The Mo-Mo bond dinuclear compounds were synthesized via oxidative coupling of tricarbonyltrimethylsilylcyclopentadienyl molybdenum anion salt and silylene-bridged bis(tricarbonyltrimethylsilylcyclopentadienylmolybdenum anion salts) E[h-Me3SiC5H3Mo(CO)3]22-Li2+, [E = SiMe2, O(SiMe2)2], resp. Compound containing molybdenum-molybdenum triple bond was also prepared by heating [h-Me2SiC5H4Mo(CO)3]2 (I) under reflux in toluene. Acetylene add to the MoYMo triple bond to give tetrahedron complex, structures of the title compounds were characterized by elemental analyses, IR and 1H NMR spectra. The crystal structures of complex I was determine

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, CRYSTAL STRUCTURE, PROTON MAGNETIC RESONANCE SPECTROMETRY, MOLYBDENUM COMPLEX, COUPLING REACTION, DINUCLEAR COMPLEX