新型二维七核簇合物[WS_4Cu_6Br_4(Py)_4]的合成及晶体结构  

Synthesis and Crystal Structure of a Novel Two-dimensional Heptanuclear Cluster Compound [ WS_4Cu_6Br_4 ( Py)_4 ]

作　　者：郎建平[1] 郁开北[2] 忻新泉[3] 

机构地区：[1]苏州大学化学系,苏州215006 [2]中国科学院成都分析测试中心,成都610041 [3]南京大学化学系,南京210008

出　　处：《化学学报》1996年第3期276-280,共5页Acta Chimica Sinica

基　　金：江苏省教委自然科学基金资助的课题

摘　　要：标题化合物是通过(NH_4)_2WS_4,CuBr和(n-Bu)_4NBr的低热固相反应,其固相产物的乙腈溶液和吡啶发生取代反应来合成的.此簇合物为四方晶系,空间群I(?)2d,晶胞参数:a=1.4612(2)nm,c=1.5125(3)nm,V=3.2300(3)nm^3,Z=4,μ=126.90cm^(-1),Dc=2.73g/cm^3,F(000)=2479,最终偏差因子R=0.040.X射线单晶衍射法证实由六个Cu原子所组成的稍畸变的八面体,包围着近似正四面体的WS_4核,形成WS_4Cu_6单元,通过-Cu_(eq)-Br-Cu_(eq)-桥,此单元连接其最近的另一个单元,形成一个二维网络结构.The title compound [WS4Cu6Br4(Py)4] were obtained by the reaction of (NH4)2WS4, CuBr and (n - Bu)4NBr in the solidstateand pyridine substitution of the solid state product in acetonitrile. Its red crystal is tetragonal, space group I4 2d with unit cell parameters a =1.4612(2)nm, c = 1.5125(3)nm, V = 3.2300(3)nm3, Z = 4, μ= 126.90cm-1, Dc= 2. 73g/cm3, F (000) =2479, R = 0. 040 for 560 observed reflections. The X - ray analysis confirms that the structure, which possesses acrystallo- graphic 4 symmetry axis running through Br(1), Cu(1), W, Cu(1a), Br(1a)atoms, consists of a tetrahedral WS4 core envelopedby an octahedral array of six copper atoms, forming an WS4Cu6 aggregate. Linked by - Cueq - Br - Cueq - bridges, this aggregate connects with its nearest, neighbours and develops a two- dimentional network.

关 键 词：簇合物 晶体结构 钨 硫 铜 溴 吡啶 

分 类 号：O641.4[理学—物理化学]