Notes. Heterobimetallic clusters derived from [MS4]2–(M = Mo or W): synthesis and structural characterization of [NMe4]4[(CuCl)5Cl2WS4], a double cubane-like complex

Abstract

Reaction of [NMe4]2[MS4](M = Mo or W) with CuCl (1:3.5) in CH3CN produces a hexanuclear complex anion [(CuCl)5Cl2MS4]4–. Crystals of [NMe4]4[(CuCl)5Cl2WS4] are monoclinic, space group C2/c with cell dimensions a= 21.610(4), b= 9.340(2), c= 19.570(5), β= 92.84(2)°, and Z= 4. Least-squares refinement based on 2 708 reflections with I 3σ(I) converged at R= 0.032. The anion has crystallographically imposed C2 symmetry. The crystal structure determination shows that five of the six edges of the [WS4]2– tetrahedron are co-ordinated by CuCl units forming an open double cubane-like structure; the cubic geometry is achieved by chlorine atoms.