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F 3 SiSH and (F 3 Si) 2 S: Conflicting Observations Resolved by Unambiguous Syntheses
Author(s) -
Beckers Helmut,
Bürger Hans
Publication year - 2001
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/1521-3749(200106)627:6<1217::aid-zaac1217>3.0.co;2-b
Subject(s) - chemistry , raman spectroscopy , bond cleavage , medicinal chemistry , stereochemistry , crystallography , physics , organic chemistry , catalysis , optics
The reaction between liquid F 3 SiI and red HgS mainly yields the disilylsulfane (F 3 Si) 2 S and, in smaller amounts, hitherto unknown (F 3 SiS) 2 SiF 2 . These fluorosilylsulfanes have different thermal stabilities. (F 3 Si) 2 S is a versatile precursor for F 3 Si derivatives, and at ambient temperature it is stable, while (F 3 SiS) 2 SiF 2 decomposes rapidly. F 3 SiSH has been obtained, along with F 3 SiBr, by selective cleavage of one of the Si–S bonds in (F 3 Si) 2 S with HBr in the liquid phase and was for the first time unambiguously characterized. Contrary to previous reports, (F 3 Si) 2 O rather than (F 2 SiS) 2 is formed when SiF 4 is passed over SiS 2 at 1298 K in a quartz tube. Raman and infrared spectra of (F 3 Si) 2 S, F 3 SiSH and its deuterated derivative F 3 SiSD have been measured and assigned to vibrational fundamentals. Multinuclear NMR spectra have been recorded.