The reaction of NaCo(CO)4-x(PR3)x (x = 0,1) with Au(PR3)Cl was examined in THF. The products were characterized by single crystal X-ray analysis and/or XPS spectroscopy. When the THF solution of NaCo(CO)4-x(PR3)x which was in situ prepared by the reduction of the corresponding cobalt carbonyl dimer with Na amalgam was filtered, the main product was (R3P)Au-Co(CO)4 and (R3P)Au-Co(CO)4-x (PR3)x (x=1,2); phosphine migration from the Au to the Co site was observed for bulky phosphines during the recrystallization process. When the THF solution of NaCo(CO)4-x(PR3)x was not filtered, the main product had the composition of M[Co(CO)3(PR3)]2. The element M was clearly determined to be Hg by XPS spectroscopy. The reaction of NaMn(CO)5 with Au(PR3)Cl, however, afforded R3PAu-Mn(CO)5. The bonding parameters such as Au-M and Hg-Co bond-lengths were interpreted in terms of the electronic nature of the R group of the monodentate PR3 ligand.
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