Chapter 4 - Jacobs University

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<strong>Chapter</strong> 3 The Wheel-Shaped Cu 20 Table 3.1: Crystal Data and Structure Refinement for K 12 Li 13 [Cu 20 Cl(OH) 24 (H 2 O) 12( P 8 W 48 O 184 )] ·22H 2 O (1a) 1a emp formula H92 K12 Li13 O242Cu20Cl P8 W48 fw (g/mol) 29440 crystal system tetragonal space group (No.) I4/m (87) a (Å) 26.754(3) c (Å) 21.241(3) γ ( o ) 100.737(3) vol (Å 3 ) 15202.61(4) Z 2 temp (°C) -120(2) d calcd (Mg m -3 ) 3.215 abs coeff. (mm -1 ) 19.744 transmission 0.2624 and 0.2085 Data / parameters 9102 /255 Goodness-of-fit on F 2 1.169 R [I > 2s(I)] 0.068 R w (all data) 0.179 63
<strong>Chapter</strong> 3 The Wheel-Shaped Cu 20 3.4 Results and discussion 3.4.1 Synthesis and structure Polyanion [Cu 20 Cl(OH) 24 (H 2 O) 12 (P 8 W 48 O 184 )] 25- (1) (Figures 3.2 - 3.4) crystallized as a mixed potassium-sodium salt K 12 Li 13 [Cu 20 Cl(OH) 24 (H 2 O) 12( P 8 W 48 O 184 )]·22H 2 O(1a) which crystallized in the tetragonal space group I4/m. As a result the asymmetric unit of 1 includes only 6 tungsten and 3 copper atoms (Figure 3.5). The title polyanion 1 is unprecedented in structure, size and composition. This supramolecular assembly represents the first transition metal substituted derivative of [H 7 P 8 W 48 O 184 ] 33- and it incorporates more paramagnetic ions than any other polyoxometalate known to date. [12a,b,16] The structure of the wheel-shaped [H 7 P 8 W 48 O 184 ] 33- precursor is maintained in 1 and the cavity has been filled with a highly symmetrical copper-hydroxo cluster (Figures 3.2,3.3,3.6). This emphasizes that the template effect plays an important role during formation of 1. We have shown (in disagreement with Tézé and Contant) that the oxo-groups in the cavity of the tungstophosphate precursor [H 7 P 8 W 48 O 184 ] 33- actually do interact with transition metal ions in aqueous medium, but some heating is required (Exp. Sect.). Therefore, [H 7 P 8 W 48 O 184 ] 33- can indeed be considered as a superlacunary polyanion precursor and we expect that other transition metal ions besides Cu 2+ can also be incorporated. 64
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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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Chapter 8 Collaborative Work 8.2.1
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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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