Jove
Visualize
Contact Us
JoVE
x logofacebook logolinkedin logoyoutube logo
ABOUT JoVE
OverviewLeadershipBlogJoVE Help Center
AUTHORS
Publishing ProcessEditorial BoardScope & PoliciesPeer ReviewFAQSubmit
LIBRARIANS
TestimonialsSubscriptionsAccessResourcesLibrary Advisory BoardFAQ
RESEARCH
JoVE JournalMethods CollectionsJoVE Encyclopedia of ExperimentsArchive
EDUCATION
JoVE CoreJoVE BusinessJoVE Science EducationJoVE Lab ManualFaculty Resource CenterFaculty Site
Terms & Conditions of Use
Privacy Policy
Policies

Related Concept Videos

¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.7K
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...
1.7K
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

3.8K
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...
3.8K
Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

853
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...
853
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

1.8K
The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse....
1.8K
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

2.2K
Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal and vicinal coupling are observed. For example, consider the COSY spectrum of ethyl acetate, where its 1D proton NMR spectrum is plotted along the vertical and horizontal axes with their corresponding chemical shift scale. Three spots on the diagonal corresponding to the three peaks in the 1D proton spectrum are called diagonal peaks. The COSY...
2.2K
¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

1.4K
At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
1.4K

You might also read

Related Articles

Articles linked to this work by shared authors, journal, and citation graph.

Sort by
Same author

Probing Hydrogen Activation in a Dimetal Dihydride Complex by Symmetric Exchange with Parahydrogen.

Journal of the American Chemical Society·2026
Same author

Chemical hydrodynamics of nuclear spin states.

Science advances·2025
Same author

Simulation of pulsed dynamic nuclear polarization in the steady state.

The Journal of chemical physics·2025
Same author

Leveraging relaxation-optimized <sup>1</sup>H-<sup>13</sup>C<sub>F</sub> correlations in 4-<sup>19</sup>F-phenylalanine as atomic beacons for probing structure and dynamics of large proteins.

Nature chemistry·2025
Same author

Instrumental distortions in quantum optimal control.

The Journal of chemical physics·2025
Same author

MXene synthesis in a semi-continuous 3D-printed PVDF flow reactor.

Nanoscale advances·2025

Related Experiment Video

Updated: Apr 5, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

16.2K

(14)N overtone transition in double rotation solid-state NMR.

Ibraheem M Haies1, James A Jarvis, Lynda J Brown

  • 1School of Chemistry, University of Southampton, SO17 1BJ, Southampton, UK. m.carravetta@soton.ac.uk.

Physical Chemistry Chemical Physics : PCCP
|August 25, 2015
PubMed
Summary

Solid-state NMR overtone spectroscopy of nitrogen-14 nuclei offers direct detection without labeling. Double rotation further enhances spectral resolution, approaching high-resolution techniques for nitrogen-15.

More Related Videos

Author Spotlight: Exploring Intrinsically Disordered Protein Dynamics Through NMR Relaxation Experiments
09:25

Author Spotlight: Exploring Intrinsically Disordered Protein Dynamics Through NMR Relaxation Experiments

Published on: November 1, 2024

3.0K
Practical Aspects of Sample Preparation and Setup of 1H R1&#961; Relaxation Dispersion Experiments of RNA
08:17

Practical Aspects of Sample Preparation and Setup of 1H R1ρ Relaxation Dispersion Experiments of RNA

Published on: July 9, 2021

5.4K

Related Experiment Videos

Last Updated: Apr 5, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

16.2K
Author Spotlight: Exploring Intrinsically Disordered Protein Dynamics Through NMR Relaxation Experiments
09:25

Author Spotlight: Exploring Intrinsically Disordered Protein Dynamics Through NMR Relaxation Experiments

Published on: November 1, 2024

3.0K
Practical Aspects of Sample Preparation and Setup of 1H R1&#961; Relaxation Dispersion Experiments of RNA
08:17

Practical Aspects of Sample Preparation and Setup of 1H R1ρ Relaxation Dispersion Experiments of RNA

Published on: July 9, 2021

5.4K

Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Quantum Mechanics and Spectroscopy
  • Materials Science

Background:

  • Solid-state NMR overtone transitions of spin-1 (14)N nuclei are largely unaffected by nuclear quadrupole interactions to first order.
  • Magic-angle sample spinning (MASS) of (14)N overtone spectra yields narrow lines (kHz range), enabling direct detection of nitrogen compounds without isotopic labeling.
  • Second-order quadrupolar interactions still broaden (14)N overtone resonances, limiting spectral resolution.

Purpose of the Study:

  • To investigate the potential of double rotation (DOR) to further enhance spectral resolution in solid-state (14)N NMR overtone spectroscopy.
  • To reduce spectral linewidths caused by second-order quadrupolar effects in (14)N solid-state NMR.
  • To bring the resolution of (14)N solid-state NMR closer to that achieved with (15)N spectroscopy.

Main Methods:

  • Application of double rotation (DOR) technique to solid-state (14)N NMR experiments.
  • Acquisition and analysis of (14)N overtone NMR spectra under DOR conditions.
  • Comparison of spectral linewidths obtained with DOR versus traditional MASS techniques.

Main Results:

  • Double rotation (DOR) successfully reduced spectral linewidths by an order of magnitude compared to MASS.
  • The achieved linewidths approach those typically observed in high-resolution solid-state NMR spectroscopy of (15)N.
  • Demonstrated significant improvement in spectral resolution for (14)N solid-state NMR.

Conclusions:

  • Double rotation (DOR) is a powerful technique for suppressing second-order quadrupolar broadening in solid-state (14)N NMR overtone spectroscopy.
  • This advancement significantly improves spectral resolution, making (14)N NMR more comparable to (15)N NMR in terms of resolution.
  • Further development of pulsed methodologies could potentially offer even greater suppression of second-order effects, advancing high-resolution solid-state NMR.