Research Article

The determination of 17O NMR parameters of hydroxyl oxygen: A combined deuteration and DOR approach

  1. Alan Wong1,
  2. Ivan Hung1,
  3. Andy P. Howes1,
  4. Tiit Anupõld2,
  5. Jaan Past2,
  6. Ago Samoson2,
  7. Steven P. Brown1,
  8. Mark E. Smith1,
  9. Ray Dupree1,*

Article first published online: 21 DEC 2007

DOI: 10.1002/mrc.2088

Issue

Magnetic Resonance in Chemistry

Magnetic Resonance in Chemistry

Special Issue: New techniques in solid-state NMR

Volume 45, Issue S1, pages S68–S72, December 2007

Additional Information

How to Cite

Wong, A., Hung, I., Howes, A. P., Anupõld, T., Past, J., Samoson, A., Brown, S. P., Smith, M. E. and Dupree, R. (2007), The determination of 17O NMR parameters of hydroxyl oxygen: A combined deuteration and DOR approach. Magn. Reson. Chem., 45: S68–S72. doi: 10.1002/mrc.2088

Author Information

  1. 1

    Physics Department, University of Warwick, Coventry, CV4 7AL, UK

  2. 2

    National Institute for Chemical Physics and Biophysics, Akadeemia Tee 23, Tallinn, Estonia

*Physics Department, University of Warwick, Coventry, CV4 7AL, UK.

Publication History

  1. Issue published online: 21 DEC 2007
  2. Article first published online: 21 DEC 2007
  3. Manuscript Accepted: 20 AUG 2007
  4. Manuscript Revised: 17 AUG 2007
  5. Manuscript Received: 12 JUL 2007

Funded by

  • BBSRC. Grant Number: BB/C000471/1

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Keywords:

  • NMR;
  • 17O;
  • double rotation;
  • NMR parameters;
  • deuteration;
  • hydroxyl oxygen;
  • glycine

Abstract

The direct detection of hydroxyl oxygen (O[BOND]H) by 17O double-rotation (DOR) NMR is very challenging because of the strong O[BOND]H dipole interaction. It is shown that deuteration of the hydroxyl site overcomes this using glycine·HCl as an illustration. Two well-separated sets of narrow (linewidth ∼80–100 Hz) resonances with their spinning-sidebands are observed for the carboxyl and hydroxyl oxygens in the DOR spectrum of [17O,2H]glycine·HCl. The chemical shift anisotropy of these sites is obtained from a simulation of the DOR spinning-sideband intensities. The chemical shift span (Ω) for the carboxyl oxygen is found to be much larger than that of the hydroxyl oxygen, with Ω values of 540 ± 15 and 210 ± 10 ppm, respectively. Copyright © 2007 John Wiley & Sons, Ltd.

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