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Synthesis, characterization, and spectral features of six-coordinated dioxomolybdenum(VI) complexes of the type, [MoO2(tscz)2] (where Htscz represents the thiosemicarbazone moiety) are reported. These have been characterized by elemental analysis, conductance measurements, molecular weight determinations, and magnetic studies. Based on IR, 1H NMR, 13C NMR, and electronic spectral studies, an octahedral geometry with cis-MoO2 structure has been proposed. The antibacterial and fungicidal activities of two representative ligands and their dioxomolybdenum complexes have also been evaluated and discussed.