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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)

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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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2D NMR: Overview of Heteronuclear Correlation Techniques01:18

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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: 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: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

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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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¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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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...
1.5K
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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Through-space NMR correlations between two different half-integer quadrupolar nuclei using T-HMQC sequences.

Yury G Kolyagin1, Julien Trébosc2, Olivier Lafon1

  • 1Univ. Lille, CNRS, Centrale Lille, Univ. Artois, UMR 8181, UCCS - Unité de Catalyse et de Chimie du Solide, F-59000, Lille, France.

Solid State Nuclear Magnetic Resonance
|October 9, 2025
PubMed
Summary

This study introduces T-HMQC, a novel NMR technique for probing proximities between quadrupolar nuclei. T-HMQC offers wider excitation bandwidth, beneficial for analyzing complex materials like glasses.

Keywords:
D-HMQCQuadrupolar nucleiT-HMQCTRAPDORThrough-space correlations

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Materials science, particularly the study of glasses and amorphous materials.

Background:

  • Heteronuclear Multiple-Quantum Correlation (HMQC) experiments are used to study proximities between spin-1/2 nuclei.
  • TRAnsfer of Population in DOuble-Resonance (TRAPDOR) experiments utilize specific irradiation techniques.

Purpose of the Study:

  • To demonstrate the applicability of T-HMQC for probing proximities between distinct half-integer spin quadrupolar isotopes.
  • To introduce novel selective variants of T-HMQC to reduce spectral complexity.
  • To analyze the influence of experimental parameters on T-HMQC efficiency.

Main Methods:

  • Development and application of T-HMQC (TRAPDOR-HMQC) sequences for quadrupolar nuclei.
  • Introduction of selective T-HMQC variants using echo-antiecho quadrature detection or central-transition (CT)-selective pulses.
  • Experimental analysis of 11B-27Al T-HMQC on a magnesium aluminoborate glass.

Main Results:

  • T-HMQC effectively probes proximities between half-integer spin quadrupolar isotopes.
  • Optimized TRAPDOR pulse conditions involve separation by integer rotor periods and maximum rf field strength.
  • Selective T-HMQC variants reduce spectral complexity but may decrease sensitivity compared to D-HMQC.

Conclusions:

  • T-HMQC is a valuable technique for studying quadrupolar nuclei interactions in materials.
  • TRAPDOR pulse synchronization and rf amplitude are critical for efficient T-HMQC.
  • T-HMQC offers a wider excitation bandwidth, advantageous for broad NMR spectra, especially at high fields.