Chapter 4 - Jacobs University

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<strong>Chapter</strong> 6 U-peroxo-Polyoxometalate 6.3 X-ray crystallography A yellow rod of 4a with dimensions 0.27 x 0.03 x 0.03 mm 3 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 Ka radiation (l = 0.71073 Å). Of the 407786 reflections collected (2q max = 49.78°, 99.4% complete), 42978 were unique (R int = 0.2848) and 22961 reflections were considered observed (I > 2s(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 uranium atoms (SHELXS-97). Then the remaining atoms were found from successive Fourier maps (SHELXL-97). The final cycle of refinement, including the atomic coordinates, anisotropic thermal parameters (W, U, P, and K atoms) and isotropic thermal parameters (O and Li atoms) converged at R = 0.0806 (I > 2s(I)) and R w = 0.1966 (all data). In the final difference map the deepest hole was -3.6 e - Å -3 (1.03 Å from U6) and the highest peak 4.0 e - Å -3 (0.09 Å from U7). The data for this crystal is summarized in Table 6.1. 111
<strong>Chapter</strong> 6 U-peroxo-Polyoxometalate Table 6.1: Crystal data and structure refinement for K 6 Li 19 [Li(H 2 O)K 4 (H 2 O) 3 {(UO 2 ) 4 (O 2 ) 4 (H 2 O) 2 } 2 (PO 3 OH) 2 P 6 W 36 O 136 ]×74H 2 O (4a) 4a empirical formula H166 K10 Li20 O248 P8 U8 W36 Formula weight 13607.49 Temperature 173(2) K Wavelength 0.71073 Å Crystal system Monoclinic Space group (No.) P2 1 /n (14) a(Å) 29.343(4) b(Å) 26.706(4) c(Å) 32.229(6) α( o ) 90 β( o ) 100.288(8) γ ( o ) 90 vol(Å 3 ) 24848(7) Z 4 Density (calculated)( Mg/m3) 3.636 Absorption coefficient(mm-1) 22.114 Max. and min. transmission 0.6079 and 0.1442 Data / restraints / parameters 42978 / 0 / 1448 Goodness-of-fit on F2 1.016 R[I>2s (I)] R1 = 0.0806, wR2 = 0.1966 R w (all data) R1 = 0.1623, wR2 = 0.2439 112
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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 1 Introduction (84) Isabell
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Chapter 2 were block-diagonal least
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Chapter 2 Experimental 2.2.3 Synthe
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Chapter 2 Experimental 2.2.7 Synthe
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Chapter 2 Experimental 2.2.11 Synth
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Chapter 2 Experimental 2.3Reference
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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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