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化学学报
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化学学报 ›› 2002, Vol. 60 ›› Issue (11): 1993-1998. 上一篇    下一篇

研究论文

闭式十二顶双镍十硼烷簇合物[(μ-Cl)(Ph_2PC_6H_4)_2Ni_2B_(10)H_6Cl(PPh_3)]的合成与结构

窦建民;胡春华;姚海军;李越生;金若水;郑培菊   

  1. 复旦大学分析测试中心.上海(200433);复旦大学化学系.上海(200433);复旦 大学材料系.上海(200433)
  • 发布日期:2002-11-15

Synthesis and Crystal Structure of closo Twelve-vertex Cluster [(μ- Cl)(Ph_2PC_6H_4)_2Ni_2B_(10)H_6Cl(PPh_3)]

Dou Jianmin;Hu Chunhua;Yao Haijun;Li Yuesheng;Jin Ruoshui;Zheng Peiju   

  1. Research Center of Analysis and Measurement Fudan University. Shanghai(200433);Department of Chemistry Fudan University.Shanghai (200433);Department of Material Science, Fudan University.Shanghai (200433)
  • Published:2002-11-15

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研究了[NiX_2(PPh_3)_2](X=F, Cl, SCN)在二氯甲烷中与B_(10)H_(10)~(2-) 的反应，对形成的产物[(μ-Cl)(Ph_2PC_6H_4)_2-Ni_2B_(10)H_6Cl(PPh_3)]·0. 25CH_2Cl_2 (1)通过元素分析、红外光谱、飞行时间二次离子质谱等进行了表征， 并通过单晶X射线衍射测定了簇合物的结构。1的晶体学数据：单斜晶系，空间群 P2_1/c,a = 1.1703(2)nm, b = 2.1082(4) nm, c = 2.2068 (8) nm, β = 99.98 (2) °, V = 5.3622(2)nm~3, Z = 4, F(000) = 2274, D_(calcd)=1.373g/cm~3. R_1 = 0.0358, wR_2 = 0.0807. 1为闭式十二项双镍十硼烷簇合物，具有两个邻 位环化的Ni-P-C-C-B五元环，镍-镍之间还存在氯桥。结构分析表明：邻位环化增 强了镍与硼之间的成键作用。

关键词: 镍化合物, 硼烷 P, 簇状化合物, 构型, 元素分析, 飞行时间质谱法, 晶体结构

The reactions of [NiX_2(PPh_3)_2] (X = F, Cl, SCN) with B_(10)H_(10) ~(2-) in CH_2Cl_2 were investigated and the cluster [(μ-Cl) (Ph_2PC_6H_4)_2Ni_2B_(10)H_6Cl(PPh_3)]·0.25CH_2Cl_2 (1) was characterized by elemental analysis, IR, time-of-flight secondary ion mass spectrum and single crystal diffraction analysis. Crystal data for 1: triclinic crystal system, space group P2_1/c with cell dimensions, a = 1.1703(2)nm, b = 2.1082(4) nm, c = 2.2068(8)nm β=99. 82(2) °, V=5.3622(2)nm~3, Z = 4, F(000) = 2274, D_(calcd) = 1.373 g/cm~3. R_1=0.0358, wR_2 = 0.0807. The cluster possesses closo twelve- vertex configuration and has two ortho-cycloboronated Ni-P-C-C-B five- membered rings. There is a Cl-bridge between two Ni atoms. The structure analysis shows that the cyclization can strengthen the nickel-to-boron bonding.

Key words: NICKEL COMPOUNDS, BORANE P, CLUSTER COMPOUND, CONFIGURATION, ELEMENTAL ANALYSIS, TIME-OFF FLIGHT MASS SPECTROMETRY, CRYSTAL STRUCTURE

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