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The determination of 17 O NMR parameters of hydroxyl oxygen: A combined deuteration and DOR approach
Author(s) -
Wong Alan,
Hung Ivan,
Howes Andy P.,
Anupõld Tiit,
Past Jaan,
Samoson Ago,
Brown Steven P.,
Smith Mark E.,
Dupree Ray
Publication year - 2007
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.2088
Subject(s) - chemistry , oxygen , laser linewidth , oxygen 17 , chemical shift , spinning , dipole , molecule , analytical chemistry (journal) , nuclear magnetic resonance , organic chemistry , polymer chemistry , laser , physics , optics
The direct detection of hydroxyl oxygen (OH) by 17 O double‐rotation (DOR) NMR is very challenging because of the strong OH 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 [ 17 O, 2 H]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.