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Dissertations / Theses on the topic 'Cyclopentadienyl'

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Published: 4 June 2021

Last updated: 16 June 2025

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1

Sams, David W. I. "Studies on complexes bearing phosphaallyl, chiral cyclopentadienyl, di- or tri- cyclopentadienyl ligands." Thesis, University of Bristol, 1994. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.238828.

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2

Roy, Karin. "Kinetische Untersuchungen zur Hochtemperaturpyrolyse und -oxidation von Cyclopentadien und Cyclopentadienyl mit Hilfe der Stosswellentechnik." [S.l. : s.n.], 1999. http://deposit.ddb.de/cgi-bin/dokserv?idn=958163359.

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3

Roy, Karin. "Kinetische Untersuchungen zur Hochtemperaturpyrolyse und -oxidation von Cyclopentadien und Cyclopentadienyl mit Hilfe der Stoßwellentechnik." [S.l.] : Universität Stuttgart , Fakultät Chemie, 1999. http://www.bsz-bw.de/cgi-bin/xvms.cgi?SWB8385926.

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4

Harrison, Stephen Anthony. "Novel chiral cyclopentadienyl metal complexes." Thesis, University of Southampton, 2002. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.442873.

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5

Veighy, Clifford Robert. "Novel cyclopentadienyl transition metal complexes." Thesis, University of Southampton, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.327366.

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6

Ling, Xiaolan. "Silylated-cyclopentadienyl derivatives of zirconium." Thesis, University of Sussex, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.368492.

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7

Mackey, Olivia Nicola Denise. "Cyclopentadienyl derivatives of Main Group Elements." Thesis, Queen's University Belfast, 1990. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.334507.

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8

Beaumont, Ian R. "The chemistry of cyclopentadienyl cobalt complexes." Thesis, University of Nottingham, 1991. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.291970.

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9

Kuma, Karl Earl Adjetey. "A study of palladium cyclopentadienyl complexes." Thesis, University of Salford, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.299126.

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10

Plews, M. J. "Cyclopentadienyl uranium, neptunium and plutonium chemistry." Thesis, University of Manchester, 1985. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.355913.

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11

Duckett, Simon Benedict. "Silicon-hydride activation at cyclopentadienyl-rhodium." Thesis, University of York, 1989. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.329690.

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12

Wilden, Andreas. "Synthese chiraler metallorganischer Amino-Cyclopentadienyl-Komplexe /." Aachen : Mainz, 2009. http://d-nb.info/994128207/04.

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13

Piotrowski, Ingo. "Synthese von verbrückten, bifunktionellen Cyclopentadienyl-Imidazolyliden-Übergangsmetallkomplexen." [S.l.] : [s.n.], 2007. http://opus.kobv.de/tuberlin/volltexte/2007/1610.

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14

Marsh, Sarah Margaret Beatrice. "New amine-substituted cyclopentadienyl and indenyl ligands." Thesis, Durham University, 1997. http://etheses.dur.ac.uk/5012/.

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This thesis concerns the new amine-substituted cyclopentadiene and indene ligands C(_5)H(_5)(CH(_2))(_3)N((^t)Bu)H and C(_9)H(_7)(CH(_2))(_3)N((^t)Bu)H which can co-ordinate to a metal through all five carbon atoms of the five-membered ring (η(^5)) and/ or through the nitrogen (σ). Chapter 1 reviews the recent literature concerning Lewis-base functionalised cyclopentadienyl and indenyl ligands and their compounds with s-, p-, d- and f-block metals. Chapter 2 contains a brief review of possible synthetic routes to amine-substituted cyclopentadienyl and indenyl ligands with some examples from the recent literature, and a detailed account of the synthesis of C(_5)H(_5)(CH(_2))(_3)N((^t)Bu)H and C(_9)H(_7)(CH(_2))(_3)N((^t)Bu)H. The amino alcohol (^t)BuNH(CH(_2))(_3) OH was synthesised by the conjugate addition of (^t)BuNH(_2) to ethyl acrylate and reduction of the product ester (^t)BuNH(CH(_2))(_2)C0(_2)Et using LiAIH(_4). (^t)BuNH(CH(_2))(_3)OH was converted into (^t)BuNH(CH(_2))(_3)Br.HBr and (^t)BuNH(CH(_2)(_3)Cl.HCl by reaction with HBr or SOCI(_2). Reaction between (^t)BuNH(CH(_2))(_3)C1.HC1 and two equivalents of Na(C(_5)H(_5)) gave C(_5)H(_5)(CH(_2))(_3)N((^t)Bu)H in good yield. Treatment of (^1)BuNH(CH(_2))(_3)C1.HC1 with excess NaOH followed by reaction with Li(C(_9)H(_7)) gave C(_9)H(_7)(CH(_2))(_3)N((^t)Bu)H, also in good yield. Chapter 3 describes the synthesis of various main group and iron compounds of C(_5)H(_5)(CH(_2))(_3)N((^t)Bu)H and C(_9)H(_7)(CH(_2))(_3)N((^t)Bu)H. Lithium salts Li[C(_5)H(_4)(CH(_2))(_3)N((^t)Bu)H], Li[C(_5)H(_4)(CH(_2))(_3)N((^t)Bu)]Li, Li[C(_9)H(_6)(CH(_2))(_3)N((^t)Bu)H] and Li[C(_9)H(_6)(CH(_2))(_3)N((^t)Bu)]Li were prepared for use as reactive intermediates and Li[C(_5)H(_4)(CH(_2))(_3)N((^t)Bu)H] was characterised as its THF-adduct by (^t)H NMR spectroscopy. The silyl derivatives (Me(_3)Si)C(_5)H(_4)(CH(_2))(_3)NH(^t)Bu and (Me(_3)Si)C(_5)H(_4)(CH(_2))(_3)N((^t)Bu)SiMe(_3) were synthesised and characterised by NMR spectroscopy, and (Me(_3)Si)C(_9)H(_6)(CH(_6))(_3)N((^t)Bu)H and (Me(_3)Si)C(_9)H(_6)(CH(_2))(_3)N((^t)Bu)(SiMe(_3)) were also synthesised. The anune-substituted ferrocene Fe{η(^5)-C(_5)H(_4)(CH(_2))(_3)N((^t)Bu)H}(_2) was synthesised and oxidised to the corresponding ferricenium ion which was isolated as its PF(_6)(^-) salt. Exploratory work was carried out into the preparation of heterobimetallic species by reaction between Fe{η(^5)-C(_5)H(_4)(CH(_2))(_3)N((^t)Bu)H}(_2) and MX(_2) (M = Co, Ni, X = CI, M = Mn, X = Br). The substituted bis(indenyl) iron(II) complex Fe{η(^5)-C(_9)H(_6)(CH(_2))(_3)N((^t)Bu)H}(_2) was also synthesised. Chapter 4 is an account of the chemistry of {η(^5) :σ-C(_5)H(_4) (CH(_2))(_3)N(^t)Bu}Ti(NMe(-2))(_2) which was synthesised by an aminolysis reaction between C(_5)H(_5)(CH(_2))(_3)NH(^t)Bu and Ti(NMe(_2))(_4) Reaction between this compound and various weak acids gave a range of new compounds including{η(^5):σ-C(_5)H(_4)(CH(_2))(-3)N(^t)Bu} Ti(O(^t)Pr)(_2), {η(^5):σ-C(_5)H(_4)(CH(_2))(_3)N(^t)Bu)(_2), {η(^5):σC, {η(^5):σ-C(_5)H(_4)(CH(_2))(_3)N(^t)Bu}Ti(C(_5)H(_5))(NMe(_2)) , {η(^5):σ-C(_5)H(_4)(CH(_2))(_3)N(^t)Bu}Ti(SnBu(_3))(_z) and the imido-bridged dimer [{η(^5):σ-C(_5)H(_4)(CH(_2))(_3)N(^t)Bu}Ti(NHPh)](_2)(µ-NPh)2, the X-ray structure of which is reported. Chapter 5 describes the experimental procedures used, and chapter 6 gives lists of characterising data for each compound. Appendix A gives details of the methods used for magnetic susceptibility determinations; appendix B lists X-ray crystallographic data for [ {η(^5):σ-C(_5)H(_4)(CH(_2))(_3)N(^t)Bu}Ti(NHPh)](_2)(µ-NPh)(_2) and appendix C lists departmental colloquia attended.

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15

Gathergood, Nicholas Keith Peter. "Chiral cyclopentadienyl lanthanide and transition metal complexes." Thesis, University of Southampton, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.284648.

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16

Russell, Christopher Alan. "Reactive post d'1'0 organometallics." Thesis, University of Cambridge, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.388482.

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17

Hussain, Mazhar. "Cyclopentadienyl nickel complexes bearing a pendant phosphane tether." [S.l.] : [s.n.], 2005. http://deposit.ddb.de/cgi-bin/dokserv?idn=979445892.

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18

Sohns, Andreas. "Halfsandwich iron complexes with silanol-functionalized cyclopentadienyl ligands." Doctoral thesis, [S.l.] : [s.n.], 2005. http://deposit.ddb.de/cgi-bin/dokserv?idn=978871782.

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19

McGowan, Patrick Columba. "Studies in the chemistry of tungsten cyclopentadienyl compounds." Thesis, University of Oxford, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.314905.

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20

Konidaris, Peter Christopher. "New cyclopentadienyl imido compounds of molybdenum and tungsten." Thesis, University of Oxford, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.306573.

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21

Dicks, James Paul. "Dithiolene complexes of Î·âµ-cyclopentadienyl cobalt centres." Thesis, University of Nottingham, 2005. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.422748.

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22

Joly, KeÌvin. "Synthesis of novel hybrid cyclopentadienyl-amino acid ligands." Thesis, University of Birmingham, 2005. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.422784.

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23

Furtado, Stephen John. "Amino functionalised cyclopentadienyl complexes of vanadium and iron." Thesis, University of Leeds, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.275695.

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24

Carmichael, Adrian John. "Synthesis of cationic bis(cyclopentadienyl)tungsten(IV) complexes." Thesis, University of Warwick, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.245955.

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25

Collins, Sibrina Michelle. "Matrix Photochemistry of various Organometallic Cyclopentadienyl Dicarbonyl Dimers /." The Ohio State University, 2000. http://rave.ohiolink.edu/etdc/view?acc_num=osu1488193665234531.

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26

Spence, Malcolm Andrew. "Organometallic thiolate complexes of the early transition metals." Thesis, Heriot-Watt University, 1998. http://hdl.handle.net/10399/1117.

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27

SABIR, SAFIA. "Etudes electrochimiques de l'oxydation des complexes cationiques (cyclopentadienyl) fe#+(ii)(arene) et de la reduction des complexes cationiques (cyclopentadienyl) fe#+(ii)(halogenoarene)." Rennes 1, 1994. http://www.theses.fr/1994REN10103.

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Le travail presente dans ce memoire concerne l'etude des complexes cationiques cpfe#+(ii)(arene). La synthese des substrats est realisee selon la methode de nesmeyanov. L'etude de la reaction de complexation et des essais d'amelioration du rendement font l'objet du premier chapitre. Le second chapitre, decrit le comportement anodique des complexes cationiques cpfe#+(ii)(arene). Lorsque l'arene libre est plus facilement oxydable que le complexe correspondant, une seule oxydation irreversible est observee. Lorsque l'arene libre est plus difficilement oxydable que le complexe correspondant, l'oxydation s'effectue en deux etapes irreversibles. Dans tous les cas l'oxydation des complexes est suivie d'une decomposition avec liberation de l'arene, de fe#3#+ et de l'anion cyclopentadienyle oxydable au meme potentiel. Le troisieme chapitre porte sur la reduction des complexes cationiques d'halogenoarenes cpfe#+(ii)(arx) en milieux organiques. La premiere reduction est un processus monoelectronique. Quel que soit le complexe, le deroulement de la reaction depend d'une competition entre la decoordination de l'arene et l'elimination de l'ion halogenure au niveau de l'intermediaire neutre cpfe(i)(arx). Une competition analogue permet d'expliquer les deshalogenations observees lors de la synthese des complexes. Le quatrieme chapitre, concerne le comportement electrochimique de complexes cpfe#+(ii)(arx) impliquant l'intermediaire cpfe#+(ii)(ar#. ) dans une reaction, catalysee par transfert d'electron, de reduction par des alcools ou des glucides

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28

Edelmann, Matthias. "Synthese homo- und heterotrimetallischer Übergangsmetallkomplexe mit verbrückten Cyclopentadienyl-Liganden." [S.l.] : [s.n.], 2002. http://deposit.ddb.de/cgi-bin/dokserv?idn=964312905.

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29

Yan, Xuefeng. "Studies on #eta#-cyclopentadienyl derivatives of early transition metals." Thesis, University of Oxford, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.337665.

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30

Man, Kwok Wai. "Novel routes to bidentate cyclopentadienyl-aloxy complexes of titanium." Thesis, University of Southampton, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.266659.

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31

Constantine, Steven Peter. "The preparation and characterisation of some bis-cyclopentadienyl metallocenes." Thesis, University of Sussex, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.360580.

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32

Giudice, Aldo Edwin. "Synthesis and reactivity of titanium cyclopentadienyl imido amidinate complexes." Thesis, University of Oxford, 2002. http://ora.ox.ac.uk/objects/uuid:a4c06c87-d305-4147-a833-f32631b637b0.

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This Thesis describes the preparation and characterisation of a range of titanium imido complexes supported by a cyclopentadienyl-amidinate ligand set. Reactivity studies of these complexes towards unsaturated organic species are presented. <strong>Chapter 1</strong> reviews transition metal complexes containing imido, cyclopentadienyl, and amidinate ligands, with an emphasis on recent work. <strong>Chapter 2</strong> describes the synthesis and characterisation of titanium cyclopentadienyl imido amidinate complexes, along with precursor complexes which have not been previously reported. X-ray crystal structures of four imidotitanium species are described. <strong>Chapter 3</strong> describes the reactivity of titanium cyclopentadienyl imido amidinate complexes towards carbon dioxide. An unprecedented reaction with two molecules of carbon dioxide is reported for the arylimido complexes. X-ray crystal structures of two of the arylimido dicarboxylate products are described. The kinetics of the insertion of the second molecule of carbon dioxide are investigated and reported. <strong>Chapter 4</strong> describes the reactivity of titanium cyclopentadienyl imido amidinate complexes towards isocyanates and carbodiimides. The X-ray crystal structures of two N, O- bound ureate complexes are described. A new series of reactions involving two molecules of p-tolyl isocyanate with arylimido complexes is reported. Reactions of isocyanates with carbamate complexes are also reported. <strong>Chapter 5</strong> explores the reactivity of titanium cyclopentadienyl imido amidinate complexes towards sulfur-containing substrates. Comparisons are drawn with the reactivity towards oxygen-bearing homologues. X-ray crystal structures of two bridging sulfido complexes are described. <strong>Chapter 6</strong> discusses the reactivity of titanium cyclopentadienyl imido amidinate complexes towards substrates containing only one unsaturated linkage. Reactions with organic carbonyls and terminal alkynes are found to afford equilibria rather than isolable products. <strong>Chapter 7</strong> details full experimental procedures for all syntheses and reactions described in the text. <strong>Chapter 8</strong> contains characterising data for all new compounds reported. Full tables of crystallographic data for all new crystallographically characterised complexes described herein are presented in <strong>Appendices A-H, J-M</strong>. <strong>Appendix I</strong> contains kinetics data relating to work discussed in Chapter 3.

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33

Blom, Burgert. "Bulky cyclopentadienyl chromium complexes as ethene trimerisation catalyst precursors." Master's thesis, University of Cape Town, 2004. http://hdl.handle.net/11427/22101.

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The process of ethene trimerisation to 1-hexene, has recently attracted considerable interest, in light of the usefulness of 1-hexene industrially. In this project the process of catalytic ethene trimerisation, using bulky cyclopentad ienyl chromium complexes was investigated. Firstly, a series of known and novel bulky cyclopentadiene ligands, of the type, C₅Ph₄RH (R = H, alkyl, aromatic or substituted aromatic group) were synthesised. Four routes were investigated. (i) Making use of an in situ generated bis-lithium intermediate, resulting in the formation of 1 ,2,3,4,5-pentaphenyl cyclopenta-1 ,3-diene and 1 ,2,3,4-tetraphenylcyclopenta-1 ,3-diene. (ii) The attempted use of a metallation I alkylation route which was unsuccessful. (iii) The use of tetracyclone as starting material, reacted with alkyl likthium reagents, or alkyl Grignard reagents which resulted in the formation of ligands, of the type C₅Ph₄R, with R in the 5 position of the ring (R = n-butyl, tertbutyl, hexyl). Unexpected side reactions afforded the isolation of two ligands of the type C₅Ph₄R, R = 1-propeneyl and ethyl, both with the terminal alkene function, saturated. (iv) The use of a Pd catalysed route, making use of Cp₂ZrCI₂ as source of cyclopentadiene, resulted in the successful isolation of the cyclopentadiene, C₅Ar₅H (Ar = C₆Me₂H₃). All new compounds were successfully characterised using NMR, IR, MS and elemental analysis. A stable Fe(II) model complex, bis-tetraphenylcyclopentadienyl iron, was prepared and cyclic voltametry conducted on it, to investigate the effect of phenyl substituents on a Cp ligand in the reduction I oxidation potential of the iron(II) centre. This study showed that phenyl rings on a cyclopentadiene ligand have a significant effect on the redox potential of Fe(II); this trend could possibly be expected with other metals, in particular chromium .

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34

Kunst, Andreas Klaus. "Synthese und Reaktivität von verbrückten und unverbrückten Cycloheptatrienyl-Cyclopentadienyl-Übergangsmetallkomplexen." [S.l.] : [s.n.], 2006. http://www.digibib.tu-bs.de/?docid=00014002.

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35

Partridge, Martin Graham. "Activation and coordination of organic ligands by cyclopentadienyl metal complexes." Thesis, University of York, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.304072.

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36

Cullin, David W. "High resolution laser spectroscopy of jet-cooled substituted cyclopentadienyl radicals /." The Ohio State University, 1991. http://rave.ohiolink.edu/etdc/view?acc_num=osu148768795996825.

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37

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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38

Biradar, A. V. "Cyclopentadienyl molybdenum acetylide complexes as novel catalyst for oxidation reactions." Thesis(Ph.D.), CSIR-National Chemical Laboratory, Pune, 2008. http://dspace.ncl.res.in:8080/xmlui/handle/20.500.12252/2712.

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39

Green, Simon Michael. "The synthesis and application of novel chiral transition metal complexes." Thesis, University of Southampton, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.285879.

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40

Thornberry, Matthew P. "Synthesis, Properties, and Reactivity of Pentafluorophenyl Substituted Cyclopentadienes and Their Transition Metal Complexes." Diss., Virginia Tech, 2001. http://hdl.handle.net/10919/28539.

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Substituent effects in eta5-cyclopentadienyl (Cp) transition metal complexes have been intensely studied since the discovery of the first such complex, ferrocene. Modifications of the Cp ligand framework effect changes in the physical properties and chemical reactivity of the coordinated transition metal. This concept is useful when applied to catalysis mediated by Cp complexes, because the performance of the catalyst can be markedly improved using well-chosen ligand substituents. Studies of electronic substituent effects ideally employ a wide range of electron-donating and electron-withdrawing groups. Unfortunately, most of the available electron-withdrawing groups suffer from problems with Cp ligand synthesis, Cp anion stability, and electron-withdrawing group stability under catalytic conditions. This dissertation shows that the pentafluorophenyl (C6F5) substituent is highly electron-withdrawing but avoids all of these problems. Several new C6F5-substituted cyclopentadienes are prepared by the reaction of sodium cyclopentadienide and hexafluorobenzene (C6F6) under varying conditions. Corresponding C6F5-substituted cyclopentadienyl ligands (sodium salts) are obtained upon deprotonating the dienes with NaH. Complexes of Mn(I), Re(I), Fe(II), Co(II), Zr(IV) are synthesized by reacting these ligands with transition metal halides. The acidities of several C6F5- and C5F4N-substituted cyclopentadienes and indenes are measured using 19F NMR spectroscopy. The electron-withdrawing fluorinated aryl groups have a substantial acidifying effect. The identity and number of substituents (C6F5, C5F4N, CH3, and t-Bu), the position of the substituents on the cyclopentadiene, and the intramolecular (vicinal) steric effects also influence acidity. The electron-withdrawing ability of the C6F5 group is also characterized by infrared spectroscopic analysis of substituted CpM(CO)3 (M = Mn(I) and Re(I)) and electrochemical analysis of substituted ferrocenes. X-ray crystal structures of several C6F5-substituted Cp complexes reveal interesting structural motifs, including pi-stacking of the C6F5 substituents, Cp-M bond elongation, and CO-C6F5 interactions. In addition, dynamic Cp-C6F5 and Cp-M rotational barriers are measured by variable temperature NMR spectroscopy. Finally, ethylene polymerizations and ethylene/1-hexene copolymerizations are conducted using C6F5- and C6H5-substituted zirconocene dichlorides as catalysts. Contrary to findings published elsewhere, this study shows that substituent electronic effects induce substantial changes in comonomer incorporation.<br>Ph. D.

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41

Micallef, Leanne S. "Preparation and Antitumour Studies of Some Ruthenium and Iron Cyclopentadienyl Complexes." Thesis, Griffith University, 2006. http://hdl.handle.net/10072/367824.

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In this work, a series of mono-, di-and pentasubstituted metallocene compounds of iron and ruthenium was prepared, with all compounds screened for their antitumour properties. Chapter 1 includes a review of the use of metals in medicine, in particular, their application to the treatment of cancer. Metal-containing compounds have been shown to possess great potential as antitumour agents, as evidenced by their current medical use and their significance in recent literature. In Chapter 2 the synthesis of a key starting material and its conversion to a large number of pentasubstituted ruthenocenes is discussed. The pentamethyl ester (1) was prepared by a modified literature method, which involved a reduction in the number of steps and the substitution of a thallium reagent for silver. On one occasion the unusual ruthenocene derivative Ru[?5-C5H4(C5(CO2CH3)5)][?5-C5(CO2CH3)5] (2) was isolated from the reaction mixture of (1). Attempts to prepare (2) by rational routes were unsuccessful. A potassium salt of ruthenocene pentacarboxylic acid was prepared using base catalysed hydrolysis of (1), while acid hydrolysis of (1) produced ruthenocene pentacarboxylic acid (6). A series of new pentasubstituted alkyl esters was produced using (6), with the general formula Ru(?5-C5H5)[?5-C5(CO2R)5]. All of these new esters were found to be oils, with the exception of the iso-propyl ester which is a waxy solid. Similarly, the synthesis of a small number of new pentasubstituted amides was achieved from (1). The pentafluorocarbonyl ruthenocene (9) was synthesised from (6) and proved to be a useful reagent for the synthesis of a number of new pentasubstituted ruthenocenes. The pentamethylcyclopentadienyl analogue of (1) was converted to the carboxylic acid and the n-propyl ester via acid catalysed hydrolysis and esterification. Synthesis of the mono-and dicarboxylic acid and fluorocarbonyl ruthenocenes gave way to the production of a range of mono-and disubstituted ruthenocene carbonyl compounds. These compounds include methyl, ethyl and propyl esters, the propyl thiocarbonyl compound, glycoconjugate compound and ethanolamides of ruthenocene. The anhydride (10) was found to be a by-product of the synthesis of the mono-and difluorocarbonyl compounds but was later able to be prepared rationally. As well as these ruthenocenes, the ferrocene mono-and di-methyl and propyl esters were prepared for later biological testing. Mono-and di-alkyl and ketone ruthenocenes, and the previously known formyl ruthenocene were prepared using methods adapted from the literature. A cationic mixed ruthenocene was prepared using two different methods, and completely characterised. All of the compounds prepared were fully characterised, with crystal structures obtained for Ru[?5-C5H4(C5(CO2CH3)5)][?5-C5(CO2CH3)5], Ru(?5-C5H5)[?5-C5(CO2H)4(CO2K)], Ru(?5-C5H5)[?5-C5(CO2H)5], [Ru(?5-C5H5)(?5-C5H4CO)]2O, Ru(?5-C5H5)[?5-C5(CO2C6H5)5], Ru(?5-C5H5)[?5-C5(CONH(CH2)2CH3)5], Ru(?5-C5H5)[?5-C5(CONHC6H11)5]. Biological testing of all of the above compounds was performed against a range of tumour cell lines and a healthy cell line. This was done in order to establish whether the compounds were active against the tumour cells, whether the activity was selective towards the tumour cell lines, and to determine any structure-activity relationship among the compounds. SRB colorimetric cell survival assays were employed for this preliminary testing. While the potency of all of the compounds was found to be low, some selectivity towards the tumour cell lines was evident when compared to their activity against healthy NFF cells. Amongst the most active compounds was the pentapropyl ester (21) which presented an IC50 of 12 µM against the ovarian tumour cell line CI80-13S. As well as gauging their level of activity, a deeper understanding of the mode of action of the compounds was also sought. Ruthenium uptake measurements, cell cycle experiments and nucleotide binding studies were carried out in order to gain information about their mechanism. Since the compounds tested did not show similar activity to that of Cd2+, nor did they affect the cell cycle, it is uncertain whether the mechanism of action involves mitochondrial function. NMR nucleotide binding studies revealed a possible interaction between the tested compounds and 5'-GMP, however, further experiments are required to obtain an understanding of the mechanism of these compounds.<br>Thesis (PhD Doctorate)<br>Doctor of Philosophy (PhD)<br>School of Science<br>Full Text

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42

Trojansek, Darlene. "The chemistry of cyclopentadienyl ruthenium disulfanes, 2-oxodisulfanes and 2-dioxodisulfanes." Thesis, McGill University, 1995. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=28940.

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The complexes CpRu(CO)$ sb2$SR(Cp = $ eta sp5$-cyclopentadienyl; R = 4-C$ sb6 rm H sb4$Me, C$ rm sb6H sb5, CH sb2C sb6H sb5$) insert sulfur from S$ sb8$ to give CpRu(CO)$ rm sb2S sb{x}$R (x = 1-3) and undergo ligand exchange with R$ rm sp prime sb2S sb{y}$ (y = 2,3) to give CpRu(CO)$ sb2 rm S sb{x}R sp prime$ (x = 1-3). The mechanisms of these reactions are discussed. Treatment of CpRu(CO)$ sb2$SH with the appropriate phthalimide sulfur transfer reagents REphth (phth = phthalimide; E = SS, SS(O); R = 4-C$ rm sb6H sb4Me, C sb6H sb5, CH sb2C sb6H sb5$) gave CpRu(CO)$ sb2$ER. The complexes CpRu(CO)$ sb2$SSR undergo sulfur redistribution in solution to give CpRu(CO)$ rm sb2S sb{x}$R (x = 1-3) and insert sulfur from S$ sb8$ to give CpRu(CO)$ sb2$SSSR. The complexes CpRu(CO)$ sb2$SS(O)R undergo spontaneous oxygen transfer in solution to form CpRu(CO)$ sb2$SSR and CpRu(CO)$ sb2$SS(O)$ sb2$R. The reaction of CpRu(CO)$ sb2$ER (E = S, SS, SS(O)) with PPh$ sb3$ in ambient light gave CpRu(PPh$ sb3$)(CO)SR. The complexes CpRu(L)(CO)SS(O)$ sb2$R were prepared by oxidation of CpRu(PPh$ sb3$)(CO)SS(O)CHMe$ sb2$ with NaIO$ sb4$ (L = PPh$ sb3$) and reaction of CpRu(CO)$ sb2$SH with RS(O)$ sb2$Cl (L = CO; R = 4-C$ rm sb6H sb4Me, C sb6H sb5$). The reaction of CpRu(CO)$ sb2$SS(O)$ sb2$R with PPh$ sb3$ gave CpRu(PPh$ sb3$)(CO)SS(O)$ sb2$R. The x-ray structures of CpRu(CO)$ sb2$SS(O)C$ rm sb6H sb5 and CpRu(CO) sb2SS(O) sb2C sb6H sb5$ were determined. Oxidation of CpRu(PPh$ sb3$)(CO)SS(O)-4-C$ rm sb6H sb4$Me by dimethyldioxirane (DMDO) gave CpRu(PPh$ sb3$)(CO)S(O)$ sb2$S(O)$ sb2$-4-C$ rm sb6H sb4$Me which was immediately hydrolyzed by trace amounts of H$ sb2$O to give CpRu(PPh$ sb3$)(CO)S(O)$ sb3$H. Cyclic voltammetry (CV) studies of CpRu(CO)$ sb2$ER (E = S, SS, SS(O), SS(O)$ sb2$) were performed. All of these complexes undergo irreversible sulfur-based oxidations.

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43

Larch, Christopher Paul. "Multidentate amide and cyclopentadienyl uranium and thorium complexes and related studies." Thesis, University of Sussex, 2007. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.436239.

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44

Vaughan, Richard Robert. "Synthesis and characterisation of cyclopentadienyl cobalt complexes of selenium-containing ligands." Thesis, Queen's University Belfast, 1991. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.334685.

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45

Downing, Stephen Paul. "Studies of N-heterocyclic carbenes functionalised with a cyclopentadienyl type moiety." Thesis, University of Southampton, 2007. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.439577.

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46

Shen, Lihong. "Preparation of substituted cyclopentadienyl ligands by nucleophilic addition to substituted fulvenes." DigitalCommons@Robert W. Woodruff Library, Atlanta University Center, 1990. http://digitalcommons.auctr.edu/dissertations/3188.

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By modifing the procedure reported by Stone and Little, we have been able to make substituted fulvenes on a large scale and maintain good yield. Treatment of 6-tert-butylfulvene with lithium diethylamine gave, upon work-up, neopentylcyclopentadiene in 83% yield. Treatment of neopentylcyclopentadiene with n-butyllithium followed by zirconium tetrachloride gave [ƞ5-C5H4CH2C(CH3)3]2ZrCl2 in 19% yield. Treatment of 6-tert-butylfulvene with lithium 1,2,3,4-tetrahydroisoquinoline gave, upon work-up, neopentylcyclopentadiene in 71% yield- and a mixture of 3,4-dihydroisoquinoline, 1,4-dihydroisoquinoline and isoquinoline in 72% combined yield. Treatment of 6-methyl-6-phenylfulvene with dilithio-Ɩ-proline at -78 °C gave, upon work-up, a 99% yield of 1-cyclopentadienyl-1-phenylethane, 17.4% ee. Treatment of 6-methyl-6-phenylfulvene with dilithio (s)-(-)-2-pyrrolidone-5-carboxylic acid at -78 °C gave, upon work-up, a 99% yield of 1-cyclopentadienyl-1-phenylethane, 8.7% ee. Treatment of 1-cyclopentadieny-11-phenylethane (8.7% ee) with one equivalent of n-BuLi followed by treatment with lithium cyclopentadienide and ferrous chloride gave, upon work-up, [C5H5][C5H4(CH(CH3)C6H5)]Fe, 10.5% ee. Treatment of 1-cyclopentadienyl-1-phenylethane (17.4% ee) with one equivalent of n-BuLi followed by treatment with cyclopentadienyltitanium trichloride gave, upon work-up, a 48% yield of [C5H5][C5H4(CH(CH3)C6H5)]TiCl2. Treatment of 1-cyclopentadienyl-1-phenyl-ethane (17.4% ee) with one equivalent of n-BuLi followed by treatment with zirconium tetrachloride gave [C5H4(CH(CH3)C6H5)]2ZrCl2 in 78% yield. Treatment of 6-tert-butylfulvene with excess of cyclopentadienyl lithium gave, upon work-up, 1, 1-bis(cyclopentadienyl)-1-tert-butylmethane in 34% yield. Treatment of 1, 1-bis(cyclopentadienyl)-1-tert-butylmethane with two equivalent of methylmagnesium bromide or isopropylmagnesium chloride followed by quenching with D2O gave 1,1-bis(cyclopentadienyl)-l-tert-butylmethane-d2 in 56.9% and 84.1% yield respectively. Treatment of fluorenyl lithium with 6-tert-butylfulvene gave, upon work-up, a 44% yield of 1-cyclopentadienyl-1-fluorenyl-2,2-dimethylpropane as a yellow solid. Treatment of this yellow solid with two equivalent of n-BuLi followed by treatment with zirconium tetrachloride gave a 72% yield of neopentyl(cyclopentadienyl-l-fluorenyl) zirconium chloride.

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47

Costa, André Pontes da. "Cyclopentadienyl-functionalised N-heterocyclic carbenes: synthesis, coordination to Mo, Ru, Rh." Doctoral thesis, Universidade Nova de Lisboa. Instituto de Tecnologia Química e Biológica, 2011. http://hdl.handle.net/10362/6858.

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Dissertation presented to obtain the Ph.D degree in Chemistry<br>This thesis deals with the synthesis of cyclopentadienyl-functionalised N-heterocyclic carbenes and its coordination to both middle and late transition metals. One of the goals was to gain chemical knowledge on the reactivity patterns of these complexes, and explore their potential applications in catalysis. The imidazolium salts synthesised in the course of this thesis represent a series containing changes in the electronic and steric parameters. The ligand precursors were coordinated to molybdenum, ruthenium, rhodium and iridium. These organometallic complexes were studied in homogeneous catalysis processes such as: olefin epoxidation (Mo), isomerisation of allylic alcohols (Ru), b-alkylation of alcohols, Nalkylation of amines and transfers hydrogenation of ketones (Ir).(...)<br>Apoio financeiro da FCT e do FSE no âmbito do Quadro Comunitário de Apoio: SFRH/BD/28490/2006

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Warren, Andrea D. "Synthesis and Characterization of Cyclopentadienyl Transition Metal Complexes Bearing Tetrafluoropyridyl Substituents." Thesis, Virginia Tech, 2001. http://hdl.handle.net/10919/34672.

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Three new tetrafluoropyridyl-substituted cyclopentadienes were synthesized. Reactions of pentafluoropyridine (C5F5N) with sodium cyclopentadienide (NaCp) in THF with excess NaH present afforded mixtures of (4-tetrafluoropyridyl)cyclopentadiene (1), 1,3-bis(tetrafluoropyridylcyclopentadiene) (2), and 1,2-bis(tetrafluoropyridylcyclo-pentadiene) (3). Selectivity for mono- and diarylation was controlled by varying the reaction time. Each of the three cyclopentadienes (1, 2, and 3) was converted to its corresponding substituted sodium cyclopentadienide (4, 5, and 6, respectively) by treatment with NaH in THF. Reaction of the monoarylated sodium cyclopentadienide (4) with M(CO)5Br in THF (M = Mn, Re) afforded the corresponding substituted CpM(CO)3 complexes (7Mn and 7Re). The diarylated sodium cyclopentadienides (5 and 6) likewise afforded the diarylated complexes 8Mn, 8Re, 9Mn, and 9Re. Infrared spectroscopic measurements of [(C5F4N)nC5H5-n]M(CO)3 (M = Mn, Re; n = 0 - 2) revealed an increase of about 6 cm-1 in the A-symmetric C-O stretching mode per C5F4N group, which is significantly higher than the average increase (4 cm-1) found earlier for C6F5 groups. Reaction of 2 equiv of 4 with FeBr2 in THF afforded the 1,1'-diarylated ferrocene (10). Analogous reactions starting with 5 and 6 afforded tetraarylated ferrocenes (11 and 12, respectively). Reaction of 2 equiv of 4 with ZrCl4 afforded (C5F4NCp)2ZrCl2 (13), whereas the reaction of CpZrCl3 with 1 equiv of 4 afforded (C5F4NCp)CpZrCl2 (14). Metallocene (13) was found to be moderately active for ethylene/1-hexene copolymerization (1 atm of C2H4, toluene solvent, methylalumoxane cocatalyst).<br>Master of Science

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NOUALI, HABIBA. "Syntheses et reactions de complexes alleniques difonctionnels de cyclopentadienyl maganese dicarbonyle." Université Louis Pasteur (Strasbourg) (1971-2008), 1990. http://www.theses.fr/1990STR13222.

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Ce travail a consiste a synthetiser des complexes d'allenes difonctionnels du methylcyclopentadienylmanganese dicarbonyle afin d'etudier leur reactivite. Une synthese generale de complexes de formylallenes portant une seconde fonction electroattractive a ete developpee. Ces nouveaux complexes stables de ligands activement reactifs ont permis l'acces a d'autres types de complexes d'allenes electrophiles, comme ceux d'alcenylallenes et plus generalement a des derives alleniques polyinsatures, complexes ou non. Une autre voie d'acces aux complexes d'alcenylallenes, permettant le controle de la stereochimie de la double liaison non allenique, a egalement ete developpee au depart d'enynes homoconjugues. La photolyse en milieu acide des complexes alcenylalleniques, ainsi synthetises, conduit generalement a la liberation du ligand avec reduction de la double liaison allenique engagee dans la complexation, conduisant a l'obtention de dienes conjugues beta fonctionnels. La stereochimie de cette reaction de photodecomplexation reductrice est fixee par la configuration ou complexe de depart (complexe exodouble liaison e; complexe endodouble liaison z). L'aspect preparatif de cette reaction d'obtention de dienes beta fonctionnalises e-e, e-z ou z-z est cependant limite par la difficulte d'obtention de complexes d'alcenylallenes stereochimiquement homogenes

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50

Lee, Sang Woo 1952. "Reduction Pathways in Cyclopentadienyl Rhenium Dicarbonyl Dibromide Deriviatives and Indenyl Rhenium Tricarbonyl: Synthesis, Structure, and Reactivity of Anionic Cyclopentadienyl Rhenium Complexes. Ring Attack vs. Metal-Halogen Exchange." Thesis, University of North Texas, 1989. https://digital.library.unt.edu/ark:/67531/metadc332212/.

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The reactions of diagonal and lateral Cp'Re(CO)2Br2 (where Cp' = n5-C5H5, n5-C5Me5) and (n5-CgH7)Re(CO)3 with reducing agents have been examined. Hydride reduction at -78 °C is observed to occur at the Cp ring in both CpRe(CO)2Br2 isomers, affording a thermally unstable [(n4 -C5Hg)Re(CO)2Br2]- complex. The product of hydride ring attack has been characterized by low-temperature IR and 1H NMR measurements in addition to 13C NOE and heteronuclear 2D NMR measurements. Reaction of lateral CpRe(CO)2Br2 with either MeLi or PhLi affords both Cp-ring attack and metalhalogen exchange, [CpRe(CO)2Br]- (1) while t-BuLi reacts exclusively via metal-halogen exchange. diag-CpRe(CO)2Br2 reacts with the above lithium reagents to yield the same metal-halogen exchange anion. Analogous reactions using diag- and lat-Cp*Re(CO)2Br2 (where Cp* = n5-CgMe5) afford only the corresponding rhenium metal-halogen exchange anion, [Cp*Re(CO)2Br] (2). The molecular structures of 1-[Li/15-Crown-5] and 2-PPP were established by X-ray crystallography. 1-[Li/15-Crown-5] crystallizes in the monoclinic space group P21 with a = 10.860(4) A, b = 13.116(5) A, c = 7.417(3) A, B = 105.26(3)0, V = 1018.7(3) A3 , and Z = 2. 2-PPP crystallizes in the orthorhombic space group Pbca with a = 20.646(5) A, b = 17.690(5) A, c = 17.553(3) A, and z = 8. Solution FT-IR studies of 2 in THF reveal the presence of only solvent-separated ion pairs when the gegencation is Li+, K+, or PPP+ from -70 °C to room temperature. 2-Na at room temperature displays a 39:61 mixture of carbonyl oxygen-sodium and solvent-separated ion pairs, respectively. These ion pairs reveals a reversible temperature-dependent equilibrium. The equilibrium constant has been determined by IR band shape analysis over the temperature range -70 °C to room temperature and values of AH and AS are reported. The reaction of the ring-attacked complex, diag-[(n4-C5H6)Re(CO)2Br2]- with PPh3, P(OPh)3, or Me3CNC leads to the formation of the CpRe(CO)2L. Treatment of [Cp'Re(CO)2Br]- with methyltriflate, TFA, and magic ethyl yields the corresponding diag-Cp'Re(CO)2Br(R) (R = CH3, H, C2H5) complexes based on in situ IR analysis. All of these functionalized complexes decomposed in solution over a period of days to give Cp'Re(CO)3 as the only isolable product (20-30 %). The reaction of the [Cp,Re(C0)2Br]- with Bu3SnH at 60 °C leads to the formation of diag-Cp'Re(CO)2(SnBu3)2, which was also synthesized independently by the deprotonation of diag-Cp'Re(CO)2H2 with Et3N in the presence of Bu3SnBr at room temperature. The reaction of Cp'Re(CO)2Br2 with Bu3SnH at room temperature was discovered to afford the dihydride in excellent yield and, thus represents an improved synthetic route for the synthesis of diag-Cp'Re(CO)2H2. The hydride reduction of (n5-CgH7)Re(CO)3 at room temperature leads to the immediate formation of [(n5-CgH7)Re(CO)2H]- complex, which has been characterized by IR analysis and 1H and 13C NMR spectroscopy.

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