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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
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
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), 38-48. (doi:10.1016/j.jmr.2005.11.003).

Record type: Article

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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More information

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
ORCID for Malcolm H. Levitt: ORCID iD orcid.org/0000-0001-9878-1180

Catalogue record

Date deposited: 07 Mar 2007
Last modified: 26 Nov 2019 01:52

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