物理化学学报 >> 1992, Vol. 8 >> Issue (06): 749-752.doi: 10.3866/PKU.WHXB19920607

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簇合物(μ-SC6H5)(μ-P(SC6H5)2)Fe2(CO)6的合成和晶体结构

吴秉芳; 阎秀英; 刘启旺; 刘树堂; 胡襄   

  1. 内蒙古大学化学系，呼和浩特 010021
  • 收稿日期:1991-07-26 修回日期:1991-12-27 发布日期:1992-12-15
  • 通讯作者: 吴秉芳

Synthesis and Crystal Structure of Cluster (μ-SC6H5)(μ-P(SC6H5)2)Fe2(CO)6

Wu Bing-Fang; Yan Xiu-Ying; Liu Qi-Wang; Liu Shu-Tang; Hu Xiang   

  1. Department of Chemistry, Nei Monggu University, Huhehot 010021
  • Received:1991-07-26 Revised:1991-12-27 Published:1992-12-15
  • Contact: Wu Bing-Fang

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摘要： 用Fe_3(CO)_(12)与亚磷酸三硫代苯酯P(SC_6H_5)_3反应得到标题化合物。P(SC_6H_5)_3以其裂解分子片SC_6H_5和P(SC_6H_5)_2配位。用X-ray衍射技术测定了该化合物的晶体结构, 晶体属正交晶系, 空间群为Pbca, a=1.7422(7), b=1.0634(6), c=2.898(12) nm; V=5.370 nm, z=8, D_c=1.579 g·cm~(-3)。由直接法和差值Fourier合成解出全部非氢原子坐标, 并用全矩阵最小二乘法修正, 最后偏离因子R=0.054, R_w=0.058, 分子结构中心的Fe_2SP折叠环沿S…P线或沿Fe—Fe键折叠的二面角(分别为76.1°和82°)比其它具有中心Fe_2S_2, Fe_2P_2和Fe_2SP折叠环的类似化合物中的相应值小, Fe—Fe键长为0.2572 nm, Fe—S(1)—Fe=68.6°, Fe—P—Fe=70.7°。

关键词: 双核铁羰基衍生物, 合成, 晶体结构, 桥联原子

Abstract: The title compound was obtained by the reaction of Fe_3(CO)_(12) with phosphorotri-thious acid triphenyl ester P(SC_6H_5)_3. Ligand precursor P(SC_6H_5)_3 coordinated to the cluster by its cleaved fragments SC_6H_5 and P(SC_6H_5)_2. The crystal structure of the compound has been determined by a single crystal X-ray diffraction method. The crystal is orthorhombic, space group belongs Pbca, a=1.7422(7), b=1.0634(6), c=2.8987(12) nm; V=5.370 nm, z=8, D_c=1. 579 g·cm~(-3). Coordinates of all nonhydrogen atoms were delermined by idrect method and difference Fourier synthesis, with 3531 observable reflections (I≥3σ(I_0)) refined by a full-matrix least-squares procedure so that the final R=0.054, R_W=0.058. The dihedral angle of the folded Fe_2SP ring along the S…P line or the Fe—Fe bond (76.1° or 82°, respectively) is much smaller than that for other similar compounds with the central Fe_2S_2 or Fe_2P_2 or Fe_2·SP folded rings. Fe—Fe=0.2572(2) nm, Fe—S(1)—Fe=68.6°(1), Fe—P—Fe=70.7°(1).

Key words: Dinuclear iron carbonyl derivative, Synthesis, Crystal structure, Bridging atom