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290ChemInform Abstract The diphosphine clusters (Ia) react with trimethylamine N-oxide in acetonitrile solution to give the acetonitrile derivatives (Ib). The acetonitrile ligand of (Ib) is readily displaced by other two-electron donor ligands to yield the derivatives (Ic), (Id). (Ib) also react with HCl or thiols to produce the chloride-or thiolate-bridged clusters (II), whereas the treatment of (Ib) (R1: Ph) with H2Oor MeOH leads to the only product Os3H(CO)8(Ph2PCH2PPhC6H4) isolated. Thermolysis of the ethylene derivative (Id) (L: C2H4) or of the corresponding decacarbonyl (Ia) gives the cyclometallated product (III). The µ-hydroxo derivative (V) (space group P21/n, Z=4), prepared from (IV) as shown, has a different structure from (IIa) as confirmed by X-ray analysis. The molecular and crystal structure of the cyclometallated cluster (III) ( P21/n, Z=4) is also determined.

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The diphosphine clusters (Ia) react with trimethylamine N‐oxide in acetonitrile solution to give the acetonitrile derivatives (Ib).