The title compound Fe3（CO）8（C6H5NC）（μ3-S）2 （Ⅰ） was synthesized bythe reaction of C6H5NCS with Fe3（CO）12 at room temperature. The crystal andmolecular structure of the title compound were determined by single ctystal diffratttionmethod- Crystal data: monoclinic, space group P21/C, a=12．718（4）A, b=26.164（10）A,c=l3.741（7）A, β=117.18（2） °, V=4067（2）A3, Z=8, Dc=1．825 g/cm3. The structure wassolved by direct method and difference Fourier synthesis, and refined by full-matrix Leastsquares with anisotropic thermal paramaters, using 1990 observed reflections [Ⅰ＞3σ（Ⅰ）].The final residual factor was R＝0．076, Rw＝0．082. The substituted ligand （C6H5NC）in Fe3（CO）8（C6H5NC）（μ3-S）2 is connected to the Fe（3） atom of the distorted tetragonalpyramid Fe3S2 framework.
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