Chapter 4 - Jacobs University

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<strong>Chapter</strong> 9 Unpublished Results 9.2.5 Synthesis of K 13 [Y(SiW 11 O 39 ) 2 ]·25H 2 O (19a) A 0.644 g (0.2 mmol) sample of K 8 [SiW 11 O 39 ]∙13H 2 O was dissolved in 20 mL of 1M KCH 3 COO (4.8 pH) and then reacted with 0.0667 g (0.2 mmol) YCl 3 ∙6H 2 O. This solution was heated to 80 °C for 60 minutes. After that, 2 mL of 30% hydrogen peroxide (1 mmol) was added to the hot solution. After heating, the solution was then filtered in hot. The resulting solution was layered with 0.5 ml of 1 M CsCl. The filtrate was allowed to evaporate in an open beaker at room temperature. After about three days a white crystalline product started to appear. After that, the evaporation was allowed to continue until the solution level approached the solid product which was then collected by filtration and air dried. Yield: 0.489g (39%). IR (cm -1 ): 1035(w), 1005(sh), 956(s), 908(vs),7 60(s), 725, 625 (sh), 540, 520, 472(sh), 430(sh). Figure 9.47 FTIR spectrum of 19a. 201
<strong>Chapter</strong> 9 Unpublished Results Figure 9.48 TGA spectrum of complex 19a. 9.2.5.1 X-ray crystallography A block like crystal of 19a with dimensions 0.23 x 0.08 x 0.03 mm3 was mounted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 281597 reflections collected (2θ max = 24.87°, 99.4% complete), 16397 were unique (R int = 0.1712) and 5632 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 202
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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 (17) Evans,
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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 2 Experimental 2.3Reference
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Chapter 3 The Wheel-Shaped Cu 20 in
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Chapter 3 The Wheel-Shaped Cu 20 Cu
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Chapter 9 Unpublished Results Figur
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