Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.2.1.1 X-ray crystallography A colorless needle of 15a with dimensions 0.38 x 0.10 x 0.03 mm 3 was mounted in a Hampton cryoloop for indexing and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 278364 reflections collected (2θmax = 46.5°, 99.6% complete), 7672 were unique (Rint = 0.1853) and 19584 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, As, Na and Cs atoms) and isotropic thermal parameters converged at R = 0.1057 (I > 2σ(I)) and and Rw = 0.2782 (all data). In the final difference map the deepest hole was -3.1e - Å -3 and the highest peak 4.0 e - Å -3 . The data for this crystal are summarized in Table 9.2. 169
<strong>Chapter</strong> 9 Unpublished Results Table 9.2: Crystal data and structure refinement for Na 23 [Cs{Y(B-a-AsW 9 O 33 )} 4 ]·58H 2 O (15a) Empirical formula H 116 As 4 Cs Na 23 O 190 W 36 Y 4 fw 11092.53 Crystal system Tetragonal Space group (No.) P4/ncc (126) a(Å) 28.5314(10) b(Å) 28.5314(10) c(Å) 26.2868(17) Vol(Å 3 ) 21398.5(17) Z 4 Temp (K) 173(2) Wavelength (Å) 0.71073 d calcd (Mg/m3) 3.443 abs coeff (mm -1 ) 21.265 R [I > 2α(I)] 0.1057 R w (all data) 0.3316 170
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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 (48) Mizuno,
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Chapter 2 Experimental 2.2.3 Synthe
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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 3 The Wheel-Shaped Cu 20 20
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Chapter 9 Unpublished Results 9.3.7
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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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