Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.1.3.1 Results and discussion The polyanion [Cu 20 N 3 (OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )] 25- (8)(Figure 9.8) is unprecedented in structure, size, and composition. This is isostructural with [Cu 20 Cl(OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )] 25- , published in 2005 by Kortz group. Instead of Cl - we successfully incorporated N - 3 , which acts as a template. The structure of the wheel-shaped [H 7 P 8 W 48 O 184 ] 33- precursor is maintained in 1 and the cavity is filled with a highly symmetrical copper-hydroxo cluster. The Cu 20 Br cluster in 8 is composed of only three structurally unique types of copper ions. All 20 copper centers are bridged to neighboring copper ions by m 3 -oxo ligands to give a highly symmetrical, cage-like assembly. Based on bond valence sum calculations all 24 bridging oxygen atoms are monoprotonated. The coordination numbers and geometries of three types of Cu are different from each other and the octahedral Cu exhibits Jahn–Teller distortion with axial elongation. Figure 9.8 Polyhedral/ball and stick type structural representation of 8. Color scheme: Cu, P and WO 6 units are shown by turquoise, blue and red respectively. 149
<strong>Chapter</strong> 9 Unpublished Results 9.1.4 Synthesis of K 12 Li 16 Co 2 (H 2 O) 6 [Co 4 (H 2 O) 16 P 8 W 48 O 184 ]·54H 2 O (9a) A sample of CoCl 2·6H 2 O (0.0785 g, 0.33 mmol) was dissolved in 1M LiCH 3 COO buffer solution (20 mL) at pH 5.3 then K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.187 g, 0.0125 mmol) was added. 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 2-3days a red-pink 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: 0.13g (73.86 %). IR : 1136(s), 1083(s), 1017(m), 931(sh), 911(sh), 793(s), 676(s), 525(w), 462 (w) cm -1 . 75 70 65 60 %Transmittance 55 50 45 40 35 30 25 1200 1100 1000 900 800 Wavenumbers (cm-1) 700 600 500 Figure 9.9 FT-IR spectrum of 9a. 150
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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 1 Introduction (17) Evans,
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Chapter 1 Introduction (48) Mizuno,
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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 Fi
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Chapter 3 The Wheel-Shaped Cu 20 Cu
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Chapter 3 The Wheel-Shaped Cu 20 20
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Chapter 9 Unpublished Results Table
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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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