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Reactions of the tetranuclear mixed-metal clusters ReM3(CO)13(µ3-thpymS) (1, M = Os; 2, M = Ru; thpymSH = tetrahydropyrimidine-2-thiol) with PPh3 are examined. At room temperature reaction between 1 and PPh3 in the presence Me3NO leads to the formation of mono- and bis-phosphine substituted clusters ReOs3(CO)12(PPh3)(µ3-thpymS) (3) and ReOs3(CO)11(PPh3)2(µ3-thpymS) (4). Cluster 3 also reacts with PPh3 under similar conditions to give 4. In contrast, a similar reaction between 2 and PPh3 furnishes only the mono-phosphine substituted clusters ReRu3(CO)12(PPh3)(µ3-thpymS) (3). All the new clusters have been characterized by analytical and spectroscopic data together with single crystal X-ray diffraction for 1, 3 and 5.

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