Synthesis and characterization of Na[cis-mer-Mo(C6F5)(CO)2{P(OMe)3}3]

Abstract

The complex [Mo(C₆F₅)(CO)₂(η-C₇H₇)] can be reduced either chemically or electrochemically by one electron. Electrochemical studies suggest that the reduction is followed by a rapid but reversible structural change. The orange intermediate reduction product has not yet been isolated in pure form. Chemical reduction with sodium amalgam in tetrahydrofuran in the presence of trimethyl phosphite initially forms this orange product, but precipitation with hexane yields the pale yellow zerovalent σ-aryl molybdenum complex Na[cis-mer-Mo(C₆F₅)(CO)₂{P(OMe)₃}₃], in which the cycloheptatrienyl ligand has been displaced by three trimethyl phosphite groups. This complex has been fully characterized by IR, ¹H and ³¹P NMR spectroscopy and X-ray crystallography.