Synthesis and Characterization of a Sb(Ⅲ)Complex with α-Diimine Ligand and a Csp3-Csp3 Coupling Production of the Original Ligand

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.