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化学学报
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化学学报 ›› 1996, Vol. 54 ›› Issue (5): 440-446. 上一篇    下一篇

研究论文

直接法合成异核羰基金属族合物及Pd3(SC6H4OH)3(PPh3)3(OH)2Cl的晶体结构分析

赵转云;刘省明;马竟涛;殷元骐;黄梁仁   

  1. 中国科学院兰州化学物理研究所;中国科学院福建物质结构研究所
  • 发布日期:1996-05-15

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

ZHAO ZHUANYUN;LIU SHENGMIN;MA JINGTAO;YIN YUANQI;HUANG LIANGREN   

  • Published:1996-05-15

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本文根据分子碎片结合原理, 用直接法由简单的单质元素, 金属盐类及配体, 通过控制反应温度、压力, 时间及配体用量在CO气氛下一步合成含羰基和不含羰基的簇合物: Pd3(SC6H4OH)3(PPh3)3(OH)2Cl(1),Fe2S2(CO)5Pd(PPh3)3(2), Fe2S2(CO)5Pt(PPh3)3(3)。对它们进行了IR, NMR,EDS, 元素分析, 金属分析和化合物1的X光单晶衍射结构分析。化合物1属单斜晶系, 离子型, P21/n空间群, 晶胞参数a=1.4629(3)nm, b=1.9263(3)nm,c=2.4908(7)nm, β=94.53(2)°, Z=4, R=0.053。

关键词: 红外分光光度法, 元素分析, 晶体结构, 铁络合物, 羰基络合物, 苯硫酚 P, 硫化物, 钯化合物, 三苯基膦 P

According to the principle of fragment combination, the metal clusters of Pd3(SC6H4OH)3(PPh3)3(OH)2Cl(1), Fe2S2(CO)5Pd(PPh3)3(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 analyzed by elements of C/H and metal, and characterized with IR, ^1H NMR, EDS. The single crystal of cluster(1) is also analyzed 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, β=94.53(2)°, V=6.9974nm^3, Z=4, Dc=1.47g.cm^-^3, R=0.053, Rw=0.065.

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, CRYSTAL STRUCTURE, IRON COMPLEX, CARBONYL COMPLEX, BENZENETHIOL P, SULFIDE, PALLADIUM COMPOUNDS, TRIPHENYLPHOSPHINE P

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