Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.3.7.1 X-ray crystallography A colorless block of 26a with dimensions 0.23 x 0.08 x 0.02 mm 3 was mounted in a Hampton cryoloop for indexing and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 Kα radiation (λ = 0.71073 Å). Of the 294738 reflections collected (2θ max = 55.26°, 99.2 % complete), 21912 were unique (R int = 0.1331) and 14901 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 hafnium 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, Hf, and K atoms) and isotropic thermal parameters converged at R = 0.0578 (I > 2σ(I)) and and R w = 0.1768(all data). The data for this crystal are summarized in Table 9.9. 231
<strong>Chapter</strong> 9 Unpublished Results Table 9.9: Crystal data and structure refinement for K 14 [Hf (BW 11 O 39 ) 2 ]·21H 2 O (26a) Empirical formula H19.50 B2 Hf K7 O97.50 W22 fw 6098.17 Crystal system Triclinic Space group (No.) Pī (2) a(Å) 14.0195(4) b(Å) 18.7256(7) c(Å) 18.9881(7) α(°) 100.568(2) β(°) 92.278(2) γ(°) 103.668(2) Vol(Å 3 ) 4743.5(3) Z 2 Temp(K) 173(2) Wavelength(Å) 0.71073 d calcd (Mg/m3) 4.270 abs coeff (mm -1 ) 28.062 R [I > 2α(I)] 0.0578 R w (all data) 0.1768 232
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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 C) Keggin a-
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Chapter 4 - Jacobs University

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