Open AccessOff-resonance 13C–2H REDOR NMR for site-resolved studies of molecular motion
Author(s) -
Martin D. Gelenter,
Kelly J. Chen,
Mei Hong
Publication year - 2021
Publication title -
journal of biomolecular nmr
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.346
H-Index - 106
eISSN - 1573-5001
pISSN - 0925-2738
DOI - 10.1007/s10858-021-00377-7
Subject(s) - dephasing , chemistry , resonance (particle physics) , deuterium , molecular physics , nuclear magnetic resonance , sideband , helicity , molecule , magic angle spinning , spectral line , nuclear magnetic resonance spectroscopy , atomic physics , physics , stereochemistry , microwave , organic chemistry , quantum mechanics , particle physics , astronomy
We introduce a 13 C- 2 H Rotational Echo DOuble Resonance (REDOR) technique that uses the difference between on-resonance and off-resonance 2 H irradiation to detect dynamic segments in deuterated molecules. By selectively inverting specific regions of the 2 H magic-angle spinning (MAS) sideband manifold to recouple some of the deuterons to nearby carbons, we distinguish dynamic and rigid residues in 1D and 2D 13 C spectra. We demonstrate this approach on deuterated GB1, H/D exchanged GB1, and perdeuterated bacterial cellulose. Numerical simulations reproduce the measured mixing-time and 2 H carrier-frequency dependence of the REDOR dephasing of bacterial cellulose. Combining numerical simulations with experiments thus allow the extraction of motionally averaged quadrupolar couplings from REDOR dephasing values.