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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
41

Molybdenum, tungsten and rhodium complexes of nitrogen-oxides.

Rajaseelan, Rajaratnam Edward. January 1989 (has links)
Complexes of the type MX(η²-NO₃)(CO)₂(PPh₃)₂, (M = Mo, X = Cl, Br; M = W, X = Br) were prepared from the reactions of MX₂(CO)₂(PPh₃)₂ with ammonium nitrate in acetone. The complexes were characterized by elemental analyses, ¹⁵N labelling, infrared and NMR spectroscopy. The nitrate ligand is bidentate and the complexes are seven-coordinate. Novel nitrite complexes of molybdenum and tungsten of the type M(NO₂)₂(PPh₃)₂ were prepared. The compounds were characterized by elemental analyses, ¹⁵N labelling, infrared and multinuclear NMR spectroscopy. Both NO₂ ligands are chelating and the two NO₂, PPh₃ and CO ligands are equivalent. Molybdenum dinitrosyl complexes were synthesized by the reduction of nitrate ions. The crystal structure of cis-dinitrosyl-cis-dichloro-trans-bis-(triphenylphosphine)molybdenum(II) was determined by x-ray diffraction. Both the nitrosyl groups are linear. Mo(NO)₂Cl₂(OPPh₃)₂ and Mo(NO)₂Cl(NO₃)(OPPh₃)₂ were synthesized by the reaction of MoCl(η²-NO₃)(CO)₂(PPh₃)₂ with NO in acetone/toluene mixture. The nitrosyl ligands are linear and the phosphineoxide ligands are cis to each other. The dinitrite complex Rh(NO)(NO₂)₂(PPh₃)₂ of the series Rh(NO)X₂(PPh₃)₂ (X - monodentate anions) was prepared as a direct derivative of Rh(NO)Cl₂(PPh₃)₂ by its reaction with sodium nitrite. The complex is square pyramidal with an apical nitrosyl ligand. The two NO₂ groups are present as the nitro and the nitrito group. Rh(NO)(NO₂)₂(PPh₃) reacted with oxygen and formed Rh(NO₃)₃(PPh₃)₂. The reaction of Rh(NO)(NO₂)₂(PPh₃)₂ with CO in acetonitrile produced Rh(CO)(NO₂)(PPh₃)₂. The complex Rh(CO)(NO₂)(PPh₃)₂ is square planar with the phosphine ligands in the trans positions.
42

Synthesis of new axially chiral diphosphines and phosphinamines for asymmetric catalysis

Long, James Maurice January 1996 (has links)
No description available.
43

Studies on functionalised crown thioethers

Sutton, Liam Richard January 1999 (has links)
No description available.
44

Polyaza redox-active acyclic and macrocyclic compounds designed to bind cations and anions

Spencer, Paul January 1994 (has links)
No description available.
45

Synthesis, structures and reactivities of low-valent late transition metal amides.

January 2001 (has links)
Chung Hei Lam. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2001. / Includes bibliographical references. / Abstracts in English and Chinese. / Table of Contents --- p.i / Acknowledgements --- p.iv / Abstracts --- p.v / 摘要 --- p.vii / List of Compounds --- p.ix / List of Tables --- p.xii / List of Figures --- p.xiv / Abbreviations --- p.xv / Chapter CHAPTER 1. --- SYNTHESIS OF LATE TRANSITION METAL AMIDES / Chapter 1.1 --- GENERAL BACKGROUND --- p.1 / Chapter 1.2 --- PREPARATIONS OF LATE TRANSITION METAL AMIDES --- p.2 / Chapter 1.3 --- OBJECTIVES OF THIS WORK --- p.3 / Chapter 1.4 --- REFERENCES FOR CHAPTER1 --- p.5 / Chapter CHAPTER 2. --- "SYNTHESIS, STRUCTURES AND REACTIVITIES OF IRON(II) AND COBALT(II) AMIDES" / Chapter 2.1 --- INTRODUCTION --- p.7 / Chapter 2.1.1 --- A General Review on Iron(II) and Cobalt (II) Amides --- p.7 / Chapter 2.1.2 --- A General Review on Iron(II) and Cobalt(II) Thiolates --- p.9 / Chapter 2.1.3 --- A General Review on Iron(II) and Cobalt(II) Alkoxides and Aryloxides --- p.11 / Chapter 2.2 --- RESULTS AND DISCUSSION --- p.13 / Chapter 2.2.1 --- Synthesis of the Ligand Precursor LH (1) and the Corresponding Lithium Reagents [Li(L)(TMEDA)] (2) and LiL (3) --- p.13 / Chapter 2.2.2 --- Synthesis´ة Structures and Reactivities of Mononuclear Iron(II) and Cobalt(II) Amides --- p.14 / Chapter 2.2.2.1 --- Synthesis of Mononuclear Iron(II) and Cobalt(II) Amides --- p.14 / Chapter 2.2.2.2 --- Reactions of Compound 4 with ArMe OH and ArSH --- p.18 / Chapter 2.2.2.3 --- Physical Characterization of Compounds 4-6 --- p.19 / Chapter 2.2.2.4 --- Molecular Structures of Compounds 4-6 --- p.20 / Chapter 2.2.3 --- "Synthesis, Structures and Reactivities of Binuclear Iron(II) and Cobalt (II) Amides" --- p.31 / Chapter 2.2.3.1 --- Synthesis of Binuclear Iron(II) and Cobalt(II) Amides --- p.31 / Chapter 2.2.3.2 --- Reactions of Compounds 7 and 8 with Protic Reagents --- p.33 / Chapter 2.2.3.3 --- "Attempted Reactions of Compounds 7 and 8 with 3,5-di-tert- butylcatechol" --- p.35 / Chapter 2.2.3.4 --- Physical Characterization of Compounds 7-14 --- p.35 / Chapter 2.2.3.5 --- Molecular Structures of Compounds 7-10 and 13-14 --- p.38 / Chapter 2.3 --- EXPERIMENTALS FOR CHAPTER 2 --- p.57 / Chapter 2.4 --- REFERENCES FOR CHAPTER 2 --- p.64 / Chapter CHAPTER 3. --- SYNTHESIS AND STRUCTURES OF MANGANESE(II) AMIDES / Chapter 3.1 --- INTRODUCTION --- p.68 / Chapter 3.2 --- RESULTS AND DISCUSSION --- p.70 / Chapter 3.2.1 --- Synthesis of Manganese(II) Amide --- p.70 / Chapter 3.2.2 --- Physical Characterization of Compound 15 --- p.72 / Chapter 3.2.3 --- Molecular Structure of Compound 15 --- p.73 / Chapter 3.3 --- EXPERIMENTALS FOR CHAPTER 3 --- p.78 / Chapter 3.4 --- REFERENCES FOR CHAPTER 3 --- p.79 / "APPENDIX 1 General Procedures, Physical Measurements and X-ray Structure Analysis" --- p.81 / APPENDIX 2 Table A-1. Selected crystallographic data for compounds 4-6. --- p.84 / Table A-2. Selected crystallographic data for compounds 7-10. --- p.85 / Table A-3. Selected crystallographic data for compounds 13-15 --- p.86
46

Transition metal phosphoranoimine complexes: synthesis, structure and catalytic study.

January 2002 (has links)
Suk-Yu Wong. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2002. / Includes bibliographical references. / Abstracts in English and Chinese. / Acknowledgements --- p.i / Abstract --- p.ii / 中文摘要 --- p.iv / List of Compounds Synthesized --- p.vi / List of Abbreviation --- p.viii / Contents --- p.x / Chapter CHAPTER 1 --- Development of Phosphoranoimine as a Ligand for the Synthesis of Metal Complexes / Chapter 1.1 --- Introduction / Chapter 1.1.1 --- General Aspects of Phosphoranoimine --- p.1 / Chapter 1.1.2 --- General Aspects of Transition Metal Phosphoranoimine Complexes --- p.3 / Chapter 1.1.3 --- Reaction with Organolithium Compounds --- p.6 / Chapter 1.1.5 --- Objective of this Work --- p.8 / Chapter 1.2 --- Results and Discussion / Chapter 1.2.1 --- Synthesis and Characterization of Phosphoranoimine Ligand (9a and 9b) --- p.11 / Chapter 1.2.2 --- Synthesis of Dilithium Phosphoranoimine Complex (10a) --- p.14 / Chapter 1.2.3 --- Synthesis of Monolithium Phosphoranoimine Complex (10b) --- p.16 / Chapter 1.2.4 --- "Molecular Structures of Dilithium Complex and Monolithium Complex [Li2{2,6-(Me3SiN=PPh2CH)2C5H3N}THF] (10a) and [Li{2,6-(Me3SiN=PPri2CH)(Me3SiN=PPri2CH2)C5H3N}] (10b)" --- p.17 / Chapter 1.3 --- Experimental Section --- p.21 / Chapter 1.4 --- References --- p.27 / Chapter CHAPTER 2 --- Synthesis and Characterization of Transition Metal Complexes Containing Phosphoranoimine Ligands / Chapter 2.1 --- Introduction --- p.30 / Chapter 2.2 --- Results and Discussion / Chapter 2.2.1 --- "Synthesis and Characterization of Titanium(IV) Phosphoranoimido Complexes [Ti{N=(2-CH2Py)PPr i2 }C13(THF)] (11) and [Ti2{ {N=PPh2CH2}2 C5H3N-2,6}{(μ-Cl)2Cl4(THF)2}]n (12)" --- p.33 / Chapter 2.2.2 --- "Molecular Structures of [Ti{N=(2-CH2Py)PPri2}Cl3(THF)] (11) and [Ti2{{N=PPh2CH2}2C5H3N-2,6}{{471}-Cl)2Cl4(THF)2}]n (12)" --- p.36 / Chapter 2.2.3 --- "Synthesis and Characterization of Iron(II) Complexes [Fe{(2-CH2Py)PR2=NSiMe3}C12] (R = Ph, 13a; Pri, 13b)" --- p.42 / Chapter 2.2.4 --- "Molecular Structures of [Fe{(2-CH2Py)PR2=NSiMe3}Cl2] (R = Ph, 13a; Pri, 13b)" --- p.43 / Chapter 2.2.5 --- "Synthesis and Characterization of Cobalt(II) Complexes [Co{(2-CH2Py)PR2=NSiMe3}Cl2] (R = Ph, 14a; Pri,14b)" --- p.46 / Chapter 2.2.6 --- "Molecular Structures of [Co{(2-CH2Py)PR2=NSiMe3}Cl2] (R = Ph, 14a; Pri, 14b)" --- p.47 / Chapter 2.2.7 --- "Synthesis and Characterization of Copper(I) Complexes [Cu{(2-CH2Py)PPh2=NSiMe3 }I]2 (15a), [Cu{ (2-CH2Py)PPri2=NSiMe3 }I] (15b) and [Cu{2,6-(Me3SiN=PPri2CH2)2C5H3N}]+ [Cul2]-(16)" --- p.50 / Chapter 2.2.8 --- "Molecular Structures of [Cu{(2-CH2Py)PPh2=NSiMe3}I]2 (15a), [Cu{(2-CH2Py)PPri2=NSiMe3} I] (15b) and [Cu{2,6-(Me3SiN=PPri2CH2)2C5H3N}]+ [Cul2]- (16)" --- p.53 / Chapter 2.2.9 --- Spectroscopic properties of compounds 11-16 --- p.58 / Chapter 2.3 --- Experimental Section --- p.60 / Chapter 2.4 --- References --- p.64 / Chapter CHAPTER 3 --- Synthesis and Characterization of Group 8 Transition Metal Complexes Containing Phosphoranoimine Ligands / Chapter 3.1 --- Introduction --- p.65 / Chapter 3.2 --- Results and Discussion / Chapter 3.2.1 --- "Synthesis and Characterization of Nickel(II) Complexes [Ni{(2-CH2Py)PR2=NSiMe3 }Br2] (R = Ph, 17a; Pri, 17b)" --- p.68 / Chapter 3.2.2 --- "Molecular Structures of [Ni{(2-CH2Py)PR2=NSiMe3}Br2] (R = Ph, 17a; Pri, 17b)" --- p.69 / Chapter 3.2.3 --- "Synthesis and Characterization of hydrolyzed Nickel(II) and Palladium(II) Complexes [Ni{2,6-(HN=PPh2CH2)(Me3SiN=PPh2CH2) C5H3N}Br]+[Br]- (18), [(EtOH)Ni{2,6-(HN=PPh2CH2)2- C5H3N}C1]+[C1]- (19) and [Pd{(2-CH2Py)PPh2=NH}Cl2] (20)" --- p.72 / Chapter 3.2.4 --- "Molecular Structures of [Ni{2,6-(HN=PPh2CH2)(Me3SiN=PPh2CH2) C5H3N }Br]+[Br]- (18) and [(EtOH)Ni{2,6-(HN=PPh2CH2)2- C5H3N}C1]+[C1]- (19),and [Pd{ (2-CH2Py)PPh2=NH}Cl2] (20 )" --- p.75 / Chapter 3.2.5 --- "Synthesis and Characterization of Ionic Palladium(II) Complex [Pd{2,6-(Me3SiN = PPh2CH2)2C5H3N}Cl]+[Cl]- (21)" --- p.80 / Chapter 3.2.6 --- "Molecular Structure of[Pd{2,6-(Me3SiN=PPh2CH2)2C5H3N}Cir[Cir]- (21)" --- p.81 / Chapter 3.2.7 --- Spectroscopic properties of compounds 17-21 --- p.83 / Chapter 3.3 --- Experimental Section --- p.84 / Chapter 3.4 --- References --- p.87 / Chapter CHAPTER 4 --- Reactivity of Phosphoranoimine Complexes on Ethylene Polymerization / Chapter 4.1 --- Introduction / Chapter 4.1.1 --- A Brief Review on Olefin Polymerization --- p.89 / Chapter 4.2 --- Results and Discussion --- p.92 / Chapter 4.3 --- Experimental Section --- p.94 / Chapter 4.4 --- References --- p.95 / APPENDIX I / Crystallographic Data and Refinement Parameters --- p.96 / APPENDIX II / Chapter A. --- General Experimental Procedures and Physical Measurement --- p.105 / Chapter B. --- X-ray Crystallography --- p.105
47

Divalent transition metal complexes supported by sterically demanding amido ligands.

January 2006 (has links)
by Au Yeung Ho Yu. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2006. / Includes bibliographical references. / Abstracts in English and Chinese. / Abstract --- p.i / 摘要 --- p.iii / Acknowledgement --- p.v / Table of Contents --- p.vi / Abbreviations --- p.ix / List of Compounds --- p.x / Chapter Chapter 1 --- A General Introduction To Late Transition Metal Amides / Chapter 1.1 --- General Background --- p.1 / Chapter 1.2 --- An Overview of Late Transition Metal Amides --- p.2 / Chapter 1.3 --- Objectives of This Work --- p.7 / Chapter 1.4 --- References for Chapter1 --- p.9 / Chapter Chapter 2 --- Late Transition Metal Complexes Derived From 2-Pyridyl Amido Ligand / Chapter 2.1 --- General Background / Chapter 2.1.1 --- A Brief Introduction to Pyridine-Functionalized Amido Ligands --- p.13 / Chapter 2.1.2 --- Late Transition Metal Complexes Supported by 2-Pyridyl Amido Ligands --- p.14 / Chapter 2.2 --- Aims of Our Study --- p.18 / Chapter 2.3 --- Result and Discussion / Chapter 2.3.1 --- Preparation of the [N(CH2But)(2-C5H3N-6-Me)]- Ligand and the Corresponding Lithium Derivatives --- p.19 / Chapter 2.3.2 --- Syntheses and Structures of Iron(II) and Cobalt(II) Amides / Chapter 2.3.2.1 --- "Synthesis of [M(L1)2(HL1)] [M = Fe (6), Co (7)]" --- p.20 / Chapter 2.3.2.2 --- Physical Characterization of Compounds 6 and7 --- p.24 / Chapter 2.3.2.3 --- Molecular Structures of Compounds 6 and7 --- p.24 / Chapter 2.4 --- Experimentals for Chapter 2 --- p.31 / Chapter 2.5 --- References for Chapter 2 --- p.34 / Chapter Chapter 3 --- Synthetic and Structural Studies of Late Transition Metal Anilides / Chapter 3.1 --- An Overview on Anilido Complexes --- p.40 / Chapter 3.2 --- Aims of Our Study --- p.45 / Chapter 3.3 --- Result and Discussion / Chapter 3.3.1 --- Aniline Precursors and The Lithium Derivatives / Chapter 3.3.1.1 --- Syntheses of the Aniline Precusors HLn (n = 2-5) --- p.46 / Chapter 3.3.1.2 --- Syntheses of Lithium Derivatives of Ln (n = 2-5) --- p.47 / Chapter 3.3.1.3 --- Physical Characterization of Compounds 11-13 --- p.48 / Chapter 3.3.1.4 --- "Molecular Structures of Compounds 11a, 12a and 12b" --- p.49 / Chapter 3.3.2 --- Syntheses and Structures of Late Transition Metal Anilides / Chapter 3.3.2.1 --- Syntheses of N-Silylated Anilides --- p.57 / Chapter 3.3.2.2 --- Physical Characterization of Compounds 14-20 --- p.64 / Chapter 3.3.2.3 --- Molecular Structures of Compounds 14-20 --- p.65 / Chapter 3.3.2.4 --- Syntheses of N-Alkylated Anilides --- p.89 / Chapter 3.3.2.5 --- Physical Characterization of Compounds 21-26 --- p.92 / Chapter 3.3.2.6 --- "Molecular Structures of Compounds 21, 23, 25 and 26" --- p.93 / Chapter 3.4 --- Experimentals for Chapter 3 --- p.103 / Chapter 3.5 --- References for Chapter 3 --- p.112 / Chapter Chapter 4 --- Reactions of Late Transition Metal Anilides and Their Derivatives / Chapter 4.1 --- General Background / Chapter 4.1.1 --- Reactions of Late Transition Metal Amides --- p.124 / Chapter 4.1.2 --- A Brief Introduction to Oxidative Coupling of Phenols --- p.129 / Chapter 4.1.3 --- A Brief Overview on the Ring-Opening Polymerization of Cyclic Esters --- p.130 / Chapter 4.2 --- Aims of Our Study --- p.132 / Chapter 4.3 --- Results and Discussion / Chapter 4.3.1 --- Reactions of Late Transition Metal Anilides and Their Derivatives / Chapter 4.3.1.1 --- Ligand Substitution --- p.133 / Chapter 4.3.1.2 --- Chloride Abstraction --- p.137 / Chapter 4.3.1.3 --- Chemical Reduction --- p.138 / Chapter 4.3.1.4 --- Reaction with Unsaturated Compounds --- p.139 / Chapter 4.3.1.5 --- Physical Characterization of Compounds 27-33 --- p.140 / Chapter 4.3.1.6 --- Molecular Structures of Compounds 27-33 --- p.142 / Chapter 4.3.2 --- Oxidation of Bisaryloxide Complexes --- p.162 / Chapter 4.3.3 --- The Ring-Opening Polymerization of e-Caprolactone --- p.167 / Chapter 4.4 --- Experimentals for Chapter 4 --- p.171 / Chapter 4.5 --- References for Chapter 4 --- p.176 / "Appendix 1 General Procedures, Physical Measurements and X-Ray Structure Analysis" --- p.187 / Appendix 2 NMR Spectra of Compounds --- p.189 / Appendix 3 Selected Crystallographic Data --- p.202
48

Synthesis of bis(phosphoranoimido)metal complexes.

January 2006 (has links)
Sze Wing Yin. / Thesis submitted in: November 2005. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2006. / Includes bibliographical references. / Abstracts in English and Chinese. / Table of Contents --- p.vi / Acknowledgements --- p.i / Abstract --- p.ii / 摘要 --- p.iv / List of Compounds Synthesized --- p.x / Abbreviation --- p.xi / Chapter Chapter 1 --- Syntheses and Characterization of Bis(phosphoranoimido)lithium and Late Transition Metal Complexes / Chapter 1.1 --- Introduction --- p.1 / Chapter 1.1.1 --- A General Review of Bis(Phosphoranoimido) Ligands --- p.1 / Chapter 1.1.2 --- Synthesis of Bis(Phosphoranoimido)metal Complexes --- p.8 / Chapter 1.2 --- Objectives --- p.13 / Chapter 1.3 --- Results and Discussion --- p.14 / Chapter 1.3.1.1 --- "Synthesis of Bis(Phosphoranoimido)lithium complexes [Li{{(Me3SiNPR2CH)(Me3SiN=PR2CH2)}C5H3N-2,6} (R = Ph, 36; R = Pr', 37)]" --- p.14 / Chapter 1.3.1.2 --- Spectroscopic Properties of Complexes 36 and 37 --- p.14 / Chapter 1.3.1.3 --- "Molecular Structures of [Li{{(Me3SiNPR2CH)- (Me3SiN=PR2CH2)}C5H3N-2,6} (R = Ph, 36; R = Pr', 37)]" --- p.16 / Chapter 1.3.2.1 --- Synthesis and Characterization of Bis(Phosphoranoimido)transition Metal Complexes --- p.21 / Chapter 1.3.2.2 --- Spectroscopic Properties of 38 - 41 --- p.21 / Chapter 1.3.2.3 --- "Molecular Structures of [MCI {{(Me3SiNPPh2CH)- (Me3SiN=PPh2CH2)}C5H3N-2,6}] (M = Co, 38; Mn, 39), [MnCl{{(Me3SiNPPri2CH)(Me3SiN=PPri2CH2)}C5H3N-2,6}] (41)" --- p.22 / Chapter 1.4 --- Experimental Section --- p.31 / Chapter 1.5 --- References for Chapter 1 --- p.36 / Chapter Chapter 2 --- Syntheses and Characterization of Bis(phosphoranoimido)zirconium(IV) Complex / Chapter 2.1 --- Introduction --- p.39 / Chapter 2.1.1 --- General Aspects of Group 4 Metal Complexes --- p.39 / Chapter 2.2 --- Results and Discussion --- p.44 / Chapter 2.2.1 --- "Synthesis and Characterization of Bis(phosphoranoimido)zirconium(IV) Complex [Zr{(Me3SiNPPh2C)(Me3SiN=PPh2CH2)C5H3N-2,6}(NMe2)2] (46)" --- p.44 / Chapter 2.2.2 --- Reaction of Bis(phosphoranoimido)zirconium(IV) Complex (46) with HC1 --- p.45 / Chapter 2.2.3 --- Spectroscopic Properties of Complex 46 --- p.45 / Chapter 2.2.4 --- Molecular Structure of [Zr{(Me3SiNPR2C)- (Me3SiN=PR2CH2)5H3N-2,6}(NMe2)2] (46) --- p.46 / Chapter 2.3 --- Experimental Section --- p.51 / Chapter 2.4 --- References for Chapter 2 --- p.52 / Chapter Chapter 3 --- Syntheses and Characterization of Bis(phosphoranoimido)samarium(III) Complexes / Chapter 3.1 --- Introduction --- p.54 / Chapter 3.1.1 --- A General Review of Lanthanide Complexes --- p.54 / Chapter 3.1.2 --- General Aspect of Bis(phosphoranoimido)lanthanide Metal Complexes --- p.58 / Chapter 3.1.3 --- Synthesis and Structure of Bis(phosphoranoimido)dilithium Complex --- p.60 / Chapter 3.2 --- Results and Discussion --- p.63 / Chapter 3.2.1 --- Synthesis and Characterization of Bis(phosphoranoimido)samarium(III) Complexes --- p.63 / Chapter 3.2.2 --- Spectroscopic Properties of 56 and 57 --- p.65 / Chapter 3.2.3 --- "Molecular Structures of [Sm {{(Me3SiNPPh2CH)2} - C5H3N-2,6}(μ-Cl2)Li(THF)2] (56) and [Sm{{(Me3SiNPPri2CH)2}C5H3N-2,6}2(μ-Cl)]2 (57)" --- p.65 / Chapter 3.3 --- Experimental Section --- p.72 / Chapter 3.4 --- References for Chapter 3 --- p.74 / Appendix I / Chapter A. --- General Procedures --- p.77 / Chapter B. --- Physical and Analytical Measurements --- p.77 / Appendix II / Table A.1. Selected Crystallographic Data for Compounds 36,37 and 38 --- p.80 / Table A.2. Selected Crystallographic Data for Compounds 39,41 and 46 --- p.81 / Table A.3. Selected Crystallographic Data for Compounds 56 and 57 --- p.82
49

Synthesis, structure and reactivity of group 4 metal complexes bearing cyclopentadienyl-carboranyl ligands. / CUHK electronic theses & dissertations collection

January 2010 (has links)
[eta5:sigma-Me2C(C5H4 )(C2B10H10]Zr[eta2-S 2C2B10H10](NHMe2)2 was prepared by amine elimination reaction between [eta5:sigma-Me 2C(C5H4)(C2B10H10)]Zr[NMe 2)2 and 1,2-(HS)2-1,2-C2B10 H10. It underwent ligand substitution reaction with XylNC to generate [eta5:sigma-Me2C(C5H 4)(C2B10H10]Zr[eta2-S 2C2B10H10][2,6-(CH3) 2C6H3N=C]2 and reacted with THE to give ring opening product [eta5:sigma-Me2C(C 5H4)(C2B10H10]ZR-[eta 2-S2C2B10H10][sigma-O(CH 2)4NHMe2)]. Zirconium-promoted nucleophilic reaction of dimethylamine with various kinds of unsaturated polar organic substrates, such as PhCN, PhNCO, nBuNCS and MA were studied. / Direct deboration of group 4 metal carboranyl complexes was achieved by reactions of [eta5:sigma-Me2C(C5H 4)(C2B10H10]M[NMe2) 2 (M = Zr, Hf), [eta5:sigma-Me2C(C 9H6)(C2B10H10]Zr[NMe 2)2 or [eta5:sigma-H2C(C 13H8)(C2B10H10]Zr[NMe 2)2 with excess diamines. The resultant metal dicarbollide complexes [eta5:eta6-Me2C(C 5H4)(C2B9H10)]Zr[eta 2-N(Me)(Ch2)2NH(Me)] and [eta5:eta 6-Me2C(C5H4)(C2B 9H10]Zr[eta2-[NMe)(CH2) 3NH(Me)] were active toward unsaturated molecules, like nBuNCS, iPr-N=C=N- iPr and nBuNC, to give mono-insertion products. [eta5:eta6-Me2C(C 5H4)(C2B9H10)]Zr[eta 2-N(Me)(CH2)3NH(Me)] was able to be deprotonated by nBuLi to give a lithium salt {[eta 5:eta-6-Me2C(C5H4)(C 2B9H10)]Zr[eta2-N(Me)(CH 2)3N(Me)Li]}2. It reacted with [HNEt3][BPh 4] to afford cationic zirconium species [eta5:eta 6-Me2C(C5H4)(C2B 9H10]Zr{eta2-NH(Me)(CH2) 3NH(ME)}][BPh4]. The dichloro species [eta5:eta 6-Me2C(C5H4)(C2B 9H10}MCl2][Li(DME)3)] (M = Zr, Hf) were reduced by sodium metal to produce a new class of metallacarbornes bearing arachno-eta6-C2B9 tetraanion. / The amine exchange reaction between [eta5:sigma-Me 2C(C5H4)(C2B10H10]M[NMe 2)2 (M = Zr, Hf, Ti) and N, N'-dimethylethylenediamine or N, N'-dimethylpropane-1,3-diamine gave [eta5:sigma-Me 2C(C5H4)(C2B10H10]M-[eta 2N(Me)(CH2)2N(Me)] (M = Zr, Ti) or [eta 5:sigma-Me2C(C5H4)(C2B 10H10]M-[eta2N(Me)(CH2) 3N(Me)] (M= Zr, Hf, Ti) in good yields. The metal-nitrogen bonds in these group 4 metal diamide complexes were very reactive toward unsaturated polar organic substrates, such as RNC, RNCS, RNCO, R-N=C=N-R and RCN to give multiple insertion products. The carbodiimide and XylNC (Xyl = 2,6-Me 2C6H3) insertion products [eta5:sigma-Me 2C(C5H4)(C2B10H10]M-[eta 3N(Me)(CH2)3N(Me)C(=NR)NR] (M = Zr, R = iPr, Cy; M = Hf, R = Cy) and [eta5:sigma-Me 2C(C5H4)(C2B10H10]M-[eta 2:eta2-N(Xyl)=CN(Me)(CH2)3N(Me)C=N(Xyl)] (M = Zr, Hf) also showed reactivities toward unsaturated molecules, resulting in the de-insertion of carbodiimide and XylNC. Different reactivity patterns were observed, depending on the nature of metal atoms and substrates. / Sit, Mei Mei. / Adviser: Zuowei Xia. / Includes supplementary digital materials. / Source: Dissertation Abstracts International, Volume: 73-01, Section: B, page: . / Thesis (Ph.D.)--Chinese University of Hong Kong, 2010. / Includes bibliographical references (leaves 247-267). / Electronic reproduction. Hong Kong : Chinese University of Hong Kong, [2012] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Electronic reproduction. [Ann Arbor, MI] : ProQuest Information and Learning, [201-] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Abstract also in Chinese.
50

Synthesis, structure and oxygenation reactivity of transition metal catecholate complexes supported by tripodal tridentate ligands.

January 2008 (has links)
Cheng, Yat Ho. / Thesis submitted in: October 2007. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2008. / Includes bibliographical references. / Abstracts in English and Chinese. / Abstract --- p.i / 摘要 --- p.iii / Acknowledgment --- p.iv / Contents --- p.v / Abbreviations --- p.xi / Chapter Chapter I. --- Model Studies for Catechol Dioxygenases / Chapter I.1 --- General Background / Chapter I.2 --- Intradiol-Cleaving Catechol Dioxygenases --- p.2-4 / Chapter I.3 --- Extradiol-Cleaving Catechol Dioxygenases --- p.5-8 / Chapter I.4 --- Selectivity of Intra- versus Extradiol-Cleaving Pathways --- p.8-10 / Chapter I.5 --- Early Studies on Model Complexes for Catechol Dioxygenases --- p.10-16 / Chapter I.6 --- Spin Crossover Study of Model Complexes --- p.16-18 / Chapter I.7 --- Model complexes for the Extradiol-Cleaving Dioxygenases --- p.19-23 / Chapter I.8 --- Objectives of this Work --- p.23 / Chapter I.9 --- References for Chapter I --- p.24-31 / Chapter Chapter II. --- "Synthesis and Reactivity Studies of Model Complexes of Catechol Dioxygenases Supported by the anionic Hydrotris-3,5-dimethylpyrazolylborate Ligand" / Chapter II.1 --- Introduction --- p.32-33 / Chapter II.2 --- Result and Discussion --- p.34-60 / Chapter II.2.1 --- Synthesis of Iron(III) Catecholate Complexes --- p.34-37 / Chapter II.2.2 --- Molecular Structures --- p.38-45 / Chapter II.2.3 --- Electrochemical Studies --- p.46-48 / Chapter II.2.4 --- UV-Vis Spectroscopic Studies --- p.49-55 / Chapter II.2.4.1 --- Oxygenation Studies of the Catecholate Complexes --- p.49-51 / Chapter II.2.4.2 --- Spectral Studies at low Temperature --- p.52-54 / Chapter II.2.4.3 --- Reactivity Studies with Excess Pyrazole --- p.54-55 / Chapter II.2.5 --- Identification of the degradation products --- p.56-60 / Chapter II.3 --- Summary --- p.61 / Chapter II.4 --- Experiments for Chapter II --- p.62-66 / Chapter II.4.1 --- Materials --- p.62 / Chapter II.4.2 --- Synthesis of complexes --- p.62-64 / Chapter II.4.3 --- Characterization of degradation products --- p.65-66 / Chapter II.5 --- References for Chapter II --- p.67-70 / Chapter Chapter III. --- "Synthesis and Reactivity Studies of Model Complexes of Catechol Dioxygenases Supported by the neutral Hydrotris-3,5-dimethylpyrazolylmethane Ligand" / Chapter III.1 --- Introduction --- p.71-72 / Chapter III.2 --- Results and Discussion --- p.73-96 / Chapter III.2.1 --- Synthesis --- p.73-78 / Chapter III.2.1.1 --- Synthesis of Iron(III)-Catecholate Complexes --- p.73-74 / Chapter III.2.2.2 --- Attempt to Synthesis Iron(III)-Catecholate Complexes with Pyrocatechol --- p.75-76 / Chapter III.2.2.3 --- Attempts to Remove the Chloride Ligand from the Iron(III) Catecholate Complexes --- p.76-77 / Chapter III.2.2.4 --- Synthesis of Iron(II)-Catecholate Complexes --- p.77-78 / Chapter III.2.2 --- Molecular Structures --- p.79-85 / Chapter III.2.3 --- Electrochemical Studies --- p.86-88 / Chapter III.2.4 --- UV-Vis Spectroscopic and Reactivity Studies on Oxygenation of / Chapter III.2.4.1 --- Oxygenation Studies of the Catecholate Complexes --- p.89-90 / Chapter III.2.4.2 --- Spectral changes with chloride removed from the catecholate complex --- p.91-93 / Chapter III.2.5 --- Identification of the degradation products --- p.94-96 / Chapter III.3 --- Summary --- p.96 / Chapter III.4 --- Experimental for Chapter III --- p.97-101 / Chapter III.4.1 --- Materials --- p.97 / Chapter III.4.2 --- Synthesis of complexes --- p.97-99 / Chapter III.4.3 --- Characterization of Oxygenation Products --- p.100 / Chapter III.5 --- References for Chapter III --- p.101-105 / Chapter Chapter IV. --- "Synthesis and Reactivity Studies of Manganese and Cobalt Catecholate Complexes Supported by the anionic Hydrotris-3,5-dimethyl -pyrazolylborate Ligand" / Chapter IV.1 --- Introduction --- p.106-109 / Chapter IV.2 --- Results and Discussion --- p.110-127 / Chapter IV.2.1 --- Synthesis of Manganese and Cobalt Catecholate Complexes --- p.110-111 / Chapter IV.2.2 --- Molecular Structures --- p.112-118 / Chapter IV.2.3 --- UV-Vis Spectroscopic Studies and Reactivity Studies --- p.119-124 / Chapter IV.2.3.1 --- Oxygenation studies of the Manganese(III)-Catecholate Complex --- p.119-121 / Chapter IV.2.3.1 --- Oxygenation studies of the Cobalt(II)-catecholate Comple --- p.x / Chapter IV.2.4 --- Identification of Degradation Products --- p.124-126 / Chapter IV.3 --- Summary --- p.126 / Chapter IV.4 --- Experimental for Chapter IV --- p.127-129 / Chapter IV.4.1 --- Materials --- p.127 / Chapter IV.4.2 --- Synthesis of complexes --- p.127-129 / Chapter IV.5 --- References for Chapter IV --- p.130-135 / Appendix I / Chapter A.I.1 --- General Procedure --- p.136 / Chapter A.I.2 --- Physical Characterization --- p.136-138 / Appendix II / Chapter A.II.1 --- "Selected Crystallographic Data for Compounds 1,2,4,5,7,9,14,15,16,17 and 18" --- p.142-147 / Chapter A.II.2 --- 1H and 13C NMR Spectra --- p.148-150 / Chapter A.II.3 --- Chromatogram and Mass spectra (El and Cl) from GCMS Analysis --- p.151-157 / Chapter A.II.4 --- Mass Spectra --- p.158-162

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