Synthesis and Characterization of a Sb(Ⅲ) Complex with α-Diimine Ligand and a C_(sp3)-C_(sp3) Coupling Production of the Original Ligand  

作　　者：马小莉 孙帅 杨鹰 

机构地区：[1]School of Chemical Engineering and Environment,Beijing Institute of Technology [2]School of Chemistry and Chemical Engineering,Central South University

出　　处：《Chinese Journal of Structural Chemistry》2013年第5期714-720,共7页结构化学（英文）

基　　金：supported by the National Natural Science Foundation of China (No. 21001016 and 20902112)

摘　　要：A Csp3-Csp3 coupling production of the original ligand molecule [（CMeN（2,6-iPr2C6H3））2]2 （1） and an antimony ionic compound with α-diimine ligand [LH3]＋[SbCl4]-（2, L = [（2,6-iPrC6H3）NC（Me）]2） were synthesized and characterized by 1H NMR, elemental analysis and single-crystal X-ray structural analysis. The crystal of compound 1 belongs to the orthorhombic system, space group Pbca with a = 21.173（4）, b = 10.1639（17）, c = 22.954（4） , V = 4939.8（14） 3, C56H78N4, Mr = 807.22, Z = 4, Dc = 1.085 g/cm3, μ（MoKα） = 0.062 mm-1, F（000） = 1768, S = 0.998, the final R = 0.0593 and wR = 0.1616 for 6481 observed reflections （Ⅰ 〉 2σ（Ⅰ）） and R = 0.0819 and wR = 0.1805 for all 28753 data. The crystal of compound 2 belongs to the triclinic system, space group P with a = 10.930（2）, b = 12.553（2）, c = 12.561（3） , α = 89.780（7）, β = 82.861（6）, γ = 68.598（4）o, V = 1590.5（5） 3, C28H43Cl4N2Sb, Mr = 671.19, Z = 2, Dc = 1.401 g/cm3, μ（MoKα） = 1.222mm-1, F（000） = 688, S = 0.989, the final R = 0.0294 and wR = 0.0616 for 7578 observed reflections （Ⅰ 〉 2σ（Ⅰ）） and R = 0.0366 and wR = 0.0639 for all 16515 data. Complex 1 can be rationalized as a result of Csp3-Csp3 coupling of two ligand molecules. The reaction of corres- ponding potassium salts with Sb（Ⅲ） chloride resulted in the antimony complex 2, in which the cationic moiety [LH3]^＋ is balanced by the presence of [SbCl4]- anion.A Csp3-Csp3 coupling production of the original ligand molecule [（CMeN（2,6-iPr2C6H3））2]2 （1） and an antimony ionic compound with α-diimine ligand [LH3]＋[SbCl4]-（2, L = [（2,6-iPrC6H3）NC（Me）]2） were synthesized and characterized by 1H NMR, elemental analysis and single-crystal X-ray structural analysis. The crystal of compound 1 belongs to the orthorhombic system, space group Pbca with a = 21.173（4）, b = 10.1639（17）, c = 22.954（4） , V = 4939.8（14） 3, C56H78N4, Mr = 807.22, Z = 4, Dc = 1.085 g/cm3, μ（MoKα） = 0.062 mm-1, F（000） = 1768, S = 0.998, the final R = 0.0593 and wR = 0.1616 for 6481 observed reflections （Ⅰ 〉 2σ（Ⅰ）） and R = 0.0819 and wR = 0.1805 for all 28753 data. The crystal of compound 2 belongs to the triclinic system, space group P with a = 10.930（2）, b = 12.553（2）, c = 12.561（3） , α = 89.780（7）, β = 82.861（6）, γ = 68.598（4）o, V = 1590.5（5） 3, C28H43Cl4N2Sb, Mr = 671.19, Z = 2, Dc = 1.401 g/cm3, μ（MoKα） = 1.222mm-1, F（000） = 688, S = 0.989, the final R = 0.0294 and wR = 0.0616 for 7578 observed reflections （Ⅰ 〉 2σ（Ⅰ）） and R = 0.0366 and wR = 0.0639 for all 16515 data. Complex 1 can be rationalized as a result of Csp3-Csp3 coupling of two ligand molecules. The reaction of corres- ponding potassium salts with Sb（Ⅲ） chloride resulted in the antimony complex 2, in which the cationic moiety [LH3]^＋ is balanced by the presence of [SbCl4]- anion.

关 键 词：Α-DIIMINE C-C coupling ANTIMONY ionic compound 

分 类 号：O641.4[理学—物理化学]