Syntheses and Crystal Structures of Homleptic Lanthanide Complexes [C_6H_5COCHC(CH_3)N-(p-ClC_6H_4)]_3Ln(THF)_n (Ln =Yb,Y,Nd)  

作　　者：仇为仁 周海荣 范玲玲 王耀荣 姚英明 沈琪 

机构地区：[1]Key Laboratory of Organic Synthesis of Jiangsu Province,College of Chemistry,Chemical Engineering and Materials Science,Soochow University

出　　处：《Chinese Journal of Structural Chemistry》2014年第7期1031-1036,共6页结构化学（英文）

基　　金：supported by the National Natural Science Foundation of China(Nos.21072146,21174095 and 21132002);Key Laboratory of Organic Synthesis of Jiangsu,Soochow University(KJS1008)

摘　　要：Three homoleptic lanthanide complexes, [C6H5COCHC（CH3）N（p-CIC6H4）]3Ln（THF）n （n = 0, Ln = Yb （1）; n = 0, Ln = Y （2）; n = 1, Ln = Nd （3））, were synthesized by amine elimination reaction of Ln[N（SiMe3）2]3 with 1-phenyl-3-N-（p-chlorophenylimino）-1-butanone. These com- plexes crystallize in triclinic, space group PI with a = 9.805（3）, b = 14.831（6）, c = 16.075（6） A, a = 111.996（9）, β = 91.570（7）, y = 93.744（6）° V= 2159.4（13） A3, Z= 2, Dc = 1.515 g/cm3, F（000） = 986, μ（MoKa） = 2.396 mm-1, R = 0.0360 and wR = 0.0850 for 9548 observed reflections with I 〉 20（I） for complex 1; a = 9.861（5）, b = 14.852（9）, c = 16.111（9） A, a = 112.362（13）,β = 91.949（11）, y = 93.678（14）°, V= 2173（2） A3, Z= 2, Dc = 1.377 g/cm3, F（000） = 924,μ（MoKa） = 1.570 mm-1, R = 0.0735 and wR = 0.1389 for 8015 observed reflections with I 〉 20（I） for complex 2; and a = 9.308（3）, b = 15.357（3）, c = 17.419（4） A, a = 66.493（13）, β = 88.61（2）, y = 86.664（19）°, V = 2279.4（9） A3, Z= 2, Dc = 1.499 g/cm3, F（000） = 1046,μ（MoKa） = 1.364 mm-1, R = 0.0843 and wR = 0.2280 for 8433 observed reflections with I 〉 20（I） for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.Three homoleptic lanthanide complexes, [C6H5COCHC（CH3）N（p-CIC6H4）]3Ln（THF）n （n = 0, Ln = Yb （1）; n = 0, Ln = Y （2）; n = 1, Ln = Nd （3））, were synthesized by amine elimination reaction of Ln[N（SiMe3）2]3 with 1-phenyl-3-N-（p-chlorophenylimino）-1-butanone. These com- plexes crystallize in triclinic, space group PI with a = 9.805（3）, b = 14.831（6）, c = 16.075（6） A, a = 111.996（9）, β = 91.570（7）, y = 93.744（6）° V= 2159.4（13） A3, Z= 2, Dc = 1.515 g/cm3, F（000） = 986, μ（MoKa） = 2.396 mm-1, R = 0.0360 and wR = 0.0850 for 9548 observed reflections with I 〉 20（I） for complex 1; a = 9.861（5）, b = 14.852（9）, c = 16.111（9） A, a = 112.362（13）,β = 91.949（11）, y = 93.678（14）°, V= 2173（2） A3, Z= 2, Dc = 1.377 g/cm3, F（000） = 924,μ（MoKa） = 1.570 mm-1, R = 0.0735 and wR = 0.1389 for 8015 observed reflections with I 〉 20（I） for complex 2; and a = 9.308（3）, b = 15.357（3）, c = 17.419（4） A, a = 66.493（13）, β = 88.61（2）, y = 86.664（19）°, V = 2279.4（9） A3, Z= 2, Dc = 1.499 g/cm3, F（000） = 1046,μ（MoKa） = 1.364 mm-1, R = 0.0843 and wR = 0.2280 for 8433 observed reflections with I 〉 20（I） for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.

关 键 词：organolanthanide p-ketoiminate ligand crystal structure 

分 类 号：O627[理学—有机化学]