Two bis-[cis-MoO2]2+ core bearing complexes, designated as [{MoVIO2}2(L1)(H2O)2] (1) and [{MoVIO2}2(L2)(H2O)2] (2), were created by reacting MoO2(acac)2 with dihydrazone ligands, namely H4L1(i) and H4L2(ii) (generated from a 2:1 ratio of hydrazide of terephthalate and salicylaldehyde or o-vanillin) in a 2:1 ratio in a methanolic solution. These complexes were extensively characterized using several spectroscopic techniques. The shape of the complex [{MoVIO2}2(L1)(H2O)2] (1) was confirmed by SC-XRD, revealing an octahedral geometry. Moreover, the crystallographic analysis of complex (1) elucidates the substitution of a single facet of the water molecule with DMF, accompanied by the inclusion of an additional DMF molecule within the crystal lattice. These synthesized compounds were evaluated as potential catalysts for the epoxidation of styrene in the existence of oxidant (H2O2). The oxidation reactions were conducted using both conventional and microwave-assisted methods, and the obtained data were compared in terms of activity and selectivity.