Preparation and crystal structure of hetero-metal clusters [η5-C5H4C(O)CH2CH2C(O)OCH3]FeCoM(μ3-S)(CO)8 (M = Mo or W)

The hetero-metal clusters [eta (5)-C5H4C(O)CH2CH2C(O)OCH3]FeCoM(mu (3)-S)(CO)(8) (M=Mo 1, M=W 2) were prepared by thermal reactions of FeCo2(CO)(9)(mu (3)-S) with metal exchange reagent [eta (5)-C5H4C(O)CH2CH2C(O)OCH3]M(CO)(3)Na (M = Mo or W) in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (mu (3)-S)CoFeMo(CO)(8)[eta (5)-C5H4C(NR)Me] [R = NHC6H3-2,4-(NO2)(2)] 3. All the compounds were characterized by elemental analyses, IR and NUR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, M, = 646.05, triclinic, space group P (1) over bar, a = 8.148(2), b = 10.685(3), c = 13.410(4) Angstrom, alpha = 100.077(5), beta =102.452(5), gamma= 91.108(6)degrees, V= 1120.4(5) Angstrom (3), Z = 2, D-c = 1.915 g/cm(3), F(000) = 636, mu = 2.071 mm(-1), the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I>2 sigma (I)).