A solution and solid state study of niobium complexes University of ...
A solution and solid state study of niobium complexes University of ... A solution and solid state study of niobium complexes University of ...
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
4.5 Crystal Structure <strong>of</strong> [NbCl2(phacac-К 2 -O,O’)(OMe)3] <strong>and</strong> [NbCl(phacac-К 2 -<br />
O,O’)(OMe)2] ...................................................................................................... 71<br />
4.5.1 Introduction ................................................................................................ 71<br />
4.6 Conclusion ....................................................................................................... 77<br />
5 Formation kinetics <strong>of</strong> [NbCl(acac)(OMe)3] ....................................... 79<br />
5.1 Introduction ...................................................................................................... 80<br />
5.2 Experimental procedures ................................................................................. 80<br />
5.2.1 Kinetic experiments ................................................................................... 80<br />
5.2.2<br />
93 Nb NMR .................................................................................................. 81<br />
5.3 Results <strong>and</strong> Discussion ................................................................................... 84<br />
5.3.1 Proposed Reaction Scheme ...................................................................... 84<br />
5.3.2 Stepwise analysis <strong>of</strong> the reaction scheme ................................................. 85<br />
5.3.3 Derivation <strong>of</strong> the rate law ........................................................................... 88<br />
5.3.1 Discussion ................................................................................................. 89<br />
5.4 Conclusion ....................................................................................................... 93<br />
6 Evaluation <strong>of</strong> Study ........................................................................... 95<br />
6.1 Results Obtained .............................................................................................. 95<br />
6.2 Future Research .............................................................................................. 96<br />
Appendix A………………………………………………………….….……... 97<br />
Appendix B…….……………………………………………………..……....114<br />
IV
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