<p>By selecting appropriate ligands, two polyoxidovanadate complexes, [Ni(en)<sub>2</sub>]<sub>3</sub>[V<sub>18</sub>O<sub>42</sub>Cl]·7H<sub>2</sub>O·2H<sub>3</sub>O<sup>+</sup> (<b>1</b>) and [H<sub>2</sub>N(CH<sub>3</sub>)<sub>2</sub>]<sub>3</sub>[PV<sub>14</sub>O<sub>42</sub>]·2TMP·6H<sub>3</sub>O<sup>+</sup> (<b>2</b>), have been synthesized at different pH values using V<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>, Ni(CH<sub>3</sub>COO)<sub>2</sub>, and H<sub>6</sub>TTHA (for <b>1</b>), VO(acac)<sub>2</sub> and TPP (for <b>2</b>) (en = C<sub>2</sub>H<sub>8</sub>N<sub>2</sub>, TPP = thiamine pyrophosphate, TMP = thiamine monophosphate, H<sub>6</sub>TTHA = 1,3,5-triazine-2,4,6-triamine hexaacetic acid). The complexes have been characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis (TG), and single crystal X-ray diffraction. The complexes catalyze the oxidation of the organic substrate phenol red in the presence of H<sub>2</sub>O<sub>2</sub> and bromide, and the reaction system is considered as a model for hydrogen peroxide determination. The reaction rate constants (<i>k</i>) for <b>1</b> and <b>2</b> are calculated as 3.729 × 10<sup>3</sup> and 4.083 × 10<sup>3</sup> (mol L)<sup>−2</sup> s<sup>−1</sup>. The maximum conversion rate of phenol red for <b>1</b> is 83.32%, while for <b>2</b> is 81.12%.</p
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