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Related Concept Videos

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

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...
Spin–Spin Coupling: Three-Bond Coupling (Vicinal Coupling)01:22

Spin–Spin Coupling: Three-Bond Coupling (Vicinal Coupling)

Vicinal or three-bond coupling is commonly observed between protons attached to adjacent carbons. Here, nuclear spin information is primarily transferred via electron spin interactions between adjacent C‑H bond orbitals. This generally favors the antiparallel arrangement of spins, so 3J values are usually positive.
The extent of coupling depends on the C‑C bond length, the two H‑C‑C angles, any electron-withdrawing substituents, and the dihedral angle between the involved orbitals. The...
¹H NMR: Long-Range Coupling01:27

¹H NMR: Long-Range Coupling

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

HMBC-like experiment based on longitudinal csa/dipolar cross-correlation.

Sabine Bouguet-Bonnet1, Sébastien Leclerc, Pierre Mutzenhardt

  • 1Laboratoire de Méthodologie RMN, Université Henri Poincaré Faculté des Sciences, BP 239, 54506 Vandoeuvre-lès-Nancy Cedex, France.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|February 12, 2005
PubMed
Summary

A new NMR method efficiently isolates longitudinal two-spin order, revealing chemical shift anisotropy/dipolar cross-correlation rates. This technique enhances spectral analysis for medium-sized molecules by highlighting specific molecular interactions.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Chemical Physics
  • Molecular Biophysics

Background:

  • Cross-correlation effects, including chemical shift anisotropy (CSA) and dipolar interactions, provide valuable structural and dynamic information in NMR.
  • Existing methods may struggle to isolate specific cross-correlation pathways, especially in complex systems like medium-sized molecules.
  • Proton detection offers superior sensitivity for NMR experiments.

Purpose of the Study:

  • To develop an efficient gradient-based NMR sequence for selectively measuring longitudinal two-spin order.
  • To characterize cross-peaks related to CSA/dipolar cross-correlation rates between protons and heteronuclei.
  • To provide a tool for analyzing complex cross-correlation effects in medium-sized molecules.

Main Methods:

  • Implementation of a novel gradient-based NMR pulse sequence.
  • Exploitation of CSA and dipolar cross-correlation effects between protons and heteronuclei.
  • Utilizing proton detection for enhanced signal sensitivity.
  • Acquisition and analysis of two-dimensional NMR spectra.

Main Results:

  • The proposed sequence effectively filters out unwanted signals, isolating the longitudinal two-spin order.
  • The resulting 2D spectra exhibit cross-peaks directly proportional to the CSA/dipolar cross-correlation rates.
  • The method demonstrates applicability to medium-sized molecules with multiple cross-correlation influences.

Conclusions:

  • The developed NMR method offers an efficient way to measure CSA/dipolar cross-correlation rates.
  • This technique provides insights into molecular dynamics and structure, particularly for molecules of intermediate size.
  • The method's spectral appearance, similar to HMBC, facilitates interpretation while revealing distinct cross-correlation information.