SULFUR COMPOUNDS .187. SYNTHESIS OF BIS(TRICHLOROMETHYL)TETRASULFANE AND BIS(TRICHLOROMETHYL) HEPTASULFANE FROM TITANOCENE POLYSULFIDE COMPLEXES AND STRUCTURE OF (CCL3)(2)S-7
R. Steudel et al., SULFUR COMPOUNDS .187. SYNTHESIS OF BIS(TRICHLOROMETHYL)TETRASULFANE AND BIS(TRICHLOROMETHYL) HEPTASULFANE FROM TITANOCENE POLYSULFIDE COMPLEXES AND STRUCTURE OF (CCL3)(2)S-7, Chemische Berichte, 128(7), 1995, pp. 725-728
CCl3SCl reacts with (C5H5)(2)TiS5 to give the heptasulfane (CCl3)(2)S-
7 which forms colorless crystals of m.p. 38 degrees C. An Xray structu
ral analysis revealed that the C-S-7-C chain is helical but the CCl3 g
roups are slightly tilted. In the triclinic crystals the molecules are
arranged parallel to each other. Decomposition of (CCl3)(2)S-7 provid
es other members of the homologous series with 4-12 sulfur atoms as sh
own by HPLC analysis. The reaction of CCl3SCl with (C5H4-CH3)(4)Ti2S4
yields colorless crystals of (CCl3)(2)S-4, demonstrating the usefulnes
s also of dinuclear titanocene polysulfide complexes for the synthesis
of organic polysulfanes. Infrared, Raman, and C-13-NMR spectra of (CC
l3)(2)S-4 and (CCl3)S-7 are reported.