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Preparation, X-ray structure, and spectroscopic characterization of 1,5-Se2S2N4
被引:20
|作者:
Maaninen, A
Laitinen, RS
Chivers, T
Pakkanen, TA
机构:
[1] Univ Oulu, Dept Chem, FIN-90570 Oulu, Finland
[2] Univ Calgary, Dept Chem, Calgary, AB T2N 1N4, Canada
[3] Univ Joensuu, Dept Chem, FIN-80101 Joensuu, Finland
关键词:
D O I:
10.1021/ic990179i
中图分类号:
O61 [无机化学];
学科分类号:
070301 ;
081704 ;
摘要:
The reaction of [(Me3Si)(2)N](2)S with equimolar amounts of SCl2 and SO2Cl2 produces S4N4 in a good yield. The new chalcogen nitride 1,5-Se2S2N4 has been prepared in high yield by two different reactions: (a) from [(Me3Si)(2)N](2)S and SeCl4 and (b) from [(Me3Si)(2)N](2)Se with equimolar amounts of SCl2 and SO2Cl2. 1,5-Se2S2N4 has a cage structure similar to those of S4N4 and Se4N4. The crystal structure is disordered with site occupation factors ca. 50% for selenium in each chalcogen atom position. The 12 eV EI mass spectrum shows Se2SN2+ as the fragment with highest mass. Both the N-14 and Se-77 NMR spectra show a single resonance (-238 and 1418 ppm, respectively). These data rule out the possibility that the crystalline sample is a solid solution of S4N4 and Se4N4 and imply the presence of 1,5-Se2S2N4. This deduction was further verified by Raman spectroscopy and vibrational analysis.
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页码:3450 / 3454
页数:5
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