Two-dimensional one-pulse rotational echo spectra.

Recently a two-dimensional representation of one-dimensional spinning sideband magic-angle spinning (MAS) spectra has been published with applications to deuteron MAS nuclear magnetic resonance (NMR). The introduction of a new time axis, based on the rotor period, allows the separation of isotropic and anisotropic chemical shifts. It is shown here that, in addition to untangling spinning sideband spectra, data-processing steps can be incorporated which enabled applications of the method to signals from nuclei with anisotropies smaller than those of the quadrupole coupling of deuterons. This is achieved by linear prediction of the rotary echo signals. Advantages and limitations of the algorithm are discussed and demonstrated with experimental results of 13C cross-polarization (CP) MAS spectra of glycine.