Preparation and Crystal Structure of Hetero-metal Clusters [h5-C5H4C(O)CH2CH2C(O)OCH3]FeCoM(m3-S)(CO)8 (M = Mo or W) |
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| Authors: | ZHANG Yu-Hua YUAN Jian-Chao ZHANG Wei-Qiang YIN Yuan-Qi ZHOU Zhong-yuan Albert SCCHAN |
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| Institution: | 1. State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences,
2. Department of Applied Biology Chemical Technology, The Hong Kong Polytechnic University, |
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| Abstract: | The hetero-metal clusters h5-C5H4C(O)CH2CH2C(O)OCH3]FeCoM(m3-S)(CO)8 (M = Mo 1, M = W 2) were prepared by thermal reactions of FeCo2(CO)9(m3-S) with metal exchange reagent h5-C5H4C(O)CH2CH2C(O)OCH3]M(CO)3Na (M = Mo or W) in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (m3-S)CoFeMo(CO)8h5-C5H4C(NR)Me] R = NHC6H3-2,4-(NO2)2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P_1, a = 8.148(2), b = 10.685(3), c = 13.410(4) ?, a = 100.077(5), b = 102.452(5), g = 91.108(6)°, V = 1120.4(5) ?3, Z = 2, Dc = 1.915 g/cm3, F(000) = 636, m = 2.071 mm-1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2s(I)). |
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