title: The determination of 17O NMR parameters of hydroxyl oxygen: a combined deuteration and DOR approach.
abstract: The direct detection of hydroxyl oxygen (O-H) by (17)O 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 approximately 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 (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.
authors.affiliation: Physics Department, University of Warwick, Coventry, UK.
authors.forename: Alan
authors.initials: A
authors.lastname: Wong
authors.forename: Ivan
authors.initials: I
authors.lastname: Hung
authors.forename: Andy P
authors.initials: AP
authors.lastname: Howes
authors.forename: Tiit
authors.initials: T
authors.lastname: Anupõld
authors.forename: Jaan
authors.initials: J
authors.lastname: Past
authors.forename: Ago
authors.initials: A
authors.lastname: Samoson
authors.forename: Steven P
authors.initials: SP
authors.lastname: Brown
authors.forename: Mark E
authors.initials: ME
authors.lastname: Smith
authors.forename: Ray
authors.initials: R
authors.lastname: Dupree
mesh_terms: D003903:Deuterium; D017665:Hydroxyl Radical / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D010103:Oxygen Isotopes / Q000737:chemistry*
chemical_list: D010103:Oxygen Isotopes; D017665:Hydroxyl Radical; D003903:Deuterium