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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...
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...
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.
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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...

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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Published on: September 17, 2017

Coherence selection in double CP MAS NMR spectroscopy.

Jen-Hsien Yang1, Fang-Chieh Chou, Der-Lii M Tzou

  • 1Institute of Chemistry, Academia Sinica, 128, Yen-Chiu-Yuan Road, Sec. 2, Nankang, Taipei 11529, Taiwan, ROC.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|September 11, 2008
PubMed
Summary

This study demonstrates double cross-polarization (CP) magic-angle spinning (MAS) NMR for selecting carbon-13 (13C) signals. Optimizing radiofrequency (rf) field strength and MAS frequency enhances signal sensitivity and enables spectral editing.

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14:44

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

Published on: December 16, 2013

Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Biophysical Chemistry
  • Materials Science

Background:

  • Double cross-polarization (CP) magic-angle spinning (MAS) NMR is a powerful technique for studying molecular structures.
  • Efficient coherence transfer is crucial for signal sensitivity and spectral editing in NMR.
  • Understanding parameter dependencies is key to optimizing NMR experiments.

Purpose of the Study:

  • To demonstrate the application of double CP MAS NMR for carbon-13 (13C) coherence selection.
  • To investigate the influence of experimental parameters on (15)N/(13)C coherence transfer.
  • To achieve spectral editing by tailoring experimental parameters.

Main Methods:

  • Utilized (1)H/(15)N and (15)N/(13)C coherence transfers in double CP MAS NMR.
  • Employed a (15)N/(13)C-labeled N-acetyl-glucosamine compound.
  • Systematically monitored (13)C signal intensity as a function of radiofrequency (rf) field strength and MAS frequency.

Main Results:

  • The (15)N/(13)C coherence transfer efficiency is highly sensitive to experimental parameters.
  • Zero-quantum coherence transfer, with specific rf field and spinning frequency conditions, yields improved signal sensitivity.
  • Demonstrated spectral editing capabilities in one- and two-dimensional double CP experiments.

Conclusions:

  • Double CP MAS NMR is effective for 13C coherence selection.
  • Optimization of rf field strength and MAS frequency is critical for enhanced sensitivity and spectral editing.
  • This technique offers precise control over NMR signal acquisition for complex molecules.