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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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When protons A and X are coupled, their nuclear spin energy levels are slightly modified. This is because the energy required to excite proton A to a spin state parallel to proton X is slightly different from the energy required for it to become anti-parallel to spin X. Consequently, there are two possible excitation frequencies for A (A1 and A2), depending on the spin state of X, and vice versa. The mutual nature of coupling implies that the difference between frequencies A1 and A2, indicated...
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Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and enhance the signals of low-abundance nuclei, such as carbon-13 and nitrogen-15, in small molecules. The fundamental principle behind INEPT is the transfer of polarization from a more abundant and highly polarizable nucleus, typically hydrogen-1, to the low-abundance nucleus of interest. This process effectively boosts the NMR signal of the...
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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.
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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
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Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling.

Evgeny Nimerovsky1, Eszter E Najbauer1, Kumar Tekwani Movellan1

  • 1Department of NMR Based Structural Biology, Max Planck Institute for Biophysical Chemistry, Am Fassberg 11, 37077 Göttingen, Germany.

The Journal of Physical Chemistry Letters
|February 8, 2022
PubMed
Summary
This summary is machine-generated.

A new selective pulse sequence, MODIST, enhances proton-proton correlations in magic-angle spinning NMR. This method improves signal intensity for determining molecular structures, especially for challenging samples like proteins in lipid bilayers.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Structural Biology
  • Biophysics

Background:

  • Homonuclear dipolar recoupling is vital for magic-angle spinning (MAS) NMR structure determination.
  • High proton density in samples limits detection of longer proton-proton distances using broadband recoupling.
  • Selective methods are needed to overcome these limitations by targeting specific spins.

Purpose of the Study:

  • To introduce and validate a novel selective pulse sequence, MODIST (Modest Offset-recoupling with Intensity and Selectivity Transfer).
  • To demonstrate MODIST's capability in selectively recoupling spins with modest chemical shift differences.
  • To enhance the detection of longer-range proton-proton correlations in MAS NMR experiments.

Main Methods:

  • Development and implementation of the MODIST selective pulse sequence.
  • Application of MODIST in magic-angle spinning NMR spectroscopy.
  • Testing the sequence across various spinning frequencies (55.555 and 100 kHz) and magnetic fields (600-1200 MHz proton Larmor frequencies).
  • Selective recording of correlations between amide protons.

Main Results:

  • MODIST demonstrates good retention of total signal, achieving up to twice the intensity for proton-proton correlations compared to existing selective methods.
  • The sequence is effective across a range of MAS conditions and magnetic field strengths.
  • Selective correlations between amide protons were successfully recorded.

Conclusions:

  • MODIST is a powerful selective recoupling method for MAS NMR, enabling detection of longer proton-proton distances.
  • The enhanced signal intensity and selectivity of MODIST facilitate more accurate structure determination.
  • Application to influenza A M2 in lipid bilayers revealed cross-peaks indicative of a helical conformation, showcasing its utility in biological systems.