The chemistry of thiosemicarbazone complexes of transition metals has been the subject of attention, primarily because of overgrowing biological properties. These activities have been correlated with their metal-chelating abilities and reductive capacity. The coordination chemistry of molybdenum receives special attention due to chemistry of its oxidation state, coordination number, ligating atom and their impact on structure and reactivity. To extend these observations, in this dissertation an attention is focused on the synthesis and characterization of new dioxidomolybdenum(VI) complexes featuring thiosemicarbazone ligands