Synthesis and Crystal Structure of Tetrakis (4-methylpyridine) bis(μ4-pentathio)-tetracopper(Ⅰ) (4-methylpyridine) solvate

摘要

The red chunk title compound [Cu4(S5)2(4-Mepy) 4]@(4-Mepy) was obtained by the reaction of copper powder with sulfur powder, potassium sulfide and excess 4-methylpyridine at ambient temperature and normal atmosphere. Its structure was determined by single-crystal X-ray diffraction analysis, and the crystal data for the compound: triclinic, P ī, a = 9.7442(2), b = 14.124(3), c = 15.410 (3) ?, α = 98.96(3), β = 93.82(3), γ = 94.08(3)°, V = 2083.7(7) ? 3, Z = 2, Dc = 1.66 g/cm3, μ(MoKα) = 1.31mm-1, F(000) = 1052,C30H35N5S10Cu4,Mr = 1040.45. The structure was refined to R = 0.0393 and wR = 0.1158 for 9281 independent reflections. The title crystal consists of a neutral complex molecule [Cu4(S5)2(4-CH3C5H4N)4] and a 4-methylpyridine solvent molecule. In the neutral complex, the four Cu atoms are in a distorted tetrahedral arrangement and the nonbonding Cu…Cu distances in the copper tetrahedron range from 3.1414 to 3.8488 ?, and the Cu-S bond lengths vary from 2.2839 to 2.3670 ?.