Rozprawy doktorskie: „Organometallic compounds”

1

Williams, Michael Lloyd. "New aspects of organometallic chemistry /". Title page, contents and abstract only, 1985. http://web4.library.adelaide.edu.au/theses/09PH/09phw725.pdf.

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2

Wu, Jingcun. "Photoelectron spectroscopy of organometallic compounds". Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1997. http://www.collectionscanada.ca/obj/s4/f2/dsk2/ftp04/mq28691.pdf.

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3

Martin, Jeffrey Thomas. "Organometallic nitrosyl hydrides of tungsten". Thesis, University of British Columbia, 1987. http://hdl.handle.net/2429/27449.

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Although hydrides of metal carbonyls are widely known, the number of hydrides in the related family of metal nitrosyls is extremely small. The preparation of a series of nitrosyl hydrides from the treatment of [CpW(NO)I₂]₂ (Cp=ƞ⁵-C₅H₅) with Na[H₂Al(OCH₂CH₂OCH₃)₂] is described. The addition of one or two equivalents of the aluminum reagent results in the formation of [CpW(NO)IH]₂ or [CpW(NO)H₂]₂ respectively. The reaction of [CpW(NO)IH]₂ with a Lewis base (L=P(OPh)₃, P(OMe)₃, PPh₃ or PMe₃) gives the monometallic CpW(NO)IHL, while [CpW(NO)H₂]₂ reacts with P(OPh)₃ or P(OMe)₃ to yield [CpW(NO)HL]₂ which undergoes further reaction to give CpW(NO)H₂L. Proton NMR spectroscopy shows that all bimetallic species contain bridging hydride ligands and are therefore best, formulated as [CpW(NO)1]₂(µ-H)₂, [CpW(NO)H]₂(µ-H)₂ and [CpW(NO)L]₂(µ-H)₂. The ¹H NMR spectrum of [CpW(NO)H]₂(µ-H)₂ shows that there is no hydride ligand exchange on the NMR time scale and that ¹jH(terminal)W ≃ ¹jH(bridging)w > ²jHW. From this finding, it is possible to develop new criteria for assessing the static or fluxional nature of hydride ligands for several families of organotungsten hydrides (Cp₂W, CpW(CO)₃, W(CO)₃ and CpW(NO)x (x=l or 2)). Within each family, the magnitude of ¹JHW strongly reflects the type of metal hydride bonding, i.e. [Formula Omitted] and suggests that bridge bonding involves all the atoms in the bridge and therefore the "fused" notation is introduced. Treatment of CpW(NO)(CH₂SiMe₃)₂ with low pressures of H₂ (60-80 psig) in the presence of Lewis bases (L=P(0Ph)₃, PMePh₂) gives the unusually stable alkyl hydride compounds CpW(NO)(H)(CH₂SiMe₃)L. This chemistry is then extended to the Cp* (Cp*=ƞ⁵ -C₅Me₅) analogues, including the preparation of the appropriate starting materials. Upon thermolysis of Cp*W(NO)(H)(CH₂SiMe₃)(PMe₃) in C₆H₆, the intermolecular C-H activation product Cp*W(N0)(H)(C₆H₅)(PMe₃) is cleanly formed. However, intermolecular activation of CH₄, C₆H₁₂ or n-C₆H₁₄ does not occur under similar experimental conditions. Hydrogenolysis of Cp*W(NO)(CH₂SiMe₃)₂ at high pressures (≃920 psig) with no Lewis base present results in the formation of isolable [Cp*W(NO)H]₂(µ-H)₂ and [Cp*W(N0)H](µ-H)₂[Cp*W(N0)(CH₂SiMe₃)]. The latter is a new example of the rare class of dinuclear alkyl hydride complexes. Proton NMR spin tickling experiments on this compound allow the complete assignment of all couplings in the spectrum and show that ¹jH(terminal)W' ¹JH(bridging)W and ²jHW have the same sign.
Science, Faculty of
Chemistry, Department of
Graduate

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4

Watkin, John Graham. "Low-valent organometallic compounds of niobium". Thesis, University of Oxford, 1989. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.236173.

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5

Tooze, R. P. "Organometallic compounds of platinum group metals". Thesis, Imperial College London, 1985. http://hdl.handle.net/10044/1/37880.

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6

Callahan, Ryan Patrick. "The synthesis of perfluorinated compounds by direct fluorination organometallic compounds and carboranes /". Access restricted to users with UT Austin EID Full text (PDF) from UMI/Dissertation Abstracts International, 2001. http://wwwlib.umi.com/cr/utexas/fullcit?p3036160.

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7

Tagg, Woo Chiat, i n/a. "Novel fluorescent organometallic materials". University of Otago. Department of Chemistry, 2009. http://adt.otago.ac.nz./public/adt-NZDU20090430.133100.

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This thesis describes the synthesis and properties of some extended donor-acceptor dyads with the donor being a ferrocenyl moiety and a fluorescent naphthalimide group as the acceptor. Two series of extended ferrocenyl-naphthalimide dyads were prepared in reasonable yield depending on the synthetic route. The first are a series of three ferrocenyl-CH=CH-spacer-C[triple bond]C-naphthalimide dyads in which the spacers are phenyl, biphenyl and anthryl and the second are a series of three ferrocenyl-C[triple bond]C-spacer-C[triple bond]C-naphthalimide dyads in which the spacers are 2,2� -bithiophene, 2,5-dimethoxybenzene and tetrafluorobenzene groups. The molecular structures of some compounds have been determined by X-ray diffraction although with many challenges because of the extensive [pi]-[pi] stacking of molecules that leads to ready aggregation in the solid state, particularly for the ferrocenyl-CH=CH-spacer-C[triple bond]C-naphthalimide dyads, in which the naphthalimide bears a methyl head group. In order to reduce the [pi]-[pi] stacking effect between the molecules and also to produce chiral molecules for the potential nonlinear optical applications, a chiral α-methylbenzylamine was introduced as the head group of naphthalimide for the ferrocenyl-C[triple bond]C-spacer-C[triple bond]C-naphthalimide dyads. The resulting comounds successfully gave crystals of sufficient quality for X-ray structural investigation. While the oxidative electrochemistry of the ferrocenyl compound in the two series of dyads was largely predictable (E� ~ 0.55 V for ferrocenyl-CH=CH- and ~ 0.72 V for ferrocenyl-C[triple bond]C-), the presence of spacers in the dyads appeared to afford stability to the reduced naphthalimide species. This was exhibited by the appearance of chemically reversible one-electron reduction processes for each of the compounds investigated. Similar unusual chemical reversibility was also shown by the spacer-C[triple bond]C-naphthalimide precursor systems. For the ferrocenyl-CH=CH-spacer-C[triple bond]C-naphthalimide dyads, the oxidation and reduction potentials closely resembled those of the simple ferrocenyl-CH=CH-spacer systems. This suggested that augmentation of the simple ferrocenyl-CH=CH-phenyl, -biphenyl and -anthryl systems with an alkyne linked naphthalimide unit showed little influence on the oxidation of the ferrocenyl moiety or the reduction of the naphthalimide unit. However, for the ferrocenyl-C[triple bond]C-spacer-C[triple bond]C-naphthalimide dyads, the oxidation and reduction potentials are influenced by the inductive effects of the spacers. While an anodic shift was observed for the dyad with the electron-withdrawing spacer tetrafluorobenzene, a cathodic shift was displayed for the dyads with the electron-donating spacers 2,2�-bithiophene and 2,5-dimethoxybenzene compared to that in the simple ferrocenyl-C[triple bond]C-naphthalimide system. The spectroscopic properties of the ferrocenyl-CH=CH-spacer-C[triple bond]C-naphthalimide dyads showed that interpolation of the aromatic spacers does not interfere with the internal charge separation. Oxidation of the ferrocenyl moiety resulted in bleaching of the metal-to-ligand charge transfer band at ~ 500 nm and the growth of a new band in the near infrared region at ~ 1000 nm. This new band can be assigned to a ligand-to-metal charge transfer transition, where the ferrocenium now acts as an acceptor to the naphthalimide donor. For the ferrocenyl-C[triple bond]C-spacer-C[triple bond]C-naphthalimide dyads, the spectroscopic properties showed that the mutually electron-withdrawing tetrafluorobenzene and naphthalimide units had little interaction despite their connection by a conductive alkyne link. In contrast, the dyads containing the electron-donating 2,2�-bithiophene and 2,5-dimethoxybenzene showed some degree of interaction between the spacer and the naphthalimide fragments. This was evidenced by the appearance of a broad absorption band in the range 410 - 440 nm, which is associated with an orbital that is delocalised between the spacer and the naphthalimide fragments. Again, the roles of donor and acceptor were reversed on oxidation of the ferrocenyl moiety. This resulted in the growth of a new near infrared band at ~750 mn for the dyad containing the tetrafluorobenzene spacer and at ~ 1000 nm for the dyads with 2,2�-bithiophene and 2,5 -dimethoxybenzene spacers. The ferrocenyl unit went from being a net donor to ferrocenium, which was acting as an acceptor, with the tetrafluorobenzene spacer adopting the donor role more reluctantly than the delocalised 2,2�-bithiophene-C[triple bond]C-naphthalimide and 2,5-dimethoxybenzene-C[triple bond]C-naphthalimide moieties. 1,3,5-Tri- and 1,2,4,5-tetra-substituted benzene cores were also used as spacers for the preparation of extended arrays of ferrocenyl-naphthalimide dyads. Utilisation of the 1,3,5 -tri-substituted benzene core enabled the core to be embellished in three directions, resulting in Y-motif extended arrays containing either one ferrocenyl unit [(ethenylferrocenyl)-C₆H₃-(C[triple bond]C-C₆H₅)₂] or one naphthalimide moiety [(4-piperidino-N-propargyl-naphthalimide)-C₆H₃-(Br)₂]. With the 1,2,4,5-tetra-substituted benzene core, the extension of the core was possible in four directions and gave extended arrays in an X-motif. Again, these systems contained either ferrocenyl units [bis(alkoxyferrocenyl)-C₆H₂-(C[triple bond]C-C₆H₅)₂] or naphthalimide moieties [(tetrakis-naphthalimide)-C₆H₂]. Attempts to incorporate both ferrocenyl and naphthalimide fragments into the X- or Y-motif extended arrays were unsuccessful. By adding C₂Co₂(CO)₆dppm across the triple bonds of two of the four alkyne groups in the X-motif naphthalimide system [(tetrakis-naphthalimide)-C₆H₂], it was possible to incorporate two oxidisable C₂Co₂(CO)₄dppm cluster units into the molecule. The electrochemistry of the resulting system showed two discrete oxidation processes, suggesting the possibility of some interaction between the dicobalt cluster redox centres.

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8

Yonchev, Raycho. "Permeation of organometallic compounds through phspholipid membranes". [S.l.] : [s.n.], 2005. http://deposit.ddb.de/cgi-bin/dokserv?idn=979680972.

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9

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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10

Rafferty, Karen. "Novel organometallic compounds as potential antitumour agents". Thesis, University of Leeds, 2008. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.487773.

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11

Davies, C. L. "Vibrational studies of inorganic and organometallic compounds". Thesis, University of Nottingham, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.380175.

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12

SoÌˆezerli, Sebnem Esen. "Organometallic compounds with bulky silyl-substituted ligands". Thesis, University of Sussex, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.388678.

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13

Quayle, Michael John. "Structural studies on organic and organometallic compounds". Thesis, University of Bristol, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.266881.

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14

McGilligan, Brian Stephen. "Organometallic and related compounds of transition metals". Thesis, Imperial College London, 1990. http://hdl.handle.net/10044/1/46441.

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15

Lee, Hui Zhi Shirley. "Organometallic compounds of osmium for cancer therapy". Palaiseau, Ecole polytechnique, 2015. https://tel.archives-ouvertes.fr/tel-01232147/document.

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Cis-platin and its derivatives are the most currently used for cancer treatment. Inspired by these metallodrugs, organometallic compounds (Ti, Ru, Fe, Rh, Au…) have been developed over the years as potential candidates for anticancer drugs, some of these have entered clinical trials. Jaouen and co-workers have developed novel therapeutic agents based on ferrocene compounds analogous to tamoxifen, which show high anti-proliferative effects against two types of breast cancer cells, namely the ER+ breast carcinoma (MCF-7) and the ER- breast carcinoma (MDA-MB-231). Similarly, Leong’s group has found a series of triosmium carbonyl clusters that shows anticancer activity against these two breast cancer cells. Thus, it would be interesting to study osmocene compounds analogous to tamoxifen. Cytotoxic activity of these tamoxifen analogues, as well as that of triosmium clusters, were studied. This work aims to study the relationship between structure and activity of triosmium cluster Os3(CO)10(NCMe)2 compound with cytotoxic properties. The results show that the presence of a vacant coordination site and good solubility are important to have a good cytotoxic activity. The second part of the study was devoted to osmocene analogues (osmocifens), especially in the comparative study between the cytotoxic activity of three metallocene series: ferrocifen, ruthenocifen and osmocen. For osmium and ruthenium complexes, only compounds containing the amino chain are active while the phenolic compounds are almost inactive.

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16

Karunatilaka, Chandana. "Rotational Spectroscopy and Structures of Organometallic Compounds". Diss., The University of Arizona, 2007. http://hdl.handle.net/10150/193621.

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High-resolution pulsed beam Fourier Transform Microwave Spectroscopy (PBFTMS) technique has been used to investigate the rotational spectra, molecular structures and electronic charge distribution of organometallic and organic molecules. The thesis reports high-resolution rotational spectral findings for nine different asymmetric-top molecules in the singlet electronic ground state including: Cyclopentadienyltungstentricarbonylhydride, Bis-(cyclopentadienyl)tungstendihydride, Tetracarbonylethyleneosmium, two substituted Ferrocenes and an organic keto-enol tautomeric system, Z-2-Hydroxypyridine and 2-Pyridone. Moreover, gas-phase rotational constants and distortion constants have also been reported for an excited vibrational state of Cyclopentadienylnickelnitrosyl complex using a high-resolution Fourier Transform Spectrometer (FTS) system at Kitt Peak Arizona, (KPNO). Preliminary microwave results for a fluxional molecule, Cyclopentadienyliridiumdicarbonyl are also presented in this work. Extensive Density Functional Theory (DFT) calculations have been performed in conjunction with the experiments to provide additional insight toward further understanding the equilibrium structures, structural isomers and electric field distributions of these molecules. These calculations were not only helpful in predicting the preliminary structure and rotational constants of the molecules of interest, but also advantageous in analyzing the observed spectra.

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17

Drouin, Brian James. "Microwave spectra and structures of organometallic compounds". Diss., The University of Arizona, 1999. http://hdl.handle.net/10150/284416.

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The technique of pulsed-beam Fourier transform microwave spectroscopy is applied to gas-phase organometallic systems for elucidation of fundamental structural properties of the compounds. Ten organometallic species with significant catalytic and reactive properties are examined and presented. This work includes complete three-dimensional structural determinations of; methylrheniumtrioxide, cyclopentadienylthallium, tetracarbonyldihydroiron, tetracarbonyldihydroruthenium and tetracarbonylethyleneiron. Quadrupole coupling parameters are presented and discussed for the compounds; methylrheniumtrioxide, cyclopentadienylrheniumtricarbonyl, cyclopentadienylindium, 'anti' and ' syn' allyltricarbonylironbromide, chloroferrocene and bromoferrocene. Partial structural determinations are given for cyclopentadienylindium, ' anti' allyltricarbonylironbromide, chloroferrocene and bromoferrocene.

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18

Agarwalla, Uday Sankar. "Oxygenation Reactions of Organic and Organometallic Compounds". Thesis, University of North Bengal, 2014. http://hdl.handle.net/123456789/1485.

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19

Wong, Chun Kin. "The chemistry of organometallic derivatives of oligoacetylenic silanes". HKBU Institutional Repository, 2002. http://repository.hkbu.edu.hk/etd_ra/424.

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20

Mock, Michael T. "Synthesis and reactivity of thioether-supported organoiron and low-valent iron complexes and cyanide-bridged binuclear complexes". Access to citation, abstract and download form provided by ProQuest Information and Learning Company; downloadable PDF file, 282 p, 2008. http://proquest.umi.com/pqdweb?did=1481668291&sid=19&Fmt=2&clientId=8331&RQT=309&VName=PQD.

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21

Peatt, Anna C. (Anna Clare-Doreen) 1976. "New reaction media for organometallic chemistry". Monash University, School of Chemistry, 2003. http://arrow.monash.edu.au/hdl/1959.1/5829.

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22

Yau, Benita Chui Kam. "Organometallic chemistry of phosphine complexes of iron and ruthenium". Thesis, The University of Sydney, 1992. https://hdl.handle.net/2123/26717.

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This thesis describes two projects involving the organometallic chemistry of iron and ruthenium complexes with DMPE ligands [DMPE = 1,2-bis(dimethylphosphino)ethane]. The first study involves an investigation into the kinetics and mechanisms of OH bond activation reactions of [Fe(DMPE)2]. The second project involves an investigation into the synthesis of RuH2(DMPE)2, the formation and properties of trans-[RuH(n2-H2)(DMPE)2]*, and the reactions of RuH2(DMPE)2 with alkyl and aryl thiols. In Part I of this work, the kinetics of the cis/trans isomerization of FeH(C6H5)(DMPE)2 and FeD(C6D5)(DMPE)2 were measured by 31P NMR spectroscopy in pentane and THF. The isomerization reactions follow first-order reversible kinetics. FeH(C6H5)(DMPE)2 and FeD(C6D5)(DMPE)2 also undergo exchange with added arenes in a concerted fashion at the iron centre. The rate of exchange is comparable to the rate of isomerization. From the equilibrium constant for the exchange reaction, it was found that FeH(C6H5)(DMPE)2 is thermodynamically more stable than FeD(C6D5)(DMPE)2 by approximately 3 kJ mol'1 in pentane. FeH(C6H5)(DMPE)2 and FeD(C6D5)(DMPE)2 react with diethyl disulfide to give Fe(SEt)2(DMPE)2. The reaction proceeds via loss of benzene or benzene-d6 followed by addition of [Fe(DMPE)2] to the 8-8 bond of EtSSEt. By following the kinetics of the reactions of EtSSEt with FeH(C6H5)(DMPE)2 and FeD(C6D5)(DMPE)2 in THF separately, the rates of reductive elimination of benzene OH and GD bonds at 283 K were found to be 3.9 x 10‘ s-1 and 6.5 x 104 s-1 respectively. The inverse deuterium isotope effect (k”/kD = 0.6) can be rationalized by the presence of a n-benzene intermediate in the elimination reaction. In solution, the phenyl ring in cis'FeH(C6H5)(DMPE)2 assumes a fixed orientation and is constantly flipping at 240 K. During this work, it was discovered that [Fe(DMPE)2] is capable of catalyzing the hydrogenation of alkenes to alkanes under photochemical conditions. The hydrogenation reaction competes with a significantly slower dehydrogenation reaction. A quantitative analysis of the efficiency of [Fe(DMPE)2] as a hydrogenation catalyst was carried out. The hydrogenation of cyclopentene is faster than that of tenninal alkenes. A reaction cycle is proposed for the hydrogenation-dehydrogenation reactions mediated by Fe(DMPE)2 complexes. Treatment of an irradiated sample of FeH(cyclopenteny1)(DMPE)2 with dibromomethane afforded FeBr2(DMPE)2 and trans-[Fe(cyclopentenyl)Br(DMPE)2]Br.2H20 whose crystal structures are presented. In Part II, a synthesis of Rqu(DMPE)2 from trans-RuC12(DMPE)2 by reduction with sodium/Z-propanol is presented. Protonation of RuH2(DMPE)2 with weak organic acids such as methanol, ethanol and thiols affords the molecular hydrogen complex trans-[RuH(T]2-H2)(DMPE)2]+ which has a nZ-bound H2 ligand and a 6-bound hydride ligand. T1 measurements and 1JHD coupling in nZ-HD ligand confirm the 'non-classical' structure. Between 220 and 300 K, the molecular hydmgen complex continuously undergoes intermolecular exchange with the protonating solvent and all the rutheniumbound hydrides undergo intramolecular exchange. In methanol, a previously unreported five-coordinate ruthenium(II) complex, trans-[RuH(DMPE)2]+, exists in equilibn'um with the molecular hydrogen complex. Reactions of the ruthenium dihydride with alkyl- and arylthiols afford trans-monothiolate hydrides. Aromatic thiols react more rapidly than alkanethiols. The reaction is believed to proceed via protonation of the dihydride (by the acidic thiol group) to give the molecular hydrogen complex, followed by substitution of the 'r12-H2 ligand with the conjugate base of the thiol. The dithiolate complex trans-[Ru(SPh)2(DMPE)2] has been isolated and its X-ray crystal structure is presented. In dithiols, dithiaruthenocycles are not formed, which is in contrast with the formation of the iron analogues. Although protonation of RuH2(DMPE)2 with alcohols is facile, substitution of trans-[RuH(T]2-H2)(DMPE)2]* by alkoxide ions does not take place in the presence of thiolate ions.

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23

Li, Jian-Jun. "Platinum(II) hydroxo, oxo, amido, imido and hydrazido complexes /". free to MU campus, to others for purchase, 1996. http://wwwlib.umi.com/cr/mo/fullcit?p9720553.

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24

Siddiqui, Rehan Ahmad. "Experimental investigations of thermodynamic properties of organometallic compounds". Dresden TUDpress, 2009. http://d-nb.info/1000184366/04.

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25

Wallner, Olov. "Palladium-Catalyzed Synthesis and Transformations of Organometallic Compounds". Doctoral thesis, Stockholm : Dept. of Organic Chemistry, Stockholm University, 2006. http://urn.kb.se/resolve?urn=urn:nbn:se:su:diva-804.

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26

Walker, Neil M. "Low-valent organometallic compounds of zirconium and hafnium". Thesis, University of Oxford, 1989. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.238179.

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27

Tolun, E. "Fast atom bombardment mass spectrometry of organometallic compounds". Thesis, University of Kent, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.370368.

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28

Armishaw, Olga Anne. "Molecular studies of organometallic carbohydrates and related compounds". Thesis, Robert Gordon University, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.360997.

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29

Jones, M. H. "Thermal decomposition of inorganic and organometallic tin compounds". Thesis, City University London, 1985. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.356325.

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30

Mills, Graham Paul. "The low pressure pyrolysis of various organometallic compounds". Thesis, University of Leicester, 1995. http://hdl.handle.net/2381/33814.

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The pyrolysis mechanisms of many organometallic compounds are of great interest because of their potential use as precursors in the production of semiconductor materials, particularly compound semiconductors of elements from groups HI and V of the periodic table. Often there are competing molecular and radical processes contributing to the overall decomposition mechanisms. This study used electron spin resonance detection of radical intermediates coupled with final product analysis to determine the relative importance of these processes. The very low pressure pyrolyses of triethylgallium, triethylindium and triisopropylgallium were shown to occur by radical pathways and to occur predominantly on the surface of the pyrolysis tube. Isopropyl radicals were observed to further decompose on the surface to yield propene, and this reaction was favoured on Ga-rich surfaces and at high temperatures. A similar reaction was not observed for ethyl radicals on any surface. Gas-phase molecular elimination reactions are shown to contribute only at high pyrolysis temperatures. Hexamethyldisilane was pyrolysed at low and very low pressures and decomposed by a radical process. The very low pressure (10-4 Torr) pyrolysis occurred on the surface of the pyrolysis tube and resulted in the formation of the unexpected (CH3)2Si(H)CH2 radical by an unknown mecanism. At 1 Torr, gas-phase reactions predominated and (CH3)3Si was the major radical formed. Pyrolysis of n5-CH3C5H4Mn(CO)3 gave a vinyl-type radical, the precise identity of which could not be determined, rather than the CH3C5H4 radical proposed in gas-phase pyrolysis studies. CH3Mn(CO)5 and CH3COMn(CO)5 were also shown to decompose by a different mechanism to that observed in gas-phase studies. Pyrolysis of n5- C5H5Mn(CO)3 produced little evidence of surface decomposition and produced radicals suggested by gas-phase studies. The difficulty in identifying the products of the pyrolysis of these compounds prevented the drawing of more detailed conclusions.

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31

McKiernan, John William. "SPECIATION OF ORGANOMETALLIC COMPOUNDS USING MASS SPECTROMETRIC DETECTION". University of Cincinnati / OhioLINK, 2000. http://rave.ohiolink.edu/etdc/view?acc_num=ucin962988114.

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32

Yu, Liwen. "A Computational Study on 18+δ Organometallics". Thesis, University of North Texas, 2002. https://digital.library.unt.edu/ark:/67531/metadc3101/.

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The B3LYP density functional has been used to calculate properties of organometallic complexes of Co(CO)3 and ReBr(CO)3, with the chelating ligand 2,3-bisphosphinomaleic anhydride, in 19- and 18-electron forms. The SBKJC-21G effective core potential and associated basis set was used for metals (Co/Re) and the 6-31G* basis set was used for all other elements. The differences of bond angles, bond distances, natural atomic charges and IR vibrational frequencies were compared with the available experimental parameters. The differences between the 19- and 18-electron systems have been analyzed. The results reveal that the 19th electron is mostly distributed over the ligand of 2,3-bisphosphinomaleic anhydride, although partially localized onto the metal fragment in 1 and 2*. Two different methods, IR-frequencies and natural atomic charges, were used to determine the value of δ. Present computed values of δ are compared with available experimental values, and predictions are made for unknown complexes.

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33

Frazier, Joy Faith. "Organo-iridium compounds : synthesis, characterization and reactivity /". Thesis, This resource online, 1991. http://scholar.lib.vt.edu/theses/available/etd-08222009-040309/.

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34

Hunter, Allen Dale. "Aspects of the organometallic nitrosyl chemistry of Cr, Mo and W". Thesis, University of British Columbia, 1985. http://hdl.handle.net/2429/25824.

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The principal organometallic products resulting from the reactions of Na[(ƞ⁵-C₅H₄R)Cr(CO)₃] (R = H or Me) with allyl chlorides in THF are the green, dimeric [(ƞ⁵-C₅H₄R)Cr(CO)₃]₂ complexes (51-67% yields). The red organometallic by-products usually formed during these conversions are novel (ƞ⁶-6-alkenylfulvene)Cr(C0)₃ complexes (5-8% yields) which have been characterized completely by conventional spectroscopic methods. Dark green [W(N0)₂Cl₂]n may be synthesized in high yields by two preparative methods. The first method involves treatment of WCl₆ in CH₂Cl₂ with an excess of NO, and it proceeds via the isolable intermediate complexes, dark violet c̲i̲̲s̲-W(N0)₂Cl₄ and bright green f̲a̲c̲-W(NO)₃Cl₃. The second method involves controlled reaction of W(CO)₆ with two equivalents of ClN0 in CH₂Cl₂. It is initiated by traces of oxidant and probably proceeds via a catalytic, radical-chain mechanism that is described. If either reaction is effected in the presence of two equivalents of CH₃CN, then yellow-green W(N0)Cl₃(CH₃CN)₂ is the only nitrosyl-containing product formed. Polymeric [W(N0)₂Cl₂]n may be cleaved by a variety of Lewis bases, L, and (n̲-Bu)₃Sn(C₅H₅) to form W(N0)₂Cl₂L₂ (L = phosphine, phosphite, CH₃CN, etc.) and CpW(N0)₂Cl (Cp - ƞ⁵-C₅H₅), respectively, in good yields. The synthesis of the electron-rich nitrosyl complexes CpM(NO)L₂ (M = Cr, Mo, or W; L = P(0Me)₃, PMePh₂, P(n̲-Bu)₃, SbPh₃ or 1/2 (dppe)) is described. They are preparable in moderate to high yields by the reduction of the iodo dimers [CpM(NO)In]₂ (M = Cr, n = 1; M = Mo or W, n = 2) with sodium amalgam in THF ln the presence of the appropriate Lewis base, L, and they exhibit metal-dependent trends in vNO (Cr » Mo > W), δ ³¹P (Cr > Mo » W), and ²J₃₁p (Cr < Mo < W). These reduction reactions proceed via a number of transient intermediates, some of which are isolable. A unified mechanism for these reductive syntheses is proposed. The novel complexes, CpMo(NO)(ƞ⁴-trans-diene) (diene = acyclic conjugated diene) and CpMo(NO)(ƞ⁴-c̲i̲s̲-2,3-dlmethyl-butadiene)t are preparable in moderate yields by the reduction of [CpMo(NO)I₂]₂ with sodium amalgam in THF in the presence of the appropriate diene. The reaction between [CpMo(NO)I₂]₂ and C₄H₆•Mg•2(THF) results in the formation of a green, isolable oligomeric complex CpMo(NO)I(ƞ³-C₃H₄R) (where R = CH₂MgI and the nitrosyl oxygen acts as a Lewis base towards Mg) that can be hydrolyzed to CpMo(NO)I(ƞ³-C₄H₇) or converted to CpMo(NO)(ƞ⁴+-t̲r̲a̲n̲s̲-C₄H₆). These diene complexes have been fully characterized by conventional spectroscopic techniques (extensive ¹H and ¹³C NMR spectra being particularly informative) and by single-crystal X-ray structural determinations of CpMo(NO)(ƞ⁴-t̲r̲a̲n̲s̲-2,5-dimethyl-2,4-hexadiene) and CpMo(N0)(ƞ⁴-c̲i̲s̲-2,3-dimethyl-butadlene). A molecular orbital rationale for the structural and spectrocopic properties and relative stabilities of these c̲i̲s̲- and t̲r̲a̲n̲s̲-diene complexes is then presented.
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Chemistry, Department of
Graduate

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35

Cloete, Jezreel. "Synthesis and applications of functionalized pyridinyl imine complexes of palladium". Thesis, University of the Western Cape, 2005. http://etd.uwc.ac.za/index.php?module=etd&amp.

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The synthesis and characterization of pyridinyl &alpha
-diimine Pd(II) complexes having a functionalized hydrocarbon attached to the imino nitrogen was performed. The catalytic activity of these complexes were then evaluated in the polymerization of ethylene and in the Heck coupling reaction of methyl acrylate with iodobenzene.

Unconjugated &beta
-diimine complexes of palladium were also synthesized and their activities towards ethylene polymerization and the Heck coupling of methyl acrylate and iodobenzene also evaluated and compared to that of the &alpha
-diimine complexes. Three of the &alpha
-diimine complexes synthesized showed activity towards ethylene polymerization, these being the complexes bearing the allyl, styrene and phenol functionalities. &omega
-Carboxylato complexes which were also synthesized showed no activity towards ethylene polymerization.

The polymer produced was found to be high density linear polyethylene with an average PDI of 2.54 with Mn values ranging between 3.42 and 6.90 x 10-5 and Mw values ranging between 6.05 and 17.6 x 10-5.

The complexes bearing the allyl, styrene and phenol functionalities, as well as the &omega
-carboxylato complexes active in the Heck coupling reactions of methyl acrylate with iodobenzene. None of the unconjugated &beta
-diimine complexes prepared showed any activity towards ethylene polymerization even at high Al/Pd ratios. The activity of these complexes towards the Heck arylation reaction was comparable to that of the &alpha
-diimine complexes showing similar activities.

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36

Makanjee, Che Azad. "An experimental and theoretical investigation of unstable Fischer chromium carbene complexes". Thesis, Rhodes University, 2013. http://hdl.handle.net/10962/d1002953.

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This organometallic study involves the use organostannanes and organolithiums as precursors to chromium Fischer carbene complexes. Fischer carbenes are typically electrophilic and are stabilized by a single π-donor substituent, and contain low oxidation state metals (often but not always from Group 6). They are highly reactive and can give access to a range of biologically active compounds through cyclopropanations, insertions, coupling and photochemical reactions. Synthesis and characterization of three MOM-protected α-alkoxy organostannanes was successfully carried out via a nucleophilic addition of tributylstannyllithium to suitable aldehydes, and immediate protection of the alcohol with MOM. Two N-BOC protected α-amino organostannanes were successfully synthesized and characterized via α-lithiation and tin-lithium exchange in the presence of TMEDA. Tin-lithium transmetallation of the organostannanes allowed access to the organolithiums required for the synthesis of novel Fischer carbenes. Addition of chromium hexacarbonyl to the organolithiums formed the acylpentacarbonyl chromate salt which was alkylated with Meerwein salt, resulting in the Fischer carbene and a by-product, tetrabutyltin, which proved difficult to remove. Several Fischer carbenes were synthesized and characterized, some simple and known and some novel. In silico work explored the reaction coordinate of the [2+2] cycloaddition towards the formation of β-lactams, and the photoactivation cycle that precedes this process. Computational work also showed the effect of the ligand on the stability and reactivity of the carbene. It was found that in some cases the oxygen on the ligand could negatively influence the stability of the carbene (when compared to a simple methyl carbene). A link between bond orders and back donation in Fischer carbenes was explored in an attempt to theoretically predict the stability of a range of carbenes.
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37

Wassink, Berend. "The redox chemistry of a variety of organometallic dinitrosyl complexes of Cr, Mo and W". Thesis, University of British Columbia, 1985. http://hdl.handle.net/2429/25993.

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An understanding of the electrochemical properties of organometallic nitrosyl compounds provides a good understanding of their chemistry and a more rational way to approach synthetic investigations. Cyclic voltammetry studies of [(ƞ)⁵-C₅H₅)Cr(NO)₂]₂ in CH₂Cl₂ and CH₃CN reveal that the dimer undergoes a single two-electron oxidation to form [(ƞ⁵⁻C₅H₅)Cr(NO)₂]⁺ which is reduced to [(ƞ⁵-C₅H₅)Cr(NO)₂]• (or [(ƞ⁵-C₅H₅)Cr(NO)₂(CH₃CN)]• in the presence of CH₃CN) in a subsequent reduction step. The radical couples to form [(ƞ⁵-C₅H₅)Cr(NO)₂]₂ or decomposes. The dimer also is reversibly reduced in a one-electron step in CH₂Cl₂ and quasi-reversibly in CH₃CN. These inferences are supported by cyclic voltammograms of (ƞ)⁵-CH₅)Cr(NO)₂BF₄ and [(ƞ⁵-C₅H₅)Cr(NO)₂(CH₃CN)]PF₆. In contrast, the isoelectronic dimer [(ƞ⁵-C₅H₅)Fe(CO)₂]₂ oxidizes in two one-electron steps (the first of which is reversible and negative of the oxidation of [(ƞ⁵-C₅H₅)Cr(NO)₂]₂) and reduces to form [(ƞ⁵-C₅H₅)Fe(CO)₂]⁻. The differing oxidation behaviours of these dimers suggest that their reactions with HBF₄•OMe₂ [(ƞ⁵-C₅H₅)Cr(NO)₂]₂ cleaves into [(ƞ⁵-C₅H₅)Cr(NO)₂]⁺ and [ƞ⁵-C₅H₅)Fe(CO)₂]₂ forms [ {(ƞ⁵-C₅H₅)Fe(CO)₂}₂H]⁺) do not occur by initial electron transfer. The new radical anion complex [(ƞ⁵-C₅H₅)Fe(ƞ⁶-C₆Me₆)] [ {(ƞ₅-C₅H₅)Cr(NO)₂}₂] can be isolated by reaction of the neutral dimer with (ƞ⁵-C₅H₅)Fe(ƞ⁶-C₆Me₆) in Et₂0. Its spectroscopic properties are consistent with derealization of the extra electron onto the NO ligands, particularly the bridging nitrosyl groups. These observations provide a better understanding of the reactivity of [(ƞ⁵-C₅H₅)Cr(NO)₂]₂ with- nucleophiles. A comparative electrochemical study of the oxidations of [(ƞ⁵-C₅H₅)M(NO)₂R (M = Cr, R = CH₃; M = Mo, W, R = CH₃, C₂H₅),(ƞ⁵-C₅H₅)Fe(CO)₂CH₃ and (ƞ⁵-C₅H₅)M(CO) ₃R (M = Cr, R = CH₃; M = Mo, W, R = CH₃, C₂H₅) in CH₂Cl₂ reveals that the dinitrosyl complexes are harder to oxidize than their related carbonyl compounds. Electrophilic cleavage reactions of M-R bonds in these complexes, which proceed differently for the nitrosyl and carbonyl complexes are proposed to involve different mechanisms, with the nitrosyl-alkyl complexes reacting with electrophiles by direct attack at the metal-alkyl bonds, rather than by prior oxidation. Interestingly, (ƞ⁵-C₅H₅)Cr(NO) ₂CH₃ reacts with NOPF₆ to form the NO-insertion product [(ƞ⁵-C₅H₅)Cr(NO)₂(CH₂NOH)]PF₆ which has been structurally and spectroscopically characterized. The reactions of (ƞ⁵-C₅H₅)M(NO)₂CH₃ (M = Mo, W) with electrophiles and oxidants result in cleavage of the M-CH₃ bonds. The complexes (ƞ⁵-C₅H₅)M(NO)₂Y (M = Cr, Y = CH₃; M = Mo, Y = CH₃, C₂H₅, Cl; M = W, Y = CH₃, C₂H₅, H, Cl), [(ƞ⁵-C₅H₅)M(NO)₂L] BF₄ (M = Mo, L = PPh₃; M = W, L = PPh₃, P(OMe)₃, ƞ²-C₈H₁₄) and W(NO)₂Cl₂L₂ (L = P(OMe)₃, PMePh₂) exhibit quite reversible, one-electron reductions in CH₂Cl₂ and the new radical complexes [(ƞ⁵-C₅H₅) ₂Co] [(ƞ⁵-C₅H₅)M(NO)₂Y] (M = Mo, Y = CH₃, C₂H₅, Cl; M = W, Y = CH₃, H, Cl) are isolable by reactions of (ƞ⁵-C₅H₅)₂Co with the neutral precursor. Spectroscopic characterization of these and an X-ray crystallogrpahic analysis of [(ƞ⁵-C₅H₅)₂Co] [(ƞ⁵-C₅H₅)Mo(NO)₂C₂H₅] suggest that the anions possess monomeric, "three-legged piano stool" geometries with delocalization of the extra electron onto the NO ligands. In light of these observations the chemistry of (ƞ⁵-C₅H₅)M(N0)₂Y complexes becomes more understandable.
Science, Faculty of
Chemistry, Department of
Graduate

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38

Habrych, Malgorzata. "Mixed-ligand strategy for the preparation of manganese based single-molecule magnets". [Gainesville, Fla.] : University of Florida, 2004. http://purl.fcla.edu/fcla/etd/UFE0004815.

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39

Gorden, John David. "Low valent and mixed valent cyclopentadienyl complexes of the group 13 elements". Access restricted to users with UT Austin EID Full text (PDF) from UMI/Dissertation Abstracts International, 2001. http://wwwlib.umi.com/cr/utexas/fullcit?p3036602.

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40

Ross, Jennifer Nicola. "Alkoxy- substituted aryl- and benzyl- organotin compounds". Thesis, University of Aberdeen, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.324880.

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New organotin compounds containing alkoxy- functionalities have been prepared. The methods of preparation of the tetraorganotin species have involved three routes. Hydrostannation reactions using triphenyltin hydride have resulted in the synthesis of triphenyltin derivatives of a series of alkoxy- substituted allyl ethers. The addition of tin IV chloride, diphenyltin dichloride and phenyltin trichloride to alkoxy- substituted aryl- and benzyl- Grignard reagents have also been successful. Alkoxy- substituted benzyltin compounds have been prepared by following an alternative preparation of benzylmagnesium halides from that commonly used to prepare Grignard reagents. Nucleophilic substitution of (iodomethyl)triphenyltin by a novel ligand has been effective. The structures of the products have been investigated by ¹H, ¹³C and ¹¹⁹Sn nmr. Single crystal X-ray diffraction studies have led to the determination of the crystal structures of tetra-2-anisyltin, tetrakis-(2-methoxybenzyl)tin and N,N'-bis(5-triphenylstannoxymethyl-2-phenyl-1,3-dioxan-5-yl)ethanediamide. Selective tin-carbon bond cleavage has been effected by the use of iodine and bromine to give rise to mono- and dihalo- organotin compounds and the crystal structures of tri-2-anisyltin iodide and di-2-anisyltin dibromide have been elucidated by X-ray crystallography. Chloro(3-ethoxypropyl)diphenyltin has been synthesised directly from diphenyltin dichloride and has been found to contain a penta-co-ordinate tin centre with a four membered chelate ring as a result of intramolecular tin-oxygen co-ordination. Other tin-carbon bond cleavage reactions by halogens have been studied by ¹H and ¹¹⁹Sn nmr and GLC and the results discussed.

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41

Reade, Thomas James. "Photoactive metal-organic frameworks and related compounds". Thesis, University of Nottingham, 2014. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.755818.

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42

Turnbull, Anthony James. "Chemistry of acetylenic iron complexes". Thesis, The University of Sydney, 2000. https://hdl.handle.net/2123/27771.

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The work presented in this thesis describes the synthesis, properties and characterisation of a number of acetylide substituted iron tetraphosphine complexes. The aim of the program was to synthesise oligomeric polynuclear species where organometallic units were linked by organic acetylenic spacer units. Anunderlyingobjective of theprogrammevas to construct condensed organometallic systems in a controlled fashion. A variety of precursors to acetylenic compounds was synthesised . The complexes synthesised all contained the iron(Il) dmpe and depe skeletons (dmpe = 1,2-bis( dimethylphosphino )ethane; depe = 1,2-bis( diethylphosphino )ethane). Halide, hydride, alkyl, and triflate ligands were assessed systematically for their ability to form acetylenic complexes by substitution reactions. Combinations of these ligands were assessed to chemoselectively form unsymmetrically disubstituted acetylenic complexes. A range of iron(II) bisacetylide complexes of the type trans-[Fe(O::CRh(dmpeh] (R = C(CH3)3 (90), 􀀞s (91), 4-CH3C6Ri (92), 4-CH30C6lii (93), 4-FC􀀢 (94), 3,5-(CF3)24H3 (95), adamantyl (98), 4'-C6H4C6RiC=CH (99), Si(CH3)J (100) and (CH2)4C=CH (101)) was synthesised and characterised. The photochemical metathesis reactions of trans-[Fe(CH3)2(dmpeh] (71b) with terminal alkynes were examined as a novel reaction to synthesise iron(Il) bisacetylide complexes. A range of iron(Il) monoacetylide complexes was synthesised and characterised including cis/trans-[Fe(C-.=CR)(CH3)( dmpe )2], trans-[Fe(C=CR)(OS02CF3)(depe)z], trans-[Fe(C-.=CR)(CH3)( depe h], trans-[Fe(C=CR)(OS02CF3)(dmpe)z], trans-[Fe(C=CR)(Cl)(depe)2], and trans-[Fe(O::CR)(Cl)(dmpe)i]. The iron(Il) monoacetylide complexes were considered as intermediates in the systematic synthesis of iron(Il) bisacetylide complexes. Each category of iron(Il) monoacetylide complexes underwent unique reactions with alkynes to produce a variety of acetylenic products. The structure of one of these iron(Il) monoacetylide complexes, trans-[Fe(C-=CC􀀒s)(CH3)(dmpeh] (132b) was determined by X ray diffraction. The reactions of iron(m acetylide chloride and iron(m acetylide alkyl complexes with alkynes to form iron(m bisacetylide complexes was examined. The suitability of precursor iron(m monoacetylide complexes was scrutinised with regard to their ability to form the unsymmetrically substituted iron(m bisacetylide complexes. Photochemical metathesis reactions of complexes of the type trans-[Fe(C=CR)(CH3)(dmpe)2] were found to give the pure unsymmetrical iron(m bisacetylide complexes. The structure of the unsymmetrical iron(m bisacetylide complex, trans-[Fe(C-=CC6Hs)(C-=CCJl40CH3)2)(dmpeh] (144) was determined by X-ray diffraction. Using this approach with difunctional acetylenes such as 1, 7-octadiyne, bridged species including trans, trans-[Fe2(µ-C=C(CH2)4O=C)( C=CC􀀒sh( dmpe )4] (159) were synthesised. The synthesis and properties of 1,4-disubstituted iron(m butenynyl complexes from iron(m bisacetylide complexeswere investigated. The synthesis of symmetrically substituted iron(m butenynyl complexes from iron(m bisacetylides was achieved and was extended to the synthesis of unsymmetrically 1 ,4-disubstituted iron(m butenynyl complexes from unsymmetrical iron(m bisacetylide complexes. The structures of the two regioisomeric iron(m butenynyl complexes, cis-[Fe{113-C(O=CPh)=CH'Bu}(dmpe)2][PF6] (190) and cis-[Fe{1,3-C(C=C'Bu)=CHPh}(dmpe)2][PF6] (193) were determined by X-ray diffraction. A unique dimeric iron(m butenynyl complex cis,cis-[Fe2 { C(C=C􀀾s)=CH(CH2)4CH=(C=CC6Hs)C}( dmpe)4] 2[C02CF3] (206) was synthesised by rearrangement of the dimeric iron(II) bisacetylide complex trans,trans-[Fe2(µ-C=- C(CH2)4C=- C)(C=CC6Hs)2(dmpe)4] (159). The synthesis of iron(m butenynyl complexes from iron(m acetylide triflate complexes in the presence of added acetylene was examined and a number of mechanisms for the formation of the mixture of products were proposed.

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43

Cooke, Jason. "Fe(CO)¦4(eta²-alkyne) compounds, an organometallic renaissance". Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1998. http://www.collectionscanada.ca/obj/s4/f2/dsk2/ftp02/NQ34751.pdf.

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44

Lind, Per. "Organic and organometallic compounds for nonlinear absorption of light". Doctoral thesis, Umeå : Department of Chemistry, Umeå University, 2007. http://urn.kb.se/resolve?urn=urn:nbn:se:umu:diva-965.

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45

Wong, L.-L. "Studies in reactivity and dynamic processes of organometallic compounds". Thesis, University of Oxford, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.382707.

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46

Stevenson, Maya. "The study of structure and dynamics in organometallic compounds". Thesis, University of Oxford, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.302332.

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47

Podesta, David Mark. "Thermolysis and autoxidation of selected group IVB organometallic compounds". Thesis, University of Nottingham, 1991. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.293619.

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48

Bedson, Thomas Robert. "Nanostructure fabrication using electron beam irradiation of organometallic compounds". Thesis, University of Birmingham, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.369333.

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49

Hart, Suzanne L. "Synthesis and applications of chiral-at-titanium organometallic compounds". Thesis, University of Warwick, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.245941.

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50

El-Hamruni, Salima Maherize. "Organometallic compounds containing the (dimethylaminodimethylsilyl)bis(trimethylsilyl) methyl ligand". Thesis, University of Sussex, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.326949.

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