SYNTHESIS AND MOLECULAR-STRUCTURE OF DISULFANE

The synthesis and structure of disulfane, H2S2, has been obtained by the cracking distillation of raw sulfane mixtures in a rotary evaporator, thus substituting the classical cracking column for the rotating flask of the evaporator. Pure, gaseous dideuterodisulfane could be generated by the solvolysis of bis(methyldiphenylsilyl)disulfane, (MePh2Si)2S2, with D2O in the presence of trichloroacetic acid as stabilizing agent. Partially deuterated disulfane has been prepared by H,D exchange between pure H2S2 and DCl. For the first time the molecular structure of HSSH has been determined based solely on microwave spectroscopy with the following parameters: r(SS) = 2.0564 angstrom, r(SH) = 1.342 angstrom, dihedral angle gamma = 90.34-degrees, and < (SSH) = 97.88-degrees.