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Amal H. Ismail Ph.D. Thesis Figure 3.23. Polyhedral (left) and ball-and-stick (right) representation of [La 2 (H 2 O) 8 As 2 W 19 O 67 (H 2 O)] 8− (14). The color code is the same as in Figure 3.21, and La (blue). ..................................................................................................................................... 105 Figure 3.24. Polyhedral representation of 14 forming a 1D chain in the solid state. The color code is the same as in Figure 3.23. ......................................................................................... 106 Figure 3.25. IR spectra of Na-14 (top) and its cerium analogue (bottom)............................ 107 Figure 3.26. Polyhedral (left) and ball-and-stick (right) representations of [Sb 2 W 22 O 74 (OH) 2 ] 12− polyanion precursor (Sb 2 W 22 ). The color code is as follows: WO 6 octahedra (red) and rotated WO 6 octahedra (yellow), W (black), Sb (green), O (red). ......... 114 Figure 3.27. IR spectra of the three compounds Na-15 (blue curve), Na-16 (green curve), and Na-17 (balck curve) (from bottom to top). ............................................................................ 118 Figure 3.28. IR spectra of the three compounds Na-18 (pink line), Na-19 (balck line), and Na-20 (green line) (from bottom to top). ............................................................................... 120 Figure 3.29. Polyhedral (left) and ball-and-stick (right) representation of [Ln(H 2 O) 3 Sb 2 W 21 O 72 (OH))] 10− (Ln = Yb (15), Lu(16), Y(17)). The color code is as follows: WO 6 octahedra (red) and rotated WO 6 octahedra (yellow), W (black), Sb (green), Ln (blue), H 2 O (pink), O (red), OH (gray), the rotated triad was colored yellow for clarification. ....... 123 Figure 3.30. Polyhedral representation of 15–17 forming a dimer in the solid state. The color code is as follows: WO 6 octahedra (red), Sb (green), Ln (blue), H 2 O (pink). ....................... 124 Figure 3.31. Polyhedral (left) and ball-and-stick (right) representation of [Ln 2 (H 2 O) 6 Sb 2 W 20 O 70 )] 8− (Ln = Yb (18), Lu(19), Y(20)). The color code is the same as in Figure 3.29. ............................................................................................................................ 126 Figure 3.32. Polyhedral representation of polyanions 16-20 forming a 1D chain in the solid state. The color code is as follows: WO 6 octahedra (red), Sb (green), Ln (blue), H 2 O (pink), O (red). ....................................................................................................................................... 126 Figure 3.33. Thermograms of Na-15 – Na-17. ..................................................................... 128 xiv
Amal H. Ismail Ph.D. Thesis Figure 3.34. Thermograms of Na-18 – Na-20. ..................................................................... 128 Figure 3.35. (a) 183 W-NMR spectra of Na-16 and Na-17 (upper spectra) and (b) 183 W-NMR spectrum of Na-19 (lower spectrum). .................................................................................... 130 Figure 3.36. 89 Y-NMR of Na-17 dissolved in H 2 O/ D 2 O. .................................................... 131 Figure 3.37. IR spectra of the K-21 (blue line), K-22 (balck line), and KCsNa-23 (red line) (from bottom to top). .............................................................................................................. 137 Figure 3.38. Combined polyhedral/ball-and-stick representation of [{Ln(- CH 3 COO)(H 2 O) 2 (-GeW 11 O 39 )} 2 ] 12− (21–23). The color code is as follows: WO 6 octahedra (red), Ge (green), Ln (blue), H 2 O (pink), O (red). No hydrogen atoms shown. .................... 139 Figure 3.39. Thermograms of K-21 – KCsNa-23. ................................................................ 141 Figure 3.40. 183 W-NMR spectrum of KCsNa-23 dissolved in H 2 O/D 2 O. ............................ 142 Figure 3.41. 13 C-NMR spectrum of KCsNa-23 dissolved in H 2 O/D 2 O. .............................. 142 Figure 3.42. 1 H-NMR spectrum of KCsNa-23 dissolved in D 2 O. ........................................ 143 Figure 4.1. Combined polyhedral/ball-and-stick representation of the previously reported Fe 16 P 8 W 48 . The color code is as follows: WO 6 octahedral (red); PO 4 tetrahedral (green); W (black); Fe (yellow); O (red). ................................................................................................. 148 Figure 4.2. Combined polyhedral/ball-and-stick representation of open-ring-shaped polyanions 24 and 25. The color code is as follows: WO 6 octahedral (red); PO 4 tetrahedral (green); W (black); Fe (yellow); Ln (blue); H 2 O (pink); O (red)........................................... 153 Figure 4.3. Ball-and-stick representation of {Fe 16 O 2 (OH) 23 (H 2 O) 9 WO 3 } showing the protonation within the cleaved Fe 16 cluster and its coordination to the extra tungsten. The color code is as follows: W (black); Fe (yellow); O (red); HO as mono-protonated μ 2 -oxygen (gray); H 2 O as di-protonated μ 2 -oxygen (pink); disordered H 2 O or HO as protonated μ 2 - oxygen (turquoise).................................................................................................................. 154 xv
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