Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.3.3.2 Results and discussion The structure of [{Zr(O 2 )(GeW 11 O 39 )} 2 ] 12- (22) (Figure 9.61) reveals that the novel polyanion consists of two [α-GeW 11 O 39 ] 8- anions linked by a {Zr 2 (O 2 ) 2 } 4+ group in a head-on fashion, resulting in an assembly with C i symmetry. The Zr 4+ ion is located in an antiprismatic coordination environment with eight oxygen atoms, four of them being connected to the polyanion and other four being connected to the two peroxo oxygen groups. The BVS calculation indicates that none the four oxygen atoms from the peroxo groups are protonated. We performed TGA measurements on 22a (Figure 9.60) from room temperature to 900 °C which is fully consistent with the formula of 22a provided above. Figure 9.61 Polyhedral/ball and stick type structural representation of 22. Color scheme: Zr, Ge, and WO 6 units are shown by deep green, turquoise and red respectively. 217
<strong>Chapter</strong> 9 Unpublished Results 9.3.4 Synthesis of Cs 10 Na[Hf 6 (µ 3 - O) 4 (OH) 4 (H 2 O) 2 (CH 3 COO) 5 (AsW 9 O 33 ) 2 ]·73H 2 O (23a) A 0.493 g (0.2 mmol) of Na 9 [α-AsW 9 O 33 ] was dissolved in 20 mL of 0.5 M LiH 3 COO buffer solution (pH 4.0), and then 0.128 g (0.4 mmol) of HfCl 4 was added. The solution was heated at 80 o C for 1h and filtered while hot. Then 1M CsCl (0.5 mL) solution was added after filtration. Slow evaporation at room temperature led to the appearance of white crystalline product after about one week. Evaporation was allowed to continue until the solution level approached the solid product, which was filtered off and air-dried. Yield 0.18g. (60%). IR: 1637(m), 1617(m), 1577(m), 948(m), 874(s),784(m), 729(w), 693(w), 649(w), 457(m) cm -1 . 80 78 76 74 72 70 68 66 %Transmittance 64 62 60 58 56 54 52 50 48 46 44 1800 1600 1400 1200 1000 Wavenumbers (cm-1) 800 600 Figure 9.62 FTIR spectrum of 23a. 218
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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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