Cu_2I_2(PPh_3)_3·DMF的合成和晶体结构  

Synthesis and Crystal Structure of Dinuclear Copper(I)\= Cu2I2(PPh3)3DMF

作　　者：梁玉仓[1] 卢绍芳[1] 吴锵金[1] 黄小荥[1] 黄建全[1] 

机构地区：[1]中国科学院福建物质结构研究所,结构化学国家重点实验室

出　　处：《Chinese Journal of Structural Chemistry》1999年第3期169-174,共6页结构化学（英文）

基　　金：国家自然科学基金;福建省自然科学基金;结构化学国家重点实验室资助

摘　　要：Ｃｕ２Ｉ２（ＰＰｈ３）３·ＤＭＦ（Ｐｈ＝Ｃ６Ｈ５，ＤＭＦ＝ＨＣＯＮ（ＣＨ３）２）是通过Ｗ２Ｓ４〔Ｓ２ＣＮ－（ＣＨ２ＣＨ２ＯＨ）２〕２，ＰＰｈ３和ＣｕＩ在ＣＨ２Ｃｌ２和ＤＭＦ为溶剂，在室温条件下合成的晶体产物。其空间群为Ｐ２１／ｃ，晶胞参数：Ｃ５７Ｈ５２Ｃｕ２Ｉ２ＮＯＰ３，ａ＝１５．８６３（５），ｂ＝１９．６１９（７），ｃ＝１８．２３２（４），β＝１０９．５３（２）°，Ｖ＝５３４８（３）３，Ｚ＝４，Ｍｒ＝１２４０．８７，Ｄｃ＝１．５４ｇ／ｃｍ３，μ（Ｍｏ－Ｋα）＝２０．６６ｃｍ－１，Ｆ（０００）＝２４７２，对于Ｉ＞３σ（Ｉ）的５９５４个衍射点，最终的Ｒ＝０．０４６，Ｒｗ＝０．０６９。晶体结构由二核铜化合物和溶剂ＤＭＦ组成，两个Ｃｕ原子呈现不对称配位结构，ＤＭＦ在三配位Ｃｕ原子的近邻，它的氧原子和配位ＰＰｈ３的碳原子最近距离在３．３２（２）－３．４４（２）。From the reaction of a mixture of CuI and PPh3 in dichloromethane with W2S4S2CN(CH2CH2OH)22 in N,Ndimethyformamide, the compound Cu2I2(PPh3)3DMF was isolated unexpectedly. The crystal structure consists of dinuclear copper(I) compound and DMF solvent. Two copper atoms show an asymmetrical coordination geometry. DMF lies near threecoordinated copper atom with the closest nonbonded contacts between oxygen atom of DMF and the pheny ring carbon atoms at a distance of 3.32(2)￣3.44(2) . The presence of DMF may have a significant influence on the structure of the dinuclear copper complex and the molecular packing. Crystal data: C57H52Cu2I2NOP3, Mr=1240.87, monoclinic, space group P21/c, unit cell parameters: a=15.863(3), b=19.619(7), c=18.232(4), =109.53(2), V=5348(3)3, Z=4, Dc=1.54g/cm3, (MoK)=20.66cm-1, F(000)=2472, for 5954 observed reflections with I>3(I), final R=0.046, Rw=0.069.

关 键 词：二核铜 合成 晶体结构 铜 原子簇 配合物 

分 类 号：O614.121[理学—无机化学]