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Rummel, Ian Ammon. "Cyanometallate coordination polymer nanostructures and thin films synthesis and applications /." [Gainesville, Fla.] : University of Florida, 2009. http://purl.fcla.edu/fcla/etd/UFE0041117.
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GARAU, FEDERICA. "DESIGN, SYNTHESIS AND CHARACTERISATION OF POLYFUNCTIONAL COORDINATION POLYMERS." Doctoral thesis, Università degli studi di Padova, 2010. http://hdl.handle.net/11577/3427373.
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The research group where I performed my PhD researches is interested in the synthesis and characterisation of Coordination Polymers (CPs). CPs are infinite systems built up with metal ions (connectors) and organic ligands (linkers) as main elementary units, connected via coordination bonds and other weak interactions [Robin & Fromm, Coord. Chem. Rev., 2006, 250, 2127]. One of the interests in building CPs is the creation of new tuneable functional materials, since CPs are promising materials for applications in gas storage, anion exchange, catalysis, conductivity, luminescence, chirality, magnetism, spin transition behaviour, NLO or deposition of thin films. CPs can be normally prepared by reacting a suitable polynucleating ligand with a transition metal ion, having at least two coordination sites available. In order to obtain new CPs, during the first year of my PhD studies, two different classes of new potentially polynucleating nitrogen containing ligands were designed, synthesised and fully characterised. Unfortunately, some preliminary tests on the reactivity of these linkers with Cu(II), Ag(I), Zn(II) and Ru(II) in hydroalcoholic solvents evidenced the relatively easy hydrolysis of the ligands. For these reasons, at the moment, the study of the coordination properties of these ligands to transition metal ions has been set aside, and the attention has been focused on the understanding of the decomposition mechanism upon treatment with transition metal compounds [Casarin et al. Inorg. Chim. Acta, 2009,
362, 4358; Casarin et al. J. Phys. Chem. A, 2008,
112, 6723]. Moreover, we continued some other studies, concerning the synthesis of trinuclear triangular Cu(II) clusters. The latter can be easily prepared by reacting copper(II) carboxylates with pyrazole (Hpz) in hydroalcoholic solvents, obtaining 1D, 2D or 3D CPs [Casarin et al. Inorg. Chem., 2004, 43, 5865; Casarin et al. Inorg. Chem., 2005, 44, 6265; Di Nicola et al. Inorg. Chem., 2007, 46, 221]. Particularly, during my PhD studies some other trinuclear triangular Cu(II) clusters (starting both from saturated and unsaturated Cu(II) carboxylates) were synthesised and characterised [Di Nicola et al. Eur. J. Inorg. Chem., 2009, 666; Contaldi et al. Dalton Trans., 2009, 4928]. We started also to study the reactivity of the trinuclear triangular copper(II)/carboxylate/pyrazolate clusters towards substitution reactions. Particularly, we examined first the stability of the trinuclear triangular moiety by treating [Cu3(μ3-OH)(μ-pz)3(CH3COO)2(Hpz)], 2, with strong acids, observing that the trinuclear moiety was in a good extent maintained, and obtaining new hexanuclear and
heptanuclear coordination polymers, in some cases porous [Casarin et al. Cryst.
Growth Des., 2007, 4, 676]. Since the trinuclear moieties resulted to be quite stable towards decomposition, we decided to use them as starting material to synthesise new different CPs, having the trinuclear Cu(II) clusters directly
bridged by polynucleating ligands. We decided to follow two different approaches: i) substitution of the monocarboxylates with bicarboxylates; and ii) replacement of the neutral ligands coordinated to the Cu(II) centres (pyrazole and/or solvent molecules) with neutral bidentate nitrogen-containing ligands.
First attempts under bench-top conditions to replace the carboxylate ions by reacting the trinuclear compounds with bicarboxylic acids were not successful, leading to the isolation of the starting materials, while reactions carried out upon deprotonation of the acids led to the instantaneous precipitation of insoluble powders. The reaction with bidentate nitrogen-containing ligands gave instead interesting results, and numerous new CPs were isolated and fully characterised. Noteworthy, upon reaction between [Cu3(μ3-OH)(μ-pz)3(HCOO)2(Hpz)2(H2O)], 1, and an excess of 4,4’-bipyridine, a porous coordination polymer was obtained. The electrochemical properties of some selected copper(II) CPs isolated by us were examined; we also investigated the catalytic activities of some of these compounds in the peroxidative oxidation of cyclohexane. Both of these researches were performed in prof. Armando J. L. Pombeiro laboratories, at the Centro de Química Estrutural of the Instituto Superior Técnico (Lisbon). Finally, more recently,
we started to investigate the catalytic activity of 2 in the oxidation of methyl-p-tolyl sulfide to the corresponding sulfoxide. Preliminary results indicated that 2 is able to bind reversibly oxygen coming from H2O2 and transfer it to the sulfide.Il gruppo di ricerca presso cui ho svolto il Dottorato di Ricerca si occupa della sintesi e caratterizzazione di Polimeri di Coordinazione (CP). I CP sono dei sistemi polimerici infiniti, costruiti a partire da ioni metallici (connettori) e leganti organici (linkers) come principali unità di base, connessi tra loro attraverso legami di coordinazione e altre interazioni relativamente deboli [Robin & Fromm, Coord. Chem. Rev., 2006, 250, 2127]. Uno dei principali interessi nella costruzione di CP è l'ottenimento di nuovi materiali funzionali, dotati di proprietà modulabili; i CP, infatti, presentano potenziali applicazioni in diversi settori, quali ad esempio immagazzinamento di gas, scambio ionico, catalisi, conduttività, luminescenza, chiralità, magnetismo, ottica non lineare o deposizione di strati sottili. I CP vengono generalmente sintetizzati per “copolimerizzazione” di un opportuno legante polinucleanti con uno ione di un metallo di transizione avente almeno due siti di coordinazione disponibili. Al fine di ottenere nuovi CP, durante il primo anno del Dottorato di Ricerca sono state progettate e sintetizzate due diverse classi di nuovi leganti azotati potenzialmente polinucleanti. Test preliminari sulla reattività di questi composti con Cu(II), Ag(I), Zn(II) e Ru(II) in solventi protici hanno messo in evidenza la relativamente facile idrolisi dei leganti. Per questo motivo, lo studio delle loro proprietà coordinative a metalli di transizione è stato momentaneamente accantonato, e l’attenzione è stata focalizzata sulla comprensione del meccanismo della decomposizione in seguito al trattamento con metalli di transizione [Casarin et al. Inorg. Chim. Acta, 2009, 362, 4358; Casarin et al. J. Phys. Chem. A, 2008, 112, 6723]. E’ stato inoltre sviluppato un secondo progetto, riguardante la sintesi di cluster trinucleari triangolari di rame(II). Questi composti possono essere preparati facendo reagire carbossilati di Cu(II) con pirazolo (Hpz) in solvente protico (H2O, MeOH o EtOH). L’autoassemblaggio dei building blocks porta alla formazione di CP di diversa dimensionalità (1D, 2D o 3D) [Casarin et al. Inorg. Chem., 2004, 43, 5865; Casarin et al. Inorg. Chem., 2005, 44, 6265; Di Nicola et al. Inorg. Chem., 2007, 46, 221]. Sono stati quindi sintetizzati e caratterizzati nuovi cluster trinucleari triangolari di Cu(II) (partendo sia da carbossilati di Cu(II) saturi che insaturi) [Di Nicola et al. Eur. J. Inorg. Chem., 2009, 666; Contaldi et al. Dalton Trans., 2009, 4928]. Abbiamo inoltre esaminato la stabilità del frammento trinucleare [Cu3(μ3-OH)(μ-pz)3]2+ facendo reagire il composto [Cu3(μ3-OH)(μ-pz)3(CH3COO)2(Hpz)], 2, con diversi acidi forti. Benché in tutti i casi siano stati isolati complessi mononucleari, derivanti dalla parziale decomposizione del cluster trinucleare, la contemporanea formazione di derivati tri-, esa- ed eptanucleari, in alcuni casi porosi [Casarin et al. Cryst. Growth Des., 2007, 4, 676], ha messo in evidenza la relativa stabilità del frammento [Cu3(μ3-OH)(μ-pz)3]2+. Si è deciso quindi di utilizzare i differenti cluster trinucleari come materiale di partenza per la sintesi di nuovi CP, in cui più unità trinucleari fossero connesse tra loro tramite leganti polinucleanti. Abbiamo deciso di seguire due diversi approcci: i) sostituzione dei monocarbossilati con bicarbossilati; e ii) sostituzione dei leganti neutri coordinati ai centri di Cu(II) (pirazolo e/o molecole di solvente) con leganti azotati neutri bidentati. I primi tentativi in condizioni bench-top di sostituire gli ioni carbossilato facendo reagire i composti trinucleari con acidi bicarbossilici non hanno avuto successo, portando all’isolamento dei composti di partenza, mentre le reazioni condotte utilizzando i bicarbossilati hanno portato all’istantanea precipitazione di polveri insolubili. Le reazioni con leganti azotati neutri bidentati hanno invece portato all’ottenimento di risultati interessanti; infatti, sono stati isolati e caratterizzati numerosi nuovi CP. In particolare, dalla reazione di [Cu3(μ3-OH)(μ-pz)3(HCOO)2(Hpz)2(H2O)], 1, con un largo eccesso di 4,4’-bipiridina, è stato isolato un polimero di coordinazione poroso. Infine, sono state esaminate sia le proprietà elettrochimiche di alcuni CP di rame(II) da noi isolati che l’attività catalitica di alcuni di questi composti nella reazione di ossidazione perossidativa del cicloesano. Entrambi questi studi sono stati condotti nei laboratori del prof. Armando J. L. Pombeiro, presso il Centro de Química Estrutural dell’Instituto Superior Técnico (Lisbona). Più recentemente, abbiamo iniziato a studiare l’attività catalitica di 2 nell’ossidazione del metil-p-tolil solfuro al corrispondente solfossido. Risultati preliminari indicano che 2 è in grado di legare in modo reversibile l’ossigeno proveniente da H2O2 e di trasferirlo al solfuro.
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Knichal, Jane. "Design, synthesis and characterisation of advanced switchable functional materials." Thesis, University of Bath, 2017. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.760896.
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Choi, Ming Fai. "Design and synthesis of coordination polymer gels and high dichroic ratio azo dyes /." View Abstract or Full-Text, 2002. http://library.ust.hk/cgi/db/thesis.pl?CHEM%202002%20CHOI.
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Akiyama, George. "Studies on Synthesis and Application of Water Durable Porous Coordination Polymers." 京都大学 (Kyoto University), 2015. http://hdl.handle.net/2433/198948.
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Konkol, Kristine Louise. "Synthesis and Design of Thiophene Materials: Effects of Ring Fusion and Metal Coordination." Diss., North Dakota State University, 2019. https://hdl.handle.net/10365/31608.
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Conjugated organic materials comprise a field of materials chemistry focused on the development of semiconducting organic plastics, popular applications of which are plastic solar cells and display technologies. One of the reasons these materials have gained so much attention is that their optical and electronic properties can be tuned through engineering at the molecular level. Thiophene, an aromatic heterocycle, is a popular building block in the synthesis of many conjugated materials, prized for both the ease in which it can be synthetically functionalized and its ability to form highly conductive and low band gap materials.
The Rasmussen group has previously reported on the generation of two classes of materials, the inorganic metal thiophenedithiolenes and the fused-ring heterocycle unit thieno[3,4-b]pyrazine (TP), both of which have applications in conducting materials. In an effort to expand upon the applicability and versatility of these materials, a series of interconnected projects were performed to further tune their optical, electronic, and physical (e.g. solubility) properties. This involved synthetic molecular design, including judicious consideration of structure-function relationships, and characterization of the resulting materials. Highlights include a sterics vs. electronics consideration of the catalyzed hydrodebromination of the molecular building-block 2,3,5-tribromothiophene, variation of the coordinating metal in thiophenedithiolenes to tune the optics and electronics, and characterization of the effects of ring-fusion on TP-based terthienyl homopolymers. Additionally, a new application of the TP monomer was found, whereby it was successfully incorporated as a bridging ligand into a multi-metallic Ru(II) supramolecular assembly, which demonstrated good metal-metal communication.
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Ritch, Grayson D. "Synthesis, Characterization, and Reactivity of Novel Zinc Coordination Complexes." Kent State University Honors College / OhioLINK, 2014. http://rave.ohiolink.edu/etdc/view?acc_num=ksuhonors1399675758.
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Wojtecki, Rudy James. "Toward the Design and Synthesis of Mechanically Interlocked Polymers." Case Western Reserve University School of Graduate Studies / OhioLINK, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=case1380061061.
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Itakura, Tomoya. "Synthesis and Characterization of Proton Conducting Coordination Polymers Working under Low-humidity Condition." Kyoto University, 2017. http://hdl.handle.net/2433/217993.
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Pollino, Joel Matthew. "The "Universal Polymer Backbone" concept." Diss., Available online, Georgia Institute of Technology, 2004:, 2004. http://etd.gatech.edu/theses/available/etd-11112004-143714/unrestricted/pollino%5Fjoel%5Fm%5F200412%5Fphd.pdf.pdf.
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Thesis (Ph. D.)--Chemistry and Biochemistry, Georgia Institute of Technology, 2005.Weck, Marcus, Committee Chair ; Jones, Christopher, Committee Member ; Collard, David, Committee Member ; Liotta, Charles, Committee Member ; Bunz, Uwe, Committee Member. Includes bibliographical references.
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Kishida, Keisuke. "Studies on Synthesis of Flexible Microporous Coordination Polymers and Ethylene Separation from Gas Mixtures." 京都大学 (Kyoto University), 2014. http://hdl.handle.net/2433/189641.
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Kleinhans, Dewald Johannes. "Studies in the selective synthesis of bidentate resorcinarene ligands." Thesis, Stellenbosch : University of Stellenbosch, 2010. http://hdl.handle.net/10019.1/4194.
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Thesis (MSc (Chemistry and Polymer Science))--University of Stellenbosch, 2010.ENGLISH ABSTRACT: Resorcinarenes are macrocyclic products formed from the condensation of aldehydes (aliphatic or aromatic) and resorcinol and have been used in a wide range of applications since their first synthesis. Applications include: HPLC stationary phases for the separation of pyrimidine bases, racemic drugs and isomers, the selective extractions of lanthanides and actinides, as molecular receptors, catalysis, NMR chiral shift agents, GC separations and as starting materials for the synthesis of macrocyclic compounds (e.g. cavitands and carcerands) to name but a few. The use of resorcinarenes in catalysis is still quite new and unexplored, while catalysis using calix[4]arenes, a related macrocycle, has been widely studied. In this thesis it was attempted to synthesise a C2v symmetric resorcinarene precursor that could be further functionalised to form distal bidentate ligands for coordination to transition metals. These compounds would then ultimately be used in catalytic testing, especially for Pd catalysed C-C bond formation. A dibromo resorcinarene precursor was synthesised starting from resorcinarene, using methodology developed by Shivanyuk. This molecule was functionalised with a small range of different electrophiles using lithium halogen exchange methodology, although low yields were returned for the expected distal resorcinarene compounds. Other methods of functionalisation of the resorcinarene, using an anionic ortho-Fries rearrangement and the reduction of a dinitrile resorcinarene to amine and aldehyde functionalities proved unsuccessful. Using a dithioether resorcinarene a di-nuclear coordination compound was formed with Pd(II). This compound was tested for catalytic activity with a Heck reaction, showing low yields for the coupling of styrene with bromobenzene.
AFRIKAANSE OPSOMMING: Resorsinarene is makrosikliese produkte wat gevorm word deur die kondensasie van aldehiede (alifaties of aromaties) met resorsinol en word in ‘n verskeidenheid van toepassings gebruik sedert hulle eerste sintese. Tipiese voorbeelde sluit in: stationêre fases vir die HPLC-skeiding van pirimidien-basisse, rasemiese farmaseutiese middels en isomere, die selektiwe ekstraksie van lantaniede en aktiniede, molekulêre reseptore, katalise, chirale verskuiwingsreagense vir KMR spektrometrie, GC-skeidings en as uitgangverbindings vir die sintese van ander makrosikliese verbindings (bv. kavitande en karserande). Die gebruik van resorsinarene in katalise is ’n splinternuwe onontginde veld. In teenstelling hiermee is calix[4]areen, ’n verwante makrosikliese verbinding, baie meer bestudeer en vir katalise gebruik. Die doel van hierdie tesis was om ’n C2v simmetriese uitgangstof te sintetiseer wat verder gefunksionaliseer kan word om distale, bidentate ligande vir koordinasie met oorgangsmetale te lewer. Daar is beplan om die katalitiese eienskappe van die komplekse te toets, veral vir Pd-gekataliseerde C–C-koppelings reaksies. Deur gebruik te maak van ’n protokol wat deur Shivanyuk ontwikkel is, is ’n dibromo-resorsinareen gesintetiseer uit resorsinareen. Verskillende elektrofiele is in ’n litium-halogeen uitruilreaksie gebruik om ’n beperkte verskeidenheid nuwe ligande te sintetiseer wat verskillende funksionele groepe besit. Ongelukkig was die opbrengste aan distale ligande baie laag en ander metodes is dus ook ondersoek om die funksionalisering te bewerkstellig. ’n Anioniese orto-Fries herrangskikkingsreaksie en die reduksie van ’n dinitriel-resorsinareen om amien- en aldehiedfunksies te lewer, was ook onsuksesvol. Die reaksie tussen ‘n Pd(II) sout en ‘n ditioeter-gederivatiseerde resorsinareen het ‘n koordinasie verbinding met twee metaalkerne gelewer. Hierdie kompleks is deur middel van ‘n Heck-koppelingsreaksie vir katalitiese aktiwiteit getoets, maar het lae opbrengste gelewer in die koppeling van stireen en bromobenseen.
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Godber, Stephen C. "Synthesis and characterization of uncapped and capped poly(oxy-methylene) [POM] polymer produced from various bimettalic oxide coordination catalysts." Thesis, Georgia Institute of Technology, 1996. http://hdl.handle.net/1853/30569.
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Eubank, Jarrod F. "Rational synthesis toward the design of functional metal-organic materials." [Tampa, Fla] : University of South Florida, 2008. http://purl.fcla.edu/usf/dc/et/SFE0002408.
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Bulicanu, Vladimir. "Synthesis and study of magnetic molecular materials based on Co(II) and Cr(II) trinuclear clusters containing M-M bonds." Thesis, Bordeaux, 2016. http://www.theses.fr/2016BORD0239.
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Dans cette thèse est décrite la synthèse et les propriétés magnétiques des composés de coordination contenant des liaisons Co-Co ou Cr-Cr. Le contexte général sera discuté dans la première partie de ce travail en considérant l'évolution historique de ce type de chimie de coordination. Dans le deuxième chapitre, la possibilité d'intégrer un cluster {Co3} avec des ligands dipyridylamide et liaisons intermétalliques, dans des polymères de coordination unidimensionnels est discutée. Les interactions entre les porteurs de spin et l'effet du ligand pontant sont étudiés. Les changements des propriétés de transition de spin sont contrôlés en comparant par rapport au précurseur. Dans le troisième chapitre, les propriétés de molécule aimant d'un cluster de {Cr3} analogue à celui du {Co3}, sont étudiées. L'influence du ligand axial et la symétrie de la molécule sont également considérés et corrélées avec les propriétés de la molécule. Dans le quatrième chapitre, l'effet de la transition de spin induite par la coordination est étudié sur un exemple de cluster de {Co3} avec des ligands dipyridylformamidinate. La rupture et le rétablissement d'une liaison Co-Co est contrôlée par le biais de la température et de la lumière. L'effet de la rupture de la liaison intermétallique sur les propriétés magnétiques et structurales est aussi étudiéIn this thesis is described the synthesis, structures and magnetic properties of coordination compounds containing Co-Co or Cr-Cr bonds. In the first part of this work a general background is given on the historical evolution of this type of coordination chemistry. In the second chapter the possibility of incorporating a {Co3} cluster with dipyridylamide ligands and intermetallic bonds into one-dimentional coordination polymers is discussed. The interactions between spin centers and the effect of the bridging ligand were studied, and changes in the spin crossover properties were monitored and compared to the precursor. In the third chapter the Single-Molecule Magnet properties of a series of {Cr3} clusters are presented. The influence of the axial ligand and the symmetry of the molecule was considered and correlated to the magnetic properties. In the fourth chapter the phenomenon of coordination induced spin transition in a {Co3} cluster with dipyridylformamidinate ligands is discussed. Changes in magnetism and optical properties as a result of the breaking and restoring of a Co-Co bond were monitored as a function of temperature and light irradiation
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Daire, Fabrice. "Etude d'electrodes modifiees par fixation de composes de coordination sur un support conducteur du type polypyrrole : application en electrosynthese organique." Paris 6, 1988. http://www.theses.fr/1988PA066176.
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Proprietes electrochimiques des complexes co-l, cu-l, ni-l (ou l=methyl-4, bipyridine-2,2', derive du pyrrole) dans l'acetonitrile. Polymerisation electrolytique de ces complexes sur des electrodes d'or, platine et carbone. Proprietes electrochimiques du polymere co-bipyridyl-polypyrrole; utilisation dans la reduction catalytique des derives allyliques
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Ivy, Joshua F. "Optoelectronically Active Metal-Inorganic Frameworks and Supramolecular Extended Solids." Thesis, University of North Texas, 2018. https://digital.library.unt.edu/ark:/67531/metadc1248495/.
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Metal-organic frameworks (MOFs) have been intensely researched over the past 20 years. In this dissertation, metal-inorganic frameworks (MIFs), a new class of porous and nonporous materials using inorganic complexes as linkers, in lieu of traditional organic linkers in MOFs is reported. Besides novel MIF regimes, the previously described fluorous MOF "FMOF-1", is re-categorized herein as "F-MIF1". F-MIF-1 is comprised of [Ag4Tz6]2- (Tz = 3,5-bis-trifluoromethyl-1,2,4-triazolate) inorganic clusters connected by 3-coordinate Ag+ metal centers. Chapter 2 describes isosteric heat of adsorption studies of F-MIF1 for CO2 at near ambient temperatures, suggesting promise for carbon capture and storage. We then successfully exchanged some of these Ag(I) centers with Au(I) to form an isostructural Au/F-MIF1. Other, nonporous MIFs have been synthesized using Ag2Tz2 clusters with bridging diamine linkers 4,4'-bipyridine, pyrazine, and a Pt(II) complex containing two oppositely-situated non-coordinating pyridines. This strategy attained luminescent products better-positioned for photonic devices than porous materials due to greater exciton density.
Chapter 3 overviews work using an entirely inorganic luminescent complex, [Pt2(P2O5)4]4- (a.k.a. "PtPOP") to form new carbon-free MIFs. PtPOP is highly luminescent in solution, but as a solid shows poor quantum yield (QY ~0.02) and poor stability under ambient conditions. By complexing PtPOP to various metals, we have shown a dramatic enhancement in its solid-state luminescence (by an order of magnitude) and stability (from day to year scale). One embodiment (MIF-1) demonstrates microporous character.
Chapter 4 overviews the design and application of new MIF linkers. Pt complexes based upon (pyridyl)azolates, functionalized with carboxylic acid groups, have been synthesized. These complexes, and their esterized precursors, show strong luminescence on their own. They have been used to generate new luminescent MIFs. Such new MIFs may be useful toward future inorganic (LEDs) or organic (OLEDs) light-emitting diodes, respectively. The electronic communication along their infinite coordination structures is desirable for color tuning and enhanced conductivity functions, compared to the small molecules used in such technologies, which rely on intermolecular interactions for these functions.
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Maclaren, Jana K. [Verfasser], and Christoph [Akademischer Betreuer] Janiak. "Synthesis and charactarization of chiral coordination polymers = Synthese und Charakterisierung von chiralen koordinations Polymeren." Freiburg : Universität, 2012. http://d-nb.info/1123468699/34.
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Ahmed, Ejaz, Joachim Breternitz, Matthias Friedrich Groh, and Michael Ruck. "Ionic liquids as crystallisation media for inorganic materials." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2014. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-138932.
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Ionic liquids (ILs) have made a great impact on materials science and are being explored for potential applications in several disciplines. In this article, we briefly highlight the current state-of-the-art techniques employing ILs as new crystallisation media, working as neutral solvent, template or charge compensating species. The use of an IL as environmental friendly solvent offers many advantages over traditional crystallisation methods. The change from molecular to ionic reaction media leads to new types of materials being accessible. Room temperature ILs have been found to be excellent solvent systems for the crystallisation of a wide range of substances and morphologies ranging from nanoscopic crystals to micro- and even to macroscopic crystals. Moreover, high temperature routes, such as crystallisation from melts or gas phase deposition, have been replaced by convenient room or low temperature syntheses, employing ILs as reaction mediaDieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich
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Ahmed, Ejaz, Joachim Breternitz, Matthias Friedrich Groh, and Michael Ruck. "Ionic liquids as crystallisation media for inorganic materials." Royal Society of Chemistry, 2012. https://tud.qucosa.de/id/qucosa%3A27794.
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Ionic liquids (ILs) have made a great impact on materials science and are being explored for potential applications in several disciplines. In this article, we briefly highlight the current state-of-the-art techniques employing ILs as new crystallisation media, working as neutral solvent, template or charge compensating species. The use of an IL as environmental friendly solvent offers many advantages over traditional crystallisation methods. The change from molecular to ionic reaction media leads to new types of materials being accessible. Room temperature ILs have been found to be excellent solvent systems for the crystallisation of a wide range of substances and morphologies ranging from nanoscopic crystals to micro- and even to macroscopic crystals. Moreover, high temperature routes, such as crystallisation from melts or gas phase deposition, have been replaced by convenient room or low temperature syntheses, employing ILs as reaction media.Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.
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Gorlamari, Kranthikkumarreddy. "Synthesis and self-assembly of coordination lipid polymers." To access this resource online via ProQuest Dissertations and Theses @ UTEP, 2008. http://0-proquest.umi.com.lib.utep.edu/login?COPT=REJTPTU0YmImSU5UPTAmVkVSPTI=&clientId=2515.
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CABRAS, VALENTINA. "Green Synthesis Approach to Coordination Polymers by Mechanochemistry." Doctoral thesis, Università degli Studi di Cagliari, 2017. http://hdl.handle.net/11584/249603.
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The field of Metal-Organic Frameworks, also known with the abbreviation MOFs, has been subjected to an accelerated growth in the last 15 years. The process of mixing quickly available metal precursors with organic ligands—many of which are commercially available—to produce a wide range of frameworks, is capturing the interest of chemists and materials scientists worldwide.
There is an important link between MOF chemistry and fields of inorganic and coordination chemistry, there is also a conceptual link into the field of materials chemistry that has evolved applications ranging from catalysis to energy storage. Organic chemistry is also able to contribute to the MOFs design by the synthesis of new ligands with the aim of giving different properties to the MOF wall. X-ray crystallography and solid-state chemistry provide information about the structures of MOFs so that the process of designing and synthesizing MOFs can be refined to control a targeted property of those frameworks.
My PhD thesis aims to explore, especially from the point of view of synthetic and structural, morphological, thermal and textural characterizations, the chemistry of Coordination Polymers (CPs) and Metal-Organic Frameworks (MOFs). Mechanochemical synthesis has been adopted as a powerful method for environmentally-friendly CPs and MOFs synthesis. The experimental section, have been divided in four parts: the first part concerns the efficient mechanosynthesis of an iron(III) trimesate MOF and its usage for the adsorption of 4,6-dimethyldibenzothiophene (4,6-DMDBT) from a simulated low-sulfur diesel fuel. In the second, the structural, thermal and morphological properties of CPs based on unsatured Ni(II) dithiophostato/ dithiophospnonato complexes and 4,4’-bipyridine as linker are outlined. The third part dials with an array study of reactivity under mechanochemical conditions of a set of CPs based on the same unsatured Ni(II) complexes with different topologies of polydentate ligands. The final part is dedicated to the attempt to obtain thio-functionalized ligands for design, synthesis and future application in CP/ MOF architecture.
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Haja, Mohideen Mohamed Infas. "Novel metal organic frameworks : synthesis, characterisation and functions." Thesis, University of St Andrews, 2011. http://hdl.handle.net/10023/1892.
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The synthesis and properties of novel Metal Organic Frameworks were investigated and reported in this thesis. Thirteen new materials have been synthesized and their properties have been discussed with nine of the structures being solved. The most interesting and useful MOF among the thirteen materials is STAM-1, a copper-based Metal Organic Framework in which the starting linker (Benzene-1,3,5-tricarboxylic acid) undergoes selective in situ monoesterification during the synthesis. The monoesterified BTC can be recovered easily from the MOF, opening up MOF synthesis as a “protection” tool for unexpected selectivity in preparative chemistry that is difficult to accomplish using standard organic chemistry approaches. The selective linker derivatisation leads to the formation of a porous MOF with two types of accessible channel; one hydrophilic lined by copper and the other hydrophobic, lined by the ester groups. The unique structure of the pores leads to unprecedented adsorption behaviour, which reacts differently to gases or vapours of dissimilar chemistry and allows them to access different parts of the structure. The structural flexibility of STAM-1 shows significant differences in the kinetics of O₂ and N₂ adsorption, showing potential for new materials to be developed for air separation. Having two types of channel systems, adsorption can be switched between the two channels by judicious choice of the conditions; a thermal trigger to open the hydrophilic channel and a chemical trigger to open the hydrophobic channel. The storage and release capability of NO in STAM-1 was investigated for use in biomedical applications. Successful studies showed the strength of the antibacterial effects of NO loaded STAM-1, by using three different bacterial strains as a test of performance and were found to be bactericidal. Furthermore the antibacterial effects of NO free STAM-1 were also probed and found to be bactericidal even with low concentrations of the material such as 5 wt%. STAM-1 showed some complex magnetic behaviour by displaying strong antiferromagnetic properties at room temperature and ferromagnetic properties at lower temperatures. The antiferromagnetic coupling was observed within the dimer and ferromagnetic coupling between the dimers. This property of ferromagnetism can only be attributed to the corporation of magnetic dimers in the framework. STAM-2 displays a different magnetic behaviour than STAM-1 which shows paramagnetic properties at room temperature and antiferromagnetic properties at lower temperatures. Other novel MOFs were also successfully characterised and their properties were investigated for potential applications.
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Portolés, Gil Núria. "Green synthesis of coordination polymers using supercritical carbon dioxide." Doctoral thesis, Universitat Autònoma de Barcelona, 2019. http://hdl.handle.net/10803/669382.
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Recentment l’interès per la investigació en polímers de coordinació (CPs) i en xarxes metal·lorgàniques (MOFs) ha crescut degut al potencial d’aquests materials per nombroses aplicacions com per exemple, l’alliberació controlada de fàrmacs, la catàlisi i l’emmagatzematge i la separació de gasos. Generalment aquests materials són sintetitzats utilitzant dissolvents orgànics tòxics i altes temperatures. Per aquest motiu, és necessari desenvolupar rutes sintètiques més sostenibles per accelerar l'expansió industrial d'aquests productes. L’objectiu principal del treball és sintetitzar CPs utilitzant tecnologies sostenibles basades en l’ús del diòxid de carboni supercrític (scCO2) com a dissolvent. Fins avui, la utilització d’aquest dissolvent en l’àrea dels CPs i MOfs ha estat restringida a etàpes d’activació o neteja post-sintètica. No obstant l’ús de scCO2 pot anar més enllà i pot ser utilitzat també com a solvent en la síntesi d’aquest materials. Per tant, l’objectiu principal d’aquesta tesi és demostrar aquesta possibilitat, establir un protocol sintètic.
Per tal d’aconseguir aquest objectiu, s’ha desenvolupat una nova metodologia per explorar la síntesis de nous polímers de coordinació homometàl·lics o heterometal·lics de diferents dimensionalitats. Els CPs s’han obtingut mitjançant la reacció de complexos metàl·lics insaturat i els lligands orgànics en scCO2. S’han seleccionat diferents complexes organometàl·lics fluorats i lligands orgànics N-donadors tenint en compte la seva solubilitat en scCO2. Pels sistemes on s’utilitzen complexos metàl·lics amb baixa solubilitat, s’ha desenvolupat una alternativa basada en la utilització de lligands auxiliars pel metall. També s’han utilitzat connectors tipus bipiridina lineals o polipiridina trigonals. L’interès en la utilització d’aquests N-donadors per la síntesi de CPs està relacionat amb la geometria plana del nucli, que és ideal per generar estructures molt simètriques. Degut al caràcter sostenible de la síntesi s’ha considerat també el seu ús per la síntesi de materials biocompatibles. Per aquest motiu, com a prova de concepte, s’han utilitzat els productes naturals curcumina i àcid ferúlic com a lligands biocompatibles per la síntesi de bioMOFs de dos i de tres dimensions.
En resum, al llarg dels diferents capítols de la tesis es demostra la viabilitat de la utilització del scCO2 per la síntesis de CPs i MOFs. S’ha aconseguit cristal·litzar 17 nous CPs i la majoria s’han pogut resoldre cristal·logràficament. A través dels diversos capítols es descriu la manera de superar els obstacles sintètics trobats al emprar scCO2 com a solvent, tals com la baixa solubilitat dels reactius o la ràpida precipitació de les fases cinètiques. També són presentades aplicacions en adsorció de gasos, magnetisme i alliberació controlada de fàrmacs.Recently, the research in coordination polymers (CPs) and porous metal-organic frameworks (MOFs) has raised a large interest, since these materials are considered potential candidates for numerous applications, including drug delivery, catalysis, gas separation and storage. Generally, these materials are synthetized using toxic organic solvents and high temperatures. Therefore, the development of sustainable synthetic approaches becomes necessary to speed up the industrial expansion of these products. The main aim of this work is to synthetize CPs using a green technology based on supercritical carbon dioxide (scCO2) solvent. To date, the use of scCO2 in the field of CPs and MOFs has been mainly limited to the post-synthetic activation or cleaning steps. The use of scCO2 can go further, including the synthesis of these materials. Hence, the main objective of this work is to demonstrate this possibility, stablishing a synthetic protocol. In order to achieve the main aim, a new methodology has been developed to explore the synthesis of new single and mixed-metal CPs with different dimensionalities. CPs have been obtained by reacting a metallic complex and an organic linker in scCO2. Fluorinated organometallic complexes (i.e., hexafluoroacetylacetonate) and N-donor organic linkers have been selected taking into account their significant solubility in scCO2. Alternatives for systems involving metal complexes with low solubility have been also developed, based on the use of ancillary ligands for the metal. Linear bipyridyl and trigonal polypyridyl connectors have also been used. The growing interest in the synthesis of these CPs based on N-donor organic linkers is related to their core’s planar geometry, ideally suited to generate highly symmetrical structures. Most importantly, the green character of the synthesis allows to consider its use for the synthesis of biocompatible materials. Therefore, as a proof of concept the use of bio-linkers, e.g., curcumin and ferulic acid, for 2D and 3D bioMOFs synthesis has been explored. In short, along the different Chapters the viability of the easy, fast and eco-friendly synthesis of CPs and MOFs using scCO2 has been demonstrated. Using diverse metal nodes and linkers, 17 new CPs have been crystallized in this solvent, most of them elucidated crystallographically. The way in which synthetic obstacles in scCO2, such as low solubility of reagents or fast precipitation of kinetic phases are overcome, has been described along the different Chapters. Applications in gas adsorption, magnetism and drug delivery have also been presented.
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Dobrawa, Rainer Anton. "Synthesis and characterization of terpyridine-based fluorescent coordination polymers." Doctoral thesis, [S.l.] : [s.n.], 2004. http://deposit.ddb.de/cgi-bin/dokserv?idn=973411813.
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Low, Kam-hung, and 魯錦鴻. "Synthesis, structural characterization and applications of homoleptic organosulfur and organoselenium metal polymers." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2009. http://hub.hku.hk/bib/B43703859.
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Beldon, Patrick John. "New synthetic methods & applications for coordination polymers." Thesis, University of Cambridge, 2014. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.708056.
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Horike, Satoshi. "Syntheses and dynamic properties of functional porous coordination polymers." 京都大学 (Kyoto University), 2007. http://hdl.handle.net/2433/136253.
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Kitaura, Ryo. "Studies on syntheses and functions of microporous coordination polymers." 京都大学 (Kyoto University), 2003. http://hdl.handle.net/2433/148881.
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Kim, Chi Won. "Synthesis of Porous Coordination Polymers for Controlled Nitric Oxide Release." 京都大学 (Kyoto University), 2016. http://hdl.handle.net/2433/204585.
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Stackhouse, Chavis Andrew. "Azamacrocyclic-based Frameworks: Syntheses and Characterizations." Scholar Commons, 2018. https://scholarcommons.usf.edu/etd/7646.
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Research in metal-organic frameworks (MOFs) has risen greatly in recent decades Owing to their unequaled potential tunability and structural diversity. MOFs may be described as crystalline structures composed of metal cations or clusters of cations, commonly referred to as secondary building units (SBUs), and custom-designed organic ligands. The variety of structural motifs, ligands, and SBUs that may be incorporated promote the attainment of essentially countless potential MOFs and application in numerous areas of interest, such as gas adsorption, catalysis, gas separation, and sensing. Further functionalization of MOF materials by means of post-synthetic modification(PSM)33–37 of metal clusters or organic ligands, constructing frameworks using functional ligands or metal clusters, and incorporating advantageous molecules including organometallic molecules,38–41 enzymes,42–45 metal nanoparticles (NPs),8,46–48 heteropolyacids49–51 within the pores advance the diverse number of species, including organic ligands, inorganic metal ions/clusters, and guests, used to construct MOFs materials lead to MOFs materials possessing phenomenal properties. Implementation of these materials in sensing arises from the frameworks’ characteristic ability to increase the concentration of a desired analyte to a greater degree than its overall presence within the system; imparting an inherent sensitivity to the aforementioned analyte. MOFs materials also possess the potential for selectivity for specific analytes or classes of analytes through mechanisms such as size exclusion (molecular sieving), chemically specific interactions between the adsorbate and framework, and the directed design of pore and aperture size through the selection of appropriate organic linkers or struts.
Flexible azamacrocycle-based ligands are constructed through the use of pliable carboxylate pendant arms and azamacrocycles, e.g cyclen and tacn, and used in the pursuit of novel metal macrocycle frameworks (MMCF). Polyazamacrocycles represent a popular class of macrocyclic ligands for supramolecular chemistry and crystal engineering. This popularity may be due to their complexes’ high thermodynamic stability, relative kinetic inertness, basicity, transition metal-ion coordinating ability and rigid structure. Furthermore, their utilization promotes intriguing network topologies as coordination in complexes containing tetradentate azamacrocycles generally produces only two isomers differing via the coordination ligand’s conformation. The highly reported equatorial N4¬ ¬coordination of the macrocycle allows for interaction at the two vacant trans-axial positons, whilst the folded conformations permits interaction at two vacant cis positions. Azamacrocycle complexes differ from those of other classes of macrocycles due to the fact the macrocyclic cavity is commonly occupied by metal cations. Materials containing azamacrocycles have found use in applications such as bleaching and oxidative catalysis and molecular recognition. Cyclen units have reportedly been incorporated to construct pH-dependent selective receptors for copper (II), zinc(II), yttrium(III), and lanthanum(III) ions. Herein, we describe the synthesis and characterizations of a new lanthanide framework, La(C40H40N4O8)(NH2(CH2)2)NO3 or MMCF-3, which retains a vacancy in the macrocycle unit encourages the utilization of the framework as a cation receptor and precursor for heterometallic frameworks. The inclusion of azamacrocycles into MOF materials combine the characteristic high thermodynamic stability, basicity, and strong metal complexation of the macrocycles with the high porosity, surface area, and tunability of the frameworks. Full realization of the potential of Azamacrocyclic-based MOFs requires the preparation of new entrants to this class of materials that espouse various topological structures while incorporating diverse azamacrocycles. It has been shown that the hierarchical porosity associated with macrocyclic based frameworks can be obtained using this class of ligands.71,99 The development of more frameworks exhibiting this characteristic is needed to fully investigate the potential applications of MOFs retaining the vacant cavities of the azamacrocycles. Effectuation of hierarchical porosity of azamacrocyclic frameworks will broaden sensing applications, e.g. azamacrocycles have performed as receptors of anions, cations, amino acids and other analyte molecules, and provide an ideal slot to integrate open metal site into MOFs.
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Kadota, Kentaro. "Studies on Syntheses and Reactivity of Coordination Polymers using Borohydride." Kyoto University, 2020. http://hdl.handle.net/2433/253297.
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Tanaka, Daisuke. "Studies on syntheses and sorption properties of porous coordination polymers." 京都大学 (Kyoto University), 2008. http://hdl.handle.net/2433/136309.
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Zhang, Zhenjie. "Template-Directed Synthesis and Post-Synthetic Modification of Porphyrin-Encapsulating Metal-Organic Materials." Scholar Commons, 2014. https://scholarcommons.usf.edu/etd/5162.
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Metal-organic materials (MOMs) represent an emerging class of materials comprised of molecular building blocks (MBBs) linked by organic linker ligands. MOMs recently attract great attention because of their ability to exhibit permanent porosity, thereby enabling study of properties in the context of gas storage, gas separation, solid supports for sensors, catalysis and so on. Although MOMs have been studied for over 60 years, the porous nature of MOMs was not systematically and widely explored until the early 1990's. This may be one of the reasons why template-directed synthesis of MOMs remains relatively underexplored, especially when compared to other classes of porous material (e.g. zeolite and mesoporous silicates). However, the study of template-directed synthesis exhibits great significance to the research field of MOMs as these considerations: (i) to access analogues of prototypal MOM platforms that cannot be prepared directly; (2) to create porous materials with new topologies; (3) to transfer the functionality of templates to MOMs; (4) to exert fine control over structural features.
In this dissertation, I chose a functional organic material, porphyrin, as templates and succeeded to synthesize a series of porphyrin-encapsulating MOMs, (porph@MOMs), in which the porphyrins were encapsulated inside the cavities as guests. Porphyrins molecules can template the formation cavities with different shapes and sizes (e.g. triangle, square or hexagon) to accommodate the porphyrins molecules when organic ligands with different size and symmetry were utilized during the synthesis. On the other hand, the porphyrins molecules can also template the formation of octahemioctahedral cages or hexahedron cages with porphyrins trapped inside, which further built the tbo, pcu, rtl, zzz, mzz networks.
By selecting templated porph@MOMs as platforms, post-synthetic modifications (PSMs) of porph@MOMs were further studied. A cadmium MOM, porph@MOM-10, can undergo PSM by Mn(II) or Cu(II) via single-crystal-to-single-crystal processes. The Mn- and Cu- exchanged PSM variants exhibit catalytic activity for epoxidation of trans-stilbene. Porph@MOM-11 can serve as a platform to undergo a new PSM process involving cooperative addition of metal salts via single-crystal-to-single-crystal processes. The incorporation of the salts leads to higher H2 and CO2 volumetric uptake and higher CO2 vs CH4 selectivity. Porph@MOM-11 was also found to be a versatile platform that can undergo metal ion exchange with Cu2+ in single-crystal-to-single-crystal fashion. The use of mixed metal salt solutions (Cu2+/Cd2+) with varying ratios of metal salts enabled systematic study of the metal exchange process in porph@MOM-11 in such a manner that, at one extreme, only the Cd porphyrin moieties undergo metal ion exchange, whereas at the other extreme both the framework and the porphyrin moiety are fully exchanged. It is also observed that a concerted PSMs approach of metal ion exchange and ligand addition towards a porphyrin-walled MOM, porphMOM-1 affords a porphyrin-encapsulating MOM, porph@MOM-14, in which porphyrin anions are encapsulated in the octahemioctahedral polyhedral cage via weak interactions.
Beside of the template-directed synthesis and post-synthetic modification of porph@MOMs, pre-synthetic control of metal-organic materials' structures was also studied in this dissertation. Due to the partial flexibility of 1,3-benzenedicarboxylate linkers, kagom[eacute] lattice and NbO supramolecular isomers were observed from a complexation of bulky 1,3-benzenedicarboxylate ligand to Cu(II) paddlewheel moieties. In addition, a new family of hybrid nanoball vanadium MOM structures (Hyballs) was prepared by the self-assemble of trimesic acid with tetranuclear and pentanuclear vanadium polyoxometalates. These hyballs are robust, permanently porous and their exterior surfaces facilitate cross-linking via hydrogen bonds or coordination bonds to generate pcu networks.
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Lin, Zhuojia. "Hydrothermal synthesis of metal coordination polymers using mixed pyridine-carboxylate ligands /." View abstract or full-text, 2005. http://library.ust.hk/cgi/db/thesis.pl?CHEM%202005%20LIN.
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Aríñez, Soriano Javier. "Design and Synthesis of Submicron Diagnostic Systems Based on Coordination Polymers." Doctoral thesis, Universitat Autònoma de Barcelona, 2016. http://hdl.handle.net/10803/399333.
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Pilfold, Jessica Lori. "The synthesis of organoiron complexes and coordination polymers containing functionalized terpyridines." Thesis, University of British Columbia, 2013. http://hdl.handle.net/2429/44251.
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Organic terpyridine derivatives were prepared via nucleophilic substitution at the 4′-position and coordinated with iron, ruthenium, or nickel to form several chelated complexes. These chelated compounds were reacted with chloro-terminated organoiron carboxylic acid complexes to afford terpyridine-based monomers containing three metal centres. A monomer containing a cationic iron complex with two terminal terpyridine moieties was synthesized by employing a Steglich esterification between a dicarboxylic acid organoiron complex and a hexanediol-functionalized terpyridine. The monomers containing multimetal centres were polymerized through nucleophilic aromatic substitution reactions with bisphenol A or hydroquinone, while the monomer containing one organoiron moiety and terminal terpyridine groups was polymerized through chelation to iron or nickel.
The thermal properties of the polymers were investigated, with differential scanning calorimetry providing glass transition temperatures of approximately -21 °C for the iron-chelated polymers. Thermogravimetric analysis showed stepwise degradation of the cationic iron moieties, followed by the aromatic backbone, with the final decomposition step representing the loss of the bonding interaction between the iron centre and the nitrogen atoms of the chelated terpyridine groups.
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Fujiwara, Yu-ichi. "Synthesis and Formation Mechanism of Carbon Materials from Porous Coordination Polymers." Kyoto University, 2018. http://hdl.handle.net/2433/232058.
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Kandanapitiye, Murthi S. "Synthesis of Biocompatible Nanoparticulate Coordination Polymers for Diagnostic and Therapeutic Applications." Kent State University / OhioLINK, 2015. http://rave.ohiolink.edu/etdc/view?acc_num=kent1429019837.
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Tse, Hiu Wah. "Hydrothermal synthesis of metal carboxylate polymers using high coordination number metals /." View abstract or full-text, 2004. http://library.ust.hk/cgi/db/thesis.pl?CHEM%202004%20TSE.
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Shimomura, Satoru. "Studies on Syntheses and Properties of TCNQ based Porous Coordination Polymers." 京都大学 (Kyoto University), 2011. http://hdl.handle.net/2433/142185.
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Matsuda, Ryotaro. "Studies on syntheses, structures and porous properties of microporous coordination polymers." 京都大学 (Kyoto University), 2005. http://hdl.handle.net/2433/144533.
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Kyoto University (京都大学)0048
新制・課程博士
博士(工学)
甲第11794号
工博第2554号
新制||工||1354(附属図書館)
23534
UT51-2005-F824
京都大学大学院工学研究科合成･生物化学専攻
(主査)教授 北川 進, 教授 村上 正浩, 教授 宮原 稔
学位規則第4条第1項該当
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李鼎威 and Ting-wai Lee. "Self-assembly and crystal structure analysis of some first-row transition metal coordination polymers of 1,3-bis(4-pyridyl)propane." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2001. http://hub.hku.hk/bib/B31224660.
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Low, Kam-hung. "Synthesis, structural characterization and applications of homoleptic organosulfur and organoselenium metal polymers." Click to view the E-thesis via HKUTO, 2009. http://sunzi.lib.hku.hk/hkuto/record/B43703859.
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Price, David James 1976. "Synthesis, structure and magnetism in clusters and networks containing dicyanamide and related ligands." Monash University, School of Chemistry, 2003. http://arrow.monash.edu.au/hdl/1959.1/9365.
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Sushrutha, S. R. "Syntheses, Structures and Characterization of New Coordination Polymer Compounds." Thesis, 2016. http://etd.iisc.ac.in/handle/2005/2978.
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The present thesis provides a systematic investigation of coordination polymers of 3d, rare-earth (4f) and main group element (Bi) using both rigid aromatic, flexible aliphatic linkers. Luminescent sensing behavior towards nitro aromatics, metal ions and ferroelectric behavior have been investigated using some of the prepared compounds. The possible usefulness of lone pair on the structure has been investigated using bismuth based coordination polymers. The thermal and optical behavior of lanthanide coordination polymers (Ce, Pr and Nd) have also been studied.
Chapter 1 An Overview of Coordination Polymer (CP) Compounds
This chapter presents a brief introduction to coordination polymer (CP) compounds. Starting from the brief historical background on coordination compounds, this chapter shed light on some earlier developments in this family of compounds by Yaghi, Robson and others. The usefulness of carboxylate and imidazolates in construction of some important coordination polymer compounds like MOF-5, HKUST-1, ZIFs, MIL-53, UiO-66, CD-MOF-1 etc has been described in detail along with its properties. The coordination polymers exhibit many important properties and some of the properties like sorption, separation, ionic conductivity, catalysis and ferroelectricity have been discussed briefly and summerized. Chapter 1 also provides the general synthetic and characterization approaches that have been employed during the present studies.
Chapter 2
Part A: Adenine Based Coordination Polymers with Cyclohexane dicarboxylic acids
This chapter presents the synthesis, structure and properties of four new coordination polymers [Zn4(C8H10O4)2.5(C5H4N5)3.2H2O].7H2O.2DMA (I), [Cd3(C8H10O4)2(C5H4N5)2.H2O] (II), [Cd(C8H11O4)2(C5H5N5)2.2H2O] (III), [Cd(C8H10O4)(C7H8N5O).H2O]. 4H2O (IV), (CHDA = cyclohexane dicarboxylic acid, ad = adenine, DMA = dimethylacetamide, 9-HEA = 9-hydroxyethyl adenine). The compound I and II forms three-dimensional structure having distinct arrangements of 1,4-CHDA and adenine units with Zn and Cd metals respectively. The molecular complex unit is observed in compound III with 1,2-CHDA and adenine. Compound IV forms two-dimensional structure with 9-HEA and 1,2-CHDA. The observation of base-pairing interactions in the above compounds is noteworthy. In compounds I, II and IV amino groups are appears to be free and utilized for the detection of nitro aromatic explosives through
fluorescence quenching. The results revealed that the emission behavior of the present compounds is greatly influenced by the hydroxyl nitroaromatic analyses like indophenol, dinitrophenyl and trinitrophenols with very low detection limits. The compound I also exhibits considerable sensitivity towards metal ion detection, especially Fe2+/Fe3+, Cr3+, Ag+ and Hg2+ ions in solution. The presence of free nitrogen sites in compound II has been explored for the base catalyzed Knoevenagel condensation reaction, the quantitative yields are observed with various aldehyde substrates.
Part B: Adenine Based Coordination Polymer with Oxydiacetic acid: [Cd2(C4H4O5)2(C5H5N5)].H2O.DMA
The synthesis, structure and properties of a Cd based coordination polymer with oxydiacetic acid and adenine, [Cd2(C4H4O5)2(C5H5N5)].H2O. DMA is described. The compound has a two-dimensional structure formed by the connectivity involving Cd and oxydiacetic acid. The adenine ligand binds with the Cd metal center through the pyrimidine nitrogen and hangs in the inter layer spaces. The layers are stacked in a ABAB.... fashion and the inter layer spaces occupied by the dimethyl amine and water molecules. The water molecules are very labile and its removal can be accomplished by heating the sample at 100°C, which is also confirmed by the single crystal XRD, PXRD and IR studies. The availability of free amino groups of adenine molecule has been utilized for the detection of nitroaromatics, especially nitrophenols with good sensitivity. The amino group was also found to be useful in catalyzing Knoevenagel condensation reactions.
Chapter 3: Rare-Earth Metal Carboxylates: Ln2(µ3-OH)(C4H4O5)2(C4H2O4)].2H2O [Ln=Ce, Pr and Nd]
This chapter describes synthesis, structure and properties of series of rare-earth based compounds, [Ln2(µ3-OH)(C4H4O5)2(C4H2O4)].2H2O (Ln = Ce, Pr and Nd). The malic acid and fumaric acid form part of the structure. The lanthanide centers are connected by the malate units to form a two dimensional layers, which are pillared by fumarate units forming the three-dimensional structure. Overall, structure can be described as I2O1 type inorganic in two-dimension (Ln-O-Ln layers) and organic in one dimension. The extra framework water molecules form a dimer and occupy the channels. The robustness of the framework was reflected in terms of facile removal and reinsertion of the water molecules, which is also confirmed by single crystal XRD, variable temperature IR and cyclic TGA study. The presence of water dimers and weakly interacting water chain suggested the possibility of proton migration in these compounds. Proton conductivity studies reveal the conductivity values of ~2.85 x 10-6 Ω-1cm-1 at 98% relative humidity. The optical studies revealed an up-conversion behavior involving more than one photon for the neodymium compound.
Chapter 4: Bismuth Carboxylates with Brucite and Fluorite Related Structures
The synthesis, structure and properties of three new bismuth based coordination polymers have been described in this chapter. The compounds [C4N2H10][Bi(C7H4NO4)(C7H3NO4)].H2O (I), [Bi(C5H3N2O4) (C5H2N2O4)] (II) and [Bi(µ2-OH)(C7H3NO4)] (III) were isolated employing hydrothermal condition with three different heterocyclicdicarboxylic acids, 3,6-pyridinedicarboxylic acid, 4,5-imidazoledicarboxylic acid and 3,4-pyridinedicarboxylic acid respectively. The structures of all the compounds have linkages between Bi2O2 and the corresponding dicarboxylate forming a simple molecular unit in I, a bilayer arrangement in II and a three-dimensional extended structure in III. The topological arrangement of the nodal building units in the structures resembles brucite related layers in II and fluorite related arrangement in compound III. By utilizing the secondary interactions, the structure of III can be correlated to a Kagome related net. The observation of such classical inorganic related structures in the bismuth carboxylates is noteworthy. Heterogeneous catalytic studies indicate Lewis acidic nature in the bismuth center in all three compounds.
Chapter 5: Solvent dependent Delamination, Restacking and Ferroelectric studies in a Two-Dimensional Compound [NH4][Ag3(C9H5NO4S)2(C13H14N2)2].8H2O
This chapter describes synthesis, structure, water dependent delamination/restacking and ferroelectric behavior in a layered coordination polymer compound, [NH4][Ag3(C9H5NO4S)2(C13H14N2)2].8H2O. The compound has a two-dimensional structure with the water molecules occupying the inter-lamellar spaces. The lattice water molecules can be fully removed and reinserted, which accompany the crystalline-amorphous-crystalline transformation. This transformation resembles the collapse/delamination and re-stacking of the layers.
This transformation has also been investigated by in-situ IR and PXRD studies. The presence of a natural dipole (anionic framework and cationic ammonium ions) along with the non-centrosymmetric space group gives rise to a room-temperature ferroelectric behavior to the compound with saturation polarization (Ps) of 1.95 μC/cm2 and remnant polarization of 0.63 μC/cm2. The temperature dependent dielectric measurements indicate that the ferroelectric-paraelectric transformation occurs at 320 K. The ferroelectric-paraelectric transformation also follows the crystalline-amorphous-crystalline transitions.
47
Sushrutha, S. R. "Syntheses, Structures and Characterization of New Coordination Polymer Compounds." Thesis, 2016. http://etd.iisc.ernet.in/handle/2005/2978.
Full textAbstract:
The present thesis provides a systematic investigation of coordination polymers of 3d, rare-earth (4f) and main group element (Bi) using both rigid aromatic, flexible aliphatic linkers. Luminescent sensing behavior towards nitro aromatics, metal ions and ferroelectric behavior have been investigated using some of the prepared compounds. The possible usefulness of lone pair on the structure has been investigated using bismuth based coordination polymers. The thermal and optical behavior of lanthanide coordination polymers (Ce, Pr and Nd) have also been studied.
Chapter 1 An Overview of Coordination Polymer (CP) Compounds
This chapter presents a brief introduction to coordination polymer (CP) compounds. Starting from the brief historical background on coordination compounds, this chapter shed light on some earlier developments in this family of compounds by Yaghi, Robson and others. The usefulness of carboxylate and imidazolates in construction of some important coordination polymer compounds like MOF-5, HKUST-1, ZIFs, MIL-53, UiO-66, CD-MOF-1 etc has been described in detail along with its properties. The coordination polymers exhibit many important properties and some of the properties like sorption, separation, ionic conductivity, catalysis and ferroelectricity have been discussed briefly and summerized. Chapter 1 also provides the general synthetic and characterization approaches that have been employed during the present studies.
Chapter 2
Part A: Adenine Based Coordination Polymers with Cyclohexane dicarboxylic acids
This chapter presents the synthesis, structure and properties of four new coordination polymers [Zn4(C8H10O4)2.5(C5H4N5)3.2H2O].7H2O.2DMA (I), [Cd3(C8H10O4)2(C5H4N5)2.H2O] (II), [Cd(C8H11O4)2(C5H5N5)2.2H2O] (III), [Cd(C8H10O4)(C7H8N5O).H2O]. 4H2O (IV), (CHDA = cyclohexane dicarboxylic acid, ad = adenine, DMA = dimethylacetamide, 9-HEA = 9-hydroxyethyl adenine). The compound I and II forms three-dimensional structure having distinct arrangements of 1,4-CHDA and adenine units with Zn and Cd metals respectively. The molecular complex unit is observed in compound III with 1,2-CHDA and adenine. Compound IV forms two-dimensional structure with 9-HEA and 1,2-CHDA. The observation of base-pairing interactions in the above compounds is noteworthy. In compounds I, II and IV amino groups are appears to be free and utilized for the detection of nitro aromatic explosives through
fluorescence quenching. The results revealed that the emission behavior of the present compounds is greatly influenced by the hydroxyl nitroaromatic analyses like indophenol, dinitrophenyl and trinitrophenols with very low detection limits. The compound I also exhibits considerable sensitivity towards metal ion detection, especially Fe2+/Fe3+, Cr3+, Ag+ and Hg2+ ions in solution. The presence of free nitrogen sites in compound II has been explored for the base catalyzed Knoevenagel condensation reaction, the quantitative yields are observed with various aldehyde substrates.
Part B: Adenine Based Coordination Polymer with Oxydiacetic acid: [Cd2(C4H4O5)2(C5H5N5)].H2O.DMA
The synthesis, structure and properties of a Cd based coordination polymer with oxydiacetic acid and adenine, [Cd2(C4H4O5)2(C5H5N5)].H2O. DMA is described. The compound has a two-dimensional structure formed by the connectivity involving Cd and oxydiacetic acid. The adenine ligand binds with the Cd metal center through the pyrimidine nitrogen and hangs in the inter layer spaces. The layers are stacked in a ABAB.... fashion and the inter layer spaces occupied by the dimethyl amine and water molecules. The water molecules are very labile and its removal can be accomplished by heating the sample at 100°C, which is also confirmed by the single crystal XRD, PXRD and IR studies. The availability of free amino groups of adenine molecule has been utilized for the detection of nitroaromatics, especially nitrophenols with good sensitivity. The amino group was also found to be useful in catalyzing Knoevenagel condensation reactions.
Chapter 3: Rare-Earth Metal Carboxylates: Ln2(µ3-OH)(C4H4O5)2(C4H2O4)].2H2O [Ln=Ce, Pr and Nd]
This chapter describes synthesis, structure and properties of series of rare-earth based compounds, [Ln2(µ3-OH)(C4H4O5)2(C4H2O4)].2H2O (Ln = Ce, Pr and Nd). The malic acid and fumaric acid form part of the structure. The lanthanide centers are connected by the malate units to form a two dimensional layers, which are pillared by fumarate units forming the three-dimensional structure. Overall, structure can be described as I2O1 type inorganic in two-dimension (Ln-O-Ln layers) and organic in one dimension. The extra framework water molecules form a dimer and occupy the channels. The robustness of the framework was reflected in terms of facile removal and reinsertion of the water molecules, which is also confirmed by single crystal XRD, variable temperature IR and cyclic TGA study. The presence of water dimers and weakly interacting water chain suggested the possibility of proton migration in these compounds. Proton conductivity studies reveal the conductivity values of ~2.85 x 10-6 Ω-1cm-1 at 98% relative humidity. The optical studies revealed an up-conversion behavior involving more than one photon for the neodymium compound.
Chapter 4: Bismuth Carboxylates with Brucite and Fluorite Related Structures
The synthesis, structure and properties of three new bismuth based coordination polymers have been described in this chapter. The compounds [C4N2H10][Bi(C7H4NO4)(C7H3NO4)].H2O (I), [Bi(C5H3N2O4) (C5H2N2O4)] (II) and [Bi(µ2-OH)(C7H3NO4)] (III) were isolated employing hydrothermal condition with three different heterocyclicdicarboxylic acids, 3,6-pyridinedicarboxylic acid, 4,5-imidazoledicarboxylic acid and 3,4-pyridinedicarboxylic acid respectively. The structures of all the compounds have linkages between Bi2O2 and the corresponding dicarboxylate forming a simple molecular unit in I, a bilayer arrangement in II and a three-dimensional extended structure in III. The topological arrangement of the nodal building units in the structures resembles brucite related layers in II and fluorite related arrangement in compound III. By utilizing the secondary interactions, the structure of III can be correlated to a Kagome related net. The observation of such classical inorganic related structures in the bismuth carboxylates is noteworthy. Heterogeneous catalytic studies indicate Lewis acidic nature in the bismuth center in all three compounds.
Chapter 5: Solvent dependent Delamination, Restacking and Ferroelectric studies in a Two-Dimensional Compound [NH4][Ag3(C9H5NO4S)2(C13H14N2)2].8H2O
This chapter describes synthesis, structure, water dependent delamination/restacking and ferroelectric behavior in a layered coordination polymer compound, [NH4][Ag3(C9H5NO4S)2(C13H14N2)2].8H2O. The compound has a two-dimensional structure with the water molecules occupying the inter-lamellar spaces. The lattice water molecules can be fully removed and reinserted, which accompany the crystalline-amorphous-crystalline transformation. This transformation resembles the collapse/delamination and re-stacking of the layers.
This transformation has also been investigated by in-situ IR and PXRD studies. The presence of a natural dipole (anionic framework and cationic ammonium ions) along with the non-centrosymmetric space group gives rise to a room-temperature ferroelectric behavior to the compound with saturation polarization (Ps) of 1.95 μC/cm2 and remnant polarization of 0.63 μC/cm2. The temperature dependent dielectric measurements indicate that the ferroelectric-paraelectric transformation occurs at 320 K. The ferroelectric-paraelectric transformation also follows the crystalline-amorphous-crystalline transitions.
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"Synthesis and characterization of b-substituted porphyrins and their metal complexes: Monomer, Dimer and coordination polymer." Chinese University of Hong Kong, 1996. http://library.cuhk.edu.hk/record=b5895715.
Full textAbstract:
by Xiang Zhou.Thesis (Ph.D.)--Chinese University of Hong Kong, 1996.
Includes bibliographical references.
Acknowledgment --- p.i
Abstract --- p.ii
Abbreviations --- p.iii
Table of Contents --- p.iv-v
Chapter Chapter I --- Synthesis of β-substituted porphyrins --- p.1
Chapter I-1 --- Introduction --- p.1
Chapter I-1-1 --- Activation of alkanes: the biomimetic approach --- p.2
Chapter I-1-2 --- Electronic effects in β-substituted porphyrins --- p.5
Chapter I-1-3 --- Synthetic approach to β-substituted porphyrins --- p.7
Chapter I-2 --- Results and discussions --- p.14
Chapter I-2-1 --- Bromination of porphyrins at β-positions --- p.14
Chapter I-2-2 --- Synthesis of boronic acids --- p.17
Chapter I-2-3 --- Synthesis of β-substituted porphyrins --- p.18
Chapter I-2-4 --- Uv spectra --- p.25
Chapter I-2-5 --- "Crystal structures of H2TPP(Ph)4, H2TPP(Me)4， H2TPP(Tol)8 and H2TMP(Ph)8" --- p.26
Chapter I-3 --- Conclusion --- p.43
Chapter I-4 --- Experimental section --- p.44
Chapter I-5 --- References --- p.58
Chapter Chapter II --- Synthesis and Properties of Diporphyrins --- p.63
Chapter II-1 --- Introduction --- p.63
Chapter II-1-1 --- Linear dimers --- p.64
Chapter II-1-2 --- Cofacial porphyrins (or strati-bisporphyrins) --- p.68
Chapter II-1-3 --- Synthetic approach --- p.71
Chapter II-2 --- Results and discussions --- p.73
Chapter II-2-1 --- Synthetic strategy --- p.73
Chapter II-2-2 --- Synthesis of diporphyrins via condensation and Suzuki cross- coupling --- p.75
Chapter II-2-3 --- Synthesis of diporphyrins via Suzuki cross-coupling and condensation --- p.75
Chapter II-2-4 --- Metalation of diporphyrins --- p.78
Chapter II-2-5 --- Spectroscopy --- p.81
Chapter II-3 --- Conclusion --- p.89
Chapter II-4 --- Experimental section --- p.90
Chapter II-5 --- Reference --- p.100
Chapter Chapter III --- Novel Rhodium Porphyrin Complexes: Intermolecular Activation of Arene Carbon-Hydrogen Bond and Formation of a Nitrile-Bridged Coordination Polymer --- p.104
Chapter III-l --- Introduction --- p.104
Chapter III-1-1 --- Activation of C-H bonds --- p.104
Chapter III-1-2 --- Activation of C-H bond by rhodium porphyrin complexs --- p.106
Chapter III-2 --- Results and discussions --- p.108
Chapter III-2-1 --- Synthesis of rhodium porphyrin complexes --- p.108
Chapter III-2-2 --- Proton NMR --- p.112
Chapter III-2-3 --- UV and binding studies of rhodium porphyrin complexes --- p.115
Chapter III-2-4 --- IR spectra --- p.117
Chapter III-2-5 --- Crystal structures of rhodium porphyrin complexes --- p.118
Chapter III-3 --- Conclusion --- p.148
Chapter III-4 --- Experimental section --- p.149
Chapter III-5 --- References --- p.154
Appendix --- p.157
NMR Spectra --- p.159
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Kuo, Chen-Tsung, and 郭承宗. "Metal-Organic Frameworks (MOFs): Synthesis, Crystal structure and Properties of metal coordination polymer." Thesis, 2005. http://ndltd.ncl.edu.tw/handle/59061327630739007512.
Full text
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Cheng, Pei-Chi, and 鄭佩琪. "Synthesis, Structures and Properties of Coordination Polymer Containing Dipyridyl Ligands Bearing Amide Groups." Thesis, 2011. http://ndltd.ncl.edu.tw/handle/46086326580260688847.
Full textAbstract:
博士中原大學
化學研究所
99
This thesis includes five parts discussing the syntheses, structures and thermal and luminescent properties of a series of metal complexes containing the flexible N,N’-di(3-pyridyl)adipoamide (L1), N,N’-di(2-pyridyl)adipoamide (L2), N,N’-di(4-pyridyl)adipoamide (L3) and N,N’-di(3-pyridyl)dodecanedioamide (L4) ligands. All complexes have been characterized by IR, UV-vis and emission spectra, EA and TGA analysis and single-crystal X-ray diffraction. In the part I, the reactions of L1 with AgPF6 and AgSbF6 in CH3CN afforded the 1D concavo-convex chains {[Ag(L1)](PF6) • 2CH3CN}∞, 1a and {[Ag(L1)](SbF6) • CH3CN • 0.5H2O}∞, 2a, while the reactions of L1 with AgBF4 and AgNO3 in CH3CN, and AgPF6, AgSbF6, AgBF4 and AgCF3SO3 in DMF gave the 1D zigzag chains {[Ag(L1)](BF4) • CH3CN}∞, 3a, and {[Ag(L1)](NO3) • CH3CN}∞, 4, and {[Ag(L1)](PF6) • 4DMF}∞, 1b, {[Ag(L1)(DMF)](SbF6)}∞, 2b, {[Ag(L1)](BF4) • 4DMF}∞, 3b and {[Ag(L1)](CF3SO3) • DMF}∞, 5, respectively. In complexes 1a and 2a which show 1D concavo-convex chains, the L1 ligands adopt the AAA trans syn-anti conformation, whereas in other complexes which show the 1D zigzag chains, the L1 ligands adopt the AAA trans syn-syn conformations. The shapes and the sizes of the anions as well as the identity of the solvents are important in determining the structural diversity. For the complexes with the CH3CN solvents, the larger PF6- and SbF6- anions which adopt the octahedral geometry induce the 1D concavo-convex chains, while the smaller BF4- and NO3- anions which adopt the tetrahedral and triangular geometries induce the 1D zigzag chains. For complexes with the DMF solvents, all the complexes adopt the 1D zigzag chain, regardless of the shapes and sizes of the anions. In the part II, the complexes {[Ag(L1)](ClO4) • CH3CN}∞, 6, {[Ag(L1)](ClO4)}∞, 7, [Ag2(L1)2](p-TsO)2 • 2CH3CN (p-TsO = p-Toluenesulfonate), 8, and [Ag(L1)(p-TsO)]∞, 9, are reported. Complexes 6 and 7 form 1D linear chains, while 8 and 9 show a 0D dinuclear metallocycle and a 2D pleated grid with a {4,82} topology, respectively. Reversible crystal to crystal transformation was observed in 6 and 7 upon removal and uptake of the acetonitrile molecules, while the process is irreversible in 8 and 9, which are concomitant with changes in supramolecular structures, ligand conformations and luminescent properties. The main driving forces for the structural transformations are the Ag---N and Ag---O interactions. In the part III, using dipyridyladipoamide ligands and benzenedicarboxylate ligands, eight Zn(II) or Cd(II) complexes have been synthesized under hydrothermal conditions. The complexes [Zn(1,2-BDC)(L1)]∞, 10; [Zn2(1,3-BDC)2(L1)(H2O)2]∞, 11; [Zn2(1,4-BDC)2(L2)(H2O)2]∞, 12; {[Zn2(1,2-BDC)2(L3)(H2O)2] • 2H2O}∞, 13; {[Cd(1,2-BDC)(L1)(H2O)] • H2O}∞, 14; [Cd2(1,3-BDC)2(L1)(H2O)4]∞, 15; {[Cd2(1,4-BDC)2(L1)2] • (H2O)3}∞, 16; [Cd2(1,4-BDC)2(L2)(H2O)2]∞, 17, are reported. Complex 10 is a 1D loop-like chains, complex 13 exhibits 1D chains with loops and complex 15 shows 1D ladder chains, whereas complexes 11, 12, 14 and 17 show 2D pleated nets, and complex 16 exhibits a 3D framework. The bonding modes of BDC2- ligands play an important role in determining the structural dimension. In complexes 10 – 15 and 17, the BDC2- ligands adopt the μ2 bonding mode, whereas in complex 16, the BDC2- ligands adopt both the μ2 and μ4 bonding modes to form 3D frameworks. In the part IV, using dipyridyladipoamide ligands and pyridinedicarboxylate or benzenetricarboxylate ligands, nine complexes have been synthesized under hydrothermal conditions. The complexes {[Zn2(2,5-PDC)2(L1)(H2O)2] • 2H2O}∞, 18; [Zn2(2,6-PDC)2(L1)]∞, 19; {[Zn2(3,4-PDC)2(L1)(H2O)6] • 4H2O}∞, 20; {[Cd(2,6-PDC)(L1)(H2O)] • 4H2O}∞, 21; [Zn(1,3,5-HBTC)(L1)]∞, 22; {[Cd(1,2,3-HBTC)(L1)(H2O)] • H2O}∞, 23; {[Cd2(1,3,5-HBTC)2(L1)(H2O)2] • 2H2O}∞, 24; {[Zn3(1,2,4-BTC)2(L1)(H2O)4] • 4H2O}∞, 25; {[Cd3(1,3,5BTC)2(L3)3(H2O)3] • 3H2O}∞, 26, are reported. Complexes 20 and 21 exhibit 1D ladder chains. Complexes 18, 19 and 22 possess 2D pleated nets and complex 24 shows a 2D layer structure. Complexes 23, 25 and 26 show 3D frameworks. In complexes 25 and 26, the BTC3- ligands adopt the μ4 and μ3 bonding modes to form 3D frameworks. In the part V, using N,N’-di(3-pyridyl)dodecanedioamide (L4)ligands and multicarboxylate ligands, five complexes have been synthesized under hydrothermal conditions. The complexes [Zn(2,4-PDC)(L4)(H2O)]∞, 27; {[Zn(1,3,5-HBTC)(L4)] • 2H2O}∞, 28; {[Zn(3,4-PDC)(L4)] • 0.5L4}∞, 29; {[Cd(1,2-BDC)(L4)(H2O)] • 0.5L4}∞, 30; {[Cd(1,3,5-HBTC)(L4)1.5] • 2H2O}∞, 31, are reported. Complex 27 exhibits 1D tube like chains, while complex 28 possess 1D infinite chains and complex 29 shows 1D fish-bone chains. Complexes 30 and 31 show 2D pleated nets.