The reaction of antitumor active dirhodium(II) tetraacetate, Rh2(AcO)4, with S-methyl-L-cysteine (HSMC) was studied at the pH of mixing (= 4.8) in aqueous media at various temperatures under aerobic conditions. The results from UV-vis spectroscopy and electrospray ionization mass spectrometry (ESI-MS) showed that HSMC initially coordinates via its sulfur atom to the axial positions of the paddlewheel framework of the dirhodium(II) complex, and was confirmed by the crystal structure of [Rh2(AcO)4(HSMC)2]. After some time (48 hours at 25 o C), or at elevated temperature (40 •C), Rh-SMC chelate formation causes breakdown of the paddlewheel structure,
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