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] 1 and an antimony ionic compound with α-diimine ligand [LH3] + [SbCl4] = [(2,6-iPrC6H3) NC (Me)] 2) was 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 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.