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Chapter 3 Unpublished Results We also decided to investigate the solution properties of the diamagnetic derivatives (Lu and Y analogues) by 183 W and 89 Y NMR spectroscopy. The experiments were carried out on Na-16, Na-17, Na-19, and Na-20 redissolved in H 2 O/D 2 O. Many attempts were made to produce solution NMR spectra of the diamagnetic derivatives 16, 17, 19 and 20 (Lu and Y analogues). The major difficulty was the low solubility of the compounds, since a high concentration of the polyanion (> 0.1 M) is needed in order to get good signals in the 183 W NMR spectrum. Attempts to dissolve the compounds by heating eventually lead to partial decomposition of the polyanions and showed a less number (< 12) for both 16 and 17 (Figure 3.35 (a)), and a large number (> 6) peaks in the 183 W NMR spectra of Na-19 (Figure 3.35 (b)), probably arising from a mixture of species in the solution. On the other hand, the 89 Y NMR spectrum for 17 showed a singlet at 19 ppm (Figure 3.36) which could not be assigned whether for the mono- or di-yttrium derivative of {Sb 2 W 22 }. We also tried ion exchange using Li + loaded resin, which led eventually to the total dissolution of the compounds due to the replacement of the countercations with lithium. However, the 183 W NMR spectra for 16, 17, 19 and 20 were not conclusive and gave a less number (< 6) peaks. We speculate that the ion exchange method may have stripped the Lu 3+ and Y 3+ from the polyanion framework and thus lead to partial decomposition to various side products. 129
Chapter 3 Unpublished Results (a) (b) Figure 3.35. (a) Solution 183 W-NMR spectra of Na-16 (upper spectrum) and Na-17 (lower spectrum), and (b) Na-19, all redissolved in H 2 O/D 2 O. The spectra are not conclusive and may indicate decomposition of the polyanions. 130
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