Measurement of 13C-1H dipolar couplings in solids by using ultra-fast magic-angle spinning NMR spectroscopy with symmetry-based sequences
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Updated: Jun 4, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Qiang Wang1, Xingyu Lu, Olivier Lafon
1Unit of Catalysis and Chemistry of Solids, CNRS-8181, Lille North of France University, Villeneuve d'Ascq cedex, Lille, France.
Abstract:
We show that (13)C-(1)H dipolar couplings in fully protonated organic solids can be measured by applying a Symmetry-based Resonance-Echo DOuble-Resonance (S-REDOR) experiment at ultra-fast Magic-Angle Spinning (MAS). The (13)C-(1)H dipolar couplings are recovered by using the R12 recoupling scheme, while the interference of (1)H-(1)H dipolar couplings are suppressed by the symmetry properties of this sequence and the use of high MAS frequency (65 kHz). The R12 method is especially advantageous for large (13)C-(1)H dipolar interactions, since the dipolar recoupling time can be incremented by steps as short as one rotor period. This allows a fine sampling for the rising part of the dipolar dephasing curve. We demonstrate experimentally that one-bond (13)C-(1)H dipolar coupling in the order of 22 kHz can be accurately determined. Furthermore, the proposed method allows a rapid evaluation of the dipolar coupling by fitting the S-REDOR dipolar dephasing curve with an analytical expression.
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