Two-dimensional chemical shift/heteronuclear dipolar coupling spectra obtained with polarization inversion spin exchange at the magic angle and magic-angle sample spinning (PISEMAMAS).

High-resolution two-dimensional 15N chemical shift/1H-15N dipolar coupling polarization inversion spin exchange at the magic angle (PISEMA) spectra of a polycrystalline sample of 15N-acetylvaline were obtained with and without magic-angle sample spinning. These spectra demonstrate the advantages of the PISEMA experiment over conventional approaches to separated local-field spectroscopy, especially the high resolution in the dipolar dimension where the spinning sidebands have uniformly narrow linewidths.