Synthesis and Crystal Structure of the Diiron Azadithiolate Complex [(μ-SCH_2)_2NPh]Fe_2(CO)5(Ph_2PCH_2PPh_2)  

作　　者：刘旭锋 肖勋文 刘幸海 

机构地区：[1]Department of Chemical Engineering,Ningbo University of Technology [2]College of Chemical Engineering and Materials Science,Zhejiang University of Technology

出　　处：《Chinese Journal of Structural Chemistry》2011年第10期1437-1441,共5页结构化学（英文）

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);the Foundation of the Education Committee of Zhejiang Province (Y201018479,Z200906833);the Natural Science Foundation of Ningbo (2010A610186)

摘　　要：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.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.

关 键 词：diiron azadithiolate SYNTHESIS crystal structure 

分 类 号：O627.81[理学—有机化学]