Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results Table 9.5: Crystal data and structure refinement for K 12 [{Y(CH 3 COO)GeW 11 O 39 } 2 ]·37H 2 O(18a) Empirical formula C 4 H 80 Cs Ge 2 K 11 O 119 W 22 Y 2 fw 6963.39 Crystal system Monoclinic Space group (No.) P2 1 /c (14) a(Å) 19.9920(5) b(Å) 12.5816(3) b(Å) 21.0585(4) α(°) 90 β(°) 111.40(10) γ(°) 90 Vol(Å 3 ) 4931.68(19) Z 2 Temperature (K) 173(2) Wavelength (Å) 0.71073 d calcd (Mg/m 3 ) 4.689 abs coeff (mm -1 ) 28.268 R [I > 2α(I)] 0.0593 R w (all data) 0.1862 195
<strong>Chapter</strong> 9 Unpublished Results 9.2.4.2 Results and discussion The polyanion [{Y(CH 3 COO)GeW 11 O 39 } 2 ] 12 - (18) (Figure 9.42) consists of two [a-GeW11 O 39 ] 8- anion linked by a [{(CH 3 COO)(H 2 O) 2 Y} 2 ] 4+ group in head to head fashion which results in a dimeric compound with C 2h symmetry. The compound 18a was fully characterized in the solid state by single-crystal XRD, TGA-DSC, and IR as well as in solution by 1 H, 13 C, 89 Y and 183 WNMR. The acetate molecules are bound to the Y 3+ ions in rather unexpected fashion. In this polyanion, each Y 3+ ion has completed 8 coordination numbers by bonding with 8 oxygen atoms. Out of these eight oxygen atoms four oxygen atoms are connected to the Keggin fragment. Other three oxygen atoms are part of acetate groups and remaining one coordination bonds is occupied with water molecule. The bond angle of ÐO-Y-O is 65.19° with the two oxygen atoms from two different acetate acetate groups and bond angle of ÐO-Y-O is 53.43° with two oxygen atoms from same acetyl group and the bond distance of 2.42 Å with one acetyl oxygen atoms, 2.46 Å with two other acetyl oxygen atoms and has on an average 2.27 Å - 2.32 Å bond distance with oxygen atoms from keggin fragments [a-GeW 11 O 39 ] 8- . Encapsulated Y 3+ atoms are also bonded with one water molecule with bond distance of 2.39 Å. We performed TGA measurements on 17a (Figure 9.41) from room temperature to 900 °C which is fully consistent with the formula of 17a provided above. 196
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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 2.2.11 Synth
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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 Figur
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Appendix
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6. “Two Iron-Containing Tungstoge
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Chapter 4 - Jacobs University

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