Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies

Autores
Gil, Diego Mauricio; Avila, Manuel; Reguera, Edilso; Pagola, Silvina; Gómez, María Inés; Carbonio, Raul Ernesto
Año de publicación
2012
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Pb2[Fe(CN)6]4H2O was synthesized by mixing aqueous solutions of lead(II) nitrate and potassium ferrocyanide. Its crystal structure was solved ab initio from synchrotron powder X-ray diffraction data using the direct methods and refined by the Rietveld method. Thermal analysis (TGA and DTA), Fourier Transform Infrared Spectroscopy (FTIR) and scanning electron microscopy (SEM) studies were also used for the solid state characterization of this compound and its decomposition products. The complex crystallizes in the monoclinic crystal system, space group P21/n. The Fe2+ cation is octahedrally coordinated to six cyano groups, and the Pb2+ cation is penta-fold coordinated to three N atoms from C„N ligands and two O atoms from coordinated water molecules. The most important peculiarity of the structure of this complex is the occurrence of water bridges linking two neighboring Pb2+ cations. An unusual Fe–C„N–Pb(H2O)2– Pb–N„C–Fe linkage alternates with a usual Pb–N„C–Fe one. Zeolitic water molecules are also observed in the structure; they are located in small channels in the structure and they are hydrogen bonded to coordinated water molecules forming a cumulus. Coordinated water and zeolitic water molecules in this complex can be removed without affecting the hexacyanometallate framework. The thermal decomposition in air to produce Pb2Fe2O5 and PbO as final products has been studied by thermogravimetric and differential thermal analysis, FTIR spectroscopy and laboratory powder X-ray diffraction. The crystallite size and morphology of the complex and its thermal decomposition products were evaluated by SEM.
Fil: Gil, Diego Mauricio. Universidad Nacional de Tucumán. Facultad de Bioquímica, Química y Farmacia. Instituto de Química Inorgánica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Tucumán. Instituto de Química del Noroeste. Universidad Nacional de Tucumán. Facultad de Bioquímica, Química y Farmacia. Instituto de Química del Noroeste; Argentina
Fil: Avila, Manuel. Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada; México
Fil: Reguera, Edilso. Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada; México
Fil: Pagola, Silvina. No especifíca;
Fil: Gómez, María Inés. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Departamento de Fisicoquímica; Argentina
Fil: Carbonio, Raul Ernesto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentina
Materia
Pb2[Fe(CN)6]4H2O
Crytal structure
Synchrotron
PXRD
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/241383
Acceder
id CONICETDig_bbb44090e0562f929131804a5c2a4b8c
oai_identifier_str oai:ri.conicet.gov.ar:11336/241383
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studiesGil, Diego MauricioAvila, ManuelReguera, EdilsoPagola, SilvinaGómez, María InésCarbonio, Raul ErnestoPb2[Fe(CN)6]4H2OCrytal structureSynchrotronPXRDhttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1Pb2[Fe(CN)6]4H2O was synthesized by mixing aqueous solutions of lead(II) nitrate and potassium ferrocyanide. Its crystal structure was solved ab initio from synchrotron powder X-ray diffraction data using the direct methods and refined by the Rietveld method. Thermal analysis (TGA and DTA), Fourier Transform Infrared Spectroscopy (FTIR) and scanning electron microscopy (SEM) studies were also used for the solid state characterization of this compound and its decomposition products. The complex crystallizes in the monoclinic crystal system, space group P21/n. The Fe2+ cation is octahedrally coordinated to six cyano groups, and the Pb2+ cation is penta-fold coordinated to three N atoms from C„N ligands and two O atoms from coordinated water molecules. The most important peculiarity of the structure of this complex is the occurrence of water bridges linking two neighboring Pb2+ cations. An unusual Fe–C„N–Pb(H2O)2– Pb–N„C–Fe linkage alternates with a usual Pb–N„C–Fe one. Zeolitic water molecules are also observed in the structure; they are located in small channels in the structure and they are hydrogen bonded to coordinated water molecules forming a cumulus. Coordinated water and zeolitic water molecules in this complex can be removed without affecting the hexacyanometallate framework. The thermal decomposition in air to produce Pb2Fe2O5 and PbO as final products has been studied by thermogravimetric and differential thermal analysis, FTIR spectroscopy and laboratory powder X-ray diffraction. The crystallite size and morphology of the complex and its thermal decomposition products were evaluated by SEM.Fil: Gil, Diego Mauricio. Universidad Nacional de Tucumán. Facultad de Bioquímica, Química y Farmacia. Instituto de Química Inorgánica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Tucumán. Instituto de Química del Noroeste. Universidad Nacional de Tucumán. Facultad de Bioquímica, Química y Farmacia. Instituto de Química del Noroeste; ArgentinaFil: Avila, Manuel. Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada; MéxicoFil: Reguera, Edilso. Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada; MéxicoFil: Pagola, Silvina. No especifíca;Fil: Gómez, María Inés. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Departamento de Fisicoquímica; ArgentinaFil: Carbonio, Raul Ernesto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; ArgentinaPergamon-Elsevier Science Ltd2012-04info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/241383Gil, Diego Mauricio; Avila, Manuel; Reguera, Edilso; Pagola, Silvina; Gómez, María Inés; et al.; Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies; Pergamon-Elsevier Science Ltd; Polyhedron; 33; 1; 4-2012; 450-4550277-5387CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/pii/S027753871100756Xinfo:eu-repo/semantics/altIdentifier/doi/10.1016/j.poly.2011.12.006info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-03T10:04:06Zoai:ri.conicet.gov.ar:11336/241383instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-09-03 10:04:06.893CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
title Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
spellingShingle Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
Gil, Diego Mauricio
Pb2[Fe(CN)6]4H2O
Crytal structure
Synchrotron
PXRD
title_short Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
title_full Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
title_fullStr Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
title_full_unstemmed Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
title_sort Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies
dc.creator.none.fl_str_mv Gil, Diego Mauricio
Avila, Manuel
Reguera, Edilso
Pagola, Silvina
Gómez, María Inés
Carbonio, Raul Ernesto
author Gil, Diego Mauricio
author_facet Gil, Diego Mauricio
Avila, Manuel
Reguera, Edilso
Pagola, Silvina
Gómez, María Inés
Carbonio, Raul Ernesto
author_role author
author2 Avila, Manuel
Reguera, Edilso
Pagola, Silvina
Gómez, María Inés
Carbonio, Raul Ernesto
author2_role author
author
author
author
author
dc.subject.none.fl_str_mv Pb2[Fe(CN)6]4H2O
Crytal structure
Synchrotron
PXRD
topic Pb2[Fe(CN)6]4H2O
Crytal structure
Synchrotron
PXRD
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv Pb2[Fe(CN)6]4H2O was synthesized by mixing aqueous solutions of lead(II) nitrate and potassium ferrocyanide. Its crystal structure was solved ab initio from synchrotron powder X-ray diffraction data using the direct methods and refined by the Rietveld method. Thermal analysis (TGA and DTA), Fourier Transform Infrared Spectroscopy (FTIR) and scanning electron microscopy (SEM) studies were also used for the solid state characterization of this compound and its decomposition products. The complex crystallizes in the monoclinic crystal system, space group P21/n. The Fe2+ cation is octahedrally coordinated to six cyano groups, and the Pb2+ cation is penta-fold coordinated to three N atoms from C„N ligands and two O atoms from coordinated water molecules. The most important peculiarity of the structure of this complex is the occurrence of water bridges linking two neighboring Pb2+ cations. An unusual Fe–C„N–Pb(H2O)2– Pb–N„C–Fe linkage alternates with a usual Pb–N„C–Fe one. Zeolitic water molecules are also observed in the structure; they are located in small channels in the structure and they are hydrogen bonded to coordinated water molecules forming a cumulus. Coordinated water and zeolitic water molecules in this complex can be removed without affecting the hexacyanometallate framework. The thermal decomposition in air to produce Pb2Fe2O5 and PbO as final products has been studied by thermogravimetric and differential thermal analysis, FTIR spectroscopy and laboratory powder X-ray diffraction. The crystallite size and morphology of the complex and its thermal decomposition products were evaluated by SEM.
Fil: Gil, Diego Mauricio. Universidad Nacional de Tucumán. Facultad de Bioquímica, Química y Farmacia. Instituto de Química Inorgánica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Tucumán. Instituto de Química del Noroeste. Universidad Nacional de Tucumán. Facultad de Bioquímica, Química y Farmacia. Instituto de Química del Noroeste; Argentina
Fil: Avila, Manuel. Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada; México
Fil: Reguera, Edilso. Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada; México
Fil: Pagola, Silvina. No especifíca;
Fil: Gómez, María Inés. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Departamento de Fisicoquímica; Argentina
Fil: Carbonio, Raul Ernesto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentina
description Pb2[Fe(CN)6]4H2O was synthesized by mixing aqueous solutions of lead(II) nitrate and potassium ferrocyanide. Its crystal structure was solved ab initio from synchrotron powder X-ray diffraction data using the direct methods and refined by the Rietveld method. Thermal analysis (TGA and DTA), Fourier Transform Infrared Spectroscopy (FTIR) and scanning electron microscopy (SEM) studies were also used for the solid state characterization of this compound and its decomposition products. The complex crystallizes in the monoclinic crystal system, space group P21/n. The Fe2+ cation is octahedrally coordinated to six cyano groups, and the Pb2+ cation is penta-fold coordinated to three N atoms from C„N ligands and two O atoms from coordinated water molecules. The most important peculiarity of the structure of this complex is the occurrence of water bridges linking two neighboring Pb2+ cations. An unusual Fe–C„N–Pb(H2O)2– Pb–N„C–Fe linkage alternates with a usual Pb–N„C–Fe one. Zeolitic water molecules are also observed in the structure; they are located in small channels in the structure and they are hydrogen bonded to coordinated water molecules forming a cumulus. Coordinated water and zeolitic water molecules in this complex can be removed without affecting the hexacyanometallate framework. The thermal decomposition in air to produce Pb2Fe2O5 and PbO as final products has been studied by thermogravimetric and differential thermal analysis, FTIR spectroscopy and laboratory powder X-ray diffraction. The crystallite size and morphology of the complex and its thermal decomposition products were evaluated by SEM.
publishDate 2012
dc.date.none.fl_str_mv 2012-04
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/241383
Gil, Diego Mauricio; Avila, Manuel; Reguera, Edilso; Pagola, Silvina; Gómez, María Inés; et al.; Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies; Pergamon-Elsevier Science Ltd; Polyhedron; 33; 1; 4-2012; 450-455
0277-5387
CONICET Digital
CONICET
url http://hdl.handle.net/11336/241383
identifier_str_mv Gil, Diego Mauricio; Avila, Manuel; Reguera, Edilso; Pagola, Silvina; Gómez, María Inés; et al.; Lead hexacyanoferrate(II) tetrahydrate: Crystal structure, FTIR spectroscopy and thermal decomposition studies; Pergamon-Elsevier Science Ltd; Polyhedron; 33; 1; 4-2012; 450-455
0277-5387
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/pii/S027753871100756X
info:eu-repo/semantics/altIdentifier/doi/10.1016/j.poly.2011.12.006
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
application/pdf
application/pdf
dc.publisher.none.fl_str_mv Pergamon-Elsevier Science Ltd
publisher.none.fl_str_mv Pergamon-Elsevier Science Ltd
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
_version_ 1842269838018347008
score 13.13397

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