Recoupling of Heteronuclear Dipolar Interactions with Rotational-Echo Double-Resonance at High Magic-Angle Spinning Frequencies

Christopher P. Jaroniec, Brett A. Tounge, Chad M. Rienstra, Judith Herzfeld, Robert G. Griffin

Research output: Contribution to journalArticlepeer-review

Abstract

Heteronuclear dipolar recoupling with rotational-echo double-resonance (REDOR) is investigated in the rapid magic-angle spinning regime, where radiofrequency irradiation occupies a significant fraction of the rotor period (10-60%). We demonstrate, in two model 13C-15N spin systems, [1-13C, 15N] and [2-13C, 15N]glycine, that REDOR ΔS/S0 curves acquired at high MAS rates and relatively low recoupling fields are nearly identical to the ΔS/S0 curve expected for REDOR with ideal δ-function pulses. The only noticeable effect of the finite π pulse length on the recoupling is a minor scaling of the dipolar oscillation frequency. Experimental results are explained using both numerical calculations and average Hamiltonian theory, which is used to derive analytical expressions for evolution under REDOR recoupling sequences with different π pulse phasing schemes. For xy-4 and extensions thereof, finite pulses scale only the dipolar oscillation frequency by a well-defined factor. For other phasing schemes (e.g., xx-4 and xx̄-4) both the frequency and amplitude of the oscillation are expected to change.

Original languageEnglish (US)
Pages (from-to)132-139
Number of pages8
JournalJournal of Magnetic Resonance
Volume146
Issue number1
DOIs
StatePublished - Sep 2000
Externally publishedYes

Keywords

  • Finite pulse effects
  • Hetero-nuclear dipolar recoupling
  • Magic-angle spinning
  • Rotational-echo double-resonance
  • Solid-state NMR

ASJC Scopus subject areas

  • Biophysics
  • Biochemistry
  • Nuclear and High Energy Physics
  • Condensed Matter Physics

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