Symmetry-based recoupling of (17)O-(1)H spin pairs in magic-angle spinning NMR
Symmetry-based recoupling of (17)O-(1)H spin pairs in magic-angle spinning NMR
We have performed magic-angle-spinning solid-state NM R 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.
solid-state nmr, quadrupolar nuclei, oxygen-17, correlation
spectroscopy, symmetry-based recoupling, mas, brucite
solid-state nmr, integer quadrupolar nuclei, double-resonance nmr, magnetic-resonance, neutron-diffraction, dipolar interactions, signal enhancement, rotational-echo, amino-acids, spectroscopy
38-48
van Beek, Jaco D.
b9ee7f99-ab94-4580-8920-26cce3c7fc36
Dupree, Ray
e105fcf4-75db-4379-b227-afc4baadaf31
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
2006
van Beek, Jaco D.
b9ee7f99-ab94-4580-8920-26cce3c7fc36
Dupree, Ray
e105fcf4-75db-4379-b227-afc4baadaf31
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
van Beek, Jaco D., Dupree, Ray and Levitt, Malcolm H.
(2006)
Symmetry-based recoupling of (17)O-(1)H spin pairs in magic-angle spinning NMR.
Journal of Magnetic Resonance, 179 (1), .
(doi:10.1016/j.jmr.2005.11.003).
Abstract
We have performed magic-angle-spinning solid-state NM R 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.
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Published date: 2006
Keywords:
solid-state nmr, quadrupolar nuclei, oxygen-17, correlation
spectroscopy, symmetry-based recoupling, mas, brucite
solid-state nmr, integer quadrupolar nuclei, double-resonance nmr, magnetic-resonance, neutron-diffraction, dipolar interactions, signal enhancement, rotational-echo, amino-acids, spectroscopy
Identifiers
Local EPrints ID: 44560
URI: http://eprints.soton.ac.uk/id/eprint/44560
PURE UUID: 3a477839-061a-4fda-ba5e-b93be7f1c9cb
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Date deposited: 07 Mar 2007
Last modified: 16 Mar 2024 03:18
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Author:
Jaco D. van Beek
Author:
Ray Dupree
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