Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 3 Unpublished Results [3] a) N. Haraguchi, Y. Okaue, T. Isobe, Y. Matsuda, Inorg. Chem. 1994, 33, 1015; b) L.-H. Bi, U. Kortz, S. Nellutla, A. C. Stowe, J. van Tol, N. S. Dalal, B. Keita, L. Nadjo, Inorg. Chem. 2005, 44, 1015. [4] C. Rocchiccioli-Deltcheff, M. Fournier, R. Franck, R. Thouvenot, Inorg. Chem. 1893, 22, 207. [5] a) U. Kortz, J. Clust. Sci. 2003, 14, 205; b) P. Mialane, A. Dolbecq, E. Riviere, J. Marrot, F. Sécheresse, Eur. J. Inorg. Chem. 2004, 33. [6] M. Ibrahim, S. S. Mal, B. S. Bassil, A. Banerjee, U. Kortz, Inorg. Chem. 2011, 50, 956. [7] F. Hussain, A. Degonda, S. Sandriesser, T. Fox, S. S. Mal, U. Kortz, G. R. Patzke, Inorg. Chim. Acta, 2010, 363, 4325. 145
Chapter 4 Unpublished Results Chapter IV Mixed Lanthanide/d‐Transition Metal Containing POMs Ring opening in the cyclic Phosphotungstate [Fe16O2(OH)23(H2O)9(P8W49O189)Ln4(H2O)20] 11− 4.1. Introduction Polyoxometalates (POMs) represent a class of discrete structurally and chemically diverse nanosized metal-oxygen molecular anions (hence the ‘oxometalate’ terminology). 1a Due to this diversity, POMs have acquired interesting chemical and physical properties useful for applications in fields such as photochemistry, clinical chemistry, magnetism, catalysis and materials science. 1-2 Phosphotungstates are part of a subclass of POMs known as heteropolytungstates where the metal is tungsten (VI) and the ‘heterogroup’ is phosphate. The majority of known phophotungstate structures are based on the classical Keggin [PW 12 O 40 ] 3− and Wells-Dawson [P 2 W 18 O 62 ] 6− types; the Keggin type having one heterogroup and the Wells-Dawson type having two. The Wells-Dawson type phosphotungstates are known to have distinct chemical behaviour compared to the Keggin type ones, although some common properties arise for both. 1a Mono-, tri-, and hexa-vacant species of the Wells-Dawson molecule [P 2 W 18 O 62 ] 6− (P 2 W 18 ) can be formed and isolated in aqueous solution depending on the pH and countercations present during their synthesis. The monovacant anion [P 2 W 17 O 61 ] 10− (P 2 W 17 ) is isolated as a potassium salt by hydrolysis of P 2 W 18 at pH 6-7 using KHCO 3 . The trivacant anion [P 2 W 15 O 56 ] 12− (P 2 W 15 ) is however formed by hydrolysis of P 2 W 18 using Na 2 CO 3 without the presence of potassium at pH 9-10, and is isolated as a sodium salt. Finally, the hexavacant anion [H 2 P 2 W 12 O 48 ] 12− (P 2 W 12 ) is formed by interaction of P 2 W 18 with the base (tris-hydroxymethylaminomethane) and is isolated as a potassium salt. 1f,3 Although P 2 W 12 , 146
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