摘要
Treatment of complex [（μ-SCH2）2NCH2Ph]Fe2（CO）6 with PPh3 in the presence of decarbonylating agent Me3NO-2H2O afforded the rifle complex [（μ-SCH2）2NCH2Ph]Fe2（CO）5（PPh3） in 70% yield. The new complex was characterized by elemental analysis, IR, and 1H （31p, 13C） NMR spectroscopic techniques as well as by X-ray crystallography. It crystallizes in triclinic, space group P i with a = 9.3016（19）, b = 12.698（3）, c = 13.904（3） A, V = 1519.8（7） A3, Z = 2, C32H26Fe2NOsPS2, Mr = 711.33, Dc = 1.554 g/cm3, μ（MoKa） = 1.187 mm^-1, F（000） = 728, T= 113（2） K, the final R = 0.0288 and wR = 0.0680 for 3982 observed reflections （I 〉 2σ（I））. The PPh3 ligand resides in an axial position of the square-pyramidal geometry of the neighboring Fe atom and trans to the benzene ring in order to minimize the steric repulsion between PPh3 and the benzene ring.
Treatment of complex [（μ-SCH2）2NCH2Ph]Fe2（CO）6 with PPh3 in the presence of decarbonylating agent Me3NO-2H2O afforded the rifle complex [（μ-SCH2）2NCH2Ph]Fe2（CO）5（PPh3） in 70% yield. The new complex was characterized by elemental analysis, IR, and 1H （31p, 13C） NMR spectroscopic techniques as well as by X-ray crystallography. It crystallizes in triclinic, space group P i with a = 9.3016（19）, b = 12.698（3）, c = 13.904（3） A, V = 1519.8（7） A3, Z = 2, C32H26Fe2NOsPS2, Mr = 711.33, Dc = 1.554 g/cm3, μ（MoKa） = 1.187 mm^-1, F（000） = 728, T= 113（2） K, the final R = 0.0288 and wR = 0.0680 for 3982 observed reflections （I 〉 2σ（I））. The PPh3 ligand resides in an axial position of the square-pyramidal geometry of the neighboring Fe atom and trans to the benzene ring in order to minimize the steric repulsion between PPh3 and the benzene ring.
基金
Supported by the start-up foundation of Ningbo University of Technology
the National Natural Science Foundation of China (20902051,21002090)
Foundation of the Education Committee of Zhejiang Province (Z200906833)
the Natural Science Foundation of Ningbo city (2010A610186)
