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Spin–Spin Coupling: One-Bond Coupling01:17

Spin–Spin Coupling: One-Bond Coupling

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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,...
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Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)01:20

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

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

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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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NMR Spectroscopy: Spin–Spin Coupling01:08

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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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Spin–Spin Coupling Constant: Overview01:08

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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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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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Measuring strong one-bond dipolar couplings using REDOR in magic-angle spinning solid-state NMR.

Mukul G Jain1, Kaustubh R Mote1, Johannes Hellwagner2

  • 1TIFR Centre for Interdisciplinary Sciences, Tata Institute of Fundamental Research, Sy. No. 36/P, Gopanpally, Hyderabad 500 107, India.

The Journal of Chemical Physics
|April 8, 2019
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A new pulse scheme enhances Rotational-Echo Double Resonance (REDOR) for solid-state NMR. This method allows precise measurement of dipolar couplings in challenging spin pairs, overcoming limitations of existing techniques.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Quantum spin dynamics and magnetic resonance techniques.

Background:

  • Rotational-Echo Double Resonance (REDOR) is a standard technique for measuring dipolar couplings between spin-1/2 nuclei in solid-state NMR.
  • REDOR is valuable for estimating molecular motion and internuclear distances.
  • Challenges arise with strongly coupled spin pairs (e.g., 13C-1H) due to fast dipolar dephasing, complicating measurements even at high Magic-Angle-Spinning (MAS) frequencies.

Purpose of the Study:

  • To introduce a generalized REDOR pulse scheme for robust dipolar coupling measurements.
  • To overcome the limitations of existing REDOR-based methods, such as Shifted-REDOR (S-REDOR).
  • To achieve arbitrary scaling factors of dipolar couplings while maintaining experimental simplicity and robustness.

Main Methods:

  • Development of a general REDOR pulse scheme involving the shifting of both recoupling pulses within a rotor period.
  • Application of the new scheme to isolated 13C-15N and 1H-13C spin pairs.
  • Experimental validation at high MAS frequencies (20 and 62.5 kHz).

Main Results:

  • The generalized scheme allows for arbitrary scaling factors of dipolar couplings.
  • This method avoids the disadvantages of S-REDOR, such as Fourier component mixing and the need for high radio-frequency fields.
  • The technique proved effective for challenging spin pairs at relevant MAS rates.

Conclusions:

  • The novel REDOR pulse scheme offers a versatile and robust approach for measuring dipolar couplings in solid-state NMR.
  • It provides a significant improvement over existing methods for strongly coupled spin pairs.
  • This advancement facilitates more accurate structural and dynamic studies in solid materials.