Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização
Ano de defesa: | 2022 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/24640 |
Resumo: | The current work describes the synthesis and structural characterization of a new class of compounds, the giant telluroxanes. Eleven new compounds were obtained: [{(PhTe)18{M(NO3)(H2O)}O24}2I16] (M = Y (1), La (2), Eu (3), Lu (4)), [{(PhTe)18- {Nd(dmf)2I}O24}2I16]∙4dmf∙5H2O (5), [{(PhTe)18{Y(dmf)(H2O)}O24}2Br18]∙5dmf∙6H2O (6), [{(PhTe)18{La(dmf)2(H2O)}O24}2Br18]∙8H2O (7), [{(PhTe)18{Ce(dmf)2Br)}O24}2(SO4)2Br12] (8), [{(PhTe)18{Y(NO3)(H2O)}O24}2(PhSeO2)4(NO3)12] (9), [{(PhTe)18{Ce(NO3)2}O24- (PhSeO2)}2{Ce2(NO3)6}(NO3)8]∙6C4H8O2 (10) and [{(PhTe)18{Na(diox)(H2O)}O24}2- (HNEt3)4Cl18]∙3dmf∙10H2O (11). The research about the synthesis of giant telluroxanes is scarce, despite their structural versatility and promising applications in materials science, such optical materials and CO2 trapping. The methodology used for the synthesis of these compounds is related to the hydrolysis of phenyltellurium halides (PhTeI3, PhTeBr3, [PhTeI]4 and PhTeCl – the last two prepared in situ) and subsequent aggregation and condensation in the presence of different metallic salts, forming structures containing two cationic half-spheres of composition [{(PhTe)18{ML}O24}]n+, interconnected and stabilized by chalcogen bonds Te∙∙∙X (X = Cl, Br, I) or even by covalent bonds performed by the use of a spacer ligand, as phenylseleninate. The halfspheres are composed of two macrocycles: (PhTe)12O12 and (PhTe)6O6, the latter being important for the cluster, as accommodates oxophilic metal ions in a rigid coordination environment formed by the six oxygen atoms, similar to 18-crown-6 ligand. Both macrocycles are connected by –O2- bonds. The tests carried out revealed that the choice of metal ions does not depend on their oxidation state, but depends on their ionic radii since each ion must accommodate more than six bonds in its coordination sphere. It was also verified that changes in the solvent and anion from metallic salt cause variation in the morphology of the half-spheres and, consequently, the entire cluster. Single-crystal X-ray diffraction analysis proved to be the main characterization technique, followed by infrared, Raman, UV-Vis spectroscopies, as well as elemental analysis, melting point determination and mass spectrometry. |
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2022-06-07T12:50:19Z2022-06-07T12:50:19Z2022-03-29http://repositorio.ufsm.br/handle/1/24640The current work describes the synthesis and structural characterization of a new class of compounds, the giant telluroxanes. Eleven new compounds were obtained: [{(PhTe)18{M(NO3)(H2O)}O24}2I16] (M = Y (1), La (2), Eu (3), Lu (4)), [{(PhTe)18- {Nd(dmf)2I}O24}2I16]∙4dmf∙5H2O (5), [{(PhTe)18{Y(dmf)(H2O)}O24}2Br18]∙5dmf∙6H2O (6), [{(PhTe)18{La(dmf)2(H2O)}O24}2Br18]∙8H2O (7), [{(PhTe)18{Ce(dmf)2Br)}O24}2(SO4)2Br12] (8), [{(PhTe)18{Y(NO3)(H2O)}O24}2(PhSeO2)4(NO3)12] (9), [{(PhTe)18{Ce(NO3)2}O24- (PhSeO2)}2{Ce2(NO3)6}(NO3)8]∙6C4H8O2 (10) and [{(PhTe)18{Na(diox)(H2O)}O24}2- (HNEt3)4Cl18]∙3dmf∙10H2O (11). The research about the synthesis of giant telluroxanes is scarce, despite their structural versatility and promising applications in materials science, such optical materials and CO2 trapping. The methodology used for the synthesis of these compounds is related to the hydrolysis of phenyltellurium halides (PhTeI3, PhTeBr3, [PhTeI]4 and PhTeCl – the last two prepared in situ) and subsequent aggregation and condensation in the presence of different metallic salts, forming structures containing two cationic half-spheres of composition [{(PhTe)18{ML}O24}]n+, interconnected and stabilized by chalcogen bonds Te∙∙∙X (X = Cl, Br, I) or even by covalent bonds performed by the use of a spacer ligand, as phenylseleninate. The halfspheres are composed of two macrocycles: (PhTe)12O12 and (PhTe)6O6, the latter being important for the cluster, as accommodates oxophilic metal ions in a rigid coordination environment formed by the six oxygen atoms, similar to 18-crown-6 ligand. Both macrocycles are connected by –O2- bonds. The tests carried out revealed that the choice of metal ions does not depend on their oxidation state, but depends on their ionic radii since each ion must accommodate more than six bonds in its coordination sphere. It was also verified that changes in the solvent and anion from metallic salt cause variation in the morphology of the half-spheres and, consequently, the entire cluster. Single-crystal X-ray diffraction analysis proved to be the main characterization technique, followed by infrared, Raman, UV-Vis spectroscopies, as well as elemental analysis, melting point determination and mass spectrometry.Neste trabalho estão descritas a síntese e a caracterização estrutural de uma nova classe de compostos, os teluroxanos gigantes. Foram obtidos onze novos compostos: [{(PhTe)18{M(NO3)(H2O)}O24}2I16] (M = Y (1), La (2), Eu (3), Lu (4)), [{(PhTe)18{Nd- (dmf)2I}O24}2I16]∙4dmf∙5H2O (5), [{(PhTe)18{Y(dmf)(H2O)}O24}2Br18]∙5dmf∙6H2O (6), [{(PhTe)18{La(dmf)2(H2O)}O24}2Br18]∙8H2O (7), [{(PhTe)18{Ce(dmf)2Br)}O24}2(SO4)2- Br12] (8), [{(PhTe)18{Y(NO3)(H2O)}O24}2(PhSeO2)4(NO3)12] (9), [{(PhTe)18{Ce(NO3)2}- O24(PhSeO2)}2{Ce2(NO3)6}(NO3)8]∙6C4H8O2 (10) e [{(PhTe)18{Na(diox)(H2O)}O24}2- (HNEt3)4Cl18]∙3dmf∙10H2O (11). Os trabalhos de investigação do preparo de teluroxanos gigantes são escassos, apesar de sua versatilidade estrutural e promissoras aplicações na ciência dos materiais, como materiais ópticos e capturadores de CO2. A metodologia empregada para síntese destes compostos está relacionada com a hidrólise de haletos de feniltelúrio (PhTeI3, PhTeBr3, [PhTeI]4 e PhTeCl – sendo os dois últimos formados in situ) e subsequente agregação e condensação na presença de diferentes sais metálicos, formando estruturas contendo duas meias esferas catiônicas de composição [{(PhTe)18{ML}O24}]n+, interligadas e estabilizadas por ligações de calcogênio Te∙∙∙X (X = Cl, Br, I) ou, ainda, por ligações covalentes realizadas pelo uso de um ligante espaçador, como o fenilseleninato. As meias esferas são compostas por dois macrociclos: (PhTe)12O12 e (PhTe)6O6, sendo este último importante para o cluster, pois acomoda íons metálicos oxofílicos em um ambiente de coordenação rígido formado pelos seis átomos de oxigênio, semelhante ao ligante 18-coroa-6. Ambos macrociclos estão conectados por ligações -O2-. A partir dos testes realizados, verificou-se que a escolha dos íons metálicos independe do seu estado de oxidação, mas depende do tamanho do seu raio iônico, pois estes íons necessitam acomodar mais de seis ligações em sua esfera de coordenação. Verificou-se, ainda, que modificações do solvente e do ânion do sal metálico provocam mudanças na morfologia das meias esferas e, consequentemente, do cluster inteiro. A análise estrutural por difração de raios X em monocristal se mostrou como técnica de caracterização principal, seguido das análises complementares de espectroscopia na região do infravermelho, Raman e UV-Vis, bem como análise elementar, ponto de fusão e espectrometria de massas.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessTeluroxanosCluster macromolecularSíntese inorgânicaMacromolecular clusterInorganic synthesisTelluroxanesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEstudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatizaçãoStudy about giant telluroxanes: new examples and methodologies for derivatizationinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisLang, Ernesto Schulzhttp://lattes.cnpq.br/4481982189769819Tirloni, BárbaraBatista, Alzir AzevedoIglesias, Bernardo AlmeidaBack, Davi FernandoDeflon, Victor Marcelohttp://lattes.cnpq.br/7793853870530762Rodrigues, Jéssica Fonseca1006000000006006006006006006006006000c9d7568-d5c4-466d-b807-0125a7d37b975d0c00dc-a90f-49b2-85ab-243052b42d70a6258a1c-3b1b-4b10-8de8-da9ca27f844080bc4e9e-05f7-4c77-9942-75dff3449b50bef0481f-6297-4683-a6d3-ce04e5d709e3a47fce89-23ee-429f-8ccf-d3fa1be2829f91cd8068-c6ef-4ee9-a8c8-eb8fb60839a2reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2022_RODRIGUES_JÉSSICA.pdfTES_PPGQUÍMICA_2022_RODRIGUES_JÉSSICA.pdfTese de doutoradoapplication/pdf21127327http://repositorio.ufsm.br/bitstream/1/24640/1/TES_PPGQU%c3%8dMICA_2022_RODRIGUES_J%c3%89SSICA.pdf850791663fc9cbc0ff0baaeb6a43484aMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
dc.title.alternative.eng.fl_str_mv |
Study about giant telluroxanes: new examples and methodologies for derivatization |
title |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
spellingShingle |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização Rodrigues, Jéssica Fonseca Teluroxanos Cluster macromolecular Síntese inorgânica Macromolecular cluster Inorganic synthesis Telluroxanes CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
title_full |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
title_fullStr |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
title_full_unstemmed |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
title_sort |
Estudo sobre teluroxanos gigantes: novos exemplos e metodologias para derivatização |
author |
Rodrigues, Jéssica Fonseca |
author_facet |
Rodrigues, Jéssica Fonseca |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Lang, Ernesto Schulz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4481982189769819 |
dc.contributor.advisor-co1.fl_str_mv |
Tirloni, Bárbara |
dc.contributor.referee1.fl_str_mv |
Batista, Alzir Azevedo |
dc.contributor.referee2.fl_str_mv |
Iglesias, Bernardo Almeida |
dc.contributor.referee3.fl_str_mv |
Back, Davi Fernando |
dc.contributor.referee4.fl_str_mv |
Deflon, Victor Marcelo |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7793853870530762 |
dc.contributor.author.fl_str_mv |
Rodrigues, Jéssica Fonseca |
contributor_str_mv |
Lang, Ernesto Schulz Tirloni, Bárbara Batista, Alzir Azevedo Iglesias, Bernardo Almeida Back, Davi Fernando Deflon, Victor Marcelo |
dc.subject.por.fl_str_mv |
Teluroxanos Cluster macromolecular Síntese inorgânica Macromolecular cluster Inorganic synthesis |
topic |
Teluroxanos Cluster macromolecular Síntese inorgânica Macromolecular cluster Inorganic synthesis Telluroxanes CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Telluroxanes |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The current work describes the synthesis and structural characterization of a new class of compounds, the giant telluroxanes. Eleven new compounds were obtained: [{(PhTe)18{M(NO3)(H2O)}O24}2I16] (M = Y (1), La (2), Eu (3), Lu (4)), [{(PhTe)18- {Nd(dmf)2I}O24}2I16]∙4dmf∙5H2O (5), [{(PhTe)18{Y(dmf)(H2O)}O24}2Br18]∙5dmf∙6H2O (6), [{(PhTe)18{La(dmf)2(H2O)}O24}2Br18]∙8H2O (7), [{(PhTe)18{Ce(dmf)2Br)}O24}2(SO4)2Br12] (8), [{(PhTe)18{Y(NO3)(H2O)}O24}2(PhSeO2)4(NO3)12] (9), [{(PhTe)18{Ce(NO3)2}O24- (PhSeO2)}2{Ce2(NO3)6}(NO3)8]∙6C4H8O2 (10) and [{(PhTe)18{Na(diox)(H2O)}O24}2- (HNEt3)4Cl18]∙3dmf∙10H2O (11). The research about the synthesis of giant telluroxanes is scarce, despite their structural versatility and promising applications in materials science, such optical materials and CO2 trapping. The methodology used for the synthesis of these compounds is related to the hydrolysis of phenyltellurium halides (PhTeI3, PhTeBr3, [PhTeI]4 and PhTeCl – the last two prepared in situ) and subsequent aggregation and condensation in the presence of different metallic salts, forming structures containing two cationic half-spheres of composition [{(PhTe)18{ML}O24}]n+, interconnected and stabilized by chalcogen bonds Te∙∙∙X (X = Cl, Br, I) or even by covalent bonds performed by the use of a spacer ligand, as phenylseleninate. The halfspheres are composed of two macrocycles: (PhTe)12O12 and (PhTe)6O6, the latter being important for the cluster, as accommodates oxophilic metal ions in a rigid coordination environment formed by the six oxygen atoms, similar to 18-crown-6 ligand. Both macrocycles are connected by –O2- bonds. The tests carried out revealed that the choice of metal ions does not depend on their oxidation state, but depends on their ionic radii since each ion must accommodate more than six bonds in its coordination sphere. It was also verified that changes in the solvent and anion from metallic salt cause variation in the morphology of the half-spheres and, consequently, the entire cluster. Single-crystal X-ray diffraction analysis proved to be the main characterization technique, followed by infrared, Raman, UV-Vis spectroscopies, as well as elemental analysis, melting point determination and mass spectrometry. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-06-07T12:50:19Z |
dc.date.available.fl_str_mv |
2022-06-07T12:50:19Z |
dc.date.issued.fl_str_mv |
2022-03-29 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/24640 |
url |
http://repositorio.ufsm.br/handle/1/24640 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 600 600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
bitstream.url.fl_str_mv |
http://repositorio.ufsm.br/bitstream/1/24640/1/TES_PPGQU%c3%8dMICA_2022_RODRIGUES_J%c3%89SSICA.pdf http://repositorio.ufsm.br/bitstream/1/24640/2/license_rdf http://repositorio.ufsm.br/bitstream/1/24640/3/license.txt |
bitstream.checksum.fl_str_mv |
850791663fc9cbc0ff0baaeb6a43484a 4460e5956bc1d1639be9ae6146a50347 2f0571ecee68693bd5cd3f17c1e075df |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
|
_version_ |
1794524462636335104 |