Lead hydro sodalite [Pb2(OH)(H2O)3][Al3Si 3O12]2: Synthesis and structure determination by combining x-ray rietveld refinement, 1H MAS NMR FTIR and XANES spectroscopy

Publikation: Beitrag in FachzeitschriftArtikelForschungPeer-Review

Autoren

  • Stefanie Eiden-Aßmann
  • Andreas Schneider
  • Peter Behrens
  • Michael Wiebcke
  • Günter Engelhardt
  • Jürgen Felsche

Organisationseinheiten

Externe Organisationen

  • Universität Konstanz
  • Universität Stuttgart
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Details

OriginalspracheEnglisch
Seiten (von - bis)292-297
Seitenumfang6
FachzeitschriftChemistry - a European journal
Jahrgang6
Ausgabenummer2
PublikationsstatusVeröffentlicht - Jan. 2000

Abstract

Ion exchange of the sodium hydro sodalites [Na3(H2O)4]2-[Al3Si 3O12]2, [Na4(H3O2)]2[Al3Si 3O12]2 and [Na4(OH)]2[Al3Si3O 12]2 with aqueous Pb(NO3)2 solutions yielded, whichever reactant sodalite phase was used, the same lead hydro sodalite, [Pb2(OH)-(H2O)3]2[Al 3Si3O12]2. Thus, in the case of the non-basic reactant [Na3(H2O)4]2-[Al3Si 3O12]2 an overexchange occurs with respect to the number of nonframework cationic charges. Rietveld structure refinement of the lead hydro sodalite based on powder X-ray diffraction data (cubic, a = 9.070 Å, room temperature, space group P43n) revealed that the two lead cations within each polyhedral sodalite cage form an orientationally disordered dinuclear [Pb2(μ-OH)(μ-H2O)(H2O)2] 3+ complex. Due to additional lead framework oxygen bonds the coordination environment of each metal cation (CN 3+3) is approximately spherical, and clearly the lead 6s electron lone pair is stereochemically inactive. This is also suggested by the absence of a small peak at 13.025 keV, attributed in other Pb2+-O compounds to an electronic 2p-6s transition, in the PbL3 edge XANES spectrum. 1H MAS NMR and FTIR spectra show that the hydrogen atoms of the aqua hydroxo complex (which could not be determined in the Rietveld analysis) are involved in hydrogen bonds of various strengths.

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Lead hydro sodalite [Pb2(OH)(H2O)3][Al3Si 3O12]2: Synthesis and structure determination by combining x-ray rietveld refinement, 1H MAS NMR FTIR and XANES spectroscopy. / Eiden-Aßmann, Stefanie; Schneider, Andreas; Behrens, Peter et al.
in: Chemistry - a European journal, Jahrgang 6, Nr. 2, 01.2000, S. 292-297.

Publikation: Beitrag in FachzeitschriftArtikelForschungPeer-Review

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@article{4cb2c99ec96743f1b00e0f2e2e57f36f,
title = "Lead hydro sodalite [Pb2(OH)(H2O)3][Al3Si 3O12]2: Synthesis and structure determination by combining x-ray rietveld refinement, 1H MAS NMR FTIR and XANES spectroscopy",
abstract = "Ion exchange of the sodium hydro sodalites [Na3(H2O)4]2-[Al3Si 3O12]2, [Na4(H3O2)]2[Al3Si 3O12]2 and [Na4(OH)]2[Al3Si3O 12]2 with aqueous Pb(NO3)2 solutions yielded, whichever reactant sodalite phase was used, the same lead hydro sodalite, [Pb2(OH)-(H2O)3]2[Al 3Si3O12]2. Thus, in the case of the non-basic reactant [Na3(H2O)4]2-[Al3Si 3O12]2 an overexchange occurs with respect to the number of nonframework cationic charges. Rietveld structure refinement of the lead hydro sodalite based on powder X-ray diffraction data (cubic, a = 9.070 {\AA}, room temperature, space group P43n) revealed that the two lead cations within each polyhedral sodalite cage form an orientationally disordered dinuclear [Pb2(μ-OH)(μ-H2O)(H2O)2] 3+ complex. Due to additional lead framework oxygen bonds the coordination environment of each metal cation (CN 3+3) is approximately spherical, and clearly the lead 6s electron lone pair is stereochemically inactive. This is also suggested by the absence of a small peak at 13.025 keV, attributed in other Pb2+-O compounds to an electronic 2p-6s transition, in the PbL3 edge XANES spectrum. 1H MAS NMR and FTIR spectra show that the hydrogen atoms of the aqua hydroxo complex (which could not be determined in the Rietveld analysis) are involved in hydrogen bonds of various strengths.",
keywords = "Host - Guest chemistry, Ion exchange, Lead, Sodalites, Structure elucidation",
author = "Stefanie Eiden-A{\ss}mann and Andreas Schneider and Peter Behrens and Michael Wiebcke and G{\"u}nter Engelhardt and J{\"u}rgen Felsche",
year = "2000",
month = jan,
language = "English",
volume = "6",
pages = "292--297",
journal = "Chemistry - a European journal",
issn = "0947-6539",
publisher = "Wiley-VCH Verlag",
number = "2",

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TY - JOUR

T1 - Lead hydro sodalite [Pb2(OH)(H2O)3][Al3Si 3O12]2

T2 - Synthesis and structure determination by combining x-ray rietveld refinement, 1H MAS NMR FTIR and XANES spectroscopy

AU - Eiden-Aßmann, Stefanie

AU - Schneider, Andreas

AU - Behrens, Peter

AU - Wiebcke, Michael

AU - Engelhardt, Günter

AU - Felsche, Jürgen

PY - 2000/1

Y1 - 2000/1

N2 - Ion exchange of the sodium hydro sodalites [Na3(H2O)4]2-[Al3Si 3O12]2, [Na4(H3O2)]2[Al3Si 3O12]2 and [Na4(OH)]2[Al3Si3O 12]2 with aqueous Pb(NO3)2 solutions yielded, whichever reactant sodalite phase was used, the same lead hydro sodalite, [Pb2(OH)-(H2O)3]2[Al 3Si3O12]2. Thus, in the case of the non-basic reactant [Na3(H2O)4]2-[Al3Si 3O12]2 an overexchange occurs with respect to the number of nonframework cationic charges. Rietveld structure refinement of the lead hydro sodalite based on powder X-ray diffraction data (cubic, a = 9.070 Å, room temperature, space group P43n) revealed that the two lead cations within each polyhedral sodalite cage form an orientationally disordered dinuclear [Pb2(μ-OH)(μ-H2O)(H2O)2] 3+ complex. Due to additional lead framework oxygen bonds the coordination environment of each metal cation (CN 3+3) is approximately spherical, and clearly the lead 6s electron lone pair is stereochemically inactive. This is also suggested by the absence of a small peak at 13.025 keV, attributed in other Pb2+-O compounds to an electronic 2p-6s transition, in the PbL3 edge XANES spectrum. 1H MAS NMR and FTIR spectra show that the hydrogen atoms of the aqua hydroxo complex (which could not be determined in the Rietveld analysis) are involved in hydrogen bonds of various strengths.

AB - Ion exchange of the sodium hydro sodalites [Na3(H2O)4]2-[Al3Si 3O12]2, [Na4(H3O2)]2[Al3Si 3O12]2 and [Na4(OH)]2[Al3Si3O 12]2 with aqueous Pb(NO3)2 solutions yielded, whichever reactant sodalite phase was used, the same lead hydro sodalite, [Pb2(OH)-(H2O)3]2[Al 3Si3O12]2. Thus, in the case of the non-basic reactant [Na3(H2O)4]2-[Al3Si 3O12]2 an overexchange occurs with respect to the number of nonframework cationic charges. Rietveld structure refinement of the lead hydro sodalite based on powder X-ray diffraction data (cubic, a = 9.070 Å, room temperature, space group P43n) revealed that the two lead cations within each polyhedral sodalite cage form an orientationally disordered dinuclear [Pb2(μ-OH)(μ-H2O)(H2O)2] 3+ complex. Due to additional lead framework oxygen bonds the coordination environment of each metal cation (CN 3+3) is approximately spherical, and clearly the lead 6s electron lone pair is stereochemically inactive. This is also suggested by the absence of a small peak at 13.025 keV, attributed in other Pb2+-O compounds to an electronic 2p-6s transition, in the PbL3 edge XANES spectrum. 1H MAS NMR and FTIR spectra show that the hydrogen atoms of the aqua hydroxo complex (which could not be determined in the Rietveld analysis) are involved in hydrogen bonds of various strengths.

KW - Host - Guest chemistry

KW - Ion exchange

KW - Lead

KW - Sodalites

KW - Structure elucidation

UR - http://www.scopus.com/inward/record.url?scp=0033979003&partnerID=8YFLogxK

M3 - Article

C2 - 11931109

AN - SCOPUS:0033979003

VL - 6

SP - 292

EP - 297

JO - Chemistry - a European journal

JF - Chemistry - a European journal

SN - 0947-6539

IS - 2

ER -

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