| Summary: | Molybdenum(VI) catalysts were obtained from methanol or acetonitrile by the reaction of [MoO<sub>2</sub>(C<sub>5</sub>H<sub>7</sub>O<sub>2</sub>)<sub>2</sub>] and isonicotinoyl- or nicotinoyl-based aroylhydrazones. Reactions in methanol resulted in the formation of the mononuclear complexes [MoO<sub>2</sub>(L<sup>1–4</sup>)(MeOH)] (<b>1a</b>–<b>4a</b>), while the ones in acetonitrile provided polynuclear complexes [MoO<sub>2</sub>(L<sup>1–4</sup>)]<i><sub>n</sub></i> (<b>1</b>–<b>4</b>)<i><sub>.</sub></i> Crystals of polynuclear compound, [MoO<sub>2</sub>(L<sup>3</sup>)]<i><sub>n</sub></i>∙H<sub>2</sub>O (<b>3∙H<sub>2</sub>O</b>), suitable for X-ray diffraction analysis were obtained by the solvothermal procedure at 110 °C. Complexes were characterized by infrared spectroscopy (IR-ATR), nuclear magnetic resonance (NMR), elemental analysis (EA), and thermogravimetric analysis (TGA). The prepared catalysts were tested in alcohol oxidation reactions. Carveol, cyclohexanol, and butan-2-ol were investigated substrates. Because the alcohol oxidations are very challenging due to various possible pathways, the idea was to test different oxidants, H<sub>2</sub>O<sub>2</sub>, TBHP in water and decane, to optimize the researched catalytic system.
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