Research output: Contribution to Journal/Magazine › Journal article › peer-review
Research output: Contribution to Journal/Magazine › Journal article › peer-review
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TY - JOUR
T1 - The determination of O-17 NMR parameters of hydroxyl oxygen : a combined deuteration and DOR approach
AU - Wong, Alan
AU - Hung, Ivan
AU - Howes, Andy P.
AU - Anupõld, Tiit
AU - Past, Jaan
AU - Samoson, Ago
AU - Brown, Steven P.
AU - Smith, Mark E.
AU - Dupree, Ray
PY - 2007/12/1
Y1 - 2007/12/1
N2 - The direct detection of hydroxyl oxygen (O-H) by O-17 double-rotation (DOR) NMR is very challenging because of the strong O-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 similar to 80-100 Hz) resonances with their spinning-sidebands are observed for the carboxyl and hydroxyl oxygens in the DOR spectrum of [O-17,H-2]glycine center dot HCl. The chemical shift anisotropy of these sites is obtained from a simulation of the DOR spinning-sideband intensities. The chemical shift span (Omega) for the carboxyl oxygen is found to be much larger than that of the hydroxyl oxygen, with Omega values of 540 +/- 15 and 210 +/- 10 ppm, respectively.
AB - The direct detection of hydroxyl oxygen (O-H) by O-17 double-rotation (DOR) NMR is very challenging because of the strong O-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 similar to 80-100 Hz) resonances with their spinning-sidebands are observed for the carboxyl and hydroxyl oxygens in the DOR spectrum of [O-17,H-2]glycine center dot HCl. The chemical shift anisotropy of these sites is obtained from a simulation of the DOR spinning-sideband intensities. The chemical shift span (Omega) for the carboxyl oxygen is found to be much larger than that of the hydroxyl oxygen, with Omega values of 540 +/- 15 and 210 +/- 10 ppm, respectively.
KW - NMR, O-17, double rotation, NMR parameters, deuteration, hydroxyl oxygen, glycine
U2 - 10.1002/mrc.2088
DO - 10.1002/mrc.2088
M3 - Journal article
VL - 45
SP - S68-S72
JO - Magnetic Resonance in Chemistry
JF - Magnetic Resonance in Chemistry
SN - 1097-458X
IS - Supplement 1
ER -