single-source precursors for cu and se composite ...copper(i) diselenocarbamate clusters: synthesis,...
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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 Ping-
Kuei 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
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Electronic Supplementary Material (ESI) for Dalton Transactions.This journal is © The Royal Society of Chemistry 2015
7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 ppm
36.048
24.080
1.000
24.067
Figure S1.1H NMR spectra of [Cu8(H){Se2CNnPr2}6](PF6), 2H in CDCl3
2
2.53.03.54.04.55.05.5 ppm3.072
5.300
Figure S2. 2H NMR spectra of [Cu8(D){Se2CNnPr2}6](PF6), 2D in CH2Cl2
3
7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 ppm
1.341
1.365
1.389
2.097
3.014
4.112
4.135
4.159
4.183
5.300
36.749
1.000
23.898
Figure S3. 1H NMR spectra [Cu8(H){Se2CNEt2}6], 3H in CD2Cl2
4
7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 ppm
3.094
5.304
Figure S4. 2H NMR spectra [Cu8(D){Se2CNEt2}6], 3D in CH2Cl2
5
7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 ppm
0.875
0.900
0.924
1.787
1.812
1.837
1.863
1.889
1.920
3.321
3.964
3.991
4.017
7.260
36.604
24.321
1.000
24.196
Figure S5. 1H NMR spectra of [Cu7(H){Se2CNnPr2}6], 4H in CDCl3
7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 ppm
3.339
7.260
6
Figure S6. 2H NMR spectra of [Cu7(D){Se2CNnPr2}6], 4D in CHCl3.
Figure S7. 1H NMR spectra of [Cu7(H){Se2CNEt2}6], 5H in CD2Cl2
-8-6-4-216 14 12 10 8 6 4 2 0 ppm
1.867
3.283
3.740
Figure S8. 2H NMR spectra of [Cu7(D){Se2CNEt2}6], 5D in THF
7
310315320325330335340345350355360365370375380385390395 ppm
374.
930
Figure S9. 77Se NMR spectra of [Cu8(H){Se2CNnPr2}6](PF6), 2H in CHCl3
8
325330335340345350355360365370375380385390395 ppm
364.823
Figure S10. 77Se NMR spectra of [Cu8(H){Se2CNEt2}6]PF6, 3H in CH2Cl2
370380390400410420430440450460470480490500510520530540 ppm
448.617
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).
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Figure S15. ESI-MS spectrum of [Cu7(H){Se2CNnPr2}6]+, 4H, observed an adduct species [Cu7(H){Se2CNnPr2}6(Cu)]+
, [4H + Cu]+.
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Figure S16. ESI-MS spectrum of [Cu7(H){Se2CNEt2}6], 5H, observed an adduct species [Cu7(H){Se2CNEt2}6(Cu)]+
, [5H + Cu]+.
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