Synthesis and characterization of a Sb(III) complex with α-diimine ligand and a C_sp3-C_sp3 coupling production of the original ligand

A C_sp3-C_sp3 coupling production of the original ligand molecule [(CMeN(2,6-iPr₂C₆H₃)) ₂]₂ (1) and an antimony ionic compound with a-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) Å, V = 4939.8(14) ų, C₅₆H₇₈N ₄, M_r = 807.22, Z = 4, D_c = 1.085 g/cm ³, 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 Pl̄ with a = 10.930(2), b = 12.553(2), c = 12.561(3) Å, α = 89.780(7), β = 82.861(6), γ = 68.598(4)°, V = 1590.5(5) ų, C ₂₈H₄₃Cl₄N₂Sb, M_r = 671.19, Z = 2, D_c = 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 C _sp3-C_sp3 coupling of two ligand molecules. The reaction of corresponding 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.