Preparation, crystal structure, and spectroscopic characterization of [(Se(2)SN(2)Cl](2).
The reaction of [(Me(3)Si)(2)N](2)S with an equimolar amount of SeCl(4) in dioxane at 50 degrees C affords [(Se(2)SN(2))Cl](2) (1) in excellent yield. Crystals of 1 are orthorhombic, space group Pbca, with a = 8.5721(7) A, b = 7.8336(6) A, c = 15.228(1) A, and Z = 8. The crystal structure contains two planar Se(2)SN(2)(*)(+) rings which are linked by intermolecular Se.Se interactions [d(Se-Se) = 3.0690(7) A]. The EI mass spectrum shows Se(2)SN(2)(*)(+) as the fragment of highest mass. Both the (14)N and (77)Se NMR spectra show a single resonance (-52 and 1394 ppm, respectively). The solid [(Se(2)SN(2))Cl](2) gives a strong ESR signal indicating the presence of a Se(2)SN(2)(*)(+) radical. The Raman spectrum was assigned through normal coordinate treatment involving a general valence force field. The vibrational analysis yielded a good agreement between the observed and calculated wavenumbers.
Maaninen
A
A
Departments of Chemistry, P.O. Box 3000, 90014 University of Oulu, Finland.
Konu
J
J
Laitinen
R S
RS
Chivers
T
T
Schatte
G
G
Pietikäinen
J
J
Ahlgrén
M
M