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Related Concept Videos

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

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...
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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...
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...
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...

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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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3D 1H-13C-14N correlation solid-state NMR spectrum.

Renée Siegel1, Julien Trébosc, Jean-Paul Amoureux

  • 1UCCS (CNRS-8181), University of Lille-1, Fr-59652 Villeneuve d'Ascq, France.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|June 17, 2008
PubMed
Summary

Researchers developed a new 3D Nuclear Magnetic Resonance (NMR) technique to observe the challenging Nitrogen-14 nucleus in solid-state NMR. This advancement allows for more detailed analysis of materials containing Nitrogen-14.

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Structure and Coordination Determination of Peptide-metal Complexes Using 1D and 2D 1H NMR

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Materials science.
  • Chemical analysis.

Background:

  • Nitrogen-14 (spin I=1) nuclei are historically difficult to detect using solid-state NMR.
  • Previous observations of Nitrogen-14 were limited to one-dimensional (1D) spectra, restricting detailed structural analysis.

Purpose of the Study:

  • To present the first three-dimensional (3D) 1H-13C-14N NMR correlation spectrum.
  • To demonstrate a novel method for indirectly observing Nitrogen-14 nuclei.

Main Methods:

  • Utilized a recently developed technique for indirect observation of Nitrogen-14.
  • Employed a Heteronuclear Multiple Quantum Coherence (HMQC)-type experiment with dipolar recoupling.
  • Acquired the 3D spectrum on a L-histidine.HCl.H2O test sample.

Main Results:

  • Successfully obtained the first 3D 1H-13C-14N NMR correlation spectrum.
  • Demonstrated the efficacy of the new technique for observing Nitrogen-14 in a solid-state environment.

Conclusions:

  • The developed 3D NMR technique significantly advances the observation capabilities for Nitrogen-14 in solid-state NMR.
  • This method opens new avenues for structural elucidation of nitrogen-containing materials.