Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 3 Published Results Figure 3.18. Thermograms of Na-11 and NaEu-12. 3.A.2.5. Conclusions We have successfully synthesized the V-shaped, lanthanide-containing isopolyanions [Sm 2 (H 2 O) 10 W 28 O 93 (OH) 2 ] 14− (11) and [Eu 2 (H 2 O) 10 W 28 O 93 (OH) 2 ] 14− (12) which were structurally characterized by IR spectroscopy, single-crystal X-ray diffraction, TGA and elemental analysis. The polyanions 11 and 12 were synthesized in aqueous acidic medium by simple one-pot reaction of sodium tungstate with a lanthanide(III) salt and then isolated as the hydrated sodium and mixed sodium-europium salts Na-11 and NaEu-12, respectively. Polyanions 11 and 12 are composed of a 28-tungsten isopolyanion unit {W 28 } which consists of two undeca {W 11 } and one hexa {W 6 } fragments coordinated to two external lanthanide ions bearing five terminal aqua ligands. Polyanions 11 and 12 represent only the second 91
Chapter 3 Published Results example of lanthanide-containing isopolyanions and they contain exposed lanthanide centers with labile terminal aqua ligands. The latter represent good candidates for ligand substitution with other mono- or polydentate ligands (e.g. carboxylic acids, amino acids), including chiral ones, providing a potential for catalysis. We also try to isolate 11 and 12 as lipophilic alkyl ammonium salts which would open the door for organic catalysis reactions. 3.A.2.6. References [1] a) M. T. Pope in Heteropoly and Isopoly Oxometalates, Springer-Verlag, Berlin, 1983; b) M. T. Pope, A. Müller, 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., Int. Ed. Engl. 1995, 34, 2328; e) C. Hill in Polyoxometalates: Chemical Reviews, 1998 (special thematic issue on polyoxometalates); f) 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; g) T. Yamase, M. T. Pope in Polyoxometalate Chemistry for Nano-Composite Design (Eds.: T. Yamase, M. T. Pope), Kluwer: Dordrecht, The Netherlands, 2002; h) G. R. J. Choppin, Nucl. Radiochem. Sci. 2005, 6, 1. [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. [3] N. Mizuno, M. Misono, Chem. Rev. 1998, 98, 199. 92
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