Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results Table 9.1: Crystal Data and Structure Refinement for K 12 Li 16 Co 2 (H 2 O) 6 [Co 4 (H 2 O) 16 P 8 W 48 O 184 ]·54H 2 O (9 a) emp formula K 12 Li 16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 fw 13519.42 Space group (No.) Pī (2) a (Å) 15.9934(9) b (Å) 20.4843(15) c (Å) 23.6382(14) α ( o ) 106.161(3) β ( o ) 103.673(3) γ ( o ) 95.424(3) vol (Å 3 ) 7119.9(8) Z 1 Temp (°C) 173(2) wavelength (Å) 0.71073 d calcd (Mg/m3) 3.153 abs coeff (mm -1 ) 19.96 R [I > 2α(I)] 0.071 R w (all data) 0.231 153
<strong>Chapter</strong> 9 Unpublished Results 9.1.4.2 Results and discussion The polyanion [Co 4 (H 2 O) 16 P 8 W 48 O 184 ] 32- (9) (Figure 9.11) contains two pairs of cobalt ions which are incorporated in the cavity but on opposite sides (K-3 and K-7) in figure 9.12. Additionally two disordered cobalt ions in K-4 and K-5 position are occupied by 15%. Interestingly, this difference in coordination is accompanied by a distortion of the P 8 W 48 structure and this kind of distortion observed before in other transition metal complexes. The bond distances between two terminal oxygen of two P 2 W 12 units increase to 3.81 Å from their usual bond distance 2.93 Å. There are also two extra cobalt ions linked to the outside of the polyanion in K-4 and K-5 position bridging to neighboring polyanions, form a 2D network. We also performed TGA measurements on 9a from room temperature to 900 °C in order to confirm the number of crystal waters (Figure 9.10). Figure 9.11 Polyhedral/ball and stick type structural representation of 9. Color scheme: K, Co, P and WO 6 units are shown by orange, pink, blue and red respectively. 154
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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 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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