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Related Concept Videos

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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Carbon-13 (¹³C) NMR: Overview01:10

Carbon-13 (¹³C) NMR: Overview

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Carbon-13 is a naturally occurring NMR-active isotope of carbon with a low natural abundance of 1.1%. In contrast, carbon-12 is the most abundant isotope of carbon with zero nuclear spin. Therefore, it is NMR inactive. The gyromagnetic ratio of carbon-13 is smaller than that of protons. As a result, carbon-13 resonance is about 6000 times weaker than proton resonance. For a given magnetic field strength, the resonance frequency of carbon-13 is about one-fourth of the resonance frequency for...
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Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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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.
Spin decoupling is usually achieved by...
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Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
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Other Nuclides: 31P, 19F, 15N NMR01:16

Other Nuclides: 31P, 19F, 15N NMR

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Many organic, inorganic, and biological molecules contain spin-half nuclei such as nitrogen-15, fluorine-19, and phosphorus-31. As a result, NMR studies of these nuclei have found extensive applications in chemical and biological research.
While fluorine-19 and phosphorous-31 have high natural abundances (100%) and positive gyromagnetic ratios, nitrogen-15 has a low natural abundance and a negative gyromagnetic ratio. However, nitrogen-15 is still preferred over nitrogen-14 (which has a...
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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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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Spin-state-selective methods in solution- and solid-state biomolecular 13C NMR.

Isabella C Felli1, Roberta Pierattelli1

  • 1Magnetic Resonance Center (CERM) and Department of Chemistry "Ugo Schiff", University of Florence, Via L. Sacconi 6, 50019 Sesto Fiorentino, Italy.

Progress in Nuclear Magnetic Resonance Spectroscopy
|February 12, 2015
PubMed
Summary
This summary is machine-generated.

Spin-state-selective methods improve carbon-13 detected Nuclear Magnetic Resonance (NMR) experiments for biomolecular studies. These techniques enhance homonuclear decoupling, making NMR a more powerful tool for protein analysis.

Keywords:
BiomoleculesHomodecouplingIDPParamagnetic moleculesScalar coupling

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Area of Science:

  • Biophysical Chemistry
  • Structural Biology
  • Nuclear Magnetic Resonance (NMR) Spectroscopy

Background:

  • Carbon-13 detected NMR experiments are crucial for biomolecular structure determination.
  • Homonuclear decoupling in the direct acquisition dimension is essential for spectral resolution.
  • Previous methods had limitations in efficiency and applicability.

Purpose of the Study:

  • To provide a detailed overview of spin-state-selective methods for homonuclear decoupling.
  • To summarize newly developed NMR experiments based on these methods.
  • To showcase applications of these techniques in protein studies.

Main Methods:

  • Discussion of various spin-state-selective pulse sequences.
  • Analysis of experimental data from different protein samples.
  • Comparison of different decoupling strategies.

Main Results:

  • Demonstration of effective homonuclear decoupling in (13)C detected NMR.
  • Successful application of new NMR experiments to diverse protein systems.
  • Improved spectral quality and data interpretation for proteins in various aggregation states.

Conclusions:

  • Spin-state-selective methods significantly enhance the utility of (13)C detected NMR.
  • These advancements facilitate the study of complex biomolecules.
  • The presented techniques offer broad applicability in structural biology.