Distance measurements to quadrupolar nuclei: Evolution of the rotational echo double resonance technique

Amir Goldbourt*

*Corresponding author for this work

Research output: Contribution to journalReview articlepeer-review

Abstract

Molecular structure determination is the basis for understanding chemical processes and the property of materials. The direct dependence of the magnetic dipolar interaction on the distance makes solid-state nuclear magnetic resonance (NMR) an excellent tool to study molecular structure when X-ray crystallography fails to provide atomic-resolution data. Although techniques to measure distances between pairs of isolated nuclear spin-1/2 pairs are routine and easy to implement using the rotational echo double resonance (REDOR) experiment (Gullion & Schaefer, 1989), the existence of a nucleus with a spin > 1/2, appearing in approximately 75% of the elements in the periodic table, poses a challenge due to difficulties stemming from the large nuclear quadrupolar coupling constant (QCC). This mini-review presents the existing solid-state magic-angle spinning NMR techniques aimed toward the efficient and accurate determination of internuclear distances between a spin-1/2 and a “quadrupolar” nucleus having a spin larger than one half. Analytical expressions are provided for the various recoupling curves stemming from different techniques, and a coherent nomenclature for these various techniques is suggested. Treatment of some special cases such as multiple spin effects and spins with close Larmor frequencies is also discussed. The most advanced methods can recouple spins with quadrupolar frequencies up to tens of megahertz and beyond, expanding the distance measurement capabilities of solid-state NMR to an increasingly growing number of applications and nuclear spin systems.

Original languageEnglish
Pages (from-to)908-919
Number of pages12
JournalMagnetic Resonance in Chemistry
Volume59
Issue number9-10
DOIs
StatePublished - 1 Sep 2021

Funding

FundersFunder number
United States-Israel Binational Science Foundation2016169

    Keywords

    • REDOR
    • RESPDOR
    • magic-angle spinning
    • quadrupolar nuclei
    • solid-state NMR

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