Chapter 4 - Jacobs University

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<strong>Chapter</strong> 5 Organoruthenium POM Table 5.1: Crystal Data and Structure Refinement for K 12 Li 15 [{K(H 2 O)} 3 {Ru(pcymene)(H 2 O)} 4 P 8 W 49 O 186 (H 2 O) 2 ]·87H 2 O (3a) 3a emp formula C40 H248 K16 Li16 O240 P8 Ru4 W49 fw (g/mol) 14967.71 crystal system Triclinic space group (No.) Pī (2) a (Å) 19.0968(12) b (Å) 20.2604(12) c (Å) 22.6082(10) α ( o ) 101.977(3) β ( o ) 109.431(3) γ ( o ) 100.737(3) vol (Å 3 ) 7754.3(8) Z 1 temp (°C) -100 (2) d calcd (Mg m -3 ) 3.205 abs coeff. (mm -1 ) 18.628 transmission 0.5228 and 0.1665 Data / parameters 31644 /876 Goodness-of-fit on F 2 1.061 R [I > 2s(I)] 0.065 R w (all data) 0.212 95
<strong>Chapter</strong> 5 Organoruthenium POM 5.4 Results and discussion 5.4.1 Synthesis and structure The title polyanion [{K(H 2 O)} 3 {Ru(p-cymene)(H 2 O)} 4 P 8 W 49 O 186 (H 2 O) 2 ] 27- (3) was prepared by a one-pot reaction of [Ru(p-cymene)Cl 2 ] 2 with P 8 W 48 (10:1 ratio) in aqueous 1M LiOAc/CH 3 COOH buffer solution at pH 6.0. We isolated 1 in the form of its mixed potassium-lithium salt K 12 Li 15 [{K(H 2 O)} 3 {Ru(p-cymene)(H 2 O)} 4 P 8 W 49 O 186 (H 2 O) 2 ]·87H 2 O (3a) which was structurally characterized by single crystal X-ray diffraction. The extra equivalent of tungstate which appears in 3 is most likely formed in situ by decomposition of a very minor fraction of the P 8 W 48 precursor. Compound 1a has been fully characterized in the solid state by single-crystal XRD, TGA-DSC, IR and elemental analysis. Figure 5.3 Combined polyhedral/ball-and-stick representation of 3. The color code is as follows: WO 6 (violet, blue), PO 4 (yellow), Ru (green), O (red), C (black), K (orange). No hydrogens shown for clarity. Note that the two blue WO 6 octahedra and the two adjacent potassium ions have 50% occupancy each. 96
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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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Curriculum Vitae SIB SANKAR MAL Dep
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EDUCATION PhD Jacobs University (20
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POSTER, ORAL PRESENTATION 1. Poster
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6. “Two Iron-Containing Tungstoge
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Appendix
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Appendix
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