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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Materials science and structural biology.

Background:

  • Rotational-Echo Double-Resonance (REDOR) is crucial for measuring internuclear distances between heteronuclear spins in solid-state NMR.
  • Measuring distances between strongly coupled spins at intermediate magic-angle spinning (MAS) frequencies is difficult due to rapid magnetisation dephasing.
  • Shifted-REDOR (S-REDOR) addresses this by scaling down dipolar coupling.

Purpose of the Study:

  • To introduce and evaluate a novel sine-squared pulse-positioned REDOR variant.
  • To compare its performance against standard REDOR and S-REDOR.
  • To assess its utility for measuring internuclear distances, particularly under challenging conditions.

Main Methods:

  • Theoretical analysis of the REDOR pulse sequences.
  • Numerical simulations to model magnetisation dynamics.
  • Experimental validation using solid-state NMR.

Main Results:

  • The proposed sine-squared REDOR variant exhibits similar scaling properties to S-REDOR.
  • Comparative analysis of dipolar recoupling efficiencies and experimental robustness was performed.
  • The new variant demonstrates advantages in radiofrequency field requirements at high MAS frequencies.

Conclusions:

  • The sine-squared REDOR sequence is a viable alternative to S-REDOR for heteronuclear distance measurements.
  • It offers improved performance and efficiency, especially at faster MAS rates.
  • This advancement enhances the capabilities of solid-state NMR for structural analysis.