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Related Concept Videos

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

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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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NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

3.4K
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...
3.4K
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

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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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Covariance spectroscopy in high-resolution multi-dimensional solid-state NMR.

Eugene C Lin1, Stanley J Opella1

  • 1Department of Chemistry and Biochemistry, University of California, San Diego, La Jolla, CA 92093-0307, USA.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|January 2, 2014
PubMed
Summary
This summary is machine-generated.

Covariance spectroscopy (COV) enhances sensitivity in solid-state NMR experiments. This method, combined with non-uniform sampling, allows for faster, more sensitive 3D NMR, aiding structural analysis.

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Area of Science:

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

Background:

  • High-resolution solid-state NMR experiments, like homonuclear spin-exchange spectroscopy, are crucial for molecular structure determination.
  • Traditional NMR methods can be time-consuming, limiting the complexity of achievable experiments.
  • Increased sensitivity is paramount for analyzing complex biological systems.

Purpose of the Study:

  • To investigate the application of covariance spectroscopy (COV) for enhancing sensitivity in 2D and 3D solid-state NMR.
  • To demonstrate the efficiency of combining COV with non-uniform sampling (NUS) techniques.
  • To showcase the utility of COV-enhanced 3D NMR for resonance assignment and structural restraint measurement.

Main Methods:

  • Application of covariance spectroscopy (COV), a statistical method, to enhance sensitivity in high-resolution solid-state NMR.
  • Implementation of an alternative States sampling scheme to reduce experimental time by 50%.
  • Integration of COV with non-uniform sampling (NUS) processing methods for multi-dimensional NMR experiments.

Main Results:

  • Covariance spectroscopy significantly increases sensitivity in homonuclear spin-exchange NMR experiments.
  • The combined approach of COV and NUS enables the performance of various 3D NMR experiments with substantial sensitivity gains.
  • A demonstrated 3D homonuclear spin-exchange/separated-local-field (SLF) spectrum facilitated resonance assignment and structural restraint measurement within a limited experimental time.

Conclusions:

  • Covariance spectroscopy is a powerful tool for improving sensitivity in solid-state NMR.
  • The combination of COV and NUS offers a highly efficient strategy for advanced 3D NMR experiments.
  • This integrated approach accelerates structural analysis, enabling detailed molecular insights from single, time-limited experiments.