Dissertations / Theses: 'Metal complexes. Ruthenium. Iron'

1

Guest, Ruth Winifred. "Synthesis and reactions of iron and rutheniuim dinitrogen complexes." Connect to full text, 2008. http://ses.library.usyd.edu.au/handle/2123/3533.

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Thesis (Ph. D.)--University of Sydney, 2008.
Includes tables. Includes list of publications: leaves i-ii. Title from title screen (viewed October 30, 2008). Submitted in fulfilment of the requirements for the degree of Doctor of Philosophy to the School of Chemistry, Faculty of Science. Includes bibliographical references. Also available in print form.

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2

Walters, Stephen John. "Acyl(oxy) carbene and vinylidene chemistry of iron and ruthenium half-sandwich complexes." Thesis, University of Sheffield, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.245691.

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3

Xie, Jin. "Synthesis, structures and spectroscopic properties of primary and secondary phosphine complexes of iron, ruthenium and osmium porphyrins." Click to view the E-thesis via HKUTO, 2007. http://sunzi.lib.hku.hk/HKUTO/record/B39556876.

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4

Xie, Jin, and 解錦. "Synthesis, structures and spectroscopic properties of primary and secondary phosphine complexes of iron, ruthenium and osmiumporphyrins." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2007. http://hub.hku.hk/bib/B39556876.

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5

鄧煒堂 and Wai-tong Tang. "Homogeneous oxidation of organic substrates by ruthenium, iron and manganese tertiary amine complexes." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 1989. http://hub.hku.hk/bib/B31231706.

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6

Tang, Wai-tong. "Homogeneous oxidation of organic substrates by ruthenium, iron and manganese tertiary amine complexes /." [Hong Kong : University of Hong Kong], 1989. http://sunzi.lib.hku.hk/hkuto/record.jsp?B12355203.

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7

Burgun, Alexandre. "Oxidative activation of iron- and ruthenium-alkynyl complexes : toward square-shaped molecules with four redox-active metal centres." Rennes 1, 2011. http://www.theses.fr/2011REN1S081.

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8

Turner, David Benjamin. "Photochemistry of Group 8 Metal Complexes of Type [M(bpy)2(CN)2] (M = Fe, Ru). Photosynthesis of Heteroleptic Iron(II) Compounds and Photoionization of Ruthenium(II) Compounds." The Ohio State University, 2009. http://rave.ohiolink.edu/etdc/view?acc_num=osu1253238745.

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9

Buitrago, Elina. "Transition metal-catalyzed reduction of carbonyl compounds : Fe, Ru and Rh complexes as powerful hydride mediators." Doctoral thesis, Stockholms universitet, Institutionen för organisk kemi, 2012. http://urn.kb.se/resolve?urn=urn:nbn:se:su:diva-75795.

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A detailed mechanistic investigation of the previously reported ruthenium pseudo-dipeptide-catalyzed asymmetric transfer hydrogenation (ATH) of aromatic ketones was performed. It was found that the addition of alkali metals has a large influence on both the reaction rate and the selectivity, and that the rate of the reaction was substantially increased when THF was used as a co-solvent. A novel bimetallic mechanism for the ruthenium pseudo-dipeptide-catalyzed asymmetric reduction of prochiral ketones was proposed. There is a demand for a larger substrate scope in the ATH reaction, and heteroaromatic ketones are traditionally more challenging substrates. Normally a catalyst is developed for one benchmark substrate, and a substrate screen is carried out with the best performing catalyst. There is a high probability that for different substrates, another catalyst could outperform the one used. To circumvent this issue, a multiple screen was executed, employing a variety of ligands from different families within our group’s ligand library, and different heteroaromatic ketones to fine-tune and to find the optimum catalyst depending on the substrate. The acquired information was used in the formal total syntheses of (R)-fluoxetine and (S)-duloxetine, where the key reduction step was performed with high enantioselectivities and high yield, in each case. Furthermore, a new iron-N-heterocyclic carbene (NHC)-catalyzed hydrosilylation (HS) protocol was developed. An active catalyst was formed in situ from readily available imidazolium salts together with an iron source, and the inexpensive and benign polymethylhydrosiloxane (PMHS) was used as hydride donor. A set of sterically less demanding, potentially bidentate NHC precursors was prepared. The effect proved to be remarkable, and an unprecedented activity was observed when combining them with iron. The same system was also explored in the reduction of amides to amines with satisfactory results.

At the time of doctoral defense, the following paper was unpublished and had a status as follows: Paper 2: Manuscript.

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10

Orth, Nicole [Verfasser], Ivana [Akademischer Betreuer] Ivanovic-Burmazovic, and Ivana [Gutachter] Ivanovic-Burmazovic. "Development of a Novel Inorganic Enzyme Mimetic with Dual Functionality and Characterization of Catalytically Active Copper, Iron and Ruthenium Complexes and Metal Based Self-Assemblies by Cryospray-Ionization Mass Spectrometry / Nicole Orth ; Gutachter: Ivana Ivanovic-Burmazovic ; Betreuer: Ivana Ivanovic-Burmazovic." Erlangen : Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), 2021. http://d-nb.info/1237107652/34.

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11

Whittlesey, Michael Keith. "Reactivity of iron and ruthenium dihydride complexes." Thesis, University of York, 1991. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.280400.

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12

Barthram, Anita Marie. "Metal-metal interactions in polynuclear complexes of ruthenium and osmium." Thesis, University of Bristol, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.326683.

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13

Guest, Ruth Winifred. "Synthesis and Reactions of Iron and Ruthenium Dinitrogen Complexes." University of Sydney, 2008. http://hdl.handle.net/2123/3533.

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Doctor of Philosophy (PhD)
This thesis is primarily concerned with the synthesis and reactions of iron and ruthenium dinitrogen complexes of tripodal phosphine ligands. Of particular interest is the cationic dinitrogen bridged iron complex [(FeH(PP3))2(μ-N2)]2+ 23, containing the tetradentate ligand P(CH2CH2PMe2)3, PP3 1, and its potential for facilitating the reduction of the bound dinitrogen upon treatment with acid. The synthesis of a selection of novel and known tripodal phosphine and amino phosphine ligands is described. New ligands N(CH2CH2CH2PMe2)3 N3P3 7 and P(CH2CH2CH2PiPr2)3 P3Pi3 11 were synthesised by nucleophilic displacement of bromide from the bromoalkylphosphine and bromoalkylamine precursors with the relevant phosphide. A new method for synthesis of known ligand P(CH2CH2CH2PMe2)3 P3P3 19 by the nucleophilic substitution of its chloroalkylphosphine oxide with dimethylphosphide and subsequent reduction is also reported. The reaction of [(FeH(PP3))2(μ-N2)]2+ 23 with base produced the singly deprotonated mixed valence species [(FeH(PP3))(μ-N2)(Fe(PP3))]+ 37 and subsequently the iron(0) dinuclear species (Fe(PP3))2(μ-N2) 38 and mononuclear complex Fe(N2)(PP3) 44. The 15N labelling of complexes has allowed the 15N NMR spectra of 23, 37 and 44 to be reported along with the observation of a long-range 5JP-P coupling across the bridging dinitrogen of 37. Complexes 23 and 37 were also structurally characterised by X-ray crystallography. The treatment of a variety of iron PP3 1 dinitrogen complexes, including the mononuclear species [(Fe(N2)H(PP3)]+ 22, with acid, or base then acid, did not result in the formation of ammonia from reduction of the complexed dinitrogen. The reactions of FeCl2(PP3) 24 and FeClH(PP3) 25 with ammonia and hydrazine afforded the complexes [FeCl(N2H4)(PP3)] 48, [FeH(N2H4)(PP3)] 47, [FeCl(NH3)(PP3)] 49 and [FeH(NH3)(PP3)] 46. Complexes 47 and 46 are considered potential intermediates in any reduction of the dinitrogen ligand of 23 to ammonia. Complexes 49 and 46 were also formed from the decomposition of the hydrazine complexes 48 and 47. The 15N NMR shifts, derived from both the 15N labelling of complexes and from 1H-15N 2D NMR experiments at natural abundance are reported. In addition, complex 47 was characterised by X-ray crystallography. The novel ligand P(CH2CH2PiPr2)3 PPi3 12 was used in the successful synthesis of [FeCl(PPi3)]+ 51 and [RuCl(PPi3)]+ 56. Reduction of 51 and 56 with potassium graphite under dinitrogen afforded the complexes Fe(N2)(PPi3) 52 and Ru(N2)(PPi3) 57 respectively. This is the first report of a Ru(0) dinitrogen complex. Treatment of 52 and 57 with lutidinium tetrafluoroborate resulted in protonation and oxidation of the metal centre to afford the hydrido complexes [Fe(N2)H(PPi3)]+ 53 and [Ru(N2)H(PPi3)]+ 58 respectively. 15N labelled analogues of 52, 53, 57 and 58 were achieved by exchange reactions with 15N2 gas, allowing for analysis by 15N NMR spectroscopy. Species 52, 57 and 58 have also been structurally characterised by X-ray crystallography. Treatment of 52 with excess acid in THF afforded both 53 and the dihydrogen complex [Fe(H2)H(PPi3)]+ 54. The mechanism of formation of 54 probably involves the C-H activation of the solvent THF. The complex cation [RuCl(P3Pi3)]+ 65 was synthesised using the novel ligand P3Pi3 11. A polymeric iron(II) complex, [Fe2Cl4(N3P3)2]n 66, of the tridentate ligand N3P3 7 was also synthesised. Characterisation of both 65 and 66 by X-ray crystallography is reported. (FeCl)2(μ-Cl)2(μ-Pi2)2 68, an unusual bridged dimer of the known ligand CH2(PiPr2)2 Pi2 67, and iron(II) and iron(0) tetramers of the PP3 1 ligand, namely [Fe4Cl4(PP3)5]4+ 71 and Fe4(PP3)5 72 were also characterised by X-ray crystallography.

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14

Yang, Mei. "Iron(II) and ruthenium(II) polypyridyl complexes as photosensitizers." Available to US Hopkins community, 2003. http://wwwlib.umi.com/dissertations/dlnow/3080801.

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15

Morewood, Catherine Alexandra. "π-complexes of osmium and ruthenium organometallic clusters." Thesis, University of Cambridge, 1995. https://www.repository.cam.ac.uk/handle/1810/272792.

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16

Luther, Thomas Alan. "Dicationic dihydrogen complexes of osmium and ruthenium /." Thesis, Connect to this title online; UW restricted, 1997. http://hdl.handle.net/1773/11540.

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17

Brown, Thomas Joseph. "The use of (cyclopentadienone)iron tricarbonyl complexes and ruthenium complexes for hydrogen transfer reactions." Thesis, University of Warwick, 2017. http://wrap.warwick.ac.uk/103451/.

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The synthesis of (cyclopentadienone)iron tricarbonyl complexes and the application of said complexes to the catalysis of ‘hydrogen borrowing’ reactions between amines and alcohols has been studied. A family of analogous (cyclopentadienone)iron tricarbonyl complexes were synthesised and used in ‘hydrogen borrowing’ with aniline and analogous alcohol reagents comprising increasing carbon chain length, in an attempt to gain more understanding of the effect of altering the electron environment of the hydroxy group of the active iron catalysts generated from the synthesised (cyclopentadienone)iron tricarbonyl complexes. Utilising an alternative set of reaction conditions, the scope of the ‘hydrogen borrowing’ methodology was extended to include amines derived from piperidine, benzylamine and other aliphatic amines. The incorporation of additional functionality (e.g. alkene or alkyne groups) into the product amines was also found to be an option of the new methodology. The synthesis of novel asymmetric (cyclopentadienone)iron tricarbonyl complexes was also attempted and a novel application of Ru(II)/TsDPEN hydrogen transfer catalysts was also discovered.

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18

Wong, Chun-yuen. "Ruthenium-carbon bonding interaction synthesis and spectroscopic studies of ruthenium-acetylide, -carbene, -vinylidene and -allenylidene complexes." Click to view the E-thesis via HKUTO, 2004. http://sunzi.lib.hku.hk/hkuto/record/B31040858.

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19

Greguric, Ivan. "Molecular recognition of DNA by metal co-ordination complexes /." [Campbelltown, N.S.W.] : University of Western Sydney, Macarthur, Faculty of Informatics, Science and Technology, 1999. http://library.uws.edu.au/adt-NUWS/public/adt-NUWS20030624.114833/index.html.

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20

Pokharel, Uttam Raj. "ORGANOMETALLIC HETEROCYCLES AND ACENE-QUINONE COMPLEXES OF RUTHENIUM, IRON AND MANGANESE." UKnowledge, 2012. http://uknowledge.uky.edu/chemistry_etds/6.

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A variety of organometallic-fused heterocycles and acene quinones were prepared and characterized. This work was divided into three parts: first, the synthesis of 5,5-fused heterocyclic complexes of tricarbonylmanganese and (1’,2’,3’,4’,5’-pentamethylcyclopentadienyl)ruthenium; second, the synthesis of 1,2-diacylcyclopentadienyl p-cymene complexes of ruthenium(II); and third, synthesis of cyclopentadienyl-fused polyacenequinone complexes of ruthenium, iron and manganese. The first examples of the convenient, versatile and symmetric cyclopentadienyl-fused heterocycle complexes of (1’,2’,3’,4’,5’-pentamethylcyclopentadienyl)ruthenium(II) and tricarbonylmanganese(I) were synthesized starting from (1,2-dicarbophenoxycyclopentadienyl)sodium. The sodium salt was transmetalated using [MnBr(CO)5] and 1/4 [Ru(μ3-Cl)(Cp*)]4 to give [Mn(CO)3{η5-C5H3(CO2Ph)2-1,2}] and [Ru{η5-C5H3(CO2Ph)2-1,2}(Cp*)]. The diester complexes were saponified under basic conditions to obtain the corresponding dicarboxylic acids. The dicarboxylic acids were used to synthesize unique cyclopentadienylmetal complexes including diacyl chlorides, anhydrides, thioanhydrides and p-tolyl imides of ruthenium and manganese. Similarly, a series of 1,2-diacylcyclopentadienyl-p-cymene cationic complexes of ruthenium were synthesized using thallium salt of 2-acyl-6-hydroxyfulvene and [Ru(η6-p-cymene)(μ-Cl)Cl]2 in a 2:1 ratio with an intension of converting them into heterocycle-fused cationic sandwich complexes. However, our attempts of ring closing on 1,4-diketons with sulfur or selenium were unsuccessful. A methodology involving the synthesis of metallocene-fused quinone complexes was employed starting from pentamethylruthenocene-1,2-dicarboxylic acids. The diacyl chloride was prepared in situ from the dicarboxylic acids and used for Friedel-Crafts acylation. We observed single-step room-temperature diacylation of aromatics, including benzene, o-xylene, toluene, 1,4-dimethoxybenzene and ferrocene with pentamethylruthenocene-1,2-diacyl chloride to obtain the corresponding quinone complexes. Similarly, we synthesized mononuclear and binuclear γ-quinones by aldol condensation of 1,2-diformylcyclopentadienylmetal complexes with cyclohexane-1,4-dione or 1,4-dihydroxyarenes. The third methodology involves the Friedel-Crafts acylation of ferrocene with 2-carbomethoxyaroyl chlorides followed by saponification, carbonyl reduction, and ring closing by second Friedel-Crafts acylation to give Ferrocene-capped anthrone-like tricyclic and tetracyclic ketones. The oxidation of the ketones gave [3,4-c]-fused α-quinone complexes of iron. The oxidative and reductive coupling, enolization and C-alkylation of the anthrone complex were studied. Solvolysis of α-carbinol gave α-ferrocenylcarbenium salt, which underwent dimerization on treatment with non-nucleophilic base. We were successful to trap the in situ generated trimethylsilylenol ether of ferrocene-anthrone using dienophiles like N-phenylmaleimide or dimethylacetylenedicarboxylate under Diels-Alder conditions.

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21

Wong, Chun-yuen, and 黃駿弦. "Ruthenium-carbon bonding interaction synthesis and spectroscopic studies of ruthenium-acetylide, -carbene, -vinylidene and -allenylidene complexes." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2004. http://hub.hku.hk/bib/B31040858.

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22

Vanover, Eric. "Photochemical Oxidation Studies of Porphyrin Ruthenium Complexes." TopSCHOLAR®, 2012. http://digitalcommons.wku.edu/theses/1201.

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In nature, transition metal containing enzymes display many biologically important, attractive and efficient catalytic oxidation reactions. Many transition metal catalysts have been designed to mimic the predominant oxidation catalysts in nature, namely, the cytochrome P450 enzymes. Ruthenium porphyrin complexes have been the center of this research and have successfully been utilized, as catalysts, in major oxidation reactions, such as the hydroxylation of alkanes. The present work focuses on photocatalytic studies of aerobic oxidation reactions with well characterized ruthenium porphyrin complexes. The photocatalytic studies of aerobic oxidation reactions of hydrocarbons The photocatalytic studies of aerobic oxidation reactions of hydrocarbons catalyzed by a bis-porphyrin-ruthenium(IV) μ-oxo dimer using atmospheric oxygen as the oxygen source in the absence of co-reductants were investigated. The ruthenium(IV) μ-oxo bisporphyrin (3a-d) was found to catalyze aerobic oxidation of a variety of organic substrates efficiently. By comparison, 3d was found to be a more efficient photocatalyst than the well-known 3a under identical conditions. A KIE at 298K was found to be larger than those observed in autoxidation processes, suggesting a nonradical mechanism that involved the intermediacy of ruthenium(V)-oxo species as postulated. The reactivity order in the series of ruthenium(IV) μ-oxo bisporphyrin complexes follows TPFPP>4- CF3TPP>TPP, and is consistent with expectations based on the electrophilic nature of the ruthenium(IV) μ-oxo bisporphyrin species. The trans-dioxoruthenium(VI) porphyrins have been among the best characterized metal-oxo intermediates and their involvement as the active oxidant in the hydrocarbon oxidation have been extensively studied. In addition to the well-known chemical methods, we developed a novel approach for generation of trans-dioxoruthenium( VI) porphyrins with visible light by extension of the known photoinduced ligand cleavage reactions. A series of trans-dioxoruthenium(VI) porphyrin complexes (6a-d) were photochemically synthesized and spectroscopically characterized by UV-vis, and 1H-NMR.

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23

Humphrey, Paul Andrew. "A study of transition metal complexes /." Title page, contents and summary only, 1990. http://web4.library.adelaide.edu.au/theses/09PH/09phh9262.pdf.

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24

Stuart, Clare Anne. "Reactions of ruthenium(II) diphosphine complexes with silver(I) salts." Thesis, University of Liverpool, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.366948.

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25

Klüh, Katharina. "Primary phosphine halfsandwich complexes of iron and ruthenium synthesis and hydrophosphination reactions /." [S.l.] : [s.n.], 2006. http://deposit.ddb.de/cgi-bin/dokserv?idn=981723179.

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26

Li, Yan, and 李艷. "Synthesis and reactivity of carbene complexes of iron, ruthenium and osmium porphyrins." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2004. http://hub.hku.hk/bib/B31245730.

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27

Gafoor, Mansoor Ahmed. "The synthesis and reactivity of some hydrocarbyl complexes of iron and ruthenium." Master's thesis, University of Cape Town, 1991. http://hdl.handle.net/11427/18335.

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We have reviewed the synthesis and properties of ethylene-bridged dinuclear transition metal complexes. The ethylene-bridged ruthenium complex [CpRu(CO)₂]₂[μ-(CH₂CH₂)] has been prepared. The characterization data (IR, ¹H and ¹³C NMR, and Mass spectral) and properties of this complex are discussed. The crystal structure of this complex has also been determined. The reactivity of this complex with donor ligands (CO, PMe₂Ph and PPh₃), protic acids (CF₃COOH and HCl), bromine, MeOH and with oxidants (Ph₃CPF₆ and AgBF₄) has been investigated. The new ruthenium complexes [{CpRu(CO)₂}₂{μ-(CnH₂n₋₁)}]PF₆ (n = 3 or 5), as well as their known iron analogues have been prepared. The crystal structures of [{CpM(CO)₂}₂{μ-(C₃H₅)}]PF₆ (M = Fe or Ru) have been determined. The fluxional behaviour of the complex [{CpRu(CO)₂}₂{μ-(C₃H₅)}]PF₆ has also been determined and discussed in comparison with the analogous iron complexes. A sequence of reactions of [CpM(CO)₂]₂[μ-(CH₂)₅] (M = Fe or Ru) with Ph₃CPF₆, CF₃COOH and NaI has been shown to give high yields of 1-pentene; the relevance of this reaction sequence is discussed. The synthesis and properties of the known ruthenium ethyl complex [CpRu(CO)₂(CH₂CH₃)] are compared with [CpRu(CO)₂]₂[μ-(CH₂CH₂)]. The synthesis, characterization and properties of the ruthenium haloalkyl complexes [CpRu(CO)₂{(CH₂)nX}] (n = 3, X= Cl, Br or I; n = 4 or 5, X= Br or I) are also described.

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28

Willis, Richard Ronald. "Synthesis and reactivity of heterobinuclear complexes of ruthenium-platinum and iron-platinum /." The Ohio State University, 1992. http://rave.ohiolink.edu/etdc/view?acc_num=osu1487841548268408.

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29

Bridgewater, Brian Michael. "Sterically hindered chiral transition metal complexes." Thesis, Durham University, 1998. http://etheses.dur.ac.uk/5022/.

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This thesis describes the synthesis, characterization and study of a series of organometallic compounds which all contain the same new ligand, l-phenyl-3-methyl-4,5,6,7-tetrahydroindenyl. The ligand forms a chiral complex once coordinated, and is relatively bulky when compared with ligands such as cyclopentadienyl or 4,5,6,7-tetrahydroindenyl.Chapter one of this thesis introduces cyclopentadienyl ligand chirality, cyclopentadienyl metal complex chirality and sterically demanding cyclopentadienyl systems. The synthesis and chemistry of tetrahydroindenes and some applications of chiral cyclopentadienyl metal complexes and their bulky analogues are also reviewed. Chapter two describes modifications to a literature preparation of the tetrahydroindenone precursor of the new tetrahydroindenyl ligand which lead to higher yields. The synthesis of the ligand itself is described, as well as the synthesis of a benzylidene-substituted hexahydroindene, which demonstrates a limitation in the flexibility of the synthetic route chosen. The synthesis, characterization and various properties of the following iron(II) compounds are discussed in chapter two; bis-l-phenyl-3-methyl- 4,5,6,7-tetrahydroindenyl iron (II), 2.3, l-phenyl-3-methyl-4,5,6,7-tetrahydroindenyl iron(II) dicarbonyl dimer, 2.4, and l-phenyl-3-methyl-4,5,6,7-tetrahydroindaiyl methyl dicarbonyl iron(II), 2.5. For all these iron complexes, the solid state molecular structures and the absolute configuration of the chiral ligand were determined using single crystal X-ray d iffraction. For 23 and 2.4, three isomers are possible, two enantiomers that are collectively termed the rac-isomer and a third isomer, the meso- isomer. Cyclic voltammetric studies on 2.3 indicate that it has a reversible one electron oxidation at 0.187 V (with respect to a non-aqueous Ag/AgCl standard electrode). The difference between this and the reversible one electron oxidation for (η-C(_5)H(_5))(_2)Fe (with respect to the same standard) is -0.314 V, therefore 2.3 is shown to be much more easily oxidized than (η-C(_5)H(_5))(_2)Fe. The solution-state infi-a-red spectrum of 2.4 is explained, with reference to a literature analysis of the unsubstituted analogue [CpFe(CO)(_2)](_2). The steric forces present in the various molecular environments are discussed in connection with the degree of phenyl-ring tilt relative to the cyclopentadienyl mean plane and the deviation of the other cyclopentadimyl substituents away from the metal centre. Subsequent reactions of compounds 2.4 and 2.5 are described. Attempts to make linked analogues of the new ligand are summarized in chapter two. In chapter three, two Zr(rV) compounds are prepared, bis (l-phenyl-3-methyl-4,5,6,7-tetrahydroindenyi) zirconium(fV) dichloride, 3.1, and bis (l-phenyl-3-methyl-4,5,6,7-tetrahydroindenyl) dimethyl zirconium(TV), 3.2. Upon crystallization, rac-3.1 spontaneously resolves into crystals containing only one enantiomer. The similarities and differences in the spectroscopic data for the iron(n) compounds of chapter two and the zirconium(IV) compounds of chapter three are discussed and possible explanations offered . The solid state molecular structures of 3.1 and 3.2 were determined by single crystal X-ray diffraction. Experimental details are given in chapter four, whilst the characterizing data are presented in chapter five. Details of the X-ray structure determinations are given in Appendix A.

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30

Wardell, E. M. "EXAFS studies on transition metal complexes." Thesis, University of Manchester, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.377729.

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31

Steiger, George Edward. "Synthesis and thermal decomposition of alkyl-olefin chelate complexes of iron and ruthenium." Diss., Georgia Institute of Technology, 1992. http://hdl.handle.net/1853/28052.

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32

Hansen, Craig Allen. "Carbonyl cyclopentadienylnitro complexes of iron and ruthenium and their oxygen atom transfer reactions." Diss., The University of Arizona, 1988. http://hdl.handle.net/10150/184482.

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New and reactive nitro organometallics, Fe(C₅H₅)(CO)₂(NO₂), Ru(C₅H₅)(CO)₂(NO₂), their nitrogen-15 derivatives, Fe(C₅H₅)(CO)(PPh₃)(NO₂), and [Fe(C₅H₅)(CO)(PPh₃)L]NOₓ (where L = MeOH or MeCN and x = 2 or 3), were isolated and characterized by elemental analysis, IR, and NMR. The compounds were made by reactions of [Fe(C₅H₅)(CO)₂]₂, Fe(C₅H₅)(CO)₂I, [Ru(C₅H₅)(CO)₂]₂, and Fe(C₅H₅)(CO)(PPh₃)I with silver nitrite. The molecular and packing structures of Fe(C₅H₅)(CO)₂(NO₂) and Ru(C₅H₅)(CO)₂(NO₂) were determined by single-crystal X-ray diffractometry at -100°C and 26°C, respectively. Although stable at low temperature, Fe(C₅H₅)(CO)₂(NO₂) and Fe(C₅H₅)(CO)(PPh₃)(NO₂) decomposed at room temperature with evolution of CO₂ and concomitant formation of unstable metal nitrosyl complexes. In the case of Fe(C₅H₅)(CO)₂(NO₂), the mixture of products included Fe(C₅H₅)(CO)(NO), [Fe(C₅H₅)(NO)]₂, Fe(C₅H₅)₂, N₂O, CO, intractable material, and [Fe(C₅H₅)(CO)₂]₂. The kinetics of the oxygen transfer reactions of Fe(C₅H₅)(CO)₂(NO₂) and Fe(C₅H₅)(CO)(PPh₃)(NO₂) have been studied by NMR and IR of the solution, by IR and manometry of the gas phase, and by IR and elemental analysis of the intractable residues. The enthalpies and entropies of activation were obtained from Eyring plots of the reaction rate constants of Fe(C₅H₅)(CO)₂(NO₂) at 20, 30, and 40°C. Ru(C₅H₅)(CO)₂(NO₂) decomposes slowly with evolution of CO₂ at 40°C. In addition to the experiments outlined above, the dissertation includes discussions of the coordination chemistry of the new compounds in light of the few reports of other nitro organometallics and the calculations of molecular orbitals and energies. Also, the angular orientation of the basicity of the nitrite ion was probed by extended Huckel calculations of the orbital energies of hydrogen nitrite as the proton was moved around the nitrite ion. Lastly, ⁵⁷Fe-¹³P spin-spin coupling was measured in Fe(CO)₄(PPh₃) by ³¹P NMR.

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33

Whiteoak, Christopher John. "Studies on Molybdenum, Iron and Ruthenium Complexes with Tetradentate Ligands as Oxidation Catalysts." Thesis, Imperial College London, 2009. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.516482.

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34

Chan, Ka-ho, and 陳嘉豪. "Ruthenium-N-heterocyclic carbene and ruthenium acetylide complexes supported by macrocyclic porphyrin or tetradentate schiff base ligands : synthesis, structure and catalytic applications." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2015. http://hdl.handle.net/10722/211130.

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35

Page, Simon Matthew. "Ruthenium anticancer complexes : a targeted approach to enzyme inhibition." Thesis, University of Cambridge, 2013. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.608027.

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36

Ono, Takashi. "Second-Row Transition-Metal Complexes Relevant to CO2." Doctoral thesis, Universitat Rovira i Virgili, 2014. http://hdl.handle.net/10803/276964.

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dinucleares de rutenio que contienen ligandospolypyridyl. Estos complejos se han aplicado para las reacciones catalíticas, tales como la reducción de CO2 y la oxidación del agua y sustrato orgánico. En la primera, las actividades catalíticas hacia la reducción de CO2 se han investigado desde el punto de vista de las propiedades electrónicas y estéricas de los catalizadores, así como su nuclearidad. En el segundo, la aplicación de mono-y dinucleares complejos de Ru-aqua que contienen ligando tridentadoaniónico hacia reacción de oxidación se ha estudiado. Además, una reactividad potencial de dianión molibdato, que puede ser considerado como modelo homogéneo de catalizadores de óxido de metal heterogéneos para la transformación de CO2 se ha estudiado.
This thesis has been focused on the synthesis and characterization of a series of new mono- and dinuclear ruthenium complexes containing polypyridyl ligands. These complexes have been applied for the catalytic reactions, such as CO2 reduction and oxidation of water and organic substrate. In the first, the catalytic activities toward CO2 reduction have been investigated from the viewpoint of electronic and steric properties of the catalysts as well as their nuclearity. In the second, the application of mono- and dinuclear Ru-aqua complexes containing anionic tridentate ligand toward oxidation reaction has been studied. Additionally, a potential reactivity of molybdate dianion, which can be considered as homogeneous model of heterogeneous metal oxide catalysts for CO2 transformation has been studied.

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37

Johnson, David. "A computational study of ruthenium metal vinylidene complexes : novel mechanisms and catalysis." Thesis, University of York, 2013. http://etheses.whiterose.ac.uk/6170/.

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A theoretical investigation into several reactions is reported, centred around the chemistry, formation, and reactivity of ruthenium vinylidene complexes. The first reaction discussed involves the formation of a vinylidene ligand through non-innocent ligand-mediated alkyne-vinylidene tautomerization (via the LAPS mechanism), where the coordinated acetate group acts as a proton shuttle allowing rapid formation of vinylidene under mild conditions. The reaction of hydroxy-vinylidene complexes is also studied, where formation of a carbonyl complex and free ethene was shown to involve nucleophilic attack of the vinylidene Cα by an acetate ligand, which then fragments to form the coordinated carbonyl ligand. Several mechanisms are compared for this reaction, such as transesterification, and through allenylidene and cationic intermediates. The CO-LAPS mechanism is also examined, where differing reactivity is observed with the LAPS mechanism upon coordination of a carbonyl ligand to the metal centre. The system is investigated in terms of not only the differing outcomes to the LAPS-type mechanism, but also with respect to observed experimental Markovnikov and anti-Markovnikov selectivity, showing a good agreement with experiment. Finally pyridine-alkenylation to form 2-styrylpyridine through a half-sandwich ruthenium complex is also investigated. The mechanism for this process is elucidated, along with a description of the formation of the unexpected experimental deactivation product. Additionally the chemistry and bonding of pyridylidene complexes is also studied.

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38

Ke, Mingzhe. "Synthesis, characterization and reactivity of ruthenium porphyrin complexes containing metal-carbon bonds." Thesis, University of British Columbia, 1988. http://hdl.handle.net/2429/29126.

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The thesis describes developments in the organometallic chemistry of ruthenium porphyrin complexes, particularly their preparation, characterization and reactivity. Treatment of paramagnetic Ru(rV)(porp)Br₂ species, prepared via the interaction of [Ru(porp)]₂ with HBr in CH₂CI₂, with organolithiums or Grignard reagents yields the corresponding diamagnetic Ru(IV) complexes Ru(porp)R₂, where porp = the 2,3,7,8,12,13,17,18-octaethylporphyrinato dianion(OEP): R = Ph, m-MeC₆H₄, p-MeC₆H₄, p-MeOC₆H₄, p-FC₆H₄, Me, Et; and porp = the 5,10,15,20-tetraphenylporphyrinato dianion(TPP): R = Ph. The spectral analyses (¹H NMR, UV/vis, and mass spectroscopies) of these complexes are fully consistent with the assigned structures, which are further verified by the X-ray crystallographical analyses of Ru(TPP)Br₂ and Ru(OEP)Ph₂. The dimethyl complex Ru(OEP)Me₂ is also formed along with Ru(OEP)(P[sup n]Bu₃)₂ by the reaction of Ru(III)(OEP)(P[sup n]Bu₃)Br and methyllithium, the process involving disproportionation of Ru(OEP)Me(P[sup n]Bu₃). The diamagnetic nature of the Ru(porp)R₂ complexes, as evidenced by their sharp and temperature-independent ¹H NMR chemical shifts, requires that the d⁴-electrons of the Ru(IV) are spin-paired in the lowest, doubly degenerate d[sub xz] and d[sub]yz orbitals; the porphyrin ring current results in upfield shifts for the axial ligand protons with respect to their 'normal' positions. An unusual feature in the Ru(OEP)Ph₂ structure is the considerable distortion of the (Ph)C-Ru-C(Ph) fragment from linearity. The Ru(porp)R₂ complexes are stable as solids and in solution under atmospheric conditions, but the metal-carbon bonds are readily cleaved either by reagents such as protonic acids, carbon monoxide and phosphines, or via thermolysis. A CO insertion product Ru(OEP)Ph(COPh) is observed in solution by ¹H NMR spectroscopy upon the reaction of Ru(OEP)Ph₂ with 1 atm CO in deuterated benzene at room temperature. The anaerobic thermolysis of the Ru(porp)R₂ complexes at 80 - 100°C yields the five-coordinate, low-spin, paramagnetic Ru(porp)R derivatives, and organic products that depend on the nature of the aryl or alkyl moiety R and the solvent The remarkable transformations shown below have been demonstrated, and niechanisms are proposed.[See Thesis for Diagram] The Ru(OEP)Ph complex has been characterized crystallographically and, together with Ru(OEP)Ph₂, these represent the first reported structures involving organoruthenium porphyrins. The temperature-dependent *H NMR shifts for the Ru(OEP)R species establish a single spin state (S = 1/2) over the temperature range studied (-60° to 70°C). Under appropriate conditions in benzene or toluene, the rate-(leternnning step for the thermal decomposition of the Ru(OEP)R₂ species (R = aryl) is the homolytic cleavage of the metal-carbon bond, and the temperature variation data for the rate constant of this step allow for an estimation of the Ru-C bond strength in solution. Such bond energies are critical for a better understanding of homogeneously catalyzed hydrocarbon reactions. Substitution effects on the Ru-aryl bond strengths were studied using four para- and meta-substituted phenyl complexes (p-Me, p-MeO, p-F, and m-Me); the bond energies are in the 29 - 33 kcal/mol range, and a Hammett ρ value of +1.7 describes the rate constant trend for the p-MeO, p-Me and unsubstituted phenyl systems. Because of their ccordinatively unsaturated nature, the Ru(porp)R complexes are very reactive toward reagents. The Ru(OEP)Ph species readily binds a second axial ligand L, such as pyridine or tri-n-butylphosphine, to form a six-coordinate derivative, and temperature variation data for the equilibrium constant for pyridine binding give a solution bond energy of 11.2 kcal/mol for the Ru-N(py) bond. The Ru(OEP)Me species on reaction with L (py or P[sup n]Bu₃) undergoes disproportionation to Ru(OEP)Me₂ and Ru(OEP)L₂. The Ru(OEP)Ph species reacts with carbon monoxide to generate Ru(OEP)(CO)[sub n] (n = 1 or 2). Bromination of Ru(OEP)Ph forms a paramagnetic Ru(IV)(OEP)Ph(Br) intermediate, characterized by ¹H NMR, en route to Ru(OEP)Br₂, while treatment of Ru(OEP)Ph with HX (X = Br, CI) yields the Ru(OEP)X₂ species. Reaction of the Ru(OEP)(X-C₆H₄) complexes (X = H, p-MeO) with in situ-generated phenyl radicals is close to diffusion-controlled (k ≈ (1.4 - 2.0) X 10⁹ M⁻¹h⁻¹ at 60° - 100°C), and leads to the formation of the mixed aryl species Ru(OEP)Ph(p-MeOC₆H₄). Of interest, the photosensitized O₂-oxidation of Ru(porp)R species (R = aryl) yields the μ-oxo dinuclear species [Ru(porp)R]₂O, the metal-carbon bond remaining intact, which is unusual for the interaction of organometallic metalloporphyrins with dioxygen under light.
Science, Faculty of
Chemistry, Department of
Graduate

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39

Liu, Peng. "Oxidation and nitrene transfer reactions catalyzed by iron-oligopyridine complexes." Click to view the E-thesis via HKUTO, 2009. http://sunzi.lib.hku.hk/hkuto/record/B42664275.

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40

Liu, Peng, and 劉鵬. "Oxidation and nitrene transfer reactions catalyzed by iron-oligopyridine complexes." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2009. http://hub.hku.hk/bib/B42664275.

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41

Chen, Jun. "Transition Metal Complexes of Nucleosides for Cancer Chemotherapy." University of Dayton / OhioLINK, 2016. http://rave.ohiolink.edu/etdc/view?acc_num=dayton1461516224.

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42

Faulkner, Charlotte Waveney. "A study of some ruthenium(II) and manganese(I) acetylide and vinylidene complexes." Thesis, University of Cambridge, 1994. https://www.repository.cam.ac.uk/handle/1810/272793.

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43

Bitcon, Caroline. "Synthesis and redox properties of organometallic alkynyl complexes of molybdenum, tungsten, iron and ruthenium." Thesis, University of Manchester, 1988. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.328284.

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44

Adams, Michael R. "Synthesis and reactivity of homo- and heterobinuclear iron and ruthenium phosphido-bridged carbonyl complexes /." The Ohio State University, 1990. http://rave.ohiolink.edu/etdc/view?acc_num=osu1487677267731845.

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45

何毅雯 and Ngai-man Emmie Ho. "The chemistry of ruthenium carbonyl clusters containing nitrene and nitrido ligands." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2000. http://hub.hku.hk/bib/B3124029X.

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46

Ho, Ngai-man Emmie. "The chemistry of ruthenium carbonyl clusters containing nitrene and nitrido ligands /." Hong Kong : University of Hong Kong, 2000. http://sunzi.lib.hku.hk/hkuto/record.jsp?B21982351.

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47

Zapiter, Joan Marie Diangson. "Transition Metal Complexes Anchored on Europium Oxide Nanoparticles." Thesis, Virginia Tech, 2014. http://hdl.handle.net/10919/24786.

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Polypyridyl transition metal complexes containing ruthenium, rhodium and iridium centers are mainly studied due to their light absorbing and emitting properties. Lanthanide oxides such as europium oxide absorb light as well and exhibit strong luminescence and long lifetimes. The optical properties of these materials were significant especially in solar energy utilization schemes and optical applications. Energy transfer across a surface is important in several applications including phosphors and biomedical applications. Excited states of metal complexes with a carboxylate-containing ligand such as deeb = diethyl-2,2'-bipyridine-4,4'-dicarboxylate were studied on nanoparticle surfaces. In this work, [Rh(deeb)2Cl2](PF6), [Ir(deeb)2Cl2](PF6) and [Ir(deeb)2(dpp)](PF6)3 were synthesized using the building block approach. The metal complexes were characterized using 1H NMR spectroscopy, mass spectrometry, electronic absorption spectroscopy and electrochemistry. The 1H NMR spectra of the complexes were consistent with those of their ruthenium analogs. Mass spectra contain fragmentation patterns of the (M-PF6)+ molecular ion for [Rh(deeb)2Cl2](PF6) and [Ir(deeb)2Cl2](PF6), and (M-3PF6)3+ molecular ions for [Ir(deeb)2(dpp)](PF6)3. The electronic absorption spectrum of [Rh(deeb)2Cl2](PF6) shows a maximum at 328 nm, which is assigned as 1π→π*transition. The electronic absorption spectrum of [Ir(deeb)2Cl2](PF6) shows maxima at 308 nm and 402 nm, which are assigned as 1π→π* and metal-to-ligand charge transfer transitions, respectively. The [Ir(deeb)2(dpp)](PF6)3 complex exhibits peaks due to 1π→π* transitions at 322 nm and 334 nm. [Rh(deeb)2Cl2](PF6) has emission maxima from the 3LF state at 680 nm and 704 nm for the solid and glassy solutions at 77 K, respectively. [Ir(deeb)2Cl2](PF6) has emission maxima from the 3MLCT state at 538 nm in acetonitrile and 567 nm in the solid state at room temperature, with lifetimes of 1.71 μs and 0.35 μs, respectively. [Ir(deeb)2Cl2](PF6) has an unusually higher quantum yield than analogous compounds. [Ir(deeb)2(dpp)](PF6)3 has emission maxima from the 3IL state at 540 nm in acetonitrile and 599 nm in the solid state at room temperature, with lifetimes of 1.23 μs and 0.14 μs, respectively. Cyclic voltammetry of [Ir(deeb)2Cl2](PF6) and [Ir(deeb)2(dpp)](PF6)3 yield reversible and quasi-reversible couples corresponding to deeb ligand and Ir3+/+reductions, respectively. Attachment of the complexes were conducted by equilibration of complex solutions in acetonitrile with europium oxide nanoparticles. Europium oxide nanoparticles, which were synthesized by gas-phase condensation, have 11-nm diameters and exhibit sharp f-based luminescence in the visible and near IR regions. EDX, TEM, IR and reflectance spectroscopy measurements indicate substantial coating through various modes of attachment of the nanoparticle surface by the metal complexes while retaining the excited state properties of the metal complexes. Surface adsorption studies indicate monolayer coverage of the nanoparticle surface by the metal complexes, consistent with limiting surface coverages of previously reported analogous systems. Eu2O3 nanoparticles modified with [Rh(deeb)2Cl2]+ exhibit minimal to no energy transfer from emission spectra, and a reduction in the lifetime at 77K could be due to the rhodium complex preventing the excitation of Eu3+. Upon attachment of the Ir complexes [Ir(deeb)2Cl2]+ and [Ir(deeb)2(dpp)]3+ on as-prepared nanoparticles, Eu3+ luminescence was observed for nanoparticles modified with iridium complexes at room temperature, which could be due to energy transfer among other possibilities. Efficiencies of 68% and 50%, and energy transfer rate constants of 1.1 x 10-5 and 1.0 x 10-5 were calculated from lifetime data for [Ir(deeb)2Cl2]+ and [Ir(deeb)2(dpp)]3+ on Eu2O3 nanoparticles, respectively. Since iridium complexes are used as components of light-emitting diodes, europium oxide nanoparticles modified with iridium complexes have potential in optical applications which make studies of these compounds interesting.
Master of Science

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48

Hung, Wai Yiu. "Syntheses and reactivities of osmium and ruthenium complexes with metal-carbon triple bonds /." View abstract or full-text, 2006. http://library.ust.hk/cgi/db/thesis.pl?CHEM%202006%20HUNG.

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49

Nishizawa, Keita. "Environmentally Benign Metal-Catalyzed Living Radical Polymerization：Polymerization in Water and Iron Catalysis." 京都大学 (Kyoto University), 2016. http://hdl.handle.net/2433/215960.

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50

Kirgan, Robert A. "Diimine complexes of ruthenium(ii), rhenium(i) and iron(ii): from synthesis to DFT studies." Diss., Wichita State University, 2007. http://hdl.handle.net/10057/3981.

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The chloro and pyridinate derivatives of rhenium(I) tricarbonyl complexes containing the diimine ligands 2,2’-bipyrazine (bpz) and 5,5’-dimethyl-2,2’-bipyrazine (Me2bpz) are discussed. When compared to similar rhenium(I) tricarbonyl complexes of 2,2’-bipyridine (bpy) and 2,2’-bipyrimidine (bpm), the Me2bpz complexes are comparable to bpm derivatives and their properties are intermediate between those of bpy and bpz complexes. Also discussed is the synthesis and properties of two new analogues of ruthenium(II) tris-bipyridine, a monomer and dimer. The complexes contain the ligand 6,6’-(1,2-ethanediyl)bis-2,2’-bipyridine (O-bpy) which contains two bipyridine units bridged in the 6,6’ positions by an ethylene group. Crystal structures of the two complexes formulated as [Ru(bpy)(O-bpy)](PF6)2 and [(Ru(bpy)2)2(O-bpy)](PF6)4 reveal structures of lower symmetry than D3 which affects the electronic properties of the complexes as revealed by Density Functional Theory (DFT) and Time Dependent Density Functional Theory (TDDFT) calculations. Iron(II) tris-bipyrazine undergoes dissociation in solution with loss of the three bipyrazine ligands. The rate of the reaction in acetonitrile depends on the concentration of anions present in the solution. The rate is fastest in the presence of Cl- and slowest in the presence of Br-. In a second discussion DFT calculations are used to explore four iron(II) diimine complexes. DFT calculations show the higher energy HOMO (highest occupied molecular orbital) orbitals of the four complexes are metal centered and the lower energy LUMO (lowest unoccupied molecular orbitals) are ligand centered.
Dissertation(Ph.D.)--Wichita State University, College of Liberal Arts and Sciences, Dept. of Chemistry

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Dissertations / Theses on the topic 'Metal complexes. Ruthenium. Iron'

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