@article {338, title = {High-resolution NMR of anisotropic samples with spinning away from the magic angle}, journal = {Chemical Physics Letters}, volume = {377}, year = {2003}, note = {Chem Phys Lett714CRTimes Cited:6Cited References Count:27}, month = {Aug 15}, pages = {333-339}, abstract = {
High-resolution NMR of anisotropic samples is typically performed by spinning the sample around an axis at the magic angle of 54.7degrees with the static magnetic field. Geometric and engineering constraints often prevent spinning at this specific angle. Implementations of magic angle field rotation are extremely demanding due to power requirements or an inaccessible geometry. We present a methodology for taking the magic out of MAS while still obtaining both isotropic and anisotropic spectral information during sample spinning or field rotation at arbitrary angles. Using projected-MAS, we obtained resolved scaled isotropic chemical shifts in inhomogeneously broadened spinning samples. Published by Elsevier B.V.
}, keywords = {axis}, isbn = {0009-2614}, doi = {Doi 10.1016/S0009-2614(03)01149-7}, url = {We describe here a new solid-state nuclear-magnetic-resonance (NMR) experiment for correlating anisotropic and isotropic chemical shifts of inequivalent nuclei in powdered samples. Spectra are obtained by processing signals arising from a spinning sample, acquired in independent experiments as a function of the angle between the axis of macroscopic rotation and the external magnetic field. This is in contrast to previously proposed techniques, which were based on sudden mechanical flippings or multiple-pulse sequences. We show that the time evolution of variable-angle-spinning signals is determined by a distribution relating the isotropic frequencies of the spins with their corresponding chemical shift anisotropies. Fourier transformation of these data therefore affords a two-dimensional NMR spectrum, in which line shapes of isotropic and anisotropic interactions are correlated. Theoretical and experimental considerations involved in the extraction of this spectral information are discussed, and the technique is illustrated by an analysis of C-13 NMR anisotropy in glycine, cysteine, and p-anisic acid.
}, keywords = {axis}, isbn = {0021-9606}, doi = {Doi 10.1063/1.463860}, url = {