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Related Concept Videos

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...
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...
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...
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...
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,...

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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
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Heteronuclear dipolar recoupling in multiple-spin system under fast magic-angle spinning.

Fang-Chieh Chou1, Shing-Jong Huang, Jerry C C Chan

  • 1Department of Chemistry, National Taiwan University, No. 1, Section 4, Roosevelt Road, Taipei, Taiwan.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|December 23, 2008
PubMed
Summary

We modified the C-REDOR sequence using rotary-REDOR to achieve heteronuclear recoupling in complex spin systems. This technique offers advantages for biological research due to its robustness against radiofrequency inhomogeneity.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Physical Chemistry
  • Biophysics

Background:

  • Cross-relaxation Recoupling (C-REDOR) is a technique used in solid-state NMR.
  • Radiofrequency (rf) inhomogeneity can limit the effectiveness of NMR experiments.
  • Heteronuclear recoupling is crucial for determining distances in biomolecules.

Purpose of the Study:

  • To adapt the C-REDOR sequence within the rotary-REDOR framework for enhanced heteronuclear recoupling.
  • To leverage the inherent robustness of C-REDOR against rf inhomogeneity.
  • To enable applications in biological research requiring precise structural information.

Main Methods:

  • Modification of the C-REDOR pulse sequence based on rotary-REDOR principles.
  • Implementation of active rotor synchronization for windowless C-REDOR by shortening pulse elements.
  • Validation through numerical simulations and experimental measurements on [U-(13)C,(15)N]-L-alanine.

Main Results:

  • Successful realization of heteronuclear recoupling in multiple-spin systems using the modified C-REDOR sequence.
  • Demonstration of improved performance under conditions of rf inhomogeneity.
  • Validation of the method's efficacy through both computational modeling and experimental data.

Conclusions:

  • The modified C-REDOR sequence, integrated with rotary-REDOR, effectively achieves heteronuclear recoupling in complex spin systems.
  • This approach is expected to be valuable in biological NMR studies due to its resilience to rf inhomogeneity.
  • The developed technique provides a robust tool for structural analysis of biomolecules.