The reaction of FeCo2 （CO）9(μ3-S ) with O [P（SCH2）2]2 ligand in mixed solvents of hexane and dichloromethane at 50℃ leads to the compound FeCo2 （CO）7 （μ3）-S) （O [P（SCH2）2]2）. The compound has been characterized by element analysis, IR, 1H NMR, MS spectfa and a single crystal X-ray structure determination.Its structure consists, of a distorted tetrthedral core FeCo2S in which the Co（1）, Co（2）, Fe, and S atoms occupy a vertex of the tetrahedron respectively, and the P atoms of O [P（SCH2）2]2 bonded to two Co atoms in their axial positions.
New mono- and di- substituted derivatives of Fe3 (CO) 9(μ3 - S) 2 were synthesized by reac- tion of C6H5NCS with Fe3 (CO) 1 2 atroom temperature.Their structure were characterized by means of IR(νCO) ,MS,1 H NMR,1 3 C NMR,elemental analysis and X- ray four cycle diffrac- tometer.The results showed that the formulas of the cluster compounds are Fe3 (CO) 8 (CNC6H5) (μ3 - S) 2 and Fe3 (CO) 7(CNC6H5) 2 (μ3 - S) 2 respectively.
