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: chenwei@mail.ndhu.edu.tw.

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).

12

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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