Chapter 4 - Jacobs University

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<strong>Chapter</strong> 5 Organoruthenium POM Recently, our group reported several Ru II (dmso) and Ru II (benzene) derivatives of mono-, di- and trilacunary Keggin precursors, 14 whereas the Nomiya group focussed on Wells-Dawson derivatives. 15 On the other hand, the group of Proust prepared a {Ru(p-cymene) } 2+ containing polyanion by using {Sb 2 W 22 O 74 (OH) 2 } 12- as precursor. 16 Despite the fact that P 8 W 48 has been known for over twenty years, 17 only very few metalcontaining derivatives have been reported to date. These are [Cu 20 Cl(OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )] 25- and {Ln 4 (H 2 O) 28 [KÌP 8 W 48 O 184 (H 4 W 4 O 12 ) 2 Ln 2 (H 2 O) 10 ] 13- } x (Ln = La, Ce, Pr, Nd). 18 A Cu 20 -azide derivative and a mixed-valence V 12 derivative of P 8 W 48 have also been obtained recently. 19 91
<strong>Chapter</strong> 5 Organoruthenium POM 5.2 Synthesis Preparation of 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): a sample of K 28 Li 5 [H 7 P 8 W 48 O 184 ]·92H 2 O (0.37 g, 0.025 mmol) was dissolved in aqueous 1M LiOAc/CH 3 COOH buffer solution (20mL) at pH 6.0, followed by addition of [Ru(pcymene)Cl 2 ] 2 (0.17 g, 0.28 mmol). Then the solution was heated to 80 ºC for 1h and filtered hot. After cooling to room temperature 1M KCl solution (5 mL) was added. The filtrate was allowed to evaporate in an open beaker at room temperature, resulting in a red-brown crystalline product after about two weeks. Yield: 0.19 g (49 %). IR for 3a: 1136(m), 1083(m), 1015(w), 974(sh), 925(s), 799(s), 628(s), 574(w), 528(w), 461(w), 424(w) cm -1 . Anal. found: C, 3.16; H, 1.65; P, 1.51; K, 3.61; Li, 0.79; W, 58.7; Ru, 2.51; calc for 3a: C, 3.08; H, 1.61; P, 1.59; K, 3.76; Li, 0.67; W, 57.8; Ru, 2.59. Thermal decomposition of 3a (Figigure 5.2) starts at room temperature and shows a smooth dehydration step ending in a plateau at about 280 °C. This step involves the release of ~87 water molecules [found: 10.1; calc: 10.0]. Above this temperature, we observe a slightly less regular weight loss with 3 steps up to about 690 °C. It appears that in this domain the slightly stronger bonded water ligands (e.g. K1···OH 2 , K6···OH 2 , Ru-OH 2 and W-OH 2 ) are lost (probably in this sequence) together with the four p-cymene groups [found: 4.29; calc: 4.48]. 92
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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 9 Unpublished Results Figur
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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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