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Related Concept Videos

Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
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Two NMR-active nuclei bonded to a central atom can be involved in geminal or two-bond coupling. Geminal coupling is commonly seen between diastereotopic protons in chiral molecules and unsymmetrical alkenes, among others.
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The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved...
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Spin–Spin Coupling Constant: Overview01:08

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In bromoethane, the three methyl protons are coupled to the two methylene protons that are three bonds away. In accordance with the n+1 rule, the signal from the methyl protons is split into three peaks with 1:2:1 relative intensities. The methylene protons appear as a quartet, with the relative intensities of 1:3:3:1.
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Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

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Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
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Updated: Nov 19, 2025

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Recent progress in dipolar recoupling techniques under fast MAS in solid-state NMR spectroscopy.

Yi Ji1, Lixin Liang1, Xinhe Bao2

  • 1State Key Laboratory of Catalysis, National Laboratory for Clean Energy, 2011-Collaborative Innovation Center of Chemistry for Energy Materials, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Zhongshan Road 457, Dalian, 116023, China; University of Chinese Academy of Sciences, Beijing, 100049, China.

Solid State Nuclear Magnetic Resonance
|January 28, 2021
PubMed
Summary
This summary is machine-generated.

Fast magic-angle spinning (MAS) enables high-resolution solid-state NMR. This review covers dipolar recoupling techniques crucial for structural and dynamic analysis, especially under ultrafast MAS conditions.

Keywords:
Dipolar coupling constantDipolar recouplingDipole-dipole interactionFast and ultrafast MASMagic-angle spinningSymmetry sequence

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Advanced materials characterization.
  • Molecular structure and dynamics determination.

Background:

  • Recent advances in NMR hardware allow magic-angle spinning (MAS) rates exceeding 100 kHz.
  • Fast MAS conditions significantly improve spectral resolution by suppressing anisotropic interactions.
  • This facilitates proton-detected NMR experiments in solid samples.

Purpose of the Study:

  • To review dipolar recoupling techniques optimized for fast-to-ultrafast MAS conditions.
  • To highlight techniques developed in the past two decades.
  • To emphasize their importance in modern solid-state NMR.

Main Methods:

  • Focus on the ratio of radiofrequency (RF) field strength to MAS frequency (ν1/νr) in pulse sequences.
  • Systematic comparison of heteronuclear and homonuclear dipolar recoupling schemes.
  • Highlighting schemes specifically designed for proton-detected NMR under ultrafast MAS.

Main Results:

  • Dipolar recoupling techniques are essential for molecular structure and dynamics determination under fast MAS.
  • The ν1/νr ratio is a critical parameter for assessing technique suitability for fast MAS.
  • Newer techniques are tailored for enhanced performance at ultrafast MAS rates.

Conclusions:

  • Fast MAS, coupled with effective dipolar recoupling, significantly advances solid-state NMR capabilities.
  • These techniques are vital for multi-dimensional correlation NMR experiments.
  • Specialized methods are emerging for proton-detected NMR under the most demanding MAS conditions.