One step synthesis of heteronuclear carbonyl clusters and the crystal structure analysis of Pd3(SC6H4OH)3(PPh3) 3(OH)2Cl

Acta Chimica Sinica(1996)

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摘要
According to the principle of fragment combination, the metal clusters of Pd3 (SC6H4OH)3(PPh3) 3(OH)2Cl(1), Fe2S2(CO)5Pd(PPh3)S(2), and Fe2S2(CO)5Pt(PPh3)3(3) which with carbonyl or without carbonyl groups are prepared under CO atmosphere by one step method using simple elements, metal salts and ligands as starting materials through controlling the reaction temperature, pressure, time and the amount of ligands. These clusters are analysed by elements of C/H and metal, and characterized with IR, 1H NMR, EDS. The single crystal of cluster (1) is also analysed by X-ray diffraction. The results showed that it belongs to monoclinic system, P21/n space group, the cell parameters are a = 1.4629(3)nm, b = 1.9263(3)nm, c = 2.4908(7)nm, �� = 94.53(2)��, V = 6.9974nm3, Z = 4, Dc = 1.47g��cm-3, R = 0.053, Rw = 0.065.
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