Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results Figure 9.60 TGA spectrum of complex 22a. 9.3.3.1 X-ray crystallography A yellow crystal of 22a with dimensions 0.33 x 0.13 x 0.07 mm3 was mounted in a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 227743 reflections collected (2θ max = 55.86°, 98.4% complete), 12649 were unique (R int = 0.0975) and 9638 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, Zr, Ge, and K atoms) and isotropic thermal parameters converged at R = 0.0502 (I > 2σ(I)) and and R w = 0.1518(all data). 215
<strong>Chapter</strong> 9 Unpublished Results The data for this crystal are summarized in Table 9.7. Table 9.7: Crystal data and structure refinement for K 12 [{Zr(O 2 )(GeW 11 O 39 )} 2 ]·25H 2 O (22a) Empirical formula H58 Ge2 K8 O111 W22 Zr2 fw 6519.58 Crystal system Triclinic Space group (No.) Pī (2) a(Å) 11.5114(4) b(Å) 12.6316(6) c(Å) 19.0236(10) α(°) 91.249(3) β(°) 92.891(2) γ(°) 103.628(2) Vol (Å 3 ) 2683.3(2) Z 1 Temp (K) 173(2) Wavelength (Å) 0.71073 d calcd (Mg/m3) 4.035 abs coeff (mm -1 ) 24.632 R [I > 2α(I)] 0.0502 R w (all data) 0.1518 216
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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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