配合物[Fe(OPPh_3)_4Cl_2][FeCl_4]的合成和晶体结构  被引量:2

Synthesis and crystal structure of complex [Fe(OPPh_3)_4Cl_2][FeCl_4]

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作  者:唐爱斌[1] 周健[1] 戴洁[1] 张勇[1] 刘宇[1] 卞国庆[1] 卢雯[1] 

机构地区:[1]苏州大学化学化工学院,江苏苏州215123

出  处:《化学研究与应用》2006年第9期1084-1087,共4页Chemical Research and Application

基  金:南京大学配位化学重点实验室开放基金资助项目

摘  要:A Fe(Ⅲ) compex with OPPh3,[Fe(OPPh3)4Cl2][FeCl4],has been synthesized and characterized by elemental analysis and IRspectrum.The crystal structure of the title complex has been determined by simgle crystal X-ray diffraction techmiques.The crystal belongs to monoclinic,space group P21/c.The cell parameters are :a=13.9323(13),b=27.5290(2),c=18.2095(17),β= 104.460(2)o,V=6762.9(11)3,Z=4,DC=1.412 g/cm3,μ=0.809 mm-1,F(000)=2952,R1=0.0796 and ωR2=0.1752for 10419 observed reflections(I>2σ(I)) out of 12343 unique data.In the cations[Fe(OPPh3)4Cl2]+,the Fe(Ⅲ) center adopts a slight distoned octahedral geometry comprised oftwo OPPh3 oxygen atoms and two Cl-ions at the equatorial positions,and two OPPh3 oxygenatoms at the axial positions.In the anions[FeCl4]-,The Fe(Ⅲ) ion has a sIightly distortedtetrahedI.al coordination geometry and is bonded to four Cl-ions.A Fe( Ⅲ ) compex with OPPh3, [ Fe( OPPh3 )4Cl2 ] [ FeCl4 ], has been synthesized and characterized by elemental analysis and IRspectrum. The crystal structure of the title complex has been determined by simgle crystal X - ray diffraction techmiques. The crystal belongs to monochnic, space group P21/c. The cell parameters are : a = 13. 9323 ( 13 ) A, b = 27.5290 (2)A, c = 18. 2095 (17) A,β = 104. 460 (2)°,V = 6762. 9 ( 11 )A^3 ,Z = 4, Dc = 1. 412 g/cm^3,μ = 0. 809 mm^-1, F(000) = 2952, R1 = 0. 0796 and ωR2 = 0. 1752for 10419 observed reflections ( I 〉 2or ( I ) ) out of 12343 unique data. In the cations [ Fe (OPPh3 )4Cl2 ]^+ ,the Fe(Ⅲ) center adopts a slight distoned octahedral geometry comprised ofiwo OPPh3 oxygen atoms and two CI^- ions at the equatorial positions, and two OPPh3 oxygenatoms at the axial positions. In the anions [ FeCI4 ] -, The Fe ( Ⅲ ) ion has a sIightly distortedtetrahedI, al coordination geometry and is bonded to four Cl^- ions.

关 键 词:铁的配合物 晶体结构 脱氧反应 

分 类 号:O734.741[理学—晶体学]

 

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