Reaction of [（μ-SCH2）2NPh]Fe2（CO）6 with Ph2PCH2PPh2 in the presence of Me3NO·2H2O gave the title complex [（μ-SCH2）2NPh]Fe2（CO）5（Ph2PCH2PPh2）（1）in 78% yield.The new complex 1 was characterized by ele...Reaction of [（μ-SCH2）2NPh]Fe2（CO）6 with Ph2PCH2PPh2 in the presence of Me3NO·2H2O gave the title complex [（μ-SCH2）2NPh]Fe2（CO）5（Ph2PCH2PPh2）（1）in 78% yield.The new complex 1 was characterized by elemental analysis,spectroscopy and X-ray crys-tallography.It crystallizes in triclinic,space group P1 with a = 10.832（2）,b = 12.003（2）,c = 15.579（3）,V = 1785.6（6）3,Z = 2,C32H26Fe2NO5PS2,Mr = 819.40,Dc = 1.524 g/cm3,μ（MoKα）= 1.064 mm-1,F（000）= 840,T = 113（2）K,the final R = 0.0543 and wR = 0.1218 for 6203 observed reflections（I 2σ（I））.The Ph2PCH2PPh2 ligand resides in an axial position of the square-pyramidal coordination sphere of the Fe atom and trans to the benzene ring in order to reduce the steric repulsion between Ph2PCH2PPh2 and the benzene ring.展开更多
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 cha...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.展开更多
基金supported by the National Natural Science Foundation of China (20902051,21002090)the Key Laboratory of Pesticide Chemistry and Application,Ministry of Agriculture (MOA) (No.MOAPCA201005)+1 种基金the Foundation of the Education Committee of Zhejiang Province (Y201018479,Z200906833)the Natural Science Foundation of Ningbo (2010A610186)
文摘Reaction of [（μ-SCH2）2NPh]Fe2（CO）6 with Ph2PCH2PPh2 in the presence of Me3NO·2H2O gave the title complex [（μ-SCH2）2NPh]Fe2（CO）5（Ph2PCH2PPh2）（1）in 78% yield.The new complex 1 was characterized by elemental analysis,spectroscopy and X-ray crys-tallography.It crystallizes in triclinic,space group P1 with a = 10.832（2）,b = 12.003（2）,c = 15.579（3）,V = 1785.6（6）3,Z = 2,C32H26Fe2NO5PS2,Mr = 819.40,Dc = 1.524 g/cm3,μ（MoKα）= 1.064 mm-1,F（000）= 840,T = 113（2）K,the final R = 0.0543 and wR = 0.1218 for 6203 observed reflections（I 2σ（I））.The Ph2PCH2PPh2 ligand resides in an axial position of the square-pyramidal coordination sphere of the Fe atom and trans to the benzene ring in order to reduce the steric repulsion between Ph2PCH2PPh2 and the benzene ring.
基金Supported by the start-up foundation of Ningbo University of Technologythe National Natural Science Foundation of China (20902051,21002090)+1 种基金Foundation of the Education Committee of Zhejiang Province (Z200906833)the Natural Science Foundation of Ningbo city (2010A610186)
文摘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.
