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The synthesis and characterization of a Keggin-type mono-rhenium(V)- substituted polyoxotungstate are described. The dimethylammonium salt [Me 2 NH 2 ] 4 [PW 11 Re V O 40 ] was obtained as analytically pure homogeneous black-purple crystals by reacting mono-lacunary Keggin polyoxotungstate with [Re IV Cl 6 ] 2-  in water, followed by crystallization from acetone at ca. 5 °C. Single-crystal X-ray structural analysis of [PW 11 Re V O 40 ] 4-  revealed a monomeric structure with overall  T d   symmetry. Characterization of [Me 2 NH 2 ] 4 [PW 11 Re V O 40 ] was also accomplished by elemental analysis, magnetic susceptibility, TG/DTA, FTIR, UV-vis, diffuse reflectance (DR) UV-vis, and solution  31 P-NMR spectroscopy. Furthermore, [PW 11 Re V O 40 ] 4-  and the Dawson-type dirhenium(V)-oxido-bridged polyoxotungstate [O{Re V (OH)(α 2 -P 2 W 17 O 61 )} 2 ] 14-  were supported onto anatase TiO 2  surface by the precipitation methods using CsCl and Pt(NH 3 ) 4 Cl 2 . With these materials, hydrogen evolution from water in the presence of EDTA·2Na (ethylenediamine tetraacetic acid disodium salt) under visible light irradiation (≥400 nm) was achieved.

materials

EDTA-Reduction of Water to Molecular Hydrogen Catalyzed by Visible-Light-Response TiO2-Based Materials Sensitized by Dawson- and Keggin-Type Rhenium(V)-Containing Polyoxotungstates