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Four new optically active organotin(IV) O,O'-di-(−)-menthyldithiophosphates: Me 3 SnS 2 P(OMen) 2 1, Ph 3 SnS 2 P(OMen) 2 2, Me 2 Sn[S 2 P(OMen) 2 ] 2 3 and Ph 2 Sn[S 2 P(OMen) 2 ] 2 4 (Men = Menthyl) have been prepared in ethanol from sodium O,O'-(−)-dimenthyldithiophosphate and the corresponding tri-or diorganotin(IV) chlorides. All the compounds display optical activity and were characterized by elemental analyses, IR, EM FAB + , and multinuclear NMR, ( 1 H, 13 C, 19 P 119 Sn). In addition, the molecular structures of 3 and 4 were determined by X-ray single crystal analyses. Both complexes consist of discrete molecules, where tin is bonded to two carbon atoms and the four sulfur atoms of two anisobidentate dithiophosphate ligands. The environment around the central tin atom exists in skew-trapezoidal bipyramidal geometry.