Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos
Ano de defesa: | 2006 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
Tipo de documento: | Dissertação |
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/1/10510 |
Resumo: | In this work, the structures of three alkali and alkali-earth metal complexes of phenylphosphinate ligands and ethylphosphinate ligands, (4) catena-poli- [Ba(O2PHPh)2(OH2)], (5) catena-poli-[Na(O2PHPh)] e (6) catena-poli- [Ca2(O2PHEt)4(OH2)], were determined and analysed. In a typical synthesis, the compounds were prepared by the reaction of barium and sodium acetates with phenylphosphinic acid or calcium acetate with ethylphosphinic acid, under an argon atmosphere. The mixture refluxed for 2-3 hours to give a clear, colourless solution. After removal of the solvent, a microcrystalline white powder, (1) [Ba(O2PHPh)2], (2) [Na(O2PHPh)] and (3) [Ca(O2PHPh)2]. The compound catena-poli-[Ba(O2PHPh)2(OH2)] (4) was obtained by crystallization in water/methanol. Its structure belongs to the orthorhombic system and space group Pnma. The cell parameters are a= 8.0397(3) Å, b= 32.2778(17) Å, c= 5.6487(3); the refinement gives R1 = 0.028 and wR2 = 0.0637. The Ba ion has a capped trigonal prism geometry coordination formed by seven oxygen atoms, six from phenyphosphinate ligand and one from the molecules of water. The phenylphosphinate ligand forms bridges with Ba2+ ions, creating a two-dimensional coordination polymer parallel to the ac plane. The Ba O distances range between 2.743(3) Å and 2.883(3) Å. The compound catena-poli-[Na(O2PHPh)] (5) was obtained by crystallization in water/methanol. Its structure belongs to the monoclinic system and space group P21/c with cell parameters a = 5.7065(3) Å, b = 30.6702(15) Å, c = 11.7123(5) Å, β = 91.929(3)°; the refinement gives R1 = 0.0487 and wR2 = 0.1112. The three crystallographically independent Na+ ions show pyramidal quadratic and trigonal prismatic coordination geometries. Five phenylphosphinate ligands coordinate to the Na2 and Na3 center. The Na1 ion bonds to six oxygen atoms from four phenylphosphinate ligands, with two chelating. The phenylphosphinate ligand forms bridges with Na+ ions, creating a two-dimensional coordination polymer parallel to the ix ac plane. The Na O distances range from 2.290(2) Å to 2.479(2) Å for the pyramidal quadratic Na+ ion and between 2.209(2) Å and 2.632(2) Å for trigonal prismatic Na+ ion. The compound catena-poli-[Ca2(O2PHEt)4(OH2)] (6) was obtained by crystallization in water/methanol. Its structure belongs to the monoclinic system and space group P21/c with cell parameters a= 12,2082(4) Å, b= 9,5333(3) Å, c= 18,3098(6) Å, β = 99,868(2)°; the refinement gives R1 = 0,0436 and wR2 = 0,0993. The two crystallographically independent Ca2+ ions show octahedral coordination geometries. The first bonds to six oxygen atoms each from a bridging ethylphosphinate ligand. The second bonds to six oxygen atoms, five each from a bridging ethylphosphinate ligand and one molecule of water. The ethylphosphinate ligand forms bridges with Ca2+ ions, creating a two-dimensional coordination polymer parallel to the bc plane. The Ca O distances range between 2.265(2) Å and 2.410(2) Å. |
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2013-04-242013-04-242006-03-03SILVA, Rubia Mara Siqueira da. Structural analyses of two-dimensional coordination polymer of phosphinatos of alkaline and alkaline earth metals. 2006. 85 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006.http://repositorio.ufsm.br/handle/1/10510In this work, the structures of three alkali and alkali-earth metal complexes of phenylphosphinate ligands and ethylphosphinate ligands, (4) catena-poli- [Ba(O2PHPh)2(OH2)], (5) catena-poli-[Na(O2PHPh)] e (6) catena-poli- [Ca2(O2PHEt)4(OH2)], were determined and analysed. In a typical synthesis, the compounds were prepared by the reaction of barium and sodium acetates with phenylphosphinic acid or calcium acetate with ethylphosphinic acid, under an argon atmosphere. The mixture refluxed for 2-3 hours to give a clear, colourless solution. After removal of the solvent, a microcrystalline white powder, (1) [Ba(O2PHPh)2], (2) [Na(O2PHPh)] and (3) [Ca(O2PHPh)2]. The compound catena-poli-[Ba(O2PHPh)2(OH2)] (4) was obtained by crystallization in water/methanol. Its structure belongs to the orthorhombic system and space group Pnma. The cell parameters are a= 8.0397(3) Å, b= 32.2778(17) Å, c= 5.6487(3); the refinement gives R1 = 0.028 and wR2 = 0.0637. The Ba ion has a capped trigonal prism geometry coordination formed by seven oxygen atoms, six from phenyphosphinate ligand and one from the molecules of water. The phenylphosphinate ligand forms bridges with Ba2+ ions, creating a two-dimensional coordination polymer parallel to the ac plane. The Ba O distances range between 2.743(3) Å and 2.883(3) Å. The compound catena-poli-[Na(O2PHPh)] (5) was obtained by crystallization in water/methanol. Its structure belongs to the monoclinic system and space group P21/c with cell parameters a = 5.7065(3) Å, b = 30.6702(15) Å, c = 11.7123(5) Å, β = 91.929(3)°; the refinement gives R1 = 0.0487 and wR2 = 0.1112. The three crystallographically independent Na+ ions show pyramidal quadratic and trigonal prismatic coordination geometries. Five phenylphosphinate ligands coordinate to the Na2 and Na3 center. The Na1 ion bonds to six oxygen atoms from four phenylphosphinate ligands, with two chelating. The phenylphosphinate ligand forms bridges with Na+ ions, creating a two-dimensional coordination polymer parallel to the ix ac plane. The Na O distances range from 2.290(2) Å to 2.479(2) Å for the pyramidal quadratic Na+ ion and between 2.209(2) Å and 2.632(2) Å for trigonal prismatic Na+ ion. The compound catena-poli-[Ca2(O2PHEt)4(OH2)] (6) was obtained by crystallization in water/methanol. Its structure belongs to the monoclinic system and space group P21/c with cell parameters a= 12,2082(4) Å, b= 9,5333(3) Å, c= 18,3098(6) Å, β = 99,868(2)°; the refinement gives R1 = 0,0436 and wR2 = 0,0993. The two crystallographically independent Ca2+ ions show octahedral coordination geometries. The first bonds to six oxygen atoms each from a bridging ethylphosphinate ligand. The second bonds to six oxygen atoms, five each from a bridging ethylphosphinate ligand and one molecule of water. The ethylphosphinate ligand forms bridges with Ca2+ ions, creating a two-dimensional coordination polymer parallel to the bc plane. The Ca O distances range between 2.265(2) Å and 2.410(2) Å.Neste trabalho, foram caracterizados compostos com metais alcalinos e alcalinos terrosos com ligantes do tipo fenilfosfinato e etilfosfinato. Em uma síntese típica sob atmosfera de argônio, os compostos foram facilmente sintetizados a partir da reação de acetatos de bário ou sódio com ácido fenilfosfínico e acetato de cálcio com ácido etilfosfínico. A mistura foi refluxada por 2-3 horas resultando em uma solução límpida e incolor. Removeu-se o solvente, resultando em um pó branco microcristalino, (1) [Ba(O2PHPh)2], (2) [Na(O2PHPh)] e (3) [Ca(O2PHPh)2]. Destes compostos sintetizados foram elucidadas três estruturas: (4) catena-poli-[Ba(O2PHPh)2(OH2)], (5) catena-poli-[Na(O2PHPh)] e (6) catena-poli- [Ca2(O2PHEt)4(OH2)]. O composto [Ba(O2PHPh)2] (1) foi cristalizado através da evaporação lenta de uma solução água/metanol resultando no complexo catena-poli-[Ba(O2PHPh)2(OH2)] (4), que possui cela ortorrômbica e grupo espacial Pnma, os parâmetros determinados foram a= 8,0397(3) Å, b= 32,2778(17) Å, c= 5,6487(3) Å, R1 = 0,028 e wR2 = 0,0637. O centro metálico de Ba2+ possui número de coordenação sete e geometria de coordenação do tipo prisma trigonal monoencapuzado. Coordenam ao centro metálico de Ba2+ seis ligantes fenilfosfinatos e uma molécula de água. Os ligantes fenilfosfinatos formam pontes com os íons Ba2+, gerando um polimero de coordenação bidimensional no plano cristalográfico ac. Neste composto as distâncias de ligação Ba O estão entre 2,743(3) Å e 2,883(3) Å. O composto [Na(O2PHPh)] (2) foi cristalizado através da evaporação lenta de uma solução água/metanol resultando no complexo catena-poli-[Na(O2PHPh)] (5), que possui cela monoclínica e grupo espacial P21/c, os parâmetros determinados foram a= 5,7065(3) Å, b= 30,6702(15) Å, c= 11,7123(5) Å, β = 91,929(3)°, R1 = 0,0487 e wR2 = 0,1112. O centro metálico possui dois tipos de geometria de coordenação, piramidal quadrada e prismática trigonal. O centro metálico com geometria piramidal quadrada é formado por cinco átomos de oxigênio provenientes de cinco ligantes fenilfosfinatos e o centro metálico prismático trigonal, é formado por seis átomos de oxigênio, provenientes de quatro ligantes fenilfosfinatos. Os ligantes fenilfosfinatos formam pontes com os íons Na+, gerando um polimero de coordenação bidimensional no plano cristalográfico ac. As distâncias de ligação Na O estão entre 2,290(2) Å e 2,479(2) Å no centro de coordenação piramidal quadrático e entre 2,209(2) Å e 2,632(2) Å para o centro de coordenação prismático trigonal. O composto [Ca(O2PHPh)2] (3) foi cristalizado através da evaporação lenta de uma solução água/metanol resultando no complexo catena-poli-[Ca2(O2PHEt)4(OH2)] (6), que possui cela monoclínica e grupo espacial P21/c, os parâmetros determinados foram a= 12,2082(4) Å, b= 9,5333(3) Å, c= 18,3098(6) Å, β = 99,868(2)°, R1 = 0,0436 e wR2 = 0,0993. Este complexo apresenta dois íons Ca2+ cristalograficamente independentes numa geometria de coordenação octaédrica. Coordenam ao centro metálico de Ca1 seis ligantes etilfosfinatos e no centro de metálico de Ca2 cinco ligantes etilfosfinatos e uma molécula de água. Os ligantes etilfosfinatos formam pontes com os íons Ca2+, gerando um polimero de coordenação bidimensional no plano cristalográfico bc. Neste composto as distâncias de ligação Ca O estão entre 2,265(2) Å e 2,410(2) Å.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuímicaQuímica inorgânicaPolímerosFosfinatos metálicosCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAnálise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrososStructural analyses of two-dimensional coordination polymer of phosphinatos of alkaline and alkaline earth metalsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisBurrow, Robert Alanhttp://lattes.cnpq.br/5452385625669684Peppe, Clovishttp://lattes.cnpq.br/2796064506460595Fenner, Hertonhttp://lattes.cnpq.br/2943736272592164http://lattes.cnpq.br/1215582603223545Silva, Rubia Mara Siqueira da100600000000400500500300500da77a491-2340-4bec-afed-a9ed5dd5092aaf85751a-8851-4caa-874c-7e63b8b3bdd2d21e507d-ed8e-4d15-8578-9e8f08c14b7c056fc10c-f3fe-4668-8349-3ea13df9a5f3info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALSILVA, RUBIA MARA SIQUEIRA DA.pdfapplication/pdf2263972http://repositorio.ufsm.br/bitstream/1/10510/1/SILVA%2c%20RUBIA%20MARA%20SIQUEIRA%20DA.pdf30fc3b33dda4367b30f83d9b3e12ef96MD51TEXTSILVA, RUBIA MARA SIQUEIRA DA.pdf.txtSILVA, RUBIA MARA SIQUEIRA DA.pdf.txtExtracted texttext/plain119662http://repositorio.ufsm.br/bitstream/1/10510/2/SILVA%2c%20RUBIA%20MARA%20SIQUEIRA%20DA.pdf.txtf179f72f3e75927b55b84205cdfefb47MD52THUMBNAILSILVA, RUBIA MARA SIQUEIRA DA.pdf.jpgSILVA, RUBIA MARA SIQUEIRA DA.pdf.jpgIM Thumbnailimage/jpeg5850http://repositorio.ufsm.br/bitstream/1/10510/3/SILVA%2c%20RUBIA%20MARA%20SIQUEIRA%20DA.pdf.jpg45c45cda923dd894576e9258f7d6cd50MD531/105102023-02-02 09:07:13.176oai:repositorio.ufsm.br:1/10510Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-02-02T12:07:13Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
dc.title.alternative.eng.fl_str_mv |
Structural analyses of two-dimensional coordination polymer of phosphinatos of alkaline and alkaline earth metals |
title |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
spellingShingle |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos Silva, Rubia Mara Siqueira da Química Química inorgânica Polímeros Fosfinatos metálicos CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
title_full |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
title_fullStr |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
title_full_unstemmed |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
title_sort |
Análise estrutural de polímeros bidimensionais de fosfinatos de metais alcalinos e alcalinos terrosos |
author |
Silva, Rubia Mara Siqueira da |
author_facet |
Silva, Rubia Mara Siqueira da |
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 |
Peppe, Clovis |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2796064506460595 |
dc.contributor.referee2.fl_str_mv |
Fenner, Herton |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2943736272592164 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1215582603223545 |
dc.contributor.author.fl_str_mv |
Silva, Rubia Mara Siqueira da |
contributor_str_mv |
Burrow, Robert Alan Peppe, Clovis Fenner, Herton |
dc.subject.por.fl_str_mv |
Química Química inorgânica Polímeros Fosfinatos metálicos |
topic |
Química Química inorgânica 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 three alkali and alkali-earth metal complexes of phenylphosphinate ligands and ethylphosphinate ligands, (4) catena-poli- [Ba(O2PHPh)2(OH2)], (5) catena-poli-[Na(O2PHPh)] e (6) catena-poli- [Ca2(O2PHEt)4(OH2)], were determined and analysed. In a typical synthesis, the compounds were prepared by the reaction of barium and sodium acetates with phenylphosphinic acid or calcium acetate with ethylphosphinic acid, under an argon atmosphere. The mixture refluxed for 2-3 hours to give a clear, colourless solution. After removal of the solvent, a microcrystalline white powder, (1) [Ba(O2PHPh)2], (2) [Na(O2PHPh)] and (3) [Ca(O2PHPh)2]. The compound catena-poli-[Ba(O2PHPh)2(OH2)] (4) was obtained by crystallization in water/methanol. Its structure belongs to the orthorhombic system and space group Pnma. The cell parameters are a= 8.0397(3) Å, b= 32.2778(17) Å, c= 5.6487(3); the refinement gives R1 = 0.028 and wR2 = 0.0637. The Ba ion has a capped trigonal prism geometry coordination formed by seven oxygen atoms, six from phenyphosphinate ligand and one from the molecules of water. The phenylphosphinate ligand forms bridges with Ba2+ ions, creating a two-dimensional coordination polymer parallel to the ac plane. The Ba O distances range between 2.743(3) Å and 2.883(3) Å. The compound catena-poli-[Na(O2PHPh)] (5) was obtained by crystallization in water/methanol. Its structure belongs to the monoclinic system and space group P21/c with cell parameters a = 5.7065(3) Å, b = 30.6702(15) Å, c = 11.7123(5) Å, β = 91.929(3)°; the refinement gives R1 = 0.0487 and wR2 = 0.1112. The three crystallographically independent Na+ ions show pyramidal quadratic and trigonal prismatic coordination geometries. Five phenylphosphinate ligands coordinate to the Na2 and Na3 center. The Na1 ion bonds to six oxygen atoms from four phenylphosphinate ligands, with two chelating. The phenylphosphinate ligand forms bridges with Na+ ions, creating a two-dimensional coordination polymer parallel to the ix ac plane. The Na O distances range from 2.290(2) Å to 2.479(2) Å for the pyramidal quadratic Na+ ion and between 2.209(2) Å and 2.632(2) Å for trigonal prismatic Na+ ion. The compound catena-poli-[Ca2(O2PHEt)4(OH2)] (6) was obtained by crystallization in water/methanol. Its structure belongs to the monoclinic system and space group P21/c with cell parameters a= 12,2082(4) Å, b= 9,5333(3) Å, c= 18,3098(6) Å, β = 99,868(2)°; the refinement gives R1 = 0,0436 and wR2 = 0,0993. The two crystallographically independent Ca2+ ions show octahedral coordination geometries. The first bonds to six oxygen atoms each from a bridging ethylphosphinate ligand. The second bonds to six oxygen atoms, five each from a bridging ethylphosphinate ligand and one molecule of water. The ethylphosphinate ligand forms bridges with Ca2+ ions, creating a two-dimensional coordination polymer parallel to the bc plane. The Ca O distances range between 2.265(2) Å and 2.410(2) Å. |
publishDate |
2006 |
dc.date.issued.fl_str_mv |
2006-03-03 |
dc.date.accessioned.fl_str_mv |
2013-04-24 |
dc.date.available.fl_str_mv |
2013-04-24 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
SILVA, Rubia Mara Siqueira da. Structural analyses of two-dimensional coordination polymer of phosphinatos of alkaline and alkaline earth metals. 2006. 85 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10510 |
identifier_str_mv |
SILVA, Rubia Mara Siqueira da. Structural analyses of two-dimensional coordination polymer of phosphinatos of alkaline and alkaline earth metals. 2006. 85 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
url |
http://repositorio.ufsm.br/handle/1/10510 |
dc.language.iso.fl_str_mv |
por |
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por |
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100600000000 |
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400 500 500 300 500 |
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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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BR |
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Química |
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Universidade Federal de Santa Maria |
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