Unprecedented {Fe14 }/{Fe10 } polyoxotungstate-based nanoclusters with efficient photocatalytic H2 evolution activity: synthesis, structure, magnetism, and electrochemistrySingh, V., Chen, Z., Ma, P., Zhang, D., Drew, M. G. B., Niu, J. and Wang, J. (2016) Unprecedented {Fe14 }/{Fe10 } polyoxotungstate-based nanoclusters with efficient photocatalytic H2 evolution activity: synthesis, structure, magnetism, and electrochemistry. Chemistry- A European Journal, 22 (31). pp. 10983-10989. ISSN 1521-3765 Full text not archived in this repository. It is advisable to refer to the publisher's version if you intend to cite from this work. See Guidance on citing. To link to this item DOI: 10.1002/chem.201601453 Abstract/SummaryNovel Fe10 and Fe14 clusters [Rb9Cs4H37Fe10O34(A-α-PW9O31)3(OH)3]⋅36 H2O (1) and [H3Rb3Fe14(OH)12(PO4)6(B-α-PW9O34)2]⋅21 H2O (2) were synthesized and characterized in the solid state by single-crystal X-ray diffraction, IR spectroscopy, thermogravimetric analysis (TGA), and magnetic studies, and in solution by electrochemistry. Cluster 1 is a decameric FeIII polyanionic cluster encapsulating a cesium atom in the center. Cluster 2 is a unique tetradecanuclear FeIII sandwich structure with phosphate-linked units featuring two quasicubic Fe4O4 moieties. Apparently, 2 has the highest nuclearity of all known FeIII sandwich-type polyoxometalate clusters. Clusters 1 and 2 also act as photocatalysts with platinum as cocatalyst for H2 evolution from light-driven water splitting. Changes in the cyclovoltammetric patterns with variations in pH were observed for 1 and 2, most likely due to intermolecular interactions among the high-nuclearity FeIII cluster cores and subsequent changes in the acid–base properties of the two reduced POMs. Magnetic studies provide evidence of antiferromagnetic interactions in 1 and 2. TGA showed that complexes 1 and 2 decompose between 580 and 590 °C.
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