posted on 2001-06-07, 00:00authored byArto Maaninen, Jari Konu, Risto S. Laitinen, Tristram Chivers, Gabriele Schatte, Jarkko Pietikäinen, Markku Ahlgrén
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.