新颖四核W—Cu—S簇合物[（η^5—C5Me5）WS3Cu3Br（Py）3（dppm）]（PF6）的合成和晶体结构  

Synthesis and Crystal Structure of a Novel Tetranuclear Cluster [(η5-C5Me5)WS3Cu3Br(Py)3 (dppm)] (PF6)

作　　者：陈金香[1] 魏振宏[1] 李宝龙[1] 徐庆锋[1] 刘泉[1] 郎建平[1] 

机构地区：[1]苏州大学化学化工学院,苏州215006

出　　处：《无机化学学报》2003年第5期527-530,共4页Chinese Journal of Inorganic Chemistry

基　　金：江苏省教育厅自然科学研究基金项目(No.02KJB150001);南京大学配位化学国家重点实验室开放基金资助。

摘　　要：In the presence of NH4PF6, reaction of [(η5 C5Me5)WS3Cu3Br(dppm)] with excess pyridine afforded red prismatic crystals, [(η5 C5Me5)WS3Cu3Br(Py)3(dppm)](PF6) (1). It was characterized by elemental analysis, IR, UV vis and1H NMR spectroscopy and X ray diffraction. 1 crystallizes in an orthorhombic system with space group Pna21 and unit cell parameters a=2.1124(4)nm, b=1.8944(4)nm, c=1.3338(2)nm, V=5.3375(19)nm3, Z=4, Dc=1.807g·cm-3, Mr=1452.42, F(000)=2864, μ=4.342mm-1, R1=0.0487, wR2=0.1027. The structure of the cluster cation contains an incomplete cubane like WS3Cu3 core where Cu(1) and Cu(2) atoms are bridged by a dppm ligand. Each of the three Cu atoms adopts a distorted tetrahedral coordination geometry. The W Cu(1), W Cu(2) and W Cu(3) distances are 0.27698(17)nm, 0.2772(17)nm, and 0.27065(9)nm, respectively. CCDC: 199845.In the presence of NH4PF6, reaction of [(η5 C5Me5)WS3Cu3Br(dppm)] with excess pyridine afforded red prismatic crystals, [(η5 C5Me5)WS3Cu3Br(Py)3(dppm)](PF6) (1). It was characterized by elemental analysis, IR, UV vis and1H NMR spectroscopy and X ray diffraction. 1 crystallizes in an orthorhombic system with space group Pna21 and unit cell parameters a=2.1124(4)nm, b=1.8944(4)nm, c=1.3338(2)nm, V=5.3375(19)nm3, Z=4, Dc=1.807g·cm-3, Mr=1452.42, F(000)=2864, μ=4.342mm-1, R1=0.0487, wR2=0.1027. The structure of the cluster cation contains an incomplete cubane like WS3Cu3 core where Cu(1) and Cu(2) atoms are bridged by a dppm ligand. Each of the three Cu atoms adopts a distorted tetrahedral coordination geometry. The W Cu(1), W Cu(2) and W Cu(3) distances are 0.27698(17)nm, 0.2772(17)nm, and 0.27065(9)nm, respectively. CCDC: 199845.

关 键 词：钨簇合物 铜簇合物 硫簇合物 晶体结构 光谱 四硫代金属酸盐 

分 类 号：O614.4[理学—无机化学]