Abstract
Phenyl-dithiastibolane and its d 5-phenyl analogue have been synthesized from PhSbCl 2 or d 5-PhSbCl 2 and ethanedithiol. CD 2Cl 2 solutions contain isolated molecules with half-chair conformation ( 1H NMR: CH 2-CH 2 torsion angle 48°). In the crystal (structure determination, R = 0.046) these molecules are midway between envelope and half-chair conformation (43°; Sb-S 243 and 246 pm), and form helical chains by intermolecular connection (SB⋯S 334 pm). Both types of Sb-S distances correlate to vibrational bands (ν(Sb-S) 310–340, ν(Sb⋯S) 224 cm −1).
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