A solution and solid state study of niobium complexes University of ...

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4.5 Crystal Structure of [NbCl2(phacac-К 2 -O,O’)(OMe)3] and [NbCl(phacac-К 2 - O,O’)(OMe)2] ...................................................................................................... 71 4.5.1 Introduction ................................................................................................ 71 4.6 Conclusion ....................................................................................................... 77 5 Formation kinetics of [NbCl(acac)(OMe)3] ....................................... 79 5.1 Introduction ...................................................................................................... 80 5.2 Experimental procedures ................................................................................. 80 5.2.1 Kinetic experiments ................................................................................... 80 5.2.2 93 Nb NMR .................................................................................................. 81 5.3 Results and Discussion ................................................................................... 84 5.3.1 Proposed Reaction Scheme ...................................................................... 84 5.3.2 Stepwise analysis of the reaction scheme ................................................. 85 5.3.3 Derivation of the rate law ........................................................................... 88 5.3.1 Discussion ................................................................................................. 89 5.4 Conclusion ....................................................................................................... 93 6 Evaluation of Study ........................................................................... 95 6.1 Results Obtained .............................................................................................. 95 6.2 Future Research .............................................................................................. 96 Appendix A………………………………………………………….….……... 97 Appendix B…….……………………………………………………..……....114 IV
Abbreviations and Symbols Abbreviation Meaning thd - V Tetramethylheptanedionate acacH Acetylacetone phacacH 1-phenyl-1,3-butanedione tBu2(acacH) Di-tertiarybutylacetylacetone ttbd - 1,1,1-trifluoro-4-thenoyl-2,4-butanedionate hfacacH Hexafluoroacetylacetone tropH Tropolone dbm Dibenzoylmethanato IR Infra red UV/Vis Ultraviolet/visible NMR Nuclear magnetic resonance XRD X-ray diffraction Z Number of formula units in a unit cell A Absorbance (theoretical) Aobs Observed absorbance (L,L') Bidentate ligand kx k-x Kx kobs ppm DMF THF C6D6 CD3OD ν λ ∆H ≠ ∆S ≠ mg mmol M Rate constant for a forward equilibrium reaction Rate constant for a backward equilibrium reaction Equilibrium constant for an equilibrium reaction Observed rate constant (Unit of chemical shift) parts per million Dimethyl formamide Tetrahydrofuran Deuterated benzene Deuterated methanol IR stretching frequency UV/Vis wavelength Enthalpy of activation Entropy of activation Milligram Millimol mol.dm -3
Page 1 and 2: A solution and solid state study of
Page 3 and 4: Table of contents Abbreviations and
Page 5: 3.4 Infrared Spectroscopy (IR) ....
Page 9 and 10: Abstract 93 Nb NMR was successfully
Page 11 and 12: Opsomming 93 Nb KMR is met sukses g
Page 13 and 14: Chapter 1 metals. 3 Due to Wollasto
Page 15 and 16: Synopsis... 2. Literature Review of
Page 17 and 18: Chapter 2 Niobium resembles tantalu
Page 19 and 20: 2.1.2 Uses Chapter 2 Niobium has a
Page 21 and 22: 2.2 Separation of Nb and Ta 2.2.1 M
Page 23 and 24: Chapter 2 Buachuang et al. 16 repor
Page 25 and 26: Chapter 2 Niobium oxide surfaces ex
Page 27 and 28: 2.4.6 Water absorption Chapter 2 Th
Page 29 and 30: Chapter 2 been reported in literatu
Page 31 and 32: Chapter 2 containing niobium as the
Page 33 and 34: Chapter 2 conclusions, with regard
Page 35 and 36: Chapter 2 Figure 2.5: Structure of
Page 37 and 38: 2.6.3.3 [NbCl3O(ttbd) - ] Chapter 2
Page 39 and 40: Chapter 2 (a) (b) Figure 2.10: Stru
Page 41 and 42: 2.7 Alkoxides Chapter 2 Specific kn
Page 43 and 44: Chapter 2 Reactions of dialkylamid
Page 45 and 46: Chapter 2 other NbCl5-x(OMe)x produ
Page 47 and 48: Chapter 2 In 1991 Lee et al. 83 pub
Page 49 and 50: EtO EtO EtO EtO Cl Nb Cl Cl Nb Cl R
Page 51 and 52: Chapter 2 The hemicarbonate formed
Page 53 and 54: Synopsis... 3. Synthesis and Charac
Page 55 and 56: Chapter 3 with γ = magnetogyric ra
Page 57 and 58:
Chapter 3 electromagnetic spectrum
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3.5.1 Bragg’s law Chapter 3 Bragg
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3.5.3 ‘Phase problem’ Chapter 3
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Chapter 3 A = ∑ ε cl (3.14) In
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Chapter 3 t1/2 = 54 = . 3.7 Sy
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3.7.2.4 Synthesis of [NbCl4(acac)]:
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4. Crystallographic Synopsis... Cha
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Chapter 4 packages 2 respectively.
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Chapter 4 4.3 Crystal Structure of
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Chapter 4 longer bonds (C1-C2, C2-C
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Chapter 4 Figure 4.5: Packing of [N
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Chapter 4 Figure 4.7: Molecular str
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Chapter 4 Table 4.5: Selected bond
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Chapter 4 Figure 4.11: Molecular st
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Chapter 4 Figure 4.12: The phacac p
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Chapter 4 Table 4.9: Hydrogen bonds
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Chapter 4 According to our knowledg
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5.2 Experimental procedures 5.2.1 K
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Chapter 5 corresponds to one specie
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5.3 Results and Discussion 5.3.1 Pr
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Chapter 5 Figure 5.5: Typical UV/Vi
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5.3.3 Derivation of the rate law Ch
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Chapter 5 The Stopped-flow data (fa
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Chapter 5 Figure 5.9: Eyring plot,
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Chapter 5 However, more information
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Chapter 6 second reaction entailed
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Appendix A Table 1.3: Bond angles (
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Appendix A A 2 Supplementary Data f
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Appendix A C(16)-H(16B) 0.96 C(16)-
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Appendix A O(7)-C(10)-C(11) 123.6 (
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Appendix A H(18E)-C(18B)-H(18F) 109
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Appendix A H(18F) 6243 6605 575 75
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Appendix A Table 3.3: Bond angles (
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Appendix A Table 3.4: Anisotropic d
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Appendix B Appendix B B 1 Supplemen
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A solution and solid state study of niobium complexes University of ...

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