The synthesis and catalytic properties of molybdenum acetylide complexes CpMo(CO)(3)(-C CR), R = Ph(1), C6H4-p-CF3 (2) and C6H4-p-CH3 (3) has been studied. The molybdenum acetylide complexes were synthesized from CpMo(CO)(3)Cl and aryl acetylenes via Stephens-Castro coupling reaction. These complexes were characterized by single crystal X-ray diffraction analysis, FTIR and H-1 NMR spectroscopy. These complexes on treatment with hydrogen peroxide, formed corresponding molybdenum oxo-peroxo species. These in situ formed oxo-peroxo species were found very active (up to 100 % conversion) and selective (up to 100 %) oxidation catalysts for various refractory and nonrefractory sulfides. Interestingly, even though the molybdenum acetylide complexes are homogeneous, they could be recycled very efficiently by extracting the catalytically active molybdenum oxo-peroxo species in aqueous phase.