Abstract: The Mo(0)binuclear complexes (Et4N)₂[(CO)₄Mo(μ-S)₂MoS₂](Ⅰ)and (Et<N)₂[(CO)₄Mo(μ-S)₂WS₂](Ⅱ) were synthesised with a new method, and their crystalline structures were determined by X-ray crystallography. Ⅰ and Ⅱ Crystallize in the orthogonal system and the space group is Pbcm with a=1. 8403(2), b=1.1963(1), c=1. 3482(1) nm, Z=4, R=0. 042 for Iand with α=1. 8453(2), 6=1.2004(2), c=1. 3482(3) nm, Z=4, R=0. 032 for I. The structures of the anions of Ⅰ and Ⅱ are all composed of both an octahedron around the Mo(0) atom and a tetrahedron with the Mo (Ⅵ) or W(Ⅵ) atom in the center by sharing an edge which is the line between the two bridged sulfur atoms. The bond distance of Mo-Mo is 0. 2992(2) nm and Mo-Wis 0. 3033(8) nm, and the bimetallic center Mo(μ-S)₂M(M=Mo, W) is planar. It was found in the Fourier IRspectrum of complex Ⅱ that the absorption band of Mo(0)-Sb is v=424. 3 cm^-1.

Key words: Mo(0) binuclear clusters, Synthesis, Crystal structure