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Related Concept Videos

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

Two-Dimensional (2D) NMR: Overview

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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....
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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...
1.5K
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.6K
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...
1.6K
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: 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...
713
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

1.1K
When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
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Efficient 2D double-quantum solid-state NMR spectroscopy with large spectral widths.

Katharina Märker1, Sabine Hediger, Gaël De Paëpe

  • 1Univ. Grenoble Alpes, CEA, CNRS, INAC, MEM, F-38000 Grenoble, France. gael.depaepe@cea.fr.

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Summary
This summary is machine-generated.

Supercycled recoupling sequences with Supercycle-Timing-Compensation (STiC) phase shifts enable recording 2D correlation spectra. This advances solid-state NMR for structure determination by providing long-range distance constraints.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Structural biology
  • Materials science

Background:

  • Supercycled recoupling sequences are crucial for solid-state NMR experiments.
  • Accurate spectral width control is essential for obtaining distance constraints.
  • Previous methods had limitations in spectral width applicability.

Purpose of the Study:

  • To extend the applicability of supercycled recoupling sequences.
  • To enable recording 2D correlation spectra with arbitrary spectral widths.
  • To facilitate the determination of long-range distance constraints in solid-state NMR.

Main Methods:

  • Application of Supercycle-Timing-Compensation (STiC) phase shifts.
  • Utilizing SR26 and related supercycled recoupling sequences.
  • Recording 2D double-quantum single-quantum correlation spectra.

Main Results:

  • Successful recording of 2D correlation spectra with arbitrary spectral widths.
  • Demonstration of the extended applicability of supercycled sequences.
  • Acquisition of valuable long-range distance constraints.

Conclusions:

  • STiC phase shifts significantly enhance supercycled sequences for solid-state NMR.
  • This method provides a powerful tool for molecular structure determination.
  • The approach is particularly beneficial for obtaining long-range structural information.