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Efficient symmetry-based γ-encoded DQ recoupling sequences for suppression of t1-noise in solid-state NMR spectroscopy at fast MAS

Highlights

  • Efficient DQ recoupling sequences at fast MAS is proposed.
  • γ-encoded RNnν sequences have high DQ recoupling efficiency.
  • The effect of MAS fluctuations on t1-noise is discussed in detail.
  • t1-noise in DQ/SQ experiment is reduced by γ-encoded RNnν sequences.

Abstract

Solid-state NMR spectroscopy has played a significant role in elucidating the structure and dynamics of materials and biological solids at a molecular level for decades. In particular, the 1H double-quantum/single-quantum (DQ/SQ) chemical shift correlation experiment is widely used for probing the proximity of protons, rendering it a powerful tool for elucidating the hydrogen-bonding interactions and molecular packing of various complex molecular systems. Two factors, namely, the DQ filtering efficiency and t1-noise, dictate the quality of the 2D 1H DQ/SQ spectra. Experimentally different recoupling sequences show varied DQ filtering efficiencies and t1-noise. Herein, after a systematic search of symmetry-based DQ recoupling sequences, we report that the symmetry-based γ-encoded RNnν sequences show superior performance to other DQ recoupling sequences, which not only have a higher DQ recoupling efficiency but can also significantly reduce t1-noise. The origin of t1-noise is further discussed in detail via extensive numerical simulations. We envisage that such γ-encoded RNnν sequences are superior candidates for DQ recoupling in proton-based solid-state NMR spectroscopy due to its capability of efficiently exciting DQ coherences and suppressing t1-noise.

Here is the link for the Article: https://doi.org/10.1016/j.ssnmr.2021.101734

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