title: 2H chemical shift anisotropies from high-field 2H MAS NMR spectroscopy.
abstract: 2H chemical shift anisotropies (CSAs) have been determined for the first time for polycrystalline samples employing 2H MAS NMR spectroscopy at high magnetic field strength (14.1 T). The 2H CSA is reflected as distinct asymmetries in the manifold of spinning sidebands (ssbs) observed for the two overlapping single-quantum transitions. Least-squares fitting to the manifold of ssbs allows determination of the 2H CSA parameters along with the quadrupole coupling parameters. This is demonstrated for KD2PO4, ND4D2PO4, KDSO4, KDCO3, alpha-(COOD)2, alpha-(COOD)2.2D2O, and boehmite (AlOOD) which exhibit 2H shift anisotropies in the range 13< or =deltasigma< or =27 ppm. For fixed values of the shift anisotropy and the 2H quadrupole coupling it is shown that the precision of the CSA parameters depends strongly on the asymmetry parameter (etaQ) for the quadrupole coupling tensor, giving the highest precision for etaQ approximately 0. The 2H CSA parameters (deltasigma and etasigma) are in good agreement with 1H CSA data reported in the literature for the corresponding protonated samples from 1H NMR spectra employing various homonuclear decoupling techniques. The determination of 2H quadrupole coupling parameters and 2H (1H) CSAs from the same 2H MAS NMR experiment may be particularly useful in studies of hydrogen bonding since the 2H quadrupole coupling constant and the CSA appear to characterize bond lengths in a hydrogen bond in a different manner.
authors.affiliation: Instrument Centre for Solid-State NMR Spectroscopy, Department of Chemistry, University of Aarhus, DK-8000 Aarhus C, Denmark.
authors.forename: Anne
authors.initials: A
authors.lastname: Hauch
authors.forename: Henrik
authors.initials: H
authors.lastname: Bildsøe
authors.forename: Hans J
authors.initials: HJ
authors.lastname: Jakobsen
authors.forename: Jørgen
authors.initials: J
authors.lastname: Skibsted
mesh_terms: D016880:Anisotropy; D006609:High Mobility Group Proteins / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008280:Magnetics; D008903:Minerals / Q000737:chemistry*; D013113:Spin Labels; D029867:Xenopus Proteins / Q000737:chemistry*
chemical_list: C473989:DNA unwinding factor , Xenopus; D006609:High Mobility Group Proteins; D008903:Minerals; D013113:Spin Labels; D029867:Xenopus Proteins