Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos
Ano de defesa: | 2007 |
---|---|
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
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/4151 |
Resumo: | In this work, the structures of coordination polymers and molecular compounds Cu(II), Hg(II), Pb(II) and Cd(II) with phenylphosphinate or diphenylphosphinate ligands were determined and are discussed. The reaction of phenylphosphinic or diphenylphosphinic acid with copper(II) acetate hydrate produces respectively aquaphenylphosphinate copper(II) or quadiphenylphosphinate copper(II), both insoluble polymeric compounds. The formation of adducts by dissolving these compounds in methanol in the presence of Lewis bases, such as pyridine or N, N, N , N -tetramethylethylenediamine (tmeda), breaks the polymeric chains. Slow evaporation under an inert atmosphere of solutions of the adducts formed crystals for the complexes [Cu{O2P(H)Ph}2(NC5H5)2(OH2)] (1.1), [Cu{O2PPh2}2(NC5H5)2(OH2)] (2.1) e [Cu{O2PPh2}2{(CH3)2N(CH2)2N(CH3)2}(OH2)] (2.2). There are intra and intermoleculares interactions between ligands molecules. Strong hydrogen bond interactions form a supramolecular arrangement in the two structures, those of 1.1 e 2.1. The novel diphenylphosphinate bridged coordination polymer catena- [Hg(μ2O2PPh2)] was synthesized as a colorless powder from mercury(II) acetate and diphenylphosphinic acid. Coordinating solvents were used to break the solid-state polymeric chains to allow the crystallization of new polymeric compounds. Crystallization from methylsulfoxide/methanol gave the solvent-free polymer catena-[Hg(μ2O2PPh2)] while pyridine/methanol gave the 1:2 Hg:pyridine adduct, catena-[Hg(μ2-O2PPh2)2(NC5H5)2] 3.1 and the molecular compound [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2. In the centrosymmetric title compound [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2, the approximately octahe9 dral Hg atom is coordinated by two each of phenylphosphinato, phosphinic acid and pyridine ligands. Each pair of phosphinic acid and phosphinato ligand features an intramolecular hydrogen bond to form an eight membered ring. The compounds 3 e 3.1, have a polymeric chain with two asymmetrically bridging diphenylphosphinate ligands. The latter also has two pyridine molecules coordinated to the Hg center. Bridged polymers, catena-[Pb(m2-O2PPh2)2{OCHN(CH3)2}2], 4.1, catena Pb(μ2-O2PPh2)2(NC5H5) 4.2, catena-[Pb(m2-O2PPh2)2(OS(CH3)2)2] 4.3 e [Pb(μ2-O2PPh2)2(4,4 -bipy)] 4.4 were synthesized by dissolving the polymeric [Pb(O2PPh2)2]n in coordination solvents; and, with slow evaporation, reforming the polymer in a well crystalline form of the solvent adduct, suitable for single crystal X-ray crystallography. The reaction of phenylphosphinic or diphenylphosphinic acid with cadmium(II) acetate produces respectively phenylphosphinate cadmium(II) or diphenylphosphinate cadmium(II), both insoluble polymeric compounds. The formation of adducts by dissolving these compounds in methanol in the presence of Lewis bases, such as pyridine, dimethylsulfoxide and dimethylformamide, breaks the polymeric chains. The slow evaporation formed crystals of [Cd(O2PHPh)2(OS(CH3)2)2]n 5.1 [Cd(O2PHPh)2(C5H5N)2] 5.2 [Cd(O2PPh2)2]n 6, [Cd(O2PPh2)2(C5H5N)2]n 6.1, [Cd(O2PPh2)2(OS(CH3)2)2]n 6.2 e [Cd(O2PPh2)2(OCHN(CH3)2)2] 6.3. The structures show one dimensional polymeric chains, formed by phosphinate ligands asymmetrically bridging. |
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2017-05-192017-05-192007-12-03CARDOSO, Márcia Regina Siqueira. Synthesis and Structural Analysis of new Coordination Polymer and molecular compounds of Phosphinatos Metals.. 2007. 261 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007.http://repositorio.ufsm.br/handle/1/4151In this work, the structures of coordination polymers and molecular compounds Cu(II), Hg(II), Pb(II) and Cd(II) with phenylphosphinate or diphenylphosphinate ligands were determined and are discussed. The reaction of phenylphosphinic or diphenylphosphinic acid with copper(II) acetate hydrate produces respectively aquaphenylphosphinate copper(II) or quadiphenylphosphinate copper(II), both insoluble polymeric compounds. The formation of adducts by dissolving these compounds in methanol in the presence of Lewis bases, such as pyridine or N, N, N , N -tetramethylethylenediamine (tmeda), breaks the polymeric chains. Slow evaporation under an inert atmosphere of solutions of the adducts formed crystals for the complexes [Cu{O2P(H)Ph}2(NC5H5)2(OH2)] (1.1), [Cu{O2PPh2}2(NC5H5)2(OH2)] (2.1) e [Cu{O2PPh2}2{(CH3)2N(CH2)2N(CH3)2}(OH2)] (2.2). There are intra and intermoleculares interactions between ligands molecules. Strong hydrogen bond interactions form a supramolecular arrangement in the two structures, those of 1.1 e 2.1. The novel diphenylphosphinate bridged coordination polymer catena- [Hg(μ2O2PPh2)] was synthesized as a colorless powder from mercury(II) acetate and diphenylphosphinic acid. Coordinating solvents were used to break the solid-state polymeric chains to allow the crystallization of new polymeric compounds. Crystallization from methylsulfoxide/methanol gave the solvent-free polymer catena-[Hg(μ2O2PPh2)] while pyridine/methanol gave the 1:2 Hg:pyridine adduct, catena-[Hg(μ2-O2PPh2)2(NC5H5)2] 3.1 and the molecular compound [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2. In the centrosymmetric title compound [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2, the approximately octahe9 dral Hg atom is coordinated by two each of phenylphosphinato, phosphinic acid and pyridine ligands. Each pair of phosphinic acid and phosphinato ligand features an intramolecular hydrogen bond to form an eight membered ring. The compounds 3 e 3.1, have a polymeric chain with two asymmetrically bridging diphenylphosphinate ligands. The latter also has two pyridine molecules coordinated to the Hg center. Bridged polymers, catena-[Pb(m2-O2PPh2)2{OCHN(CH3)2}2], 4.1, catena Pb(μ2-O2PPh2)2(NC5H5) 4.2, catena-[Pb(m2-O2PPh2)2(OS(CH3)2)2] 4.3 e [Pb(μ2-O2PPh2)2(4,4 -bipy)] 4.4 were synthesized by dissolving the polymeric [Pb(O2PPh2)2]n in coordination solvents; and, with slow evaporation, reforming the polymer in a well crystalline form of the solvent adduct, suitable for single crystal X-ray crystallography. The reaction of phenylphosphinic or diphenylphosphinic acid with cadmium(II) acetate produces respectively phenylphosphinate cadmium(II) or diphenylphosphinate cadmium(II), both insoluble polymeric compounds. The formation of adducts by dissolving these compounds in methanol in the presence of Lewis bases, such as pyridine, dimethylsulfoxide and dimethylformamide, breaks the polymeric chains. The slow evaporation formed crystals of [Cd(O2PHPh)2(OS(CH3)2)2]n 5.1 [Cd(O2PHPh)2(C5H5N)2] 5.2 [Cd(O2PPh2)2]n 6, [Cd(O2PPh2)2(C5H5N)2]n 6.1, [Cd(O2PPh2)2(OS(CH3)2)2]n 6.2 e [Cd(O2PPh2)2(OCHN(CH3)2)2] 6.3. The structures show one dimensional polymeric chains, formed by phosphinate ligands asymmetrically bridging.Neste trabalho, foram caracterizados compostos poliméricos de coordenação e compostos moleculares com metais do tipo Cu(II), Hg(II), Pb(II) e Cd(II), com ligantes do tipo fenilfosfinato e difenilfosfinato. Fosfinatos formam fortes interações metal oxigênio devido à polaridade da ligação P O, logo, estes ligantes tornam-se ideais na formação de cadeias poliméricas no estado sólido com um grande número de centros metálicos divalentes. Com centro metálico do tipo Cu(II), foram caracterizados três compostos monoméricos: [Cu{O2P(H)Ph}2(NC5H5)2(OH2)] (1.1), [Cu{O2PPh2}2(NC5H5)2(OH2)] (2.1) e [Cu{O2PPh2}2{(CH3)2N(CH2)2N- (CH3)2}(OH2)] (2.2), caracterizando a série dos fosfinatos do tipo Cu[R2P(=O)OH]. A característica principal desta série é a presença de fortes interações do tipo inter ou intramolecular do tipo ligações de hidrogênio no estado sólido. Já com o centro metálico Hg(II), foram sintetizados compostos poliméricos catena-[Hg(μ2-O2PPh2)2] 3, catena-[Hg(μ2-O2PPh2)2(NC5H5)2] 3.1 e o composto molecular [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2. A característica destes compostos é apresentar na forma polimérica duas pontes, entre dois centros metálicos adjacentes, formadas pelos ligantes difenilfosfinatos e no composto monomérico a presença de interações intramolecular do tipo ligações de hidrogênio. Na série dos compostos do tipo fosfinatos de Pb(II), os compostos obtidos são todos de natureza polimérica, são eles: poli-catena-[Pb(m2-O2PPh2)2{OCHN(CH3)2}2], 4.1, poli-catena [Pb(μ2-O2PPh2)2(NC5H5)] 4.2, poli-catena-[Pb(m2-O2PPh2)2(OS(CH3)2)2] 4.3 e [Pb(μ2-O2PPh2)2(4,4 -bipy)] 4.4, em todos o ligante difenilfosfinato forma duas pontes entre dois centros Pb2+ adjacentes. E a última série corresponde à série dos fosfinatos de Cd(II), novamente, todos os compostos desta série são de natureza polimérica, são eles: [Cd(O2PHPh)2(OS(CH3)2)2]n 5.1 e [Cd(O2PHPh)2(C5H5N)2] 5.2 tendo em comum o ânion fenilfosfinato e as estruturas [Cd(O2PPh2)2]n 6, [Cd(O2PPh2)2(C5H5N)2]n 6.1, [Cd(O2PPh2)2(OS(CH3)2)2]n 6.2 e [Cd(O2PPh2)2(OCHN(CH3)2)2] 6.3 tendo em comum o ânion difenilfosfinato. Nesta série novamente, a preferência dos ligantes fosfinatos é a formação de duas pontes entre os centros metálicos adjacentes, com exceção para o composto 6.2, onde os ligantes difenilfosfinatos realizam três pontes entre dois centros Cd(II). Vale salientar que, na maioria dos compostos sintetizados, a presença de solventes coordenantes teve importância fundamental, pois muitos destes polímeros são praticamente insolúveis na maioria dos solventes polares e apolares, sendo então difícil à obtenção de cristais apropriados para a difração de raios-X, logo, a presença de solventes coordenantes propiciou a quebra da cadeia polimérica, possibilitando a solubilidade destes compostos.application/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuímicaQuímica orgânicaPolímerosFosfinatos metálicosCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICASíntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicosSynthesis and Structural Analysis of new Coordination Polymer and molecular compounds of Phosphinatos Metals.info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisBurrow, Robert Alanhttp://lattes.cnpq.br/5452385625669684Bortoluzzi, Adailton Joãohttp://lattes.cnpq.br/6445841478978597Fenner, Hertonhttp://lattes.cnpq.br/2943736272592164Villetti, Marcos Antoniohttp://lattes.cnpq.br/8504489050993642Lang, Ernesto Schulzhttp://lattes.cnpq.br/4481982189769819http://lattes.cnpq.br/7747625811348115Cardoso, Márcia Regina Siqueira100600000000400300300300300500300da77a491-2340-4bec-afed-a9ed5dd5092afcef0fda-b85c-4df6-b4b4-e226fb5a131754de7942-f611-4d6f-81b7-f54b7940d6e5056fc10c-f3fe-4668-8349-3ea13df9a5f38437eadf-3a57-4c40-ac38-2583cb529b980b0a0ebf-0f7f-44ad-966c-5b1f3a0423ddinfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALMARCIAREGINACARDOSO.pdfapplication/pdf13374899http://repositorio.ufsm.br/bitstream/1/4151/1/MARCIAREGINACARDOSO.pdf31bffb5fc419b115b52cfc08c26ad673MD51TEXTMARCIAREGINACARDOSO.pdf.txtMARCIAREGINACARDOSO.pdf.txtExtracted texttext/plain407341http://repositorio.ufsm.br/bitstream/1/4151/2/MARCIAREGINACARDOSO.pdf.txtb50c41478247ce71f391403996d6c758MD52THUMBNAILMARCIAREGINACARDOSO.pdf.jpgMARCIAREGINACARDOSO.pdf.jpgIM Thumbnailimage/jpeg5238http://repositorio.ufsm.br/bitstream/1/4151/3/MARCIAREGINACARDOSO.pdf.jpg87b826e5c63d4e1e7daaded8756f5853MD531/41512023-01-05 08:20:21.197oai:repositorio.ufsm.br:1/4151Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-01-05T11:20:21Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
dc.title.alternative.eng.fl_str_mv |
Synthesis and Structural Analysis of new Coordination Polymer and molecular compounds of Phosphinatos Metals. |
title |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
spellingShingle |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos Cardoso, Márcia Regina Siqueira Química Química orgânica Polímeros Fosfinatos metálicos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
title_full |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
title_fullStr |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
title_full_unstemmed |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
title_sort |
Síntese e análise estrutural de novos polímeros de coordenação e compostos moleculares de fosfinatos metálicos |
author |
Cardoso, Márcia Regina Siqueira |
author_facet |
Cardoso, Márcia Regina Siqueira |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Burrow, Robert Alan |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5452385625669684 |
dc.contributor.referee1.fl_str_mv |
Bortoluzzi, Adailton João |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/6445841478978597 |
dc.contributor.referee2.fl_str_mv |
Fenner, Herton |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2943736272592164 |
dc.contributor.referee3.fl_str_mv |
Villetti, Marcos Antonio |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/8504489050993642 |
dc.contributor.referee4.fl_str_mv |
Lang, Ernesto Schulz |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/4481982189769819 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7747625811348115 |
dc.contributor.author.fl_str_mv |
Cardoso, Márcia Regina Siqueira |
contributor_str_mv |
Burrow, Robert Alan Bortoluzzi, Adailton João Fenner, Herton Villetti, Marcos Antonio Lang, Ernesto Schulz |
dc.subject.por.fl_str_mv |
Química Química orgânica Polímeros Fosfinatos metálicos |
topic |
Química Química orgânica Polímeros Fosfinatos metálicos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, the structures of coordination polymers and molecular compounds Cu(II), Hg(II), Pb(II) and Cd(II) with phenylphosphinate or diphenylphosphinate ligands were determined and are discussed. The reaction of phenylphosphinic or diphenylphosphinic acid with copper(II) acetate hydrate produces respectively aquaphenylphosphinate copper(II) or quadiphenylphosphinate copper(II), both insoluble polymeric compounds. The formation of adducts by dissolving these compounds in methanol in the presence of Lewis bases, such as pyridine or N, N, N , N -tetramethylethylenediamine (tmeda), breaks the polymeric chains. Slow evaporation under an inert atmosphere of solutions of the adducts formed crystals for the complexes [Cu{O2P(H)Ph}2(NC5H5)2(OH2)] (1.1), [Cu{O2PPh2}2(NC5H5)2(OH2)] (2.1) e [Cu{O2PPh2}2{(CH3)2N(CH2)2N(CH3)2}(OH2)] (2.2). There are intra and intermoleculares interactions between ligands molecules. Strong hydrogen bond interactions form a supramolecular arrangement in the two structures, those of 1.1 e 2.1. The novel diphenylphosphinate bridged coordination polymer catena- [Hg(μ2O2PPh2)] was synthesized as a colorless powder from mercury(II) acetate and diphenylphosphinic acid. Coordinating solvents were used to break the solid-state polymeric chains to allow the crystallization of new polymeric compounds. Crystallization from methylsulfoxide/methanol gave the solvent-free polymer catena-[Hg(μ2O2PPh2)] while pyridine/methanol gave the 1:2 Hg:pyridine adduct, catena-[Hg(μ2-O2PPh2)2(NC5H5)2] 3.1 and the molecular compound [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2. In the centrosymmetric title compound [Hg(O2PPh2)2(HO2PPh2)2(C5H5N)2] 3.2, the approximately octahe9 dral Hg atom is coordinated by two each of phenylphosphinato, phosphinic acid and pyridine ligands. Each pair of phosphinic acid and phosphinato ligand features an intramolecular hydrogen bond to form an eight membered ring. The compounds 3 e 3.1, have a polymeric chain with two asymmetrically bridging diphenylphosphinate ligands. The latter also has two pyridine molecules coordinated to the Hg center. Bridged polymers, catena-[Pb(m2-O2PPh2)2{OCHN(CH3)2}2], 4.1, catena Pb(μ2-O2PPh2)2(NC5H5) 4.2, catena-[Pb(m2-O2PPh2)2(OS(CH3)2)2] 4.3 e [Pb(μ2-O2PPh2)2(4,4 -bipy)] 4.4 were synthesized by dissolving the polymeric [Pb(O2PPh2)2]n in coordination solvents; and, with slow evaporation, reforming the polymer in a well crystalline form of the solvent adduct, suitable for single crystal X-ray crystallography. The reaction of phenylphosphinic or diphenylphosphinic acid with cadmium(II) acetate produces respectively phenylphosphinate cadmium(II) or diphenylphosphinate cadmium(II), both insoluble polymeric compounds. The formation of adducts by dissolving these compounds in methanol in the presence of Lewis bases, such as pyridine, dimethylsulfoxide and dimethylformamide, breaks the polymeric chains. The slow evaporation formed crystals of [Cd(O2PHPh)2(OS(CH3)2)2]n 5.1 [Cd(O2PHPh)2(C5H5N)2] 5.2 [Cd(O2PPh2)2]n 6, [Cd(O2PPh2)2(C5H5N)2]n 6.1, [Cd(O2PPh2)2(OS(CH3)2)2]n 6.2 e [Cd(O2PPh2)2(OCHN(CH3)2)2] 6.3. The structures show one dimensional polymeric chains, formed by phosphinate ligands asymmetrically bridging. |
publishDate |
2007 |
dc.date.issued.fl_str_mv |
2007-12-03 |
dc.date.accessioned.fl_str_mv |
2017-05-19 |
dc.date.available.fl_str_mv |
2017-05-19 |
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.citation.fl_str_mv |
CARDOSO, Márcia Regina Siqueira. Synthesis and Structural Analysis of new Coordination Polymer and molecular compounds of Phosphinatos Metals.. 2007. 261 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/4151 |
identifier_str_mv |
CARDOSO, Márcia Regina Siqueira. Synthesis and Structural Analysis of new Coordination Polymer and molecular compounds of Phosphinatos Metals.. 2007. 261 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007. |
url |
http://repositorio.ufsm.br/handle/1/4151 |
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por |
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100600000000 |
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Universidade Federal de Santa Maria |
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Programa de Pós-Graduação em Química |
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UFSM |
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Química |
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Universidade Federal de Santa Maria |
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