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Synthesis of Bis(trichloromethyl)tetra‐ and ‐heptasulfane from Titanocene Polysulfide Complexes and Structure of (CCl 3 ) 2 S 7
Author(s) -
Steudel Ralf,
Pridöhl Markus,
Buschmann Jürgen,
Luger Peter
Publication year - 1995
Publication title -
chemische berichte
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 0009-2940
DOI - 10.1002/cber.19951280711
Subject(s) - chemistry , polysulfide , triclinic crystal system , raman spectroscopy , molecule , crystallography , tetra , infrared spectroscopy , homologous series , sulfur , metallocene , stereochemistry , decomposition , crystal structure , medicinal chemistry , polymer chemistry , organic chemistry , physics , electrode , optics , electrolyte , polymerization , polymer
CCl 3 SCl reacts with (C 5 H 5 ) 2 TiS 5 to give the heptasulfane (CCl 3 ) 2 S 7 which forms colorless crystals of m.p. 38°C. An X‐ray structural analysis revealed that the C‐S 7 ‐C chain is helical but the CCl 3 groups are slightly tilted. In the triclinic crystals the molecules are arranged parallel to each other. Decomposition of (CCl 3 ) 2 S 7 provides other members of the homologous series with 4–12 sulfur atoms as shown by HPLC analysis. The reaction of CCl 3 SCl with (C 5 H 4 ‐CH 3 ) 4 Ti 2 S 4 yields colorless crystals of (CCl 3 ) 2 S 4 , demonstrating the usefulness also of dinuclear titanocene polysulfide complexes for the synthesis of organic polysulfanes. Infrared, Raman, and 13 C‐NMR spectra of (CCl 3 ) 2 S 7 and (CCl 3 )S 7 are reported.