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Transient effects in π-pulse sequences in MAS solid-state NMR.

Johannes Hellwagner1, Nino Wili1, Luis Fábregas Ibáñez1

  • 1Physical Chemistry, ETH Zurich, Vladimir-Prelog-Weg 2, 8093 Zurich, Switzerland.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|January 1, 2018
PubMed
Summary
This summary is machine-generated.

Pulse-transient compensation can double recoupling efficiency in solid-state NMR. This technique improves Radio-Frequency Driven Recoupling (RFDR) and explains Rotational Echo Double Resonance (REDOR) performance in biological structure analysis.

Keywords:
Floquet theoryPhase transientsPolarization transferRecoupling sequences under MASSolid-state NMR

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Biophysical chemistry
  • Structural biology

Background:

  • Dipolar recoupling techniques are crucial for determining biological molecule structures using solid-state NMR.
  • Common sequences like RFDR and REDOR offer simplicity and stability but can be affected by radio-frequency inhomogeneity.
  • A theoretical framework is needed to understand and optimize these recoupling sequences.

Purpose of the Study:

  • To develop a theoretical understanding of dipolar recoupling sequences using a Floquet treatment.
  • To investigate the impact of pulse transients and effective fields on recoupling efficiency.
  • To demonstrate the benefits of pulse-transient compensation for enhancing NMR signal.

Main Methods:

  • Application of a Floquet treatment incorporating chemical-shift offset dependence.
  • Analysis of homonuclear recoupling (RFDR) and heteronuclear recoupling (REDOR) sequences.
  • Experimental validation of theoretical predictions using model compounds and peptides.

Main Results:

  • The Floquet approach elucidates the influence of effective fields arising from pulse transients.
  • Pulse-transient compensation was experimentally shown to potentially double homonuclear recoupling efficiency.
  • Phase cycle optimization was explored to minimize effective fields, explaining REDOR's robustness.

Conclusions:

  • Pulse-transient compensation is a viable strategy to significantly enhance recoupling efficiency in solid-state NMR.
  • The theoretical framework provides insights into optimizing RFDR and understanding REDOR performance.
  • These findings contribute to more accurate structural determination of biological molecules.