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DOI: 10.1039/A701803G (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 2445-2450

Synthesis, characterisation, electrochemistry and reactivity of osmium–palladium carbonyl complexes containing 1,1′-bis(diphenylphosphino)ferrocene (dppf); molecular structures of [Os5PdC(CO)14(µ-dppf)], [OsPd(µ-I)2I2(CO)2( µ-dppf)]2 and [{Os5C(CO)14}2(µ -dppf)]

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Janesse Wing-Sze Hui and Wing-Tak Wong

Abstract

The hexanuclear osmium–palladium carbonyl carbide cluster [Os5PdC(CO)14(µ-dppf)] 1 [dppf = 1,1′-bis(diphenylphosphino)ferrocene] has been synthesized in 56% yield by the reaction of [N(PPh3)2]2[Os5C(CO) 14] with [Pd(dppf)(H2O)2][O3CCF3] 2. When treated with iodine in CH2Cl2 at ambient conditions, compound 1 underwent cluster degradation to give the macrocyclic complex [OsPd(µ-I)2I2(CO)2( µ-dppf)]2 2. Thermolysis of complex 1 in refluxing chloroform gave the dppf bridged dimeric cluster [{Os5C(CO)14}2(µ- dppf)] 3. The structures of 1–3 were characterised by IR, 1H, 31P NMR and mass spectroscopies and X-ray crystallography. Electrochemical investigations revealed that complex 1 underwent a reversible one-electron oxidation at the ferrocene centre followed by a quasi-reversible oxidation of the metal cluster core.

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