Dissertations / Theses: 'Synthesis of organometallics'

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Bott, Adrian William. "Clusters : synthesis and topology." Thesis, University of Cambridge, 1989. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.316027.

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Abdelsalam, Mansour. "Synthesis of piperidines using organometallic chemistry." Thesis, University of Sheffield, 2013. http://etheses.whiterose.ac.uk/4069/.

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Stern, James Andrew. "The synthesis and manipulation of organoiron complexes." Thesis, Imperial College London, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.321665.

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Dennehy, Robert Daniel. "The synthesis and reactivity of titanium metallacycles." Thesis, University of Southampton, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.359239.

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Amoroso, Angelo James. "The synthesis and reactivity of osmium carbonyl clusters." Thesis, University of Cambridge, 1993. https://www.repository.cam.ac.uk/handle/1810/272544.

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Loveridge, Tracey. "Chiral chromium complexes in synthesis." Thesis, University of Oxford, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.296868.

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Ward, Mark Frederick. "The synthesis and reactivity of (vinylketene) iron(0) complexes." Thesis, Imperial College London, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.294843.

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Charlton, Adam. "Synthesis, characterisation, and evaluation of novel nonlinear optical materials." Thesis, Bangor University, 1994. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.359051.

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De, Lima Geraldo Magela. "The synthesis, characterization and reactivity of some tin(II) compounds." Thesis, University of Sussex, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.360500.

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Wong, D. M. "Synthesis, structure and reactivity of chiral cyclopentadienyl ruthenium (II) complexes." Thesis, University of Salford, 1996. http://usir.salford.ac.uk/43028/.

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This thesis concerns the preparation, structural, and reactivity studies of new chiral monometallic cyclopentadienyl ruthenium(II) complexes exhibiting a combination of metal-centred and ligand-derived chirality.

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McCormick, Gillian J. "Synthesis and reactivity of naphthyne complexes of ruthenium." Thesis, Brunel University, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.389113.

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Lawrence, Heather Bunting Elizabeth. "Organometallic compounds with non-linear optical properties." Thesis, University of Oxford, 1990. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.276835.

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Martinelli, Marcia. "The synthesis and properties of some organo-ruthenium and organo-osmium clusters." Thesis, University of Cambridge, 1991. https://www.repository.cam.ac.uk/handle/1810/271906.

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Collier, Philip Edward. "Synthesis and reactivity of titanium imido complexes." Thesis, University of Nottingham, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.243752.

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Nichols, Lorna Susan. "The synthesis and structural characterisation of novel main group organometallics." Thesis, University of Southampton, 2006. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.438681.

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Barozzino, Consiglio Gabriella. "Organometallics in regio- and enantio-selective synthesis : structures and reactivity." Rouen, 2010. http://www.theses.fr/2010ROUES022.

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Ce travail présente deux études en chimie organométallique (organolithiens). Dans le premier chapitre, des réactions d'isomérisation réalisées en présence de superbases bimétalliques sont impliquées, et la transformation d'aziridines fonctionnalisées est examinée. Deux voies sont possibles : la β-élimination ou la cyclisation 4-exo intracyclique. Le processus réactionnel étant accompagné de la formation de centre(s) stéréogène(s), une approche asymétrique est explorée avec 3-APLi's. Le deuxième chapitre s'intéresse à l'étude structurale de phosphines (boranes) lithiées dans le but d'aborder la synthèse énantiosélective d'alkylphosphines P-stéréogéniques. Ce travail de thèse a permis d'examiner la structure en solution d'une phosphine borane lithiée modèle (Ph2P(BH3)Li) en solution par spectroscopie RMN multinoyaux (1H, 6Li, 13C, 11B, 31P). L'affinité du phosphure avec le BuLi puis la LDA a ensuite été examinée Questo lavoro di tesi è stato focalizzato su due tematiche alla chimica degli organometalli (ed in particolare degli organolitio derivati). Nella prima parte sono state studiate le reazioni di isomerizzazione in presenza di superbasi bimetalliche ed è stata esaminata la reattività di aziridine funzionlizzate. Due meccanismi sono possibili : la β-eliminazione e la ciclizzazione 4-exo intramolecolare. Dato che la reazione è accompagnata dalla formazione di uno o più centri stereogenici, è stata anche studiata una versione asimmetrica. La seconda parte descrive uno studio di fosfine-borani litiati. Questo lavoro è parte di un programma consistente nella sintesi di alchifosfine P-stereogeniche enantioarricchite. Il nostro contributo consiste nella determinazione della struttura di una litio fosfide-borano (Ph2P(BH3)Li) grazie alla tecnica di analisi NMR multinucleare (1H, 6Li, 13C, 11B, 31P). È stata anche analizzata l'affinità della lithio fosfide per il BuLi e poi per l'LDA This work focuses on two studies related to organometallic chemistry (organolithiums). In the first chapter, isomerisation reactions are conducted in the presence of bimetallic superbases and the evolution of functionalized aziridines is examinated. Two issues are possible for this transformation : the β-elimination or the 4-exo intracyclic cyclisation. Because the reaction leads to the formation of stereogenic center(s), an asymmetric version is also studied with 3-APLi's. The second chapter describes a structural study of lithiated phosphine-boranes. This work is part of a program consisting in the enantioselective synthesis of P-stereogenic alkylphosphines. Our contribution consists in the determination of the structure of a model lithiated phosphine-borane (Ph2P(BH3)Li) thanks to the multinuclear (1H, 6Li, 13C, 11B, 31P) NMR technique. The affinity for the phosphide to BuLi then LDA has also been examinated

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Palin, Michael G. "Synthesis and structure of diene-iron and arene-chromium complexes containing phosphine ligands." Thesis, Keele University, 1993. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.357157.

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Probert, Gareth David. "The zirconocene-mediated synthesis of amines." Thesis, University of Southampton, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.242623.

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Muldoon, David James. "Synthesis, structural and catalytic studies of some new complexes of molybdenum(II) and tungsten(II)." Thesis, Bangor University, 1994. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.385795.

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Moore, Rebecca J. "Novel approaches to natural product synthesis using organozinc intermediates." Thesis, University of Newcastle Upon Tyne, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.362516.

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Qi, Miao. "Developing an Electrochemically Redox Switchable System for Polymer Synthesis:." Thesis, Boston College, 2020. http://hdl.handle.net/2345/bc-ir:108945.

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Thesis advisor: Jeffery A. Byers This dissertation discusses the development of an electrochemically switchable system for copolymer synthesis as well as surface modifications. In Chapter one, the usage of electrochemistry to control polymerization reactivities is introduced. In Chapter two, an electrochemically redox switchable polymerization for lactide and cyclohexene oxide will be presented. In Chapter three, a surface modification method based on the electrochemically redox switchable catalysis is discussed. The surface-anchored catalyst responds to applied electrochemical potentials towards two different ring-opening polymerizations to generate binary polymer patterns in one step. The method represents a facile way to generate polymer coatings on surfaces. In Chapter four, a discussion on the detailed kinetic analysis of an iron-catalyzed epoxide polymerization will be presented, the study allows us to unveil the importance of entropy-controlled reactions. In Chapter five, future perspectives on the electrochemically redox switchable catalysis will be discussed Thesis (PhD) — Boston College, 2020 Submitted to: Boston College. Graduate School of Arts and Sciences Discipline: Chemistry

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El-Assiery, Saied Abdullah. "Synthesis of compounds containing phenolic or boronic acid residues by reaction of boron hydrides with metallated systems." Thesis, Lancaster University, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.317402.

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Matthews, Jennifer Louise. "The synthesis and potential applications of asymmetric silacycles." Thesis, Durham University, 1994. http://etheses.dur.ac.uk/5504/.

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Although the use of silicon-based reagents has undergone rapid development during the last twenty years, the application of organosilicon chemistry to asymmetric synthesis has been somewhat slower to develop. The many problems associated with the use of 'Si-centred' chiral organosilicon compounds has led to the application of 'C-centred' chiral organosilicon compounds. This work has been aimed at the synthesis and application of cyclic silicon species. Routes towards the synthesis of medium-sized rings have been investigated as a potential application of enantiomerically pure silacycles. This work has led to the discovery of an unusual tandem cycloaddition-bond fragmentation reaction of 3-(dienylacyloxy)cycloalk-2- en-l-ones, which affords a-tetralone as the principal product. Most work has been directed at the synthesis of asymmetric silacycles. Two routes have been explored. Firstly, the double asymmetric hydrosilylation of dienes, catalysts based on many transition metals were used but little evidence of hydrosilylation was observed. The second route is that of the double asymmetric hydroboration of divinylsilanes. Asymmetric stoichiometric hydroboration led to products of moderate to high enantiomeric excess, whilst rhodium-catalysed hydroboration led to high yields of the achiral syn isomer. The diastereoselectivity has been found to vary according to the length of the tether between two phosphine ligands, with maximum diastereoselectivity being observed for butanodiphosphines. NMR studies have investigated the possibility that this is related to the stability of a divinylsilane-diphosphine rhodium complex. Finally, the formation of a variety of silacycles has been attempted. Boron- redistribution of the product of hydroboration with (-)-diisopinocampheylborane has been shown to occur with retention of stereochemistry and subsequent carbonylation led to the formation of asymmetric silacyclohexanones. Oxidation of the hydroboration product led to the formation of a silyldiol species. Reactions of this silyldiol have provided the basis for encouraging preliminary attempts at the formation of other heterosilacycles.

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Hewlett, Dudley Francis. "The use of the [eta]Â²-aldehyde, ketone and benzyne complexes of Ti and Zr in organic synthesis." Thesis, University of Southampton, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.359225.

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Lian, Yiqian. "Chromium and iron organometallics in organic synthesis synthetic studies toward total synthesis of taxol and chromium to iron transfer processes /." Diss., Connect to online resource - MSU authorized users, 2006.

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Barbey, Sabine. "A novel approach to the ergot alkaloid skeleton." Thesis, University of Reading, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.294855.

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Yu, Yongfei. "Synthesis, structure and properties of some chiral-at-metal transition metal organometallics." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1998. http://www.collectionscanada.ca/obj/s4/f2/dsk1/tape10/PQDD_0015/NQ42488.pdf.

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Murphy, Don M. "Synthesis and properties of novel carboranes and organometallics for second harmonic generation." Thesis, University of Oxford, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.303617.

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Arbit, Ruslan Mikhaylovich. "I. Homologation of alpha-diketones. II. Synthesis of epiafricanol and advances toward longithorone a and paclitaxel." The Ohio State University, 2003. http://rave.ohiolink.edu/etdc/view?acc_num=osu1070356064.

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Joy, Jonathan Stuart. "Synthesis and charaterisation of mixed s-/p-block organometallics and p-block ligand systems." Thesis, University of Southampton, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.402058.

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Cardona, Laia Davin. "Exploiting cooperative effects in s-Block organometallics for new applications in synthesis and catalysis." Thesis, University of Strathclyde, 2017. http://digitool.lib.strath.ac.uk:80/R/?func=dbin-jump-full&object_id=28408.

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Focussing on group 1 and group 2 metals, this thesis advances the use of polar organometallics in catalysis, in particular intermolecular hydroamination processes; as well as other key stoichiometric transformations, namely deprotonative metallation and C-F bond activation. Group 1 alkyl compounds MCH2SiMe3 (M = Li, Na or K) have proved to be efficient catalysts for intermolecular hydroamination of a wide range of substituted vinylarenes and alkynes at room temperature and with short timescales. Similarly,advancing in the concept of s-block cooperative bimetallic catalysis, alkali-metal magnesiate complexes [MMg(CH2SiMe3)3] and [(donor)2M2Mg(CH2SiMe3)4] (M = Li,Na or K) have shown that they can also act as catalysts for these hydroamination processes, although longer times and high temperature conditions are required in some cases. Reactivity studies show an alkali-metal effect with potassium being significally more reactive than lithium. New insights into the constitution of the potential organometallic intermediates involved in these processes have also been gained by combining X-Ray crystallographic and NMR studies (including DOSY NMR).The second part of this thesis assesses cooperative effects of single-metal organomagnesium complexes in deprotonation and C-F bond activation processes. Using a specially designed metallating base, which combines within the same molecule a sterically demanding β-diketiminate ligand with a kinetically activatedTMP base [DippNacnacMg(TMP)], regioselective magnesiation of heterocyclic and aromatic molecules, including pyrazine or 1,2,4,5-tetrafluorobenzene, can be achieved at room temperature. Structural studies of these metallated intermediates have revealed a crucial stabilising role of the β-diketiminate ligand, which facilitates the trapping of the sensitive anions formed. Additionally, they have provided important clues to rationalise the stability of these species in solution. Contrastingly [DippNacnacMg(THF)Bu] complex is a much more kinetically retarded base, which fails to metallate these substrates promoting in some cases, when confronted with fluoroarenes, C-F bond activation process via nucleophilic aromatic substitution.

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Li, Chunmei. "Designing phase selective soluble polymers for applications in organic chemistry." Diss., Texas A&M University, 2003. http://hdl.handle.net/1969/105.

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Schofield, Daniel. "The synthesis and reactivity of Group 4 metal hydrazides." Thesis, University of Oxford, 2012. http://ora.ox.ac.uk/objects/uuid:8eb27904-237b-4065-ad37-6008166731e9.

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This thesis describes the synthesis, characterisation and reactivity of diamide-amine and bis(cyclopentadienyl) supported Group 4 hydrazido(2-) compounds towards unsaturated molecules. The mechanisms of these transformations are probed using a range of structural, kinetic and computational methods.

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Campbell, Michael Glenn. "Synthesis, Structure, and Reactivity of New Palladium(III) Complexes." Thesis, Harvard University, 2014. http://dissertations.umi.com/gsas.harvard:11289.

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Palladium is one of the most common and versatile transition metals used in modern organometallic chemistry. The chemistry of palladium in its 0, +II, and +IV oxidation states is well-known; by comparison, the chemistry of palladium in its +III oxidation state is in its infancy. The work in this thesis involves the study of previously unknown Pd(III) complexes, including applications in materials chemistry and catalysis. Chemistry and Chemical Biology

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Orchard, Katherine Lorraine. "The mild synthesis of zinc oxide nanoparticles and nanocomposites via hydrolysis of well-characterised zinc organometallics." Thesis, Imperial College London, 2011. http://hdl.handle.net/10044/1/17786.

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This thesis centres on the development of a clean, one step method for generating surface-functionalised zinc oxide (ZnO) nanoparticles for application in the synthesis of well-dispersed inorganic-organic nanocomposites. The nanoparticle synthesis method utilises the controlled hydrolysis of organometallic zinc compounds, employing diethylzinc as a bulk precursor and an alkylzinc carboxylate as a substoichiometric, secondary precursor to deliver the capping ligands. A series of ethylzinc carboxylate species were synthesised and studied by NMR spectroscopy (EtZn(OOCR); R = H, CH3, and (CH2)nCH3, where n = 4, 10, 16). The ligand stoichiometry of the complexes was found to depend on the nature of the solvent (coordinating vs. non-coordinating), and single crystal X-ray experiments indicated that the strength of the donor interaction of a coordinating solvent affects the nuclearity of the complex‟s repeat unit in the solid state. In addition, the isolated complexes of the acetate derivative were active catalysts for the copolymerisation of CO2 and cyclohexene oxide. The ZnO nanoparticle synthesis route was first explored in the absence of a polymer matrix and was proven to yield hydrophobic nanoparticles with a narrow size distribution without the need for size selection steps (average particle size 3.6 ± 0.2 nm, σ = 15% using stearate; HR-TEM). The effect of varying different synthesis parameters on the resulting ZnO particle size and morphology was investigated. Additional inorganic zinc phases were observed on slowing the reaction rate, allowing insight into the mechanism of delivery of carboxylate groups to the growing nanoparticle surfaces. Finally, in situ ZnO/epoxy resin nanocomposites were prepared. The degree of nanoparticle dispersion improved with surface-functionalisation in the order stearate < uncapped < benzoate (TEM), which correlated with the nature of the particle-matrix interaction (DSC). In situ prepared nanoparticles (uncapped) were also introduced into conventional microcomposites and found to improve the composite density and thermal conductivity relative to the highest loading of microparticles alone.

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Charette, Bronte J. "Synthesis, coordination chemistry and reactivity of new diarylamido and disilylamido SeNSe pincer ligands." Canadian Science Publishing, 2015. http://hdl.handle.net/1993/31830.

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This thesis presents advancements in the chemistry of selenium-bearing pincer ligands with respect to their synthesis, metal association and reactivity in addition to the overall nature of selenium as a donor atom. The synthesis of a new disilylamido ligand HN(SiMe2CH2SePh)2 2.1 and its potassium salt 2.2 is reported. The attempted metal association of these species was unsuccessful with various transition metals. Multinuclear NMR data suggests coordination to silver(I), 2.3 and copper(I), 2.4 with dπ-dπ back donation from the metal to the selenium donors. It is suggested from this data that –SePh can potentially act as a π-acceptor ligand as well as a σ- donor with heavy d metals. Another explanation for the observed shielding is conformational restrictions introduced by chelation. The preparation of new selenium-bearing diarylamine compounds RN(C7H6SeMe)2 (R=H: 3.1; R= Me: 3.10; R= Boc 3.11) via aryllithium chemistry is reported. Unsuccessful attempts to synthesize the –SePh and –SetBu derivatives are described using: aryllithium chemistry, Buchwald-Hartwig Amination cross coupling and Pd-catalyzed C-Se cross coupling. When reacted with MCl2(COD) (M= Pd, Pt), compound 3.10 coordinates with PdII forming a bidentate complex 3.12, while 3.1 forms tridentate complexes with PdII and PtII. NMR spectroscopy suggests the formation of a silver(I) complex 3.1-Ag from 3.1 and AgOTf, but X-ray diffraction data is required to determine its coordination motif. The new ligands and complexes have been fully characterized by (1H, 13C, 77Se) NMR spectroscopy and X-ray crystal structures are reported for 3.10, 3.12, 3.3 and 3.4. The NMR spectrum of 3.1-Ag exhibits a similar effect as the complexes of disilylamido ligands with suggested potential dπ-dπ back donation from the metal to the selenium donors. The catalytic ability of the new complex 3.3 has been tested in the Suzuki-Miyaura cross coupling reaction without notable improvements to existing catalysts. The instability of reactive intermediates may contribute to the low conversions or the size of the methyl group may decrease nanoparticle formation, a suggested active species. October 2016

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Kaplan, Hilan. "A General Approach to Cis-Fused Sesquiterpene Quinones and Synthesis, Characterization, and Catalytic Applications of Bis(Imino)-N-Heterocyclic Carbene Complexes of Iron." Thesis, Boston College, 2014. http://hdl.handle.net/2345/3862.

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Thesis advisor: James P. Morken Sesquiterpene quinones are a prolific class of marine natural products that are particularly interesting due to their antibacterial, antiviral, and anti-inhibitory properties. Hundreds of these biologically active molecules are based on decalin frameworks, both cis- as well as trans-fused, however, significantly less synthetic work has focused on targeting the cis-fused series of compounds. In this chapter, progress towards an asymmetric, general route to various sesquiterpene quinones in the cleordane family of natural products will be described. The key steps of the synthesis include a highly convergent and diastereoselective reductive alkylation to forge both the requisite cis-ring fusion well as the all carbon quaternary center, as well as a scandium-catalyzed ring expansion of a 6,5-ring system to deliver the decalin core of the molecule. Additionally, the chapter includes the development and substrate scope of both methodologies utilized in the key complexity building reactions. Iron complexes ligated by bis(imino)pyridine ligands are remarkably active catalysts for a vast range of organic transformations including polymerization, hydrogenation, hydrosilylation, and hydroboration. Whereas much work has been done to probe the importance of the imine-substituents on catalysis, significantly less information is known about the nature of the central pyridine donor. To study the effects of a more donating ligand in which the pyridine is replaced with an N-heterocyclic carbene, a series of novel ligands and their corresponding iron complexes were synthesized and characterized. Whereas imidazole-derived complexes exhibited exclusively bidentate binding modes, 4,5,6-trihydropyrimidylidene-based ligands adopted a tridentate pincer conformation analogous to complexes of bis(imino)pyridines. Bonding in the five-coordinate bis(imino)-N-heterocyclic carbene complex displayed considerably contracted iron-ligand bond distances compared to the analogous bis(imino)pyridine iron complex. The study of physical and electronic structure and bonding in organometallic compounds is a critical for understanding and predicting complex behavior and reactivity. Having synthesized a completely new type of N-heterocyclic carbene (NHC) ligand and the corresponding iron complex, a rigorous study of metal-NHC bonding, magnetism, and redox activity in bis(imino)-NHC (or carbenodiimine, CDI) complexes of iron was carried out. A series of oxidation and reduction reactions on CDI complexes of iron were performed, enabling access to complexes spanning from formally iron(0) to iron (III) oxidation states. A battery of spectroscopic and computational methods, including X-ray crystallography, Mössbauer spectroscopy, SQUID magnetometry, and EPR spectroscopy established the CDI ligand as a redox active chelator. Additionally, a unique iron-carbene interaction was discovered, in which the metal center antiferromagnetically couples with the carbon of the NHC. Intent on developing CDI complexes of iron into practical catalysts for both synthetic organic transformations and polymerization, a series of stoichiometric as well as catalytic reactions were carried out to evaluate the reactivity profile of the novel complexes. Halide atom abstraction generated a new cationic species, which demonstrated different coordination chemistry compared to the bis(imino)pyridine analogue. Furthermore, the addition of a hydride or alkyl lithium reagent to the parent (CDI)FeCl2 species resulted in interesting and unexpected reactivity involving the carbene ligand. Preliminary catalytic hydrogenation experiments established (CDI)FeCl2 as a competent catalyst for the reduction of simple alkenes in the presence of Na(Hg) as a reductant under 80 psi of hydrogen. Additionally, the dichloride species could be readily converted into bis(aryloxide) complexes that were active for the polymerization of lactide to produce poly(lactic acid). The polymerization is very controlled (PDI values are <1.3), and polymers with molecular weights of around 35 kDa can be obtained after 3 hours at room temperature Thesis (PhD) — Boston College, 2014 Submitted to: Boston College. Graduate School of Arts and Sciences Discipline: Chemistry

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Hlavinka, Mark Louis. "Dizinc organometallics based on pre-organized binucleating bis(amidoamine) ligands; synthesis, structure, and reactivity of zinc enolates." Diss., Connect to online resource, 2006. http://gateway.proquest.com/openurl?url_ver=Z39.88-2004&rft_val_fmt=info:ofi/fmt:kev:mtx:dissertation&res_dat=xri:pqdiss&rft_dat=xri:pqdiss:3207756.

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Mayberry, Darrell D. "Synthesis, Characterization, and Reactivity of Prochiral Ruthenium Clusters and Bimetallic Rhenium Complexes with an Unsymmetrical Diphosphine and Hard-Soft Donor Ligands." Thesis, University of North Texas, 2019. https://digital.library.unt.edu/ark:/67531/metadc1538707/.

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The reaction of [BrRe(CO)₄]₂ with 2-(diphenylphosphino)pyridine (PN) and 6-(diphenylphosphino)-2-formylpyridine (PON) was investigated. The reactions were regiospecific and exclusively produced the phosphorus-coordinated products, BrRe(CO)₄(κᵖ-PN) and BrRe(CO)₄(κᴾ-PON). The kinetics for the chelate ring closure (κᴾ→ κᴾᴺ) in BrRe(CO)₄(κᴾ-PN) were confirmed to occur by dissociative CO loss. The reaction of [BrRe(CO)₄]₂ with 2-(diphenylphosphino)pyridine (PN) was modeled computationally by DFT calculations. The preferred reaction pathway for the substitution reaction was determined to occur by direct attack of the pnictogen donor on the dimer and formation of the κᴺ isomer as the kinetic substitution product occurs. The κᴺ kinetic product then rapidly isomerizes to the κᴾ thermodynamic product by way of a reversible ligand dissociation. Treatment of the tetrahedral cluster H₂Ru₃(CO)₃(μ₃-S) (1) with 2-(diphenylphosphino)thioanisole (PS) furnishes the cluster H₂Ru₃(CO)₇(κ²-PS)(μ₃-S) (2). Cluster 2, which exhibits a chelated thiophosphine ligand (κ²-PS), exists as a pair of diastereomers with Keq = 1.55 at 298 K that differ in their disposition of ligands at the Ru(CO)(κ²-PS) center. The PS ligand occupies the equatorial sites (Peq, Seq) in the kinetic isomer and axial and equatorial sites (Pax, Seq) in the thermodynamically favored species. The reversible first-order kinetics to equilibrium have been measured experimentally by NMR spectroscopy and HPLC over the temperature range 293-323 K. The substitution reaction involving 1 and the isomerization of the PS ligand in 2 were investigated by DFT calculations. The computational results support a phosphine-induced expansion of the cluster polyhedron that is triggered by the associative addition of the PS donor to 1. The observed isomerization of the PS ligand in 2 is best explained by a tripodal rotation of the CO and PS groups at the Ru(CO)(κ²-PS) center that is preceded by a regiospecific migration of one of the edge-bridging hydrides to the non-hydride-bridged Ru-Ru bond in 2. The chiral clusters 1,2-Ru₃(μ-H)₂(μ₃-S)(CO)₇(μ-1p1,2p2-POP) (A) and 1,2-Ru₃(μ-H)₂(μ₃-S)(CO)₇(μ-1p2,2p1-POP) (B) were formed were formed from reaction of Ru₃(μ-H)₂(μ₃-S)(CO)₉ with 1-diphenylphosphino-2-[2-(diphenylphosphino)ethoxy]benzene (POP). Chiral clusters A and B were fully characterized by IR and NMR spectroscopy. Additionally, the molecular structure of A was solved by X-ray crystallography. Chiral cluster A was resolved into its enantiomers by preparative HPLC with a chiral column. The enantiomers were characterized by electronic circular dichroism (ECD) spectroscopy and their absolute stereochemical configuration was determined by X-ray crystallography.

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Thomas, Jaron Michael. "On Metal synthesis of Some Substituted Rhenium and Manganese Complexes." TopSCHOLAR®, 2012. http://digitalcommons.wku.edu/theses/1225.

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Heterocyclic organic and organometallic compounds (i.e. polypyrrole), and their derivatives, have been of great interest for conductive polymers due to their novel properties and environmental stability as compared to their non-aromatic analogs (i.e. polyacetylene). Our current interest focus upon the potential role of metal ligand bound pyridazines as the next generation of electronic devices that utilize the metal ligands bound to organics as the semiconducting material. Pyridazine is a 6-membered aromatic ring with two adjacent nitrogen atoms. These are promising candidates for a variety of materials and commercial applications; but they are difficult to get a metal ligand to fuse to the aromatic ring. Our recent efforts focused in attaching Rhenium and Manganese ligands/substituents (process in which is called doping) that would cause oxidation to occur to our polymer making it a p-type polymer. Since p-type polymers charge carriers leave a vacancy that does not delocalize completely. This vacancy (known as a hole) or a radical cation that only partially delocalizes over several monomeric units causing them to be structurally deformed. This deformed structure is at a higher energy than that of an undoped polymer. Typical carriers in organic semiconductors are holes and electrons in a π-orbital. So when these molecules of π-conjugated systems have a π-bond overlap (or π- stacking), electrons can move via these π-electron clouds overlapping thus causing an electrical current. Our worked focused on the synthesis of pyridazines and their organometallic rhenium complexes and polymer research. Several aryl-substituted 5,6-fused pyridazines have been synthesized but none have been documented until this study. The main goal of the research was to fully characterize the general synthesis of furan containing organometallic complexes, [M(CO)3{η5-1,2-C5H3(CC4H3ON)(CC4H3ON)}] (M = Re or Mn) (4B). We successfully characterized the ability to attach a metal organic ligand to pyridazine though IR and NMR. However, when attempts were made to recrystallize our product, we yielded an orange-brown, block like crystal of 1,2- C5H3(CC4H3ONH)(CC4H3ON) (5) in which our metal ligand group fell off and we were left with pyridazine and inorganics. Though, we successfully got an X-ray characterization and electronic studies of compound 5 which are reported herein.

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Clevenger, Margo. "Synthetic Routes to 3-Fold Symmetric Tridentate Oxygen Donor Ligands." Thesis, Virginia Tech, 1997. http://hdl.handle.net/10919/36964.

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The class of ligands represented by [CpCo(P(O)(OR)2)3]-, L- , were first synthesized by W. KlÃ¤ui in 1977. These ligands have been found to coordinate to a variety of low and high oxidation state metals through the use of its three P=O oxygen atoms as donors. The ligands act as mono-anionic six electron donors which make them similar to the more widely known cyclopentadienyl ligands, (C5H5-xRx)-, but have electronic properties like those of fluoride or oxide. Also, it has been found that the coordination chemistry of L- resembles the unsubstituted tris(pryrazolyl)hydroborato six electron ligand, (RB(pz)3)-. All three of these ligands can be modified by changing the substituent R. The KlÃ¤ui ligand offers a good opportunity to synthesize a chiral derivative. In the process to obtain the chiral version, (cyclopentadienyl)tris(biphenyl-phosphito-P)cobaltate(1-), 18, was synthesized from 2,2'-biphenol. This was characterized through NMR, mass spectroscopy, and XPS. Next, a racemic version, (cyclopentadienyl)tris(biphenylphosphito-P)cobaltate(1-), 17, was synthesized from (Â±)1,1â -bi-2-naphthol. A one-pot synthesis for the rac-binaphthyl phosphite derivative was developed with an increased yield from the previously published synthesis. The racemic version of the ligand was characterized by NMR and mass spectroscopy. The chiral version has not yet been synthesized, however, by following the developed procedure for the non-chiral version, the ligand could be synthesized from optically active 1,1'-bi-2-naphthol. Master of Science

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Palmer, Erick J. "Synthesis, characterization and density functional theory investigations of tris-cyclopentadienyl compounds of zirconium and hafnium." The Ohio State University, 2005. http://rave.ohiolink.edu/etdc/view?acc_num=osu1109969235.

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43

Smith, Charlene Amanda. "The synthesis and magnetochemistry of transition and lanthanide metal compounds." Thesis, University of Manchester, 2013. https://www.research.manchester.ac.uk/portal/en/theses/the-synthesis-and-magnetochemistry-of-transition-and-lanthanide-metal-compounds(1f50bd6e-19e2-4cf6-9211-e22fcef578f9).html.

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The introductory Chapter to this thesis outlines fundamental aspects of 4f lanthanide(III) coordination chemistry, in particular compounds that possess the intriguing properties of slow relaxation of magnetisation, (or the ability to behave as single-molecule magnets, SMMs). The recent renaissance into the study of the magnetic behaviour of 4f-coordination complexes has led to the consideration of utilising organometallic precursors for the development of novel lanthanide containing compounds, which may possess interesting magnetic properties, subsequently forming the basis of Chapter Two. In Chapter Two, the syntheses and structures of the novel lithiated thiolate ligand, lithium triphenylsilylthiolate, (Ph3SiS-Li) (2.1), and the sulfur-bridged, dimetallic dysprosium(III) and gadolinium(III) complexes [(MeCp)2Dy(µ-SSiPh3)]2 (2.2) and [(MeCp)2Gd(µ-SSiPh3)]2 (2.3), are described in detail. The structural and physical properties of these compounds are analysed through NMR, elemental analysis and SQUID magnetometry, alongside supporting theoretical calculations to reveal that compound 2.2 is the first dimetallic, sulfur-bridged SMM reported, giving an energy barrier to the reversal of magnetisation of Ueff = 192 ± 5 K.56bChapter Three reports on the structural development of a series of lanthanide monomers, exhibiting the general motif [Ln(OSiPh3)3(THF)3] (where Ln = Dy(3.4), Er(3.5), Ho(3.6), Gd(3.7), Tb(3.8)), exploiting the siloxide ligand Ph3SiOH through two novel synthetic routes. This Chapter also provides new analytical insight to these complexes by exploring their magnetic properties through a series of SQUID measurements and through the analysis of their electronic properties using air sensitive, variable temperature optical absorption spectroscopy. Compounds 3.4 and 3.5 were revealed to be SMMs, with 3.5 having a much higher thermal barrier to the reversal of magnetisation, Ueff = ~ 28 K, than 3.4, which are supported by theoretical analysis. Chapter Four describes the utility of ligand 2.1 and Ph3SiOH in the context of 3d transition metal cyclopentadienyl chemistry, outlining the syntheses and structures of three distinct compounds; the trimetallic, [Cp2Mn3(µ-OSiPh3)4](4.7), the hetero-cubane tetramer [CpMn(µ-SSiPh3)]4 (4.8) and the dimetallic thiolate-bridged [CpCr(µ-SSiPh3)]2 (4.9) compound. These compounds were formed in reactions exploiting organometallic manganocene and chromocene precursors. Magnetic susceptibility measurements were conducted on these compounds to gain further insight into their structural properties. The magnetic exchange coupling constants for Mn(II) compounds 4.7 and 4.8 were J = - 4.4 cm-1 and J = - 3.0 cm-1 respectively. Furthermore, having demonstrated the use of metal-cyclopentadienyl building blocks in the synthesis of novel SMMs, Chapter Five discusses the possibility of further advancement on the development of this class of magnetic molecules.

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Stokes, Francesca Alice. "Synthetic applications of polar transition metal metallocenes." Thesis, University of Cambridge, 2013. https://www.repository.cam.ac.uk/handle/1810/264975.

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Since the sandwich structure of ferrocene was elucidated in 1952, metallocenes have generated a vast amount of interest. Transition metal metallocenes have previously been shown to be suitable precursors in the syntheses of novel organometallic and metallo-organic complexes, although the use of metal halide starting materials for organometallic synthesis is much more common due to their being readily commercially available and generally easier to handle than the extremely air- and moisture-sensitive metallocene alternatives. In this project, the polar transition metal metallocenes Cp2V, Cp2Cr, Cp2Mn and Cp2Ni were employed as precursors in the synthesis of fourteen novel metal containing complexes, in several cases generating products which could not have been obtained using metal halide starting materials.

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Poulten, Rebecca. "Synthesis and reactivity of low coordinate nickel(I) complexes bearing ring expanded N-heterocyclic carbene ligands." Thesis, University of Bath, 2015. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.669038.

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This thesis describes the development of nickel(I) complexes incorporating ring expanded N-heterocyclic carbene (RE NHC) ligands and examines their electronic characterisation, activation of O2, reactivity and catalytic applications. A series of three coordinate, paramagnetic Ni(I) complexes of the form Ni(RE NHC)(PPh3)Br (1 – 10) were prepared by comproportionation of Ni(COD)2 and Ni(PPh3)2Br2 in the presence of RE NHCs. The RE NHCs employed varied in the degree of ring expansion (6-, 7- and 8-membered), extent of N-substituent steric bulk (Mes, oTol, oAnis) and the donor/acceptor properties of the carbene (diamino vs. diamido). EPR and DFT electronic characterisation of 1 – 10 confirmed that the unpaired electron was located on the nickel ion in a mixed orbital of predominantly 3dz2 character. Yellow solutions of 1 or 6 (RE NHC = 6Mes and 7Mes respectively) immediately became purple in the presence of O2 due to O2 activation and incorporation of the oxygen atoms as bridging ligands resulting from C-H activation/oxygenation of an RE NHC N-substituent. This generated the dimeric Ni(II) complexes Ni(6/7Mes)Br(µ-OH)(µ-O-6/7Mes)’NiBr (6Mes = 13; 7Mes = 14). Mass spectrometry demonstrated that the doubly activated complexes [NiBr(µ-O-6/7Mes)’]2 (15 and 16 respectively) were also formed in the reactions. UV-vis spectroscopy revealed the reactions took place rapidly, even at 190 K. Contrasting reactivity was observed when 2 or 7, bearing the less sterically encumbered N-oTol substituents 6oTol and 7oTol respectively, were exposed to O2, which led to the ligand redistribution products NiII(6/7oTol)(PPh3)Br2 (17 and 18 respectively). The less electron rich diamido analogue containing 6MesDAC (5), underwent dissociation and oxidation of the RE NHC and PPh3 ligands. Attempts to abstract the bromide from 1 generated novel two and three coordinate Ni(I) products. Reaction with additional 6Mes produced the two coordinate cation [Ni(6Mes)2]+ (19), which could be reduced with KC8 to Ni(6Mes)2 (20). SQUID analysis of 19 revealed it to be the first example of a nickel containing mononuclear single molecular magnet (SMM). Addition of [Et3Si]+ to 1 followed by work up in toluene led to the isolation of the Ni(I)-(η2-toluene) complex [Ni(6Mes)(η2-C6H5CH3)]+ (21). Mesitylene generated the analogous [Ni(6Mes)(η2-C6H3(CH3)3)]+ (23), but neither 1,4-xylene nor naphthalene gave isolable products. In all cases, cocrystallisation of [6MesH]+…arene was observed in variable amounts, which compromised reaction studies of the Ni-arene complexes. Removal of bromide from 1 with TlPF6 in THF generated the solvent coordinated cationic species [Ni(6Mes)(PPh3)(THF)]+ (24). Attempts to remove the ligated THF molecule were unsuccessful, however, it could be directly substituted by CO to form [Ni(6Mes)(PPh3)(CO)]+ (26). Similarly to 1, complex 24 activated O2, generating a dimer analogous to the singly activated complex 13 (Ni(6Mes)(PPh3)(µ-OH)(µ-O-6Mes)’NiBr (25)). Reactivity of 1 with NaBH4 produced [Ni(6Mes)(κ2-BH4)]2 (28), a Ni(I) dimer bridged by two BH4 ligands. The catalytic efficiency of neutral 1 in Kumada cross-coupling of aryl halides and PhMgCl or MesMgBr was probed. Of note was the high activity towards both aryl chlorides and aryl fluorides. Comparisons with cationic 24, larger 7- (7) and 8-membered ring (8 and 9) variants and the Ni(II) complexes Ni(6Mes/6oTol/7oTol)(PPh3)Br2 (29, 17 and 18 respectively) revealed that 1 exhibited the highest reactivity of all the precursors.

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Bertrand, Benoit. "Gold-based complexes : synthesis and evaluation as anticancer agents." Thesis, Dijon, 2015. http://www.theses.fr/2015DIJOS013.

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Depuis sa mise sur le marché à la fin des années 70, le Cisplatin est devenu l’un des pricipaux agents de chimiothérapie anticancéreuse. Actuellement, les composés à base de platine sont présents dans la majorité des coktails de chimiothérapie. Cependant, malgré leur succès clinique, ces composés présentent de nombreux inconvenients comme par exemple de nombreux et graves effets secondaires. Une des stratégies envisagées pour parer à ces défauts a été de remplacer le platine par d’autres métaux de transition. Parmi les différents métaux possibles, l’or est apparu comme particulièrement prometteur. En effet, les propriétés pharmacologiques de l’or sont bien connues depuis des siècles, et aujourd’hui encore certains complexes d’or sont utilisés comme agents anti-arthritiques. Plus récement, il a été démontré que les complexes d’or étaient actifs sur des lignées cellulaires cancéreuses résistantes au Cisplatin. Parmi les différentes classes de composés à base d’or synthétisées et testées, certaines familles de complexes organométalliques tel que les carbènes N-hétérocycliques, les complexes à ligands cyclométallés ou alkynyl ont attiré un intérêt tout particulier à cause de leur grande stabilité en milieu physiologique.Dans le présent manuscrit, nous avons présenté la synthèse de différents types de de complexes à base d’or incluant des carbènes N-hétérocycliques d’or(I), des complexes « bifonctionnels » d’or(I) basés sur le lansoprazole, des complexes (C^N) cyclométalés d’or(III) ainsi que des complexes homo- et hétérobimétalliques présentant un motif or(I)-NHC. Les différents composés ont été testés sur des panels de lignées cellulaires cancéreuses humaines et les résultats ont été comparés à un modèle de cellules rénales humaines saines. Nous avons effectué différentes études mécanistiques pour tenter d’élucider le possible mécanisme d’action de ces composés. Ces investigations ont inclus des études de toxicité sur des tissus sains ex vivo utilisant des tranches de tissus coupés avec précision ainsi que l’identification de possible cibles intracellulaires. Nous avons étudié deux possibles enzymes cibles : la thiorédoxine réductase et la poly(ADP-ribose) polymérase 1 ainsi qu’une structure non-usuelle de l’ADN : la structure G-quadruplexe. L’internalisation cellulaire de certains composés fluorescents a aussi été étudiée par microscopie confocale. Parmi les différents composés testés, certains ont montré une sélectivité pour les cellules cancéreuses qui mérite une étude plus approfondie Currently, platinum-based compounds are present in the majority of the chemotherapeutic cocktails. However, despite their clinical success, platinum-based drugs present several limitations including numerous and severe side effects. A strategy envisaged to overcome these limitations is the replacement of platinum by other transition metals. Among the different metals tested over the years, gold compounds have been shown to be promising as they can overcome resistance to cisplatin due to their different modes of action.In the present thesis, we present the synthesis of different types of gold-based complexes including gold(I)-N-heterocyclic carbenes (NHC), (C^N) cyclometalated gold(III) complexes as well as heterobimetallic complexes bearing a gold(I)-NHC moiety. These compounds show higher stability in a physiological environment compared to classical platinum complexes The different compounds have been tested in panels of human cancer cell lines and a model of human healthy kidney cells. Moreover, “bifunctional” lansoprazole-based gold(I) complexes were also evaluated for their biological properties in vitro. On selected compounds we also performed mechanistic studies to try to elucidate their possible mechanisms of action. Specifically, we investigated two possible enzyme targets: thioredoxin reductase and poly(ADP-ribose) polymerase 1, as well as DNA G-quadruplexes. The cellular uptake of some fluorescent compounds was also studied using confocal microscopy techniques. In a few cases, we also assessed their toxicity ex vivo in rat healthy tissues using the precision-cut tissue slices technique. Among the twenty gold-based compounds we synthesized, two of them presented interesting selective toxicity for cancer cells compared to healthy cells and tissues and deserve further investigations as potential anticancer drugs

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47

Qin, J. "Studies in organometallic solid state chemistry." Thesis, University of Oxford, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.379942.

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Zini, Simone. "Synthesis of manganese organometallic complexes." Master's thesis, Alma Mater Studiorum - Università di Bologna, 2021. http://amslaurea.unibo.it/22235/.

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Il presente lavoro di tesi si inserisce in un progetto di ricerca volto alla sintesi di nuovi complessi di metalli di transizione per lo sviluppo di catalizzatori da impiegare in reazioni di catalisi omogenea. In particolare il mio progetto si è concentrato sulla sintesi di complessi organometallici di manganese con leganti carbenici N-eterociclici (NHC). La scelta dei leganti è stata effettuata in modo tale da poter avere leganti chelanti NHC di tipo MIC (mesoionic carbene) sintetizzati tramite cicloaddizione tra un alchino ed un azide catalizzata da rame (CuAAC) e N-alchilazione. Lo studio di questi complessi a base di manganese è ancora tutt’oggi agli albori, leganti NHC vengono molto utilizzati grazie alla possibilità di variarne le proprietà steriche ed elettroniche e alla possibilità di formare legami forti con quasi tutti i metalli. Il manganese è stato scelto poiché un elemento abbondante, poco tossico e poco costoso. The present thesis work is part of a research project aimed at the synthesis of new transition metal complexes to be used in homogeneous catalysis reactions. In particular my project focused on the synthesis of manganese organometallic complexes with N-heterocyclic carbene ligands (NHC). The choice of ligands was carried out to have NHC chelating ligands of the class of MIC (mesoionic carbene). These ligands are synthesized by cycloaddition between alkyl and azide with a copper-catalyzed reaction (CuAAC) and N-alkylation in order to obtain MIC after deprotonation. The study of these manganese-based complexes is still in its infancy today, NHC ligands are widely used thanks to the possibility of varying their steric and electronic properties and the possibility of forming strong bonds with almost all metals. The choice of manganese was made because is an abundant, low-toxic and inexpensive element.

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Lee, Peter D. "Organometallic synthesis in supercritical fluids." Thesis, University of Nottingham, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.336862.

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50

Stewart, A. S. J. "Organometallic derivatives of amino acids and peptides." Thesis, Robert Gordon University, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.376684.

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Dissertations / Theses on the topic 'Synthesis of organometallics'

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