| 乙二醇二甲醚三苯基氧化膦三氯合铬Cr[(CH3OCH2CH2OCH3)(OPPh3)Cl3]的合成和晶体结构 |
| SYNTHESIS AND CRYSTAL STRUCTURE OF TRICHLORO-TRIPHENYLPHOSPHINE OXIDE-ETHYLENE GLYCOL DIMETHYLETHER CHROMIUM, Cr[(OPPh3)(CH3OCH2CH2OCH3)Cl3] |
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| 摘要: 标题配合物由Cr(CO)6和PPh3在50ml乙二醇二甲醚中回流5小时后过滤,在滤液中加S2Cl2,静置后得配合物单晶。晶体属单斜晶系,空间群为P21,单胞参数a=9.062(3)Å,b=11.088(3)Å,c=12.153(3)Å,β=97.93(1)°,V=1209.4(1.8)Å3,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,Rω=0.054,结构中Cr各与三个氧和三个氯原子键联,Cr-O(CH3OCH2CH2OCH3)平均距离为2.091Å,Cr-O(OPPh3)距离为2.000Å,Cr-Cl(平均)距离为2.274Å。它们形成了八面体配位构型。 |
| 关键词: 铬的配合物 八面体配合物 三苯基氧化膦 |
| 基金项目: |
| Abstract: The chromium complex Cr[(OPPhS3)(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)Å, b= 11.088(3)Å, c= 12.153(3)Å, β = 97.93(1)° V= 1209.4(1.8)Å3, 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, Rω = 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 2.091Å and 2.000Å, respectively. The mean Cr-Cl distance is 2.274Å. The coordination polyhedron can be described as a octahedron. |
| Keywords: chromium complex octahedral complex triphenylphosphine oxide |
| 投稿时间：1989-10-09 |
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| 林长增,黄锦顺,卢嘉锡.乙二醇二甲醚三苯基氧化膦三氯合铬Cr[(CH3OCH2CH2OCH3)(OPPh3)Cl3]的合成和晶体结构[J].无机化学学报,1992,8(1):38-42. |
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