NMR Characterization and Rietveld Refinement of the Structure of Rehydrated AlPO4-34
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2000
Authors
Tuel, AlainCaldarelli, Stefano
Meden, Anton
McCusker, Lynne B.
Baerlocher, Christian Baerlocher
Ristic, Alenka
Rajić, Nevenka

Mali, Gregor

Kaučič, Venčeslav
Article (Published version)

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The triclinic form of AlPO4-34, a microporous aluminophosphate with the chabazite (CHA) topology, adopts a rhombohedral symmetry upon calcination. The framework structure of this phase remains intact under ambient conditions, but it distorts dramatically, though reversibly, in the presence of water. Following these structural changes in situ by X-ray diffraction revealed that there are actually two stable rehydrated phases, which differ from each other by one water molecule in the channel. Both of these phases have triclinic unit cells that are closely related to that of the calcined rhombohedral phase. The structure of the low-temperature (10 °C), fully rehydrated phase (phase B) was elucidated by combining high-resolution synchrotron powder diffraction with solid-state NMR techniques. Coordination of three of the six Al atoms to water molecules causes the deformation of the framework and the reduction of the symmetry. Rietveld refinement of the structure of phase B in the triclinic s...pace group P1 (a = 9.026, b = 9.338, c = 9.508 Å, α = 95.1°, β = 104.1°, and γ = 96.6°) converged with RF = 0.079 and RWP = 0.176 (Rexp = 0.087). Framework connectivities derived from the structure were used to assign 31P NMR lines as well as part of the 27Al NMR signal.
Source:
The Journal of Physical Chemistry B, 2000, 104, 5697-5705Publisher:
- American Chemical Society
Funding / projects:
- Ministry of Science and Technology of the Republic of Slovenia
- Swiss National Science Foundation
Institution/Community
Tehnološko-metalurški fakultetTY - JOUR AU - Tuel, Alain AU - Caldarelli, Stefano AU - Meden, Anton AU - McCusker, Lynne B. AU - Baerlocher, Christian Baerlocher AU - Ristic, Alenka AU - Rajić, Nevenka AU - Mali, Gregor AU - Kaučič, Venčeslav PY - 2000 UR - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/6400 AB - The triclinic form of AlPO4-34, a microporous aluminophosphate with the chabazite (CHA) topology, adopts a rhombohedral symmetry upon calcination. The framework structure of this phase remains intact under ambient conditions, but it distorts dramatically, though reversibly, in the presence of water. Following these structural changes in situ by X-ray diffraction revealed that there are actually two stable rehydrated phases, which differ from each other by one water molecule in the channel. Both of these phases have triclinic unit cells that are closely related to that of the calcined rhombohedral phase. The structure of the low-temperature (10 °C), fully rehydrated phase (phase B) was elucidated by combining high-resolution synchrotron powder diffraction with solid-state NMR techniques. Coordination of three of the six Al atoms to water molecules causes the deformation of the framework and the reduction of the symmetry. Rietveld refinement of the structure of phase B in the triclinic space group P1 (a = 9.026, b = 9.338, c = 9.508 Å, α = 95.1°, β = 104.1°, and γ = 96.6°) converged with RF = 0.079 and RWP = 0.176 (Rexp = 0.087). Framework connectivities derived from the structure were used to assign 31P NMR lines as well as part of the 27Al NMR signal. PB - American Chemical Society T2 - The Journal of Physical Chemistry B T1 - NMR Characterization and Rietveld Refinement of the Structure of Rehydrated AlPO4-34 EP - 5705 SP - 5697 VL - 104 DO - 10.1021/jp000455a ER -
@article{ author = "Tuel, Alain and Caldarelli, Stefano and Meden, Anton and McCusker, Lynne B. and Baerlocher, Christian Baerlocher and Ristic, Alenka and Rajić, Nevenka and Mali, Gregor and Kaučič, Venčeslav", year = "2000", abstract = "The triclinic form of AlPO4-34, a microporous aluminophosphate with the chabazite (CHA) topology, adopts a rhombohedral symmetry upon calcination. The framework structure of this phase remains intact under ambient conditions, but it distorts dramatically, though reversibly, in the presence of water. Following these structural changes in situ by X-ray diffraction revealed that there are actually two stable rehydrated phases, which differ from each other by one water molecule in the channel. Both of these phases have triclinic unit cells that are closely related to that of the calcined rhombohedral phase. The structure of the low-temperature (10 °C), fully rehydrated phase (phase B) was elucidated by combining high-resolution synchrotron powder diffraction with solid-state NMR techniques. Coordination of three of the six Al atoms to water molecules causes the deformation of the framework and the reduction of the symmetry. Rietveld refinement of the structure of phase B in the triclinic space group P1 (a = 9.026, b = 9.338, c = 9.508 Å, α = 95.1°, β = 104.1°, and γ = 96.6°) converged with RF = 0.079 and RWP = 0.176 (Rexp = 0.087). Framework connectivities derived from the structure were used to assign 31P NMR lines as well as part of the 27Al NMR signal.", publisher = "American Chemical Society", journal = "The Journal of Physical Chemistry B", title = "NMR Characterization and Rietveld Refinement of the Structure of Rehydrated AlPO4-34", pages = "5705-5697", volume = "104", doi = "10.1021/jp000455a" }
Tuel, A., Caldarelli, S., Meden, A., McCusker, L. B., Baerlocher, C. B., Ristic, A., Rajić, N., Mali, G.,& Kaučič, V.. (2000). NMR Characterization and Rietveld Refinement of the Structure of Rehydrated AlPO4-34. in The Journal of Physical Chemistry B American Chemical Society., 104, 5697-5705. https://doi.org/10.1021/jp000455a
Tuel A, Caldarelli S, Meden A, McCusker LB, Baerlocher CB, Ristic A, Rajić N, Mali G, Kaučič V. NMR Characterization and Rietveld Refinement of the Structure of Rehydrated AlPO4-34. in The Journal of Physical Chemistry B. 2000;104:5697-5705. doi:10.1021/jp000455a .
Tuel, Alain, Caldarelli, Stefano, Meden, Anton, McCusker, Lynne B., Baerlocher, Christian Baerlocher, Ristic, Alenka, Rajić, Nevenka, Mali, Gregor, Kaučič, Venčeslav, "NMR Characterization and Rietveld Refinement of the Structure of Rehydrated AlPO4-34" in The Journal of Physical Chemistry B, 104 (2000):5697-5705, https://doi.org/10.1021/jp000455a . .