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直接法合成异核羰基金属簇合物及Pd3(SC6H4OH)3(PPh33(OH)2Cl的晶体结构分析

One Step Synthesis of Heteronuclear carbonyl Clusters and the Crystal Structure Analysis of Pd3(SC6H4OH)3(PPh33(OH)2Cl

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【作者】 赵转云刘省明马竟涛殷元骐黄梁仁

【Author】 ZHAO Zhuan - Yun LIU Xing - Ming MA Jing - Tao YIN Yuan - Qi( Lanzhou Institute of Chemical Physics, The Chinese Academy of Sciences, Lanzhou, 730000)HUANG Liang - Ren( Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, 350002)

【机构】 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 兰州730000兰州730000福建350002

【摘要】 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(PPh33(OH)2Cl(1),Fe2S2(CO)5Pd(PPh33(2),Fe2S2(CO)-5Pt(PPh33(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.

【Abstract】 According to the principle of fragment combination, the metal clusters of (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 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, β = 94.53(2)°, V = 6.9974nm3, Z = 4,Dc=1.47g·cm-3, R= 0.053, Rw = 0.065.

【关键词】 金属原子簇一步法单晶结构
【基金】 中国科学院上海有机化学研究所所金属有机开放实验室资助项目
  • 【文献出处】 化学学报 ,Acta Chimica Sinica , 编辑部邮箱 ,1996年05期
  • 【分类号】O621.13
  • 【下载频次】61
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