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Related Concept Videos

Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)01:20

Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)

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.
The central atom need not be NMR-active because its electrons are affected by the electron polarization of the spin-active atoms. However, spin information is transmitted less effectively than in one-bond coupling, and 2J values are usually weaker than 1J values. The energy of...
Spin–Spin Coupling: Three-Bond Coupling (Vicinal Coupling)01:22

Spin–Spin Coupling: Three-Bond Coupling (Vicinal Coupling)

Vicinal or three-bond coupling is commonly observed between protons attached to adjacent carbons. Here, nuclear spin information is primarily transferred via electron spin interactions between adjacent C‑H bond orbitals. This generally favors the antiparallel arrangement of spins, so 3J values are usually positive.
The extent of coupling depends on the C‑C bond length, the two H‑C‑C angles, any electron-withdrawing substituents, and the dihedral angle between the involved orbitals. The...
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
Spin–Spin Coupling: One-Bond Coupling01:17

Spin–Spin Coupling: One-Bond Coupling

Coupling interactions are strongest between NMR-active nuclei bonded to each other, where spin information can be transmitted directly through the pair of bonding electrons. While nuclei polarize their electrons to the opposite spins, the bonding electron pair has opposite spins. Configurations with antiparallel nuclear spins are expected to be lower in energy. When coupling makes antiparallel states more favorable, J is considered to have a positive value. The one-bond coupling constant, 1J,...
Spin–Spin Coupling Constant: Overview01:08

Spin–Spin Coupling Constant: Overview

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.
Qualitatively, any spin plus-half nucleus polarizes the spins of its electrons to the minus-half state. Consequently, the paired electron in the hydrogen–carbon bond must have a...
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

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 in...

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Related Experiment Video

Updated: May 23, 2026

Spin Saturation Transfer Difference NMR (SSTD NMR): A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes
11:44

Spin Saturation Transfer Difference NMR (SSTD NMR): A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes

Published on: November 12, 2016

Compensated second-order recoupling: application to third spin assisted recoupling.

Mathilde Giffard1, Sabine Hediger, Józef R Lewandowski

  • 1Laboratoire de Chimie Inorganique et Biologique, UMR-E3 (CEA/UJF) and CNRS, CEA/DSM/INAC-38054, Grenoble, France.

Physical Chemistry Chemical Physics : PCCP
|April 20, 2012
PubMed
Summary
This summary is machine-generated.

Phase shifts enhance solid-state NMR recoupling techniques like Third Spin Assisted Recoupling (TSAR), improving long-distance polarization transfer in biomolecules. These modified methods offer greater robustness and broader applicability in complex biological systems.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Advanced pulse sequence development.
  • Biomolecular structure and dynamics analysis.

Background:

  • Second-order recoupling techniques are crucial for detecting interactions in solid-state NMR.
  • Third Spin Assisted Recoupling (TSAR) is a key method for polarization transfer but can be sensitive to experimental parameters.
  • Detecting long-range interactions in biomolecules is essential for understanding their function.

Purpose of the Study:

  • To investigate the effect of phase shifts on second-order recoupling techniques in solid-state NMR.
  • To develop and demonstrate improved methods for detecting long-distance polarization transfer in biomolecular systems.
  • To enhance the robustness and applicability of TSAR-based recoupling mechanisms.

Main Methods:

  • Modification of existing recoupling pulse sequences (PAR, PAIN-CP) to incorporate phase shifts, creating AH-PS-PAR and ABH-PS-PAIN-CP.
  • Application of Average Hamiltonian Theory to analyze the impact of phase inversion on polarization transfer and matching conditions.
  • Experimental validation using a uniformly labeled 19.6 kDa protein (YajG) at high magnetic fields (900 MHz) and fast magic angle spinning (65 kHz).

Main Results:

  • Phase-shifted recoupling techniques, particularly PS-TSAR, significantly improve polarization transfer efficiency.
  • Phase inversion effectively compensates for off-resonance effects, broadening the experimental matching conditions.
  • The developed methods demonstrate enhanced robustness compared to standard TSAR, reducing sensitivity to precise radiofrequency settings.
  • Successful detection of long-distance transfer was achieved in a large protein sample.

Conclusions:

  • Phase-shifted recoupling strategies offer substantial improvements for detecting long-distance interactions in solid-state NMR of biomolecules.
  • The enhanced robustness and broader applicability of these modified techniques make them valuable tools for studying complex biological systems.
  • These advancements facilitate more reliable and sensitive NMR investigations of protein structure and dynamics.