乙二醇二甲醚三苯基氧化膦三氯合铬Cr[(CH_3OCH_2CH_2OCH_3)(OPPh_3)Cl_3]的合成和晶体结构  

SYNTHESIS AND CRYSTAL STRUCTURE OF TRICHLORO-TRIPHENYLPHOSPHINE OXIDE-ETHYLENE GLYCOL DIMETHYLETHER CHROMIUM, Cr[(OPPh_3)(CH_3OCH_2CH_2OCH_3)Cl_3]

作　　者：林长增 黄锦顺 卢嘉锡 

机构地区：[1]福建物质结构研究所结构化学开放研究实验室,福州350002

出　　处：《无机化学学报》1992年第1期38-42,共5页Chinese Journal of Inorganic Chemistry

摘　　要：标题配合物由Cr(CO)_6和PPh_3在50ml乙二醇二甲醚中回流5小时后过滤,在滤液中加S_2Cl_2,静置后得配合物单晶。晶体属单斜晶系,空间群为P2_1,单胞参数a=9.062(3)(?),b=11.088(3)(?),c=12.153(3)(?),β=97.93(1)°,V=1209.4(1.8)(?)~3,Z=2。 晶体结构是采用Patterson法和差Fourier合成解出。经全矩阵最小2乘法修正,最后偏离因子R=0.046,R_w=0.054,结构中Cr各与三个氧和三个氯原子键联,Cr-O(CH_3OCH_2CH_2OCH_3)平均距离为2.091(?),Cr-O(OPPh_3)距离为2.000(?),Cr-Cl(平均)距离为2.274(?)。它们形成了八面体配位构型。The chromium complex Cr[(OPPh3)(CH3OCH2CH2OCH3)Cl3] was prepared by the reaction of Cr(CO)6 with PPh3 in 50ml CH3OCH2CH2OCH3 under reflux, after 5 hrs, the precipitate was filtered off, then a solution of S2C12 was added to a stirred filtrate. On standing, crystal of the title complex were obtained. The X-ray crystal and molecular structure of the chromium complex has been determined from diffractometer data. Crystallographic data are as follows: monoclinic; space group P21, with a = 9.062(3)A, b= 11.088(3)A, c= 12.153(3)A, β = 97.93(1)° V= 1209.4(1.8)A3, Z=2. The structure was solved by Patterson and Fourier methods and refined by full matrix least-square techniques for 1772 reflections with I> 3 (I), R = 0.046, Rw = 0.054. The molecule consists of the Cr atom bonded to three oxygen atoms and three chlorine atoms. The mean Cr-O(CH3OCH2CH2OCH3) and Cr-O(OPPh3) distances are 2.091 A and 2.000A, respectively. The mean Cr-Cl distance is 2.274A. The coordination polyhedron can be described as a octahedron.

关 键 词：(OPPh3) 铬配合物 八面体配合物 

分 类 号：O614.611[理学—无机化学]