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)(CH(3)COCp)

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, H-1 NMR, C-13 NMR and two-dimensional chemical shift correlated H-1(C-13) NMR spectra. The results show that the metal fragment Co(CO)(3) in SFeCo2(CO)(9) could be exchanged by M(CO)(2)(RCOCp). The structure of SFeCoW(CO)(8)(CH(3)COCp) (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) Angstrom, empirical formula C15H7CoFeO9SW,M(r)=661.9 g mol(-1), Z=16, D-c=2.351 g cm(-3), mu=8.065 mm(-1), F(000)=4992, final R=0.048, Rw=0.0503.