Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.3.2.1 Results and discussion The structure of [{Zr(O 2 )(SiW 11 O 39 )} 2 ] 12- (21) (Figure 9.58) reveals that the novel polyanion consists of two [α-SiW 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 of the four oxygen atoms from the peroxo groups are protonated. We performed TGA measurements on 21a (Figure 9.57) from room temperature to 900 ° C which is fully consistent with the formula of 21a provided above. Figure 9.58 Polyhedral/ball and stick type structural representation of 21. Color scheme: Zr, Si, peroxo and WO units are shown by deep green spheres, green tetrahedra, red spheres and red octahedra, respectively. 213
<strong>Chapter</strong> 9 Unpublished Results 9.3.3 Synthesis of K 12 [{Zr(O 2 )(GeW 11 O 39 )} 2 ]·25H 2 O (22a) A 0.644g (0.2 mmol) sample of K 8 [α-GeW 11 O 39 ]·14H 2 O was dissolved in 20 mL 1M KCH 3 COO buffer solution (pH 4.8), and then 0.046g (0.2 mmol) of ZrCl 4 was added. During the reaction 5- 10 drops of 30% H 2 O 2 was introduced into the reaction mixture. The solution was heated to 80 o C for 30 min and filtered while still hot. Then, 6 drops of 1M KCl were added after filtration. Slow evaporation at room temperature led to the appearance of yellowish crystalline product within one day. The evaporation was allowed to continue until the solution level approached the solid product which was then collected by filtration and air dried. Yield: 0.46g (64.15%). IR: 959(s), 872(s), 809 (m), 770(m), 712(w), 670(sh), 530(w) ,453(m), 422(sh) cm -1 . 60 55 50 45 %Transmittance 40 35 30 25 20 15 1000 900 800 700 Wavenumbers (cm-1) 600 500 Figure 9.59 FTIR spectrum of 22a. 214
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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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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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