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.
The mono and di substituted derivatives of the parent cluster {μ3 H(Ph)C=C}FeCo2(CO)9 (1) have been synthesized by facile substitution reactions. The compound {μ3 H(Ph)C=C}FeCo2(CO)7(dppe) (2), {μ3 H(Ph)C=C}FeCo2(CO)8(PPh3) (3) and {μ3 H(Ph)C=C}FeCo2(CO)8(AsPh3) (4) were characterized by elemental analysis, IR, 1H ,31P NMR, MS and X ray crystallography. The new cluster 2 crystallizes in monoclinic space group P21/n, with a=0. 8614(5)nm, b=1.6404(8)nm, c=2.6574(14)nm, β=96.3222(12)°, V=3.732(3)nm3, Z=4, S=0.886, Δρmax=0.335e·nm-3, Δρmin=-0.379e·nm-3. Final R indices : R1=0.0432, wR2=0.0695. CCDC: 164600.
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.
