A novel mixed-trib ridged dimolybdenum(Ⅰ) compound [Bu4N][Mo2(n-SPh)2(u-Cl)(CO)6] (1) has been synthesized from the reaction of Mo2 (CO)8 (SPh)2 with ButNCl.Compound 1 was characterized by IR,UV-Vis and 1H,13C,95Mo NMR spectroscopic analyses.The electrochemical behavior was measured by cyclic voltammetry,indicating a quasi-reversible two-electron transfer in one step.The crystal structure determined by X-ray crystallography shows that 1 contains a [Mo2(u-S)2(u-Cl)]- core with a planar Mo2S2 unit and a Cl bridge.The Mo-Mo distance is 0.28709(7) nm,and the Mo-Cl-Mo angle is 66.44(4).A newface-sharing bioctahedral structure is discussed.