Abstract

A novel 2D inorganic-organic hybrid coordination polymer based on polyoxometalate [Mo<sub>8</sub>Na<sub>2</sub>O<sub>28</sub>]<sup>6-</sup>, [Ni(Btp)<sub>2</sub>(H<sub>2</sub>O)][Mo<sub>8</sub>Na<sub>2</sub>O<sub>26</sub>(<italic>μ</italic><sub>2</sub>-OH)<sub>2</sub>]<sub>0.5</sub>·H<sub>2</sub>O(1). (Btp = 1,3-bis(1,2,4-triazol-1-yl)propane), has been prepared under hydrothermal reaction with a mixture of (NH<sub>4</sub>)<sub>6</sub>Mo<sub>7</sub>O<sub>24</sub>·4H<sub>2</sub>O, NiCl<sub>2</sub>·6H<sub>2</sub>O, flexible ligand (Btp), NaOH and water, and structurally characterized by elemental analyses, IR spectroscopy, TG, and single-crystal X-ray diffraction analysis. X-ray crystal structure analysis shows that, the compound belongs to monoclinic crystal system, space group <italic>P</italic>2<sub>1</sub>/<italic>c</italic>, crystal data: <italic>a</italic> = 11.6871(8) Å, <italic>b</italic> = 21.7506(15) Å, <italic>c</italic> = 14.9208(8) Å, <italic>Z</italic> = 4, <italic>R</italic><sub>1</sub> = 0.0487, <italic>wR</italic><sub>2</sub> = 0.1409. Compound 1 contains a kind of new polyoxometalate cluster [Mo<sub>8</sub>Na<sub>2</sub>O<sub>28</sub>]<sup>6-</sup>, which could be regarded as the transformation from β-[Mo<sub>8</sub>O<sub>26</sub>]<sup>4-</sup> and with the structural characteristics similar to [V<sub>10</sub>O<sub>28</sub>]<sup>6-</sup> polyanion. The polyoxometalates are sandwiched by the 2D layer constructed by Ni<sup>II</sup> and Btp, leading to the formation of sandwich-like 2D columnar layer. The 2D columnar layer penetrates each other and finally results in the construction of an interesting 2D→3D polycatenated structure. In addition, the title complex shows good electrocatalytic and photocatalytic activity.

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