Can. J. Chem. 67, 2222Chem. 67, (1989. Tetrakis(benzonitrile)copper(I) hexachloroantimonate(V) crystallizes as a yellow solid in the triclinic space group with a = 8.217(4) A, b = 14.1 16(5) A, c = 14.296(9) A, a = 86.88(4)", P = 87.49(5)", and y = 81,92(3)". Hexakis(benzonitri1e) copper(II) bis[hexachloroantimonate(V)] is a green solid which also crystallizes in space group PI with a = 10.3286(8) A, b = 11.0954(8) A, c = 1 1.9722(5) A, a = 85.536(4)", P = 80.530(6)", and y = 84.05 l(6)". Both compounds are synthesized from cuprous chloride, benzonitrile and antimony pentachloride depending on relative concentrations, while the latter is also prepared from cupric chloride and antimony pentachloride in benzonitrile solution.Key words: copper complexes, crystal structures.