Details
| Original language | English |
|---|---|
| Pages (from-to) | 292-297 |
| Number of pages | 6 |
| Journal | Chemistry - a European journal |
| Volume | 6 |
| Issue number | 2 |
| Publication status | Published - 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.
Keywords
- Host - Guest chemistry, Ion exchange, Lead, Sodalites, Structure elucidation
ASJC Scopus subject areas
- Chemical Engineering(all)
- Catalysis
- Chemistry(all)
- Organic Chemistry
Cite this
- Standard
- Harvard
- Apa
- Vancouver
- BibTeX
- RIS
In: Chemistry - a European journal, Vol. 6, No. 2, 01.2000, p. 292-297.
Research output: Contribution to journal › Article › Research › peer review
}
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 -