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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...
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...
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...
Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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...
¹H NMR Signal Multiplicity: Splitting Patterns01:13

¹H NMR Signal Multiplicity: Splitting Patterns

When protons A and X are coupled, their nuclear spin energy levels are slightly modified. This is because the energy required to excite proton A to a spin state parallel to proton X is slightly different from the energy required for it to become anti-parallel to spin X. Consequently, there are two possible excitation frequencies for A (A1 and A2), depending on the spin state of X, and vice versa. The mutual nature of coupling implies that the difference between frequencies A1 and A2, indicated...
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...

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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Measuring dipolar and J coupling between quadrupolar nuclei using double-rotation NMR.

Frédéric A Perras1, David L Bryce

  • 1Department of Chemistry, University of Ottawa, Ottawa K1N 6N5, Canada.

The Journal of Chemical Physics
|May 10, 2013
PubMed
Summary

Double-rotation (DOR) NMR eliminates quadrupolar interactions, preserving crucial J coupling and dipolar coupling information in NMR spectra. This technique enables direct measurement of J coupling constants for quadrupolar nuclei, advancing chemical structure analysis.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Solid-State Chemistry
  • Quantum Chemistry

Background:

  • Spin-spin coupling interactions in NMR provide vital structural information for chemists.
  • Dipolar coupling measures internuclear distances, while J coupling identifies bonding interactions.
  • Quadrupolar interactions in spinning samples reintroduce dipolar interactions, but spectral broadening often obscures J coupling for quadrupolar nuclei.

Purpose of the Study:

  • To demonstrate that double-rotation (DOR) NMR can fully remove quadrupolar interaction effects from NMR spectra.
  • To show that J coupling multiplets remain observable for quadrupolar nuclei using DOR NMR.
  • To enable straightforward measurement of homonuclear J coupling constants between magnetically equivalent quadrupolar nuclei.

Main Methods:

  • Application of double-rotation (DOR) NMR to multiple spin pairs, including quadrupolar nuclei.
  • Analysis of NMR spectra to observe the persistence of J coupling multiplets.
  • Computational decomposition of J coupling constants into molecular orbital contributions.

Main Results:

  • DOR NMR effectively removes quadrupolar interaction effects, preserving dipolar and J couplings.
  • J coupling multiplets are observed for quadrupolar A2 spin pairs, unlike with spin-1/2 nuclei.
  • Homonuclear J coupling constants for quadrupolar nuclei were measured directly.

Conclusions:

  • DOR NMR is a powerful technique for studying J coupling in systems with quadrupolar nuclei.
  • The method facilitates a deeper understanding of J coupling origins and mechanisms in quadrupolar spin pairs.
  • This research advances the structural elucidation capabilities of NMR spectroscopy for complex molecules.