Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.1.5 Synthesis of K 9 Li 27 [Ni 4 (H 2 O) 16 (P 8 W 48 O 184 )(WO 4 ) 2 ]·44H 2 O(10a) A sample of NiCl 2·6H 2 O (0.0784 g, 0.33 mmol) was dissolved in 0.5 M LiCH 3 COO buffer solution (20 mL) at pH 4.0 then K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.187 g, 0.0125 mmol) was added. Then 6-10 drops of 30% H 2 O 2 was added to that solution. The solution was heated to 80 °C for 1h and filtered hot. The filtrate was allowed to evaporate in an open beaker at room temperature. After 2-3 days a green crystalline product started to appear. After that, the evaporation was allowed to continue until the solution level approached the solid product which was then collected by filtration and air dried. Yield: 0.163g (79%). IR: 1139(s), 1088(s), 1020(m), 933(sh), 918(sh), 813(s), 685(s), 468 (sh) cm -1 . 50 45 40 %Transmittance 35 30 25 20 15 10 1200 1100 1000 900 800 Wavenumbers (cm-1) 700 600 500 Figure 9.12 FT-IR spectrum of 10a. 155
<strong>Chapter</strong> 9 Unpublished Results Figure 9.13 TGA analysis of 10a. 9.1.5.1 Results and discussion The polyanion [Ni 4 (H 2 O) 16 (P 8 W 48 O 184 )(WO 4 ) 2 ] 32- (10) (Figure 9.14) contains two pairs of nickel ions which are incorporated in the cavity but on opposite sides. The extra equivalent of tungstate which appears in 10 is most likely formed in situ by decomposition of a very minor fraction of the P 8 W 48 precursor. Compound 10a has been fully characterized in the solid state by singlecrystal XRD, TGA-DSC, and IR. The molecular structure of 10 reveals that the novel polyanion has four [Ni(H 2 O) 4 ] 2+ groups 156
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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 1 Introduction heteropolyan
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Chapter 1 Introduction 1.3 Structur
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Chapter 1 Introduction C) Keggin a-
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Chapter 1 Introduction shows no suc
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Chapter 1 Introduction α-[P 2 W 18
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Chapter 1 Introduction Figure 1.7 B
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Chapter 1 Introduction [P 2 W 18 O
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Chapter 1 Introduction 1.5.3 Medici
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Chapter 2 Experimental 2.2.3 Synthe
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Chapter 2 Experimental 2.2.11 Synth
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Chapter 2 Experimental 2.3Reference
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Chapter 3 The Wheel-Shaped Cu 20 in
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Chapter 3 The Wheel-Shaped Cu 20 3.
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Chapter 3 The Wheel-Shaped Cu 20 Cu
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Chapter 9 Unpublished Results Table
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Curriculum Vitae SIB SANKAR MAL Dep
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EDUCATION PhD Jacobs University (20
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POSTER, ORAL PRESENTATION 1. Poster
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6. “Two Iron-Containing Tungstoge
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Appendix
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Appendix
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