4.3 Article

Recent progress in dipolar recoupling techniques under fast MAS in solid-state NMR spectroscopy

Journal

SOLID STATE NUCLEAR MAGNETIC RESONANCE
Volume 112, Issue -, Pages -

Publisher

ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.ssnmr.2020.101711

Keywords

Dipolar recoupling; Magic-angle spinning; Dipole-dipole interaction; Symmetry sequence; Fast and ultrafast MAS; Dipolar coupling constant

Funding

  1. National Natural Science Foundation of China [21773230, 91945302]
  2. LiaoNing Revitalization Talents Program [XLYC1807207, DICPQIBEBT UN201808]

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With recent advancements in NMR hardware technology, fast MAS conditions have enabled efficient dipolar recoupling techniques for molecular structure and dynamics determination. The ratio of RF field strength to MAS frequency in different pulse sequences is crucial for determining the suitability of dipolar recoupling techniques under fast MAS conditions. Specially developed schemes for proton-detection NMR experiments under ultrafast MAS conditions have been highlighted as well.
With the recent advances in NMR hardware and probe design technology, magic-angle spinning (MAS) rates over 100 kHz are accessible now, even on commercial solid NMR probes. Under such fast MAS conditions, excellent spectral resolution has been achieved by efficient suppression of anisotropic interactions, which also opens an avenue to the proton-detected NMR experiments in solids. Numerous methods have been developed to take full advantage of fast MAS during the last decades. Among them, dipolar recoupling techniques under fast MAS play vital roles in the determination of the molecular structure and dynamics, and are also key elements in multidimensional correlation NMR experiments. Herein, we review the dipolar recoupling techniques, especially those developed in the past two decades for fast-to-ultrafast MAS conditions. A major focus for our discussion is the ratio of RF field strength (in frequency) to MAS frequency, nu(1)/nu(r), in different pulse sequences, which determines whether these dipolar recoupling techniques are suitable for NMR experiments under fast MAS conditions. Systematic comparisons are made among both heteronuclear and homonuclear dipolar recoupling schemes. In addition, the schemes developed specially for proton-detection NMR experiments under ultrafast MAS conditions are highlighted as well.

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