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Chapter 3 Unpublished Results Figure 3.39. Thermograms of K-21 – KCsNa-23. The diamagnetic derivative (Lu analogue) allows us to investigate the stability of the polyanion 23 in solution by 183 W, 13 C NMR and 1 H NMR spectroscopy. The samples of the KCsNa-23 were redissolved in H 2 O/D 2 O to perform 183 W and 13 C NMR while in D 2 O to perform 1 H NMR spectroscopy. The 183 W NMR spectrum shows six separated peaks in an intensity ratio of 4:4:2:4:4:4 (see Figure 3.40) at -74.9, -85.5, -100.6, -111.2, -142.5, -148.7 ppm. The 13 C NMR spectrum of polyanion 23 shows two signals at 23.2 and 181.3 ppm (see Figure 3.41), which is similar to the 13 C NMR spectrum of [{Y(R- SbW 9 O 31 (OH) 2 )(CH 3 COO)(H 2 O)} 3 (WO 4 )] 17− , 6 and the 1 H NMR spectrum shows a singlet at 1.7 ppm (see Figure 3.42). Addition of free acetate to the polyanion solution did not result in additional 13 C or 1 H NMR signals, indicating that the acetate linkers in the polyanion appear to be labile. As a result the dimeric structure of 23 is expected to break down and the observed NMR spectra may indeed correspond to the monomeric decomposition product. Other 141
Chapter 3 Unpublished Results techniques (e.g. mass spectrometry) are needed to confirm this point. The situation is probably analogous for the structural analogue [{Y(-CH 3 COO)(H 2 O) 2 (-GeW 11 O 39 )} 2 ] 12− . 7 Figure 3.40. 183 W-NMR spectrum of KCsNa-23 dissolved in H 2 O/D 2 O. Figure 3.41. 13 C-NMR spectrum of KCsNa-23 dissolved in H 2 O/D 2 O. 142
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