Symmetry-based recoupling of 17O– 1H spin pairs in magic-angle spinning NMR

We have performed magic-angle-spinning solid-state NMR experiments in which protons are recoupled to oxygen-17 nuclei by applying a symmetry-based recoupling sequence at the proton Larmor frequency. Two-dimensional quadrupole-dipole correlation spectra are produced, in which the second-order quadrup...

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Bibliographic Details
Published in:Journal of magnetic resonance (1997) 2006-03, Vol.179 (1), p.38-48
Main Authors: van Beek, Jacco D., Dupree, Ray, Levitt, Malcolm H.
Format: Article
Language:English
Subjects:
Brucite
Correlation spectroscopy
MAS
Oxygen-17
Quadrupolar nuclei
Solid-state NMR
Symmetry-based recoupling
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Summary:We have performed magic-angle-spinning solid-state NMR experiments in which protons are recoupled to oxygen-17 nuclei by applying a symmetry-based recoupling sequence at the proton Larmor frequency. Two-dimensional quadrupole-dipole correlation spectra are produced, in which the second-order quadrupolar shift of the oxygen-17 central transition is correlated with the recoupled heteronuclear dipole–dipole interaction. These spectra are sensitive to the relative orientation of the electric field gradient at the site of the oxygen-17 nucleus and the O–H internuclear vector. We also demonstrate experiments in which polarization is transferred from protons to oxygen-17, and show that oxygen-17 signals may be selected according to the protonation state of the oxygen site. We discuss the small observed value of the heteronuclear dipolar splitting in the central-transition oxygen-17 spectra.
ISSN:1090-7807
1096-0856
DOI:10.1016/j.jmr.2005.11.003