Electronic Supplementary Material (ESI) for Dalton Transactions. This journal is © The Royal Society of Chemistry 2015
Copper(I) Diselenocarbamate Clusters: Synthesis, Structures and Single-Source Precursors for Cu and Se Composite Materials Rajendra S. Dhayal,a,b Jian-Hong Liao,a Hsing-Nan Hou,a Ria Ervilita,a PingKuei Liao,a and C. W. Liua* a
Department of Chemistry, National Dong Hwa University, Hualien, Taiwan 97401, R. O. C.
E-mail:
[email protected]. b
School of Chemistry and Biochemistry, Thapar University, Patiala 147004, Punjab, India
1
5.5
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
36.048
6.0
24.080
6.5
1.000
7.0
24.067
7.5
Figure S1.1H NMR spectra of [Cu8(H){Se2CNnPr2}6](PF6), 2H in CDCl3
2
ppm
3.072
5.300 5.5
5.0
4.5
4.0
3.5
3.0
2.5
ppm
Figure S2. 2H NMR spectra of [Cu8(D){Se2CNnPr2}6](PF6), 2D in CH2Cl2
3
5.0
4.5
4.0
3.014 3.0
1.000
3.5
2.5
1.389 1.365 1.341
5.5
2.0
1.5
1.0
ppm
36.749
6.0
2.097
6.5
23.898
7.0
4.183 4.159 4.135 4.112
5.300 7.5
Figure S3. 1H NMR spectra [Cu8(H){Se2CNEt2}6], 3H in CD2Cl2
4
7.0
6.5
6.0
5.5
3.094
5.304
7.5
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
ppm
Figure S4. 2H NMR spectra [Cu8(D){Se2CNEt2}6], 3D in CH2Cl2
5
5.0
4.5
4.0
3.5
2.5
2.0
0.924 0.900 0.875
1.920 1.889 1.863 1.837 1.812 1.787 3.0
1.5
1.0
0.5
ppm
36.604
5.5
24.321
6.0
1.000
6.5
24.196
7.0
3.321
4.017 3.991 3.964
7.260 7.5
7.5
3.339
7.260
Figure S5. 1H NMR spectra of [Cu7(H){Se2CNnPr2}6], 4H in CDCl3
7.0
6.5
6.0
5.5
5.0
4.5
4.0
6
3.5
3.0
2.5
2.0
1.5
1.0
0.5
ppm
Figure S6. 2H NMR spectra of [Cu7(D){Se2CNnPr2}6], 4D in CHCl3.
14
12
10
8
6
1.867
16
3.740 3.283
Figure S7. 1H NMR spectra of [Cu7(H){Se2CNEt2}6], 5H in CD2Cl2
4
2
0
-2
-4
-6
-8
Figure S8. 2H NMR spectra of [Cu7(D){Se2CNEt2}6], 5D in THF
7
ppm
374.930 395
390
385
380
375
370
365
360
355
350
345
340
335
330
325
320
315
310
ppm
Figure S9. 77Se NMR spectra of [Cu8(H){Se2CNnPr2}6](PF6), 2H in CHCl3
8
364.823 395
390
385
380
375
370
365
360
355
350
345
340
335
330
325
ppm
448.617
Figure S10. 77Se NMR spectra of [Cu8(H){Se2CNEt2}6]PF6, 3H in CH2Cl2
540
530
520
510
500
490
480
470
460
450
440
430
420
410
400
390
380
370
ppm
Figure S11.77Se NMR spectra [Cu7(H){Se2CNnPr2}6], 4H in CHCl3
9
Figure S12. 77Se NMR spectra of [Cu7(H){Se2CNEt2}6], 5H in CH2Cl2
10
Figure S13. ESI-MS spectrum of [Cu8(H){Se2CNnPr2}6]+, 2H. The inset shows experimental (a) and theoretical one (b).
11
Figure S14. ESI-MS spectrum of [Cu8(H){Se2CNEt2}6]+, 3H. The inset shows experimental (a) and theoretical one (b).
12
Figure S15. ESI-MS spectrum of [Cu7(H){Se2CNnPr2}6]+, 4H, observed an adduct species [Cu7(H){Se2CNnPr2}6(Cu)]+, [4H + Cu]+.
13
Figure S16. ESI-MS spectrum of [Cu7(H){Se2CNEt2}6], 5H, observed an adduct species [Cu7(H){Se2CNEt2}6(Cu)]+, [5H + Cu]+.
14
