Frequency-selective homonuclear dipolar recoupling in solid state NMR

Abstract

We introduce a new approach to frequency-selective homonuclear dipolar recoupling in solid state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). This approach, to which we give the acronym SEASHORE, employs alternating periods of double-quantum recoupling and chemical shift evolution to produce phase modulations of the recoupled dipole-dipole interactions that average out undesired couplings, leaving only dipole-dipole couplings between nuclear spins with a selected pair of NMR frequencies. In principle, SEASHORE is applicable to systems with arbitrary coupling strengths and arbitrary sets of NMR frequencies. Arbitrary MAS frequencies are also possible, subject only to restrictions imposed by the pulse sequence chosen for double-quantum recoupling. We demonstrate the efficacy of SEASHORE in experimental ${}^{13}\mathrm{C}$ NMR measurements of frequency-selective polarization transfer in uniformly ${}^{15}\mathrm{N}$ , ${}^{13}\mathrm{C}$ -labeled L-valine powder and frequency-selective intermolecular polarization transfer in amyloid fibrils formed by a synthetic decapeptide containing uniformly ${}^{15}\mathrm{N}$ , ${}^{13}\mathrm{C}$ -labeled residues.