The synthesis and crystal structure of a Dawson-type dirhenium(V)-oxido-bridged polyoxotungstate are described. 2-in water, followed by crystallization from an aqueous HCl solution in the dark. Single-crystal X-ray structure analysis revealed that the dimeric dirhenium(V)-oxido-bridged structure has overall C 2h symmetry. Characterization of K-1 was also accomplished by elemental analysis, TG/DTA, and FTIR, UV/Vis absorption, ESR, and solution 31 P NMR spectroscopy. Furthermore, the black-purple compound K-1 was grafted onto a TiO 2 surface by electrostatic binding to give TiO 2 with a cationic quaternary ammonium moiety (1-grafted TiO 2 ). Elemental analysis of 1-
The synthesis and characterization of a Keggin-type mono-rhenium(V)- substituted polyoxotungstate are described. The dimethylammonium salt [Me2NH2]4[PW11ReVO40] was obtained as analytically pure homogeneous black-purple crystals by reacting mono-lacunary Keggin polyoxotungstate with [ReIVCl6]2- in water, followed by crystallization from acetone at ca. 5 °C. Single-crystal X-ray structural analysis of [PW11ReVO40]4- revealed a monomeric structure with overall Td symmetry. Characterization of [Me2NH2]4[PW11ReVO40] was also accomplished by elemental analysis, magnetic susceptibility, TG/DTA, FTIR, UV-vis, diffuse reflectance (DR) UV-vis, and solution 31P-NMR spectroscopy. Furthermore, [PW11ReVO40]4- and the Dawson-type dirhenium(V)-oxido-bridged polyoxotungstate [O{ReV(OH)(α2-P2W17O61)}2]14- were supported onto anatase TiO2 surface by the precipitation methods using CsCl and Pt(NH3)4Cl2. 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.
A Dawson-Type Dirhenium(V)-Oxido-Bridged Polyoxotungstate: X-Ray Crystal Structure and Hydrogen Evolution from Water Vapor under Visible Light Irradiation. -The new polyoxotungstate (III) crystallizes in the triclinic space group P1 with Z = 1 (single crystal XRD). The dimeric dirhenium(V)-oxido-bridged structure has overall C2h symmetry. (III) is grafted onto a TiO2 surface by electrostatic binding to give TiO2 with a cationic quaternary ammonium moiety (III-grafted TiO2), in which seven K + ions are replaced by Si(CH 2 ) 3 cations. (III)-grafted TiO 2 is able to produce H2 from water vapor under visible light irradiation (>400 nm). -(KATO*, C. N.; HARA, K.; HATANO, A.; GOTO, K.; KURIBAYASHI, T.; HAYASHI, K.; SHINOHARA, A.; KATAOKA, Y.; MORI, W.; NOMIYA, K.; Eur. J. Inorg. Chem.
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