Chapter 4 - Jacobs University

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<strong>Chapter</strong> 3 The Wheel-Shaped Cu 20 (1.926(15) Å), Cu1-O2C3 (1.980(14) Å) and Cu1-O1Cu (1.986(14) Å) bonds. The two axial bonds are Cu1-O1C3 (2.358(16) Å) and a very long bond Cu1-O5W (2.504(17) Å) to a terminal water molecule. [19] The angle O1C3-Cu1-O5W is only 145° which reflects steric hindrance for the latter. Cu2 has square-pyramidal coordination geometry with two Cu2-O2C3 (1.922(14) Å) and two Cu2-O1Cu (1.925(14) Å) bonds in the equatorial plane and a long bond to a terminal water ligand, Cu2-O1C2 (2.29(3) A). Finally, Cu3 has a square-planar coordination geometry which is composed of Cu3-O1C3 (1.905(16) Å), Cu3-O1Cu (1.933(14) Å), Cu3-O1C3’ (1.947(16) Å) and Cu3-O2C3 (1.948(14) Å) bonds. The copper-copper distances in 1 are as follows: Cu1···Cu2, 2.812(3) Å; Cu1···Cu3, 3.045(4) Å and Cu1···Cu3’, 3.052(4) Å. O2C3 Cu3 O1C3 O1Cu O1P2 O1C2 Cu2 O3P2 O1A P1 O2P1 P2 O1P1 O2P2 O2A O3P1 O4A O12 O24 O46 O1B W1 Cu1 W2 W4 O23 O45 O13 W3 O5A W5 O56 O1T O3A O35 O2T O4T W6 O6A O6T O3T O5T Figure 3.5 Ball-and-stick representation of the asymmetric unit of 1, thermal ellipsoids shown are set at 50% probability. 67
<strong>Chapter</strong> 3 The Wheel-Shaped Cu 20 Cu1 Cu1 Cu3 Cu3 Cu3 Cu1 Cu3 Cu1 Cu2 Cu2 Cu2 Cu2 Cu1 Cu3 Cu1 Cu3 Cu3 Cu3 Cu1 Cu1 Figure 3.6 Ball and stick representation of the copper-hydroxo cluster in 1 showing all structurally equivalent copper atoms with the same label. Only the oxo-ligands bridging neighboring copper ions are shown. 3.4.2 Solution NMR We also investigated the solution properties of 1 by 31 P NMR at room temperature in D 2 O using a 400 MHz JEOL ECX instrument. We observed a singlet at –29.3 ppm (Figures 3.7) indicating that all 8 P atoms in 1 are equivalent, which is in complete agreement with the solid state structure (Figures 3.2 and 3.3). We have not yet obtained a good 183 W spectrum for 1 (expected are 3 peaks of equal intensity), probably due to solubility problems. 68
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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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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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