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.