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NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

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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...
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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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Spin–Spin Coupling: One-Bond Coupling01:17

Spin–Spin Coupling: One-Bond Coupling

1.5K
Coupling interactions are strongest between NMR-active nuclei bonded to each other, where spin information can be transmitted directly through the pair of bonding electrons. While nuclei polarize their electrons to the opposite spins, the bonding electron pair has opposite spins. Configurations with antiparallel nuclear spins are expected to be lower in energy. When coupling makes antiparallel states more favorable, J is considered to have a positive value. The one-bond coupling constant, 1J,...
1.5K
Spin–Spin Coupling Constant: Overview01:08

Spin–Spin Coupling Constant: Overview

1.5K
In bromoethane, the three methyl protons are coupled to the two methylene protons that are three bonds away. In accordance with the n+1 rule, the signal from the methyl protons is split into three peaks with 1:2:1 relative intensities. The methylene protons appear as a quartet, with the relative intensities of 1:3:3:1.
Qualitatively, any spin plus-half nucleus polarizes the spins of its electrons to the minus-half state. Consequently, the paired electron in the hydrogen–carbon bond must...
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Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)01:20

Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)

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Two NMR-active nuclei bonded to a central atom can be involved in geminal or two-bond coupling. Geminal coupling is commonly seen between diastereotopic protons in chiral molecules and unsymmetrical alkenes, among others.
The central atom need not be NMR-active because its electrons are affected by the electron polarization of the spin-active atoms. However, spin information is transmitted less effectively than in one-bond coupling, and 2J values are usually weaker than 1J values. The energy of...
1.7K
Spin–Spin Coupling: Three-Bond Coupling (Vicinal Coupling)01:22

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

1.5K
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...
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Simultaneous homonuclear and heteronuclear spin decoupling in magic-angle spinning solid-state NMR.

Kaustubh R Mote1, Perunthiruthy K Madhu2

  • 1Tata Institute of Fundamental Research Hyderabad, Survey No. 36/P, Gopanapally Village, Serilingampally Mandal, Ranga Reddy District, Hyderabad, 500 107, India.

Solid State Nuclear Magnetic Resonance
|January 27, 2018
PubMed
Summary

This study introduces an effective method for simultaneous homonuclear and heteronuclear dipolar decoupling in solid-state NMR. This technique enhances spectral resolution by reducing proton-proton and proton-carbon interactions.

Keywords:
Heteronuclear dipolar decouplingHomonuclear dipolar decouplingMagic-angle spinningSolid-state NMRrCWwPMLG

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Advanced spectroscopic techniques for molecular structure determination.

Background:

  • Homonuclear and heteronuclear dipolar interactions cause significant line broadening in solid-state NMR spectra.
  • Effective decoupling methods are crucial for obtaining high-resolution spectra in magic-angle spinning (MAS) NMR.

Purpose of the Study:

  • To develop and demonstrate an effective method for simultaneous homonuclear and heteronuclear dipolar decoupling in MAS solid-state NMR.
  • To improve spectral resolution in 1H NMR spectra by suppressing 1H-1H and 1H-13C interactions.

Main Methods:

  • Implementation of simultaneous homonuclear decoupling on the 1H channel.
  • Application of heteronuclear decoupling on the 13C channel.
  • Observation of 1H spins in a windowed fashion during experiments conducted at ~60 kHz MAS frequencies.

Main Results:

  • Successful simultaneous homonuclear and heteronuclear dipolar decoupling was achieved.
  • Significant attenuation of line broadening from both 1H-1H and 1H-13C interactions was observed.
  • Enhanced resolution in the resulting 1H NMR spectra.

Conclusions:

  • The presented method offers an effective approach for simultaneous dipolar decoupling in MAS solid-state NMR.
  • This technique leads to improved spectral quality, particularly beneficial for 13C labeled samples.
  • The findings contribute to advancements in high-resolution solid-state NMR spectroscopy.