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Synthesis, Characterization and Crystal Structure of a Diiron Azadithiolate Complex [(μ-SCH2)2NCH2Ph]Fe2(CO)5(PPh3)
引用本文:刘旭锋,肖勋文,沈梁钧,房江华,王家荣,高浩其,刘幸海.Synthesis, Characterization and Crystal Structure of a Diiron Azadithiolate Complex [(μ-SCH2)2NCH2Ph]Fe2(CO)5(PPh3)[J].结构化学,2011,30(7):1016-1020.
作者姓名:刘旭锋  肖勋文  沈梁钧  房江华  王家荣  高浩其  刘幸海
作者单位:Department of Chemical Engineering;Ningbo University of Technology;College of Chemical Engineering and Materials Science;Zhejiang University of Technology;
基金项目: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)
摘    要:Treatment of complex (μ-SCH 2) 2 NCH 2 Ph]Fe 2 (CO) 6 with PPh 3 in the presence of decarbonylating agent Me 3 NO·2H 2 O afforded the title complex (μ-SCH 2) 2 NCH 2 Ph]Fe 2 (CO) 5 (PPh 3) in 70% yield.The new complex was characterized by elemental analysis,IR,and 1 H (31 P,13 C) NMR spectroscopic techniques as well as by X-ray crystallography.It crystallizes in triclinic,space group P 1 with a=9.3016(19),b=12.698(3),c=13.904(3),V=1519.8(7)3,Z=2,C 32 H 26 Fe 2 NO 5 PS 2,M r=711.33,D c=1.554 g/cm 3,μ(MoKα)=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 PPh 3 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 PPh 3 and the benzene ring.

关 键 词:晶体结构  膦配体  苯基  CO  合成  表征  X射线晶体学  元素分析
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