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Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9<br />

Unpublished Results<br />

isomer. The BVS calculation suggests that the four oxygen atoms are monoprotonated. We<br />

performed TGA measurements on 20a (Figure 9.52) from room temperature to 900 ° C which is<br />

fully consistent with the formula of 20a provided above.<br />

Figure 9.53 Polyhedral/ball and stick type structural representation of 20. Color scheme: Zr, As, C and WO 6 units<br />

are shown by deep green, yellow, blue, red and light green respectively.<br />

9.3.1.2 Solution NMR<br />

To complement our solid state XRD results on 20 with solution studies, we performed room<br />

temperature 1 H and 13 C NMR on 20a redissolved in H 2 O/D 2 O. The 1 H NMR (Figure 9.54)<br />

spectrum exhibits one signal at 1.70 ppm, and the 13 C NMR (Figure 9.55) spectrum exhibits two<br />

signals 24.14 and 182.03 ppm which are fully consistent with the solid state structure.<br />

209

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