Preparation, Crystal Structure, and Spectroscopic Characterization of [(Se<sub>2</sub>SN<sub>2</sub>)Cl]<sub>2</sub>
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The reaction of [(Me3Si)2N]2S with an equimolar amount of SeCl4 in dioxane at 50 °C affords [(Se2SN2)Cl]2 (1) in excellent yield. Crystals of 1 are orthorhombic, space group Pbca, with a = 8.5721(7) Å, b = 7.8336(6) Å, c = 15.228(1) Å, and Z = 8. The crystal structure contains two planar Se2SN2•+ rings which are linked by intermolecular Se···Se interactions [d(Se−Se) = 3.0690(7) Å]. The EI mass spectrum shows Se2SN2•+ as the fragment of highest mass. Both the 14N and 77Se NMR spectra show a single resonance (−52 and 1394 ppm, respectively). The solid [(Se2SN2)Cl]2 gives a strong ESR signal indicating the presence of a Se2SN2•+ 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.
