Treatment of dithiirane 1-oxides 9 with (Ph 3 P) 2 Pt(η 2 -CH 2 = CH 2 ) (3) yielded the corresponding four-membered (sulfenato−thiolato)Pt II complexes 7 in high yields. The structures of 7 were determined by 31 P NMR spectroscopy and, for 7e, X-ray crystallography. Treatment of dithiirane 8 with

3,3-Disubstituted dithiirane 1-oxides were efficiently reduced with Lawesson's reagent (LR) to give the corresponding dithiiranes. X-ray diffraction analysis of 3,3-di(1-adamantyl)dithiirane is reported. Reaction of (34)S-labeled 3,3-di(1-adamantyl)dithiirane 1-oxide with LR produced the corresponding dithiirane in which the (34)S atoms were retained quantitatively.

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