Synthesis and characterization of chiral SFeCoM(CO)8(RCOCp) (M = Mo, W; R = H, CH3, C2H5O) clusters and the crystal structure of SFeCoW(CO)8(CH3COCp)

Abstract

Abstract Several chiral cluster derivatives SFeCoM(CO)8(RCOCp)(M = Mo, W; R = H, CH3, C2H5O) were synthesized by the thermal reaction of SFeCo2(CO)9 with the metal carbonyl anions [M(CO)3(RCOCp)]− without using benzophenone ketyl to initiate the reaction. The clusters were characterized by C/H analysis, IR, 1H NMR, 13C NMR and two-dimensional chemical shift correlated 1H(13C) NMR spectra. The results show that the metal fragment Co(CO)3 in SFeCo2(CO)7 could be exchanged by M(CO)2(RCOCp). The structure of SFeCoW(CO)8(CH3COCp) (3b) was determined by single crystal X-ray diffraction. The crystals of cluster 3b are orthorhombic with space group, Pbca, a = 17.937(3), b = 15.956(4), c = 26.137(7) A , empirical formula C15H7CoFeO9SW, M5 = 661.9 g mol−1, Z = 16, Dc = 2.351 g cm−3, μ = 3.65 mm−1 F(000) = 4992, final R = 0.048, Rw = 0.0503.