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The complex [ C~M O ( C O )~]~ (Cp = C5H5) reacts with S2C2(CF3)2 in refluxing methylcyclohexane solution to give C~(CO)~MO[~-S~C~(CF~)~]~MOCP (1). Complex 1 loses its CO ligands on photolysis in solution to give [ C~M O (~-S~C~( C F~)~) ]~ (2). Complexes 1 and 2 were characterized by l H and 19F NMR spectroscopy, elemental analysis, mass spectrometry, and X-ray diffraction techniques. Electrochemical properties of both compounds were also studied. Crystals of 1 are monoclinic of space group E 1 / m with a = 7.153 (1) A, b = 13.404 (9) A, c = 13.690 (4) A, p = 98.54 (2)O, and 2 = 2. The structure was solved and refined to R = 0.043 and R, = 0.053 by using 1895 independent reflections. The complex contains two asymmetrically bridging S2C (CF3)2 ligands, and both CO ligands are attached to the same Mo atom. The Mo-Mo distance of 3.256 (1) A suggests minimal Mo-Mo bonding. Crystals of 2 are monoclinic of space group E 1 / a with a = 13.030 (1) A, b = 17.336 (2) A, c = 10.741 (7) A, p = 93.29 (4)', and Z = 4. The structure was solved and refined to R = 0.044 and R, = 0.057 by using 2848 independent reflections. Complex 2 contains two symmetrically bridging S2Cz(CF3)2 ligands and has an Mo-Mo bond of 2.584 (1) A.

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