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Homonuclear dipolar recoupling under ultra-fast magic-angle spinning: probing 19F-19F proximities by solid-state NMR
Qiang Wang1, Bingwen Hu, Olivier Lafon
1UCCS, CNRS-8181, Lille-University, 59652, Villeneuve d'Ascq, France; State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Center for Magnetic Resonance, WIPM, Chinese Academy of Sciences, Wuhan 430071, China; Graduate School of the Chinese Academy of Sciences, Beijing, China.
Abstract:
We describe dipolar recoupling methods that accomplish, at high magic-angle spinning (MAS) frequencies, the excitation of double-quantum (DQ) coherences between spin-1/2 nuclei. We employ rotor-synchronized symmetry-based pulse sequences which are either gamma-encoded or non-gamma-encoded. The sensitivity and the robustness to both chemical-shift anisotropy and offset are examined. We also compare different techniques to avoid signal folding in the indirect dimension of two-dimensional double-quantum<-->single-quantum (DQ-SQ) spectra. This comprehensive analysis results in the identification of satisfactory conditions for dipolar (19)F-(19)F recoupling at high magnetic fields and high MAS frequencies. The utility of these recoupling methods is demonstrated with high-resolution DQ-SQ NMR spectra, which allow probing (19)F-(19)F proximities in powered fluoroaluminates.
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