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Related Concept Videos

2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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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...
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2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

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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...
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2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

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

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

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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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¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

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The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...
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¹H NMR: Long-Range Coupling01:27

¹H NMR: Long-Range Coupling

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The coupling interactions of nuclei across four or more bonds are usually weak, with J values less than 1 Hz. While these are usually not observed in spectra, the presence of multiple bonds along the coupling pathway can result in observable long-range coupling.
In alkenes, spin information is communicated via σ–π overlap, as seen in allylic (four-bond) and homoallylic (five-bond) couplings. These coupling interactions are stronger when the σ bond is parallel to the alkene...
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Updated: Dec 1, 2025

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Fast remote correlation experiments for 1H homonuclear decoupling in solids.

Pinelopi Moutzouri1, Bruno Simões de Almeida1, Lyndon Emsley1

  • 1Institut des Sciences et Ingéniere Chimiques, École Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|November 6, 2020
PubMed
Summary
This summary is machine-generated.

This study introduces a faster method for analyzing solid-state nuclear magnetic resonance (NMR) spectra by combining anti-z-COSY with a two-dimensional one-pulse (TOP) transformation. This TAZ-COSY technique significantly reduces experiment time while improving spectral resolution.

Keywords:
(1)H resolutionAnti-z-COSYMagic angle spinningSolid-state NMRTOP

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Advanced NMR pulse sequence development
  • Materials characterization

Background:

  • Solid-state 1H MAS NMR spectra often exhibit residual homogeneous broadening from higher-order shifts and splittings.
  • Previous methods like 2D anti-z-COSY can remove splittings but require long experiment times due to high resolution needs in the indirect dimension (t1).

Purpose of the Study:

  • To develop a time-efficient method for removing spectral broadening in solid-state NMR.
  • To adapt the anti-z-COSY experiment for faster acquisition without compromising line narrowing effects.
  • To demonstrate the utility of the new method for both solid and liquid samples.

Main Methods:

  • Adaptation of the anti-z-COSY experiment by combining it with the two-dimensional one-pulse (TOP) transformation, creating the TAZ-COSY sequence.
  • Application of the TAZ-COSY sequence to a powdered sample of L-histidine monohydrochloride monohydrate at 100 kHz MAS.
  • Adaptation of the methodology for liquid-state 1H homodecoupled data acquisition, demonstrated with testosterone.

Main Results:

  • The TAZ-COSY sequence significantly reduces experimental time compared to traditional anti-z-COSY.
  • A factor of 1.6 to 2.3 increase in spectral resolution was achieved for L-histidine monohydrochloride monohydrate in just 20 minutes.
  • The method successfully acquired liquid-state 1H homodecoupled data for testosterone.

Conclusions:

  • The TAZ-COSY sequence offers a substantial improvement in spectral resolution and a significant reduction in experimental time for solid-state NMR.
  • This adapted methodology is effective for both solid and liquid samples, enhancing NMR data acquisition efficiency.
  • The TAZ-COSY approach provides a valuable tool for detailed molecular structure analysis in various states of matter.