Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results coordinates, anisotropic thermal parameters (W, Y, Si, and K atoms) and isotropic thermal parameters converged at R = 0.0563 (I > 2σ(I)) and and R w = 0.1450 (all data). In the final difference map the deepest hole was -3.4 e - Å-3 and the highest peak 3.9 e - Å-3. The data for this crystal are summarized in Table 9.6. Table 9.6: Crystal data and structure refinement for K 13 [Y(SiW 11 O 39 ) 2 ]·25H 2 O (19a) Empirical formula H50 K13 O103 Si2 W22 Y fw 6396.49 Crystal system Triclinic Space group (No.) Pī (2) a(Å) 13.6252(3) b(Å) 19.6239(10) c(Å) 20.4279(7) α(°) 110.496(2) β(°) 105.399(2) γ(°) 98.506(2) Vol(Å 3 ) 4754.9(3) Z 2 Temp (K) 173(2) Wavelength (Å) 0.71073 d calcd (Mg/m3) 4.468 abs coeff (mm -1 ) 27.809 R [I > 2α(I)] 0.0563 R w (all data) 0.1672 203
<strong>Chapter</strong> 9 Unpublished Results 9.2.5.2 Results and discussion The polyanion [Y(SiW 11 O 39 ) 2 ] 13- (19) (Figure 9.49) is composed of one yttrium and two units of [α-SiW 11 O 39 ] 8- . The compound 19a was characterized in the solid state by single-crystal XRD, TGA-DSC, and IR as well as in solution by 89 YNMR. The structure contains an yttrium sandwiched between two [α-SiW 11 O 39 ] 8- units. The central Y 3+ is of antiprismatic geometry. It is coordinated by eight oxygen atoms, four from each [α-SiW 11 O 39 ] 8- lacunary species (Figure 9.48). The yttrium oxygen bond distances range from 2.3 Å to 2.42Å .The bond angle between two adjacent oxygen atoms of the silicotungstate precursor is 74.2°. We performed TGA measurements on 19a (Figure 9.48) from room temperature to 900 °C which is fully consistent with the formula of 19a provided above. 204
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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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