Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results Figure 9.63 TGA spectrum of complex 23a. 9.3.4.1 Results and discussion The structure of [Hf 6 (µ 3 -O) 4 (OH) 4 (CH 3 COO) 5 (AsW 9 O 33 ) 2 ] 11- (23) (Figure 9.64) reveals that the novel polyanion consists of two [α-AsW 9 O 33 ] 9- anions linked by {Hf 6 (µ 3 - O) 4 (OH) 4 (H 2 O) 2 (CH 3 COO) 5 } 7+ group, resulting in an assembly of chiral C 1 symmetry. There are two types of coordination geometry present in zirconium. There are two types coordination geometry present in zirconium. The polyanion 23 is composed of two units of [α-AsW 9 O 33 ] 9- , six hafnium and five acetate groups. There are five acetate groups which are attached to the five hafnium atoms and the other hafnium does not have any acetate group. The BVS calculation suggests that the four oxygen atoms are monoprotonated. We performed TGA measurements on 219
<strong>Chapter</strong> 9 Unpublished Results 23a (Figure 9.63) from room temperature to 900 ° C which is fully consistent with the formula of 23a provided above. Figure 9.64 Polyhedral/ball and stick type structural representation of 23. Color scheme: Hf, As, C and WO 6 unit are shown by light green, yellow, blue and red respectively. 9.3.4.2 Solution NMR To complement our solid state XRD results on 23 with solution studies, we performed room temperature 1 H and 13 C NMR on 23a redissolved in H 2 O/D 2 O. 1 H NMR (Figure 9.65) spectrum exhibits one signal at 2.77 ppm, and the 13 C NMR (Figure 9.66) spectrum exhibits two signals 24.08 and 182.18 ppm which are fully consistent with the solid state structure. 220
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Synthesis, Structure and Properties
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"The greatest book of philosophy, w
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system, space group I4/m, unit cell
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Acknowledgements The accomplishment
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teaching, and Professor Maravanji S
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2.1.2 Single crystal X-ray diffract
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5.5 Conclusion…………………
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9.1.6.1 Results and discussion…
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9.3.5 Synthesis of K 12 [Hf 4 (µ 2
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Crespo………………………
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Figure 5.4 ORTEP view of the asymme
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Figure 9.6 31 P NMR of 7a in H 2 O/
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Figure 9.34 TGA spectrum of 17a…
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Figure 9.62 FTIR spectrum of 23a…
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Table 9.6 Crystal data and structur
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Chapter 4 - Jacobs University

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