Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.3.6.1 X-ray crystallography A yellow block of 22a with dimensions 0.28 x 0.17 x 0.08 mm 3 was mounted in a Hampton cryoloop for indexing and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 157193 reflections collected (2θ max = 56.14°, 99.2 % complete), 12952 were unique (R int = 0.0994) and 9964 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, Hf, Si, K, and Rb atoms) and isotropic thermal parameters converged at R = 0.0589 (I > 2σ(I)) and and R w = 0.1885(all data). The data for this crystal are summarized in Table 9.8. 227
<strong>Chapter</strong> 9 Unpublished Results Table 9.8: Crystal data and structure refinement for K 8 Rb 4 [{Hf(O 2 )(SiW 11 O 39 )} 2 ]·20H 2 O (25a) Empirical formula H44 Hf2 K5 O150 Rb3 Si2 W22 fw 7439.59 Crystal system Triclinic Space group (No.) Pī (2) A(Å) 11.5111(6) b(Å) 12.5996(7) c(Å) 19.0734(9) α(°) 91.487(3) β(°) 92.993(3) γ(°) 103.241(3) Vol(Å 3 ) 2687.1(2) Z 1 Temp (K) 173(2) Wavelength (Å) 0.71073 d calcd (Mg/m 3 ) 4.598 abs coeff (mm -1 ) 27.538 R [I > 2α(I)] 0.0589 R w (all data) 0.1885 228
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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 4 - Jacobs University

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