$Os_3(CO)_7(μ-Ph_2PCH_2PPh_2)$ $(μ_3-η^2:η^2:η^2-C_{60})$ (1) has been prepared by decarbonylation of $Os_3(CO)_9 $(μ_3-η^2:η^2:η^2-C_{60})$ with $Me_3NO$ followed by the substitution of dppm (bisdiphenylphosphinomethane) ligand. The structure of 1 has determined by single crystal X-ray diffraction study. Reaction of 1 with $Re_3(μ-H)_3(CO)_{11}(CH_3CN)$ in refluxing chlorobenzene affords ${Os_3(CO)_7(μ-Ph_2PCH_2PPh_2)}$ ${Re_3(μ-H)_3(CO)9}$ $(μ_3-η^2:η^2:η^2-C_{60})$ (2). Compound 2 has been characterized by NMR and Mass spectroscopy. Cyclic voltammetry study of 1 reveals same half-wave potentials as $Os_3(PMe_3)_2(CO)_7$ $(μ_3-η^2:η^2:η^2-C_{60})$. Cyclic voltammetry study of 2 reveals all reduction waves of compound 1 and $Re_3(μ-H)_3(CO)_9(μ_3- η^2: η^2: η^2-C_{60})$, but the reduction potentials of 2 further shifted to more negative relative to compound 1 and $Re_3(μ-H)_3(CO)_9(μ_3-η^2: η^2: η^2-C_{60})$.
