Synthesis, characterization and crystal structure analysis of tetrahedral hetero-metal carbonyl clusters

Three new tetrahedral hetero-metal carbonyl clusters were synthesized by refluxing a solution of precursor PhCCo(3)(CO)(9) with complexes NaMo(CO)(3)(RCp)(R = HCO, CH3CO, C2H5 OCO) in THF using metal exchange reaction. Compared with metal exchange reagent NaMo-(CO)(3)Cp, the results exhibited that electron - withdrawing group C = O on cyclopentadienyl decrease exchange activity of metal exchange reagent NaMo(CO)(3)(RCp) and conversion degree to product was accelerated thermally. The results further showed the generality of this kind of metal exchange reaction. The clusters were characterized by C/H analysis, IR and H-1 NMR spectra and X-ray structure determination of cluster PhCCo(2)Mo(CO)(8)(C2H5 OCOCp). This cluster is monoclinic space group P2(1)/c with a = 1.1356(2)nm, b = 1.4030(2)nm, c = 1.6076(3)nm, beta = 107.19(1)degrees, Z = 4, D-c = 1.80g/cm(3), R = 0.048 and R(w) = 0.057.