High-pressure δ-Al(OH)3 and δ-AlOOH phases and isostructural hydroxides/oxyhydroxides: New structural insights from high-resolution1H and27Al NMR

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Abstract

In order to shed light on the proton distributions and order/disorder in high-pressure δ-Al(OH)3 and δ-AlOOH phases, two-dimensional, high-resolution 1H CRAMPS (FSLG)-MAS NMR and 27Al 3QMAS NMR spectra have been obtained. For δ-Al(OH) 3, the 1H CRAMPS-MAS NMR revealed two peaks with an intensity ratio close to 2:1. The 27Al MAS and 3QMAS NMR suggest a single Al site with a well-defined local structure. For δ-AlOOH, the 1H and 27Al NMR indicate the presence of a single H and Al site each. These results are consistent with crystal structures refined from X-ray diffraction. For comparison, 1H MAS and CRAMPS-MAS NMR spectra were also obtained for several other hydroxides/oxyhydroxides, including In(OH)3 and InOOH that have similar structures to δ-Al(OH) 3 and δ-AlOOH, respectively. These data not only provide additional insights into the proton distributions in these important crystal structure classes but also together provide a better defined quantitative correlation between 1H chemical shift and hydrogen-bonding O⋯O distance.

Original languageEnglish
Pages (from-to)13156-13166
Number of pages11
JournalJournal of Physical Chemistry B
Volume111
Issue number46
DOIs
Publication statusPublished - Nov 22 2007

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Hydroxides
hydroxides
Nuclear magnetic resonance
nuclear magnetic resonance
Protons
Crystal structure
crystal structure
Order disorder transitions
protons
Chemical shift
chemical equilibrium
aluminum oxide hydroxide
Hydrogen bonds
disorders
X ray diffraction
high resolution
hydrogen
diffraction

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry

Cite this

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title = "High-pressure δ-Al(OH)3 and δ-AlOOH phases and isostructural hydroxides/oxyhydroxides: New structural insights from high-resolution1H and27Al NMR",
abstract = "In order to shed light on the proton distributions and order/disorder in high-pressure δ-Al(OH)3 and δ-AlOOH phases, two-dimensional, high-resolution 1H CRAMPS (FSLG)-MAS NMR and 27Al 3QMAS NMR spectra have been obtained. For δ-Al(OH) 3, the 1H CRAMPS-MAS NMR revealed two peaks with an intensity ratio close to 2:1. The 27Al MAS and 3QMAS NMR suggest a single Al site with a well-defined local structure. For δ-AlOOH, the 1H and 27Al NMR indicate the presence of a single H and Al site each. These results are consistent with crystal structures refined from X-ray diffraction. For comparison, 1H MAS and CRAMPS-MAS NMR spectra were also obtained for several other hydroxides/oxyhydroxides, including In(OH)3 and InOOH that have similar structures to δ-Al(OH) 3 and δ-AlOOH, respectively. These data not only provide additional insights into the proton distributions in these important crystal structure classes but also together provide a better defined quantitative correlation between 1H chemical shift and hydrogen-bonding O⋯O distance.",
author = "Xianyu Xue and Masami Kanzaki",
year = "2007",
month = "11",
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doi = "10.1021/jp073968r",
language = "English",
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T2 - New structural insights from high-resolution1H and27Al NMR

AU - Xue, Xianyu

AU - Kanzaki, Masami

PY - 2007/11/22

Y1 - 2007/11/22

N2 - In order to shed light on the proton distributions and order/disorder in high-pressure δ-Al(OH)3 and δ-AlOOH phases, two-dimensional, high-resolution 1H CRAMPS (FSLG)-MAS NMR and 27Al 3QMAS NMR spectra have been obtained. For δ-Al(OH) 3, the 1H CRAMPS-MAS NMR revealed two peaks with an intensity ratio close to 2:1. The 27Al MAS and 3QMAS NMR suggest a single Al site with a well-defined local structure. For δ-AlOOH, the 1H and 27Al NMR indicate the presence of a single H and Al site each. These results are consistent with crystal structures refined from X-ray diffraction. For comparison, 1H MAS and CRAMPS-MAS NMR spectra were also obtained for several other hydroxides/oxyhydroxides, including In(OH)3 and InOOH that have similar structures to δ-Al(OH) 3 and δ-AlOOH, respectively. These data not only provide additional insights into the proton distributions in these important crystal structure classes but also together provide a better defined quantitative correlation between 1H chemical shift and hydrogen-bonding O⋯O distance.

AB - In order to shed light on the proton distributions and order/disorder in high-pressure δ-Al(OH)3 and δ-AlOOH phases, two-dimensional, high-resolution 1H CRAMPS (FSLG)-MAS NMR and 27Al 3QMAS NMR spectra have been obtained. For δ-Al(OH) 3, the 1H CRAMPS-MAS NMR revealed two peaks with an intensity ratio close to 2:1. The 27Al MAS and 3QMAS NMR suggest a single Al site with a well-defined local structure. For δ-AlOOH, the 1H and 27Al NMR indicate the presence of a single H and Al site each. These results are consistent with crystal structures refined from X-ray diffraction. For comparison, 1H MAS and CRAMPS-MAS NMR spectra were also obtained for several other hydroxides/oxyhydroxides, including In(OH)3 and InOOH that have similar structures to δ-Al(OH) 3 and δ-AlOOH, respectively. These data not only provide additional insights into the proton distributions in these important crystal structure classes but also together provide a better defined quantitative correlation between 1H chemical shift and hydrogen-bonding O⋯O distance.

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