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Chapter 4 Unpublished Results 4.5. Conclusions We have synthesized two 16-iron(III)-containing phosphotungstates coordinated to four lanthanide centers and composed of an unprecedented open-ring P 8 W 49 unit, [Fe 16 O 2 (OH) 23 (H 2 O) 9 (P 8 W 49 O 189 )Ln 4 (H 2 O) 20 ] 11− (Ln = Eu (24) and Gd (25)). They are synthesized in simple, one-pot reactions of Ln(III) and Fe(III) salts with the large superlacunary polyanion precursor P 8 W 48 and isolated as hydrated mixed potassium-lithiumsodium-lanthanide salts KLiNa-24 and KLiNa-25. These salts have been studied in the solid state by IR spectroscopy, single-crystal X-ray diffraction, TGA and elemental analysis. It is apparent that the presence of lanthanide ions is a crucial parameter in the synthesis of 24 and 25. However, the mechanism cleavage of the wheel-shaped P 8 W 48 is still unclear. Attempts to synthesize the open-ring Fe 16 P 8 W 49 in the absence of lanthanides ions are still underway using different synthetic procedures. Furthermore, isolation the novel P 8 W 49 or P 8 W 48 * as new precursors, starting from either the wheel-shaped P 8 W 48 or other phosphotungstate precursors such as P 2 W 12 and P 4 W 24 will be the scope of further studies. 161
Chapter 4 Unpublished Results 4.6. References [1] a) M. T. Pope in Heteropoly and Isopoly Oxometalates, Springer-Verlag, Berlin, 1983; b) M. T. Pope, A. Müller, Angew. Chem. 1991, 103, 56, Angew. Chem. Int. Ed. Engl. 1991, 30, 34; c) M. T. Pope, A. Müller in Polyoxometalates: From Platonic Solids to Anti- Retroviral Activity (Eds.: M. T. Pope, A. Müller), Kluwer: Dordrecht, The Netherlands, 1994; d) A. Müller, H. Reuter, S. Dillinger, Angew. Chem. 1995, 107, 2505, Angew. Chem. Int. Ed. Engl. 1995, 34, 2328; e) C. Hill in Polyoxometalates: Chemical Reviews, 1998 (special thematic issue on polyoxometalates); f) J. J. Borrás-Almenar, E. Coronado, A. Müller, M. T. Pope, in Polyoxometalate Molecular Science (Eds.: J. J. Borrás-Almenar, E. Coronado, A. Müller, M. T. Pope), Kluwer: Dordrecht, The Netherlands, 2001; g) M. T. Pope, A. Müller in Polyoxometalate Chemistry: From Topology via Self-Assembly to Applications (Eds.: M. T. Pope, A. Müller), Kluwer: Dordrecht, The Netherlands, 2001; h) T. Yamase, M. T. Pope in Polyoxometalate Chemistry for Nano-Composite Design (Eds.: T. Yamase, M. T. Pope), Kluwer: Dordrecht, The Netherlands, 2002; i) D.-L. Long, E. Burkholder, L. Cronin, Chem. Soc. Rev. 2007, 36, 101; j) D.-L. Long, R. Tsunashima, L. Cronin, Angew. Chem. 2010, 122, 1780, Angew. Chem. Int. Ed. 2010, 49, 1736. [2] a) A. Mylonas, A. Hiskia, E. Papaconstantinou, J. Mol. Catalysis A: Chem. 1996, 114, 191; b) A. Hiskia, A. Troupis, E. Papaconstantinou, Int. J. Photoenergy 2002, 4, 35; c) E. Gkika, P. Kormali, S. Antonaraki, D. Dimoticali, E. Papaconstantinou, A. Hiskia, Int. J. Photoenergy 2004, 6, 227; d) A. Hiskia, A. Troupis, S. Antonaraki, E. Gkika, P. Kormali, E. Papaconstantinou, Int. J. Envir. Anal. Chem. 2006, 233; e) P. Kormali, A. Troupis, T. Triantis, A. Hiskia, E. Papaconstantinou, Catalysis Today 2007, 124, 149; f) G. R. J. Choppin, Nucl. Radiochem. Sci. 2005, 6, 1. [3] R. Contant. Inorg. Synth. 1990, 27, 108. 162
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