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.
Maaninen
Arto
A
Departments of Chemistry, University of Oulu, Linnanmaa, 90570 Oulu, Finland, University of Calgary, 2500 University Drive N.W., Calgary, Alberta, Canada T2N 1N4, and University of Joensuu, P.O. Box 111, 80101 Joensuu, Finland.
Laitinen
Risto S.
RS
Chivers
Tristram
T
Pakkanen
Tapani A.
TA