factor = 0.225; data-to-parameter ratio = 16.3.
In the crystal structure of the title salt, [Cr3(C2H3O2)6O(H2O)3]NO3CH3CO2H, the trinuclear [Cr3(CH3CO2)6O(H2O)3] cluster cation has an oxide O atom that is connected to three water-coordinated CrIII atoms, the three metal atoms forming the points of an equilateral triangle. Each of the six acetate carboxylate groups bridges a Cr–O–Cr fragment. The cluster cation interacts with the nitrate counter-ion and solvent molecules through O—H O hydrogen bonds, forming a three-dimensional hydrogen-bonded network.
R[F 2 > 2(F 2)] = 0.067 wR(F 2) = 0.224 S = 1.38 5836 reflections
359 parameters H-atom parameters constrained ˚ 3 max = 1.77 e A ˚ 3 min = 1.33 e A
Table 1
˚ , ). Hydrogen-bond geometry (A D—H A
D—H
H A
D A
D—H A
O1w—H11 O16 O1w—H12 O12i O2w—H21 O14 O2w—H22 O18ii O3w—H31 O14iii O3w—H32 O5iii O15—H15 O18iv
0.84 0.84 0.84 0.84 0.84 0.84 0.84
1.96 2.06 1.92 1.93 2.28 2.42 1.81
2.769 2.873 2.668 2.725 2.781 3.244 2.624
162 162 147 157 118 165 163
Symmetry codes: (i) x þ 1; y þ 1; z þ 1; x; y þ 32; z 12; (iv) x 1; y þ 32; z þ 12.
(ii)
(6) (5) (6) (6) (5) (6) (6)
x þ 1; y 12; z þ 32;
(iii)
Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XSEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2008).
Related literature For crystal structure reports of [Cr3(C2H3O2)6O(H2O)3]+ salts, see: Anson et al. (1997); Fujihara et al. (1998); Glowiak et al. (1996); Karu et al. (1993); Winpenny et al. (2005).
We thank the University of Malaya (JPJ Vote) for supporting this sudy. Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2306).
References
Experimental Crystal data [Cr3(C2H3O2)6O(H2O)3]NO3C2H4O2 Mr = 702.37
m1310
Maah et al.
Monoclinic, P21 =c ˚ a = 11.7034 (1) A ˚ b = 14.5102 (2) A
Anson, C. E., Bourke, J. P., Cannon, R. D., Jayasooriya, U. A., Molinier, M. & Powell, A. K. (1997). Inorg. Chem. 36, 1265–1267. Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Fujihara, T., Aonahata, J., Kumakura, S., Nagasawa, A., Murakami, K. & Ito, T. (1998). Inorg. Chem. 37, 3779–3784. Glowiak, T., Kozlowski, H., Erre, L. S. & Micera, G. (1996). Inorg. Chim. Acta, 248, 99–102. Karu, E., Anson, C. E., Cannon, R. D., Jayasooriya, U. A. & Powell, A. K. (1993). Acta Cryst. C49, 1929–1932. Sheldrick, G. M. (1996). SADABS. University of Go¨ttingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Westrip, S. P. (2008). publCIF. In preparation. Winpenny, R., Smith, A., Parkin, A., Parsons, S. & Messenger, D. (2005). Private communication (deposition No. 278285). CCDC, Cambridge, England.
doi:10.1107/S1600536808029681
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Acta Cryst. (2008). E64, m1310
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