Preparation, X-ray Structure, and Spectroscopic Characterization of 1,5-Se(2)S(2)N(4)

The reaction of [(Me(3)Si)(2)N](2)S with equimolar amounts of SCl(2) and SO(2)Cl(2) produces S(4)N(4) in a good yield. The new chalcogen nitride 1,5-Se(2)S(2)N(4) has been prepared in high yield by two different reactions: (a) from [(Me(3)Si)(2)N](2)S and SeCl(4) and (b) from [(Me(3)Si)(2)N](2)Se with equimolar amounts of SCl(2) and SO(2)Cl(2). 1,5-Se(2)S(2)N(4) has a cage structure similar to those of S(4)N(4) and Se(4)N(4). 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 Se(2)SN(2)(+) as the fragment with highest mass. Both the (14)N and (77)Se 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 S(4)N(4) and Se(4)N(4) and imply the presence of 1,5-Se(2)S(2)N(4). This deduction was further verified by Raman spectroscopy and vibrational analysis.