“…In particular, in an earlier study it was shown that the reaction of [PtMe 2 (2,2′-bipyridine)], 1, with diphenyl disulfide occurred according to Scheme 1, with initial formation of a diplatinum (III) complex [Pt 2 (SPh) 2 Me 2 (bipy) 2 ], 2a, which finally gave the dithiolatoplatinum(IV) complex [Pt(SPh) 2 Me 2 (bipy)], 3a [9]. This article shows that the disulfides R 2 S 2 with R = CH 2 CH 2 CO 2 H or C 6 H 3 -4-NO 2 -3-CO 2 H can give the first examples of thiolate-carboxylate complexes of platinum(IV) [12,13].The reaction of complex 1 [9,14] with the disulfide R 2 S 2 , R=CH 2-CH 2 CO 2 H, in either acetone or dimethylsulfoxide occurred according to Scheme 2 to give the 3-thiolatopropionate complex [PtMe 2 (SCH 2-CH 2 CO 2 )(bipy)], 4, which was isolated as a red-brown solid. Complex 4 was characterized in the 1 H NMR by the presence of two methylplatinum resonances at δ = 0.43 [s, 3 H, 2 J(PtH) = 73 Hz, MePt trans to O] and 1.56 [s, 3 H, 2 J(PtH) = 69 Hz, MePt trans to N] and by four overlapping multiplet resonances, integrating to a total of four protons, for the CH 2 CH 2 protons in the range δ = 2.3-2.6.…”