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Chapter 3 Unpublished Results Figure 3.36. 89 Y-NMR of Na-17 dissolved in H 2 O/ D 2 O. 3.B.2.5. Conclusions The mono- and di-lanthanide(III) tungstoantimonates(III) [Ln(H 2 O) 3 Sb 2 W 21 O 72 (OH))] 10− (Ln = Yb (15), Lu(16), Y(17)) and [Ln 2 (H 2 O) 6 Sb 2 W 20 O 70 )] 8− (Ln = Yb (18), Lu(19), Y(20)) have been structurally characterized in the solid state by IR spectroscopy, single-crystal XRD, TGA and elemental analyses. Polyanions 15–20 were synthesized in simple, one-pot reactions of Ln 3+ ions with the trilacunary polyanion precursor SbW 9 or the Sb 2 W 22 precursor. Polyanions 15–20 crystallize as sodium salts in the triclinic system, space group P1̅. The structure of 15–17 comprises the Sb 2 W 20 fragment with one incorporated Ln 3+ ion, whereas two ions of 18–20. Different synthetic strategies were needed to deliberately and selectively prepare mono- and di-lanthanide derivatives of Sb 2 W 20 . In this context it was the pH a crucial 131
Chapter 3 Unpublished Results parameter as well-known in the synthesis of polyoxometalates using the trilacunary polyanion precursor SbW 9 . The terminal, labile water ligands in 15–20 are of interest for structural modifications and applications. We currently explore aqua ligand substitution for other monoand polydentate exogenous ligands, including chiral ones, and we envision potential applications in Lewis acid catalysis. Efforts to isolate lipophilic salts of 15–20 in order to study their catalytic properties in organic media are also underway. 3.B.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., 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) E. V. Chubarova, M. H. Dickman, B. Keita, L. Nadjo, M. Mifsud, I. W. C. E. Arends, U. Kortz, Angew. Chem., 2008, 47, 9542; b) N. V. Izarova, R. Ngo Biboum, B. Keita, M. Mifsud, I. W. C. E. Arends, G. B. Jameson, U. Kortz, Dalton Trans. 2009, 9385; c) N. V. Izarova, M. H. Dickman, R. Ngo Biboum, B. Keita, L. Nadjo, V. Ramachandran, N. S. Dalal, U. Kortz, 132
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