Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.2.3.1 X-ray crystallography A block crystal of 17a with dimensions 0.16 x 0.14 x 0.05 mm 3 was mounted in a Hampton cryoloop for indexing and intensity data collection at 173 K on a Bruker D8 APEX II CCD single-crystal diffractometer using Mo K α radiation (λ = 0.71073 Å). Of the 149004 reflections collected (2θ max = 57.64°, 99.2% complete), 10856 were unique (R int = 0.1383) and 13046 reflections were considered observed (I >2σ (I)). Routine Lorentz and polarization corrections were applied and an absorption correction was performed using the SADABS program (Sheldrick, G. M.; Acta Crystallogr. 2007, A64, 112). Direct methods were used to locate the tungsten and yttrium atoms (SHELXS-97). Then the remaining atoms were found from successive Fourier maps (SHELXL-97). The final cycle of refinement, including the atomic coordinates, anisotropic thermal parameters (W, Y, Si, K and Na atoms) and isotropic thermal parameters converged at R = 0.0484 (I > 2σ(I)) and and R w = 0.1350 (all data). In the final difference map the deepest hole was -3.1 e - Å-3 and the highest peak 4.6 e - Å-3. The data for this crystal are summarized in Table 9.4. 185
<strong>Chapter</strong> 9 Unpublished Results Table 9.4: Crystal data and structure refinement for K 12 [{Y(CH 3 COO)SiW 11 O 39 } 2 ]·30H 2 O (17a) Empirical formula C 4 H 66 K 10 Na 2 O 112 Si 2 W 22 Y 2 fw 6622.25 Crystal system Monoclinic Space group (No.) P2 1 /c (14) a(Å) 20.1156(8) b(Å) 12.6432(4) c(Å) 21.1275(5) α(°) 90 β(°) 110.63(10) γ(°) 90 Vol(Å 3 ) 5028.5(3) Z 2 d calcd (Mg/m 3 ) 4.374 abs coeff (mm -1 ) 26.762 Temp (K) 173(2) Wavelength (Å) 0.71073 R [I > 2α(I)] 0.0484 R w (all data) 0.1547 186
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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 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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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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