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Chapter 3 Unpublished Results Figure 3.42. 1 H-NMR spectrum of KCsNa-23 dissolved in D 2 O. 3.B.3.5. Conclusions The lanthanide-substituted polyoxometalates [{Ln(-CH 3 COO)(H 2 O) 2 (-GeW 11 O 39 )} 2 ] 12− (Ln = Eu (21), Gd (22), Lu(23)) have been synthesized and characterized by IR spectroscopy and elemental analysis. Single-crystal X-ray analyses were carried out on the potassium salts of 21 and 22 while on the mixed-potassium cesium of 23. The head-on dimer 21–23 consist of two (-GeW 11 O 39 ) 8− fragments connected by a lanthanide-acetate dimer, (Ln 2 (- CH 3 COO) 2 (H 2 O) 4 ) 4+ . Each Ln 3+ ion is eight-coordinated in a distorted square-antiprismatic fashion. The solution properties of the diamagnetic derivatives (Lu analogue) by 183 W, 13 C NMR and 1 H NMR spectroscopy were also investigated. 143
Chapter 3 Unpublished Results 3.B.3.6. 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) 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) D.-L. Long, E. Burkholder, L. Cronin, Chem. Soc. Rev. 2007, 36, 101; i) D.-L. Long, R. Tsunashima, L. Cronin, Angew. Chem. 2010, 122, 1780, Angew. Chem. Int. Ed. 2010, 49, 1736. [2] a) K. Wassermann, M. H. Dickman, M. T. Pope, Angew. Chem., Int. Ed. Engl. 1997, 36, 1445; b) M. Sadakane, M. H. Dickman, M. T. Pope, Angew. Chem., Int. Ed. Engl. 2000, 39, 2914; c) M. Sadakane, M. H. Dickman, M. T. Pope, Inorg. Chem. 2001, 40, 2715; d) Q. H. Luo, R. C. Howell, M. Dankova, J. Bartis, C. W. Williams, W. D. Horrocks, V. G. Young, A. L. Rheingold, L. C. Francesconi, Inorg. Chem. 2001, 40, 1894 ; e) G. L. Xue, J. Vaissermann, P. Gouzerh, J. Clust. Sci. 2002, 13, 409 ; f) Q. H. Luo, R. C. Howell, J. Bartis, M. Dankova, W. D. Horrocks, A. L. Rheingold, L. C. Francesconi, Inorg. Chem. 2002, 41, 6112; g) M. Sadakane, M. H. Dickman, M. T. Pope, Angew. Chem. 2000, 112, 3036; Angew. Chem. Int. Ed. 2000, 39, 2914; h) P. Mialane, L. Lisnard, A. Mallard, J. Marrot, E. Antic-Fidancev, P. Aschehoug, D. Vivien, F. Sécheresse, Inorg. Chem. 2003, 42, 2102. 144
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