Hiroyuki Suzuki, N. Tokitoh, R. Okazaki
Oct 16, 1998
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Journal
Journal of the American Chemical Society
Abstract
Diaryltetrathiasilolanes 2a,b, bearing bulky aryl groups such as 2,4,6-tris[bis(trimethylsilyl)methyl]phenyl (Tbt), mesityl (Mes), and 2,4,6-triisopropylphenyl (Tip), were obtained by thermal reaction of dihydrosilane 3a with elemental sulfur, reaction of highly hindered disilene 4 with sulfur, or reduction of dibromosilane 6 followed by addition of sulfur. The molecular structure of 2a was determined by X-ray crystallographic analysis. Desulfurization of 2a at −78 °C afforded a silicon−sulfur double bond compound (silanethione 7a). Although the formation of 7a was confirmed by various trapping reactions, 7a dimerized at room temperature to give 1,3,2,4-dithiadisiletane 8, whose molecular structure was determined by X-ray crystallographic analysis. Desulfurization of 2b afforded the first stable silanethione, Tbt(Tip)SiS (7b), as yellow crystals, which were thermally stable under inert gas up to its melting point (185−189 °C) and showed λmax (n→π*) at 396 nm and νSiS (Raman) at 724 cm-1. The chemical shif...