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Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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...
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
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...
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

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 in...
Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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...
Atomic Nuclei: Magnetic Resonance01:05

Atomic Nuclei: Magnetic Resonance

The number of nuclear spins aligned in the lower energy state is slightly greater than those in the higher energy state. In the presence of an external magnetic field, as the spins precess at the Larmor frequency, the excess population results in a net magnetization oriented along the z axis. When a pulse or a short burst of radio waves at the Larmor frequency is applied along the x axis, the coupling of frequencies causes resonance and flips the nuclear spins of the excess population from the...

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Updated: May 24, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

Cristalografía de RMN de estado sólido a través de restricciones paramagnéticas.

Claudio Luchinat1, Giacomo Parigi, Enrico Ravera

  • 1Magnetic Resonance Center (CERM), University of Florence, via Sacconi 6, Sesto Fiorentino, Italy. luchinat@cerm.unifi.it

Journal of the American Chemical Society
|March 8, 2012
PubMed
Resumen

La espectroscopia NMR de estado sólido (SS-NMR) utilizando desplazamientos de pseudocontacto (PCS) en metaloproteínas paramagnéticas permite la cristalografía NMR. Este método determina tanto la estructura de proteínas como el empaque de cristales con alta precisión.

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Área de la Ciencia:

  • La biofísica es la biofísica.
  • Biología Estructural Biología estructural.
  • Espectroscopia de RMN en estado sólido Espectroscopia de RMN en estado sólido

Sus antecedentes:

  • Las metaloproteínas paramagnéticas son cruciales para comprender los procesos biológicos.
  • La espectroscopia de RMN de estado sólido (SS-NMR) es una técnica poderosa para estudiar la estructura de las proteínas.
  • La cristalografía RMN combina los datos de RMN con los principios cristalográficos.

Objetivo del estudio:

  • Demostrar la utilidad de los desplazamientos de pseudocontacto (PCS) en RMN en estado sólido para determinar las estructuras de las proteínas.
  • Para validar la aplicación de restricciones derivadas de SS-NMR para un análisis preciso de envasado de cristales.

Principales métodos:

  • Medición de desplazamientos por pseudocontacto (PCS) en polvos microcristalinos de una metaloproteína paramagnética mediante el uso de SS-NMR.
  • Integración de los PCS con otras restricciones experimentales SS-NMR.
  • Aplicación de los principios de la cristalografía RMN para analizar los datos obtenidos.

Principales resultados:

  • Determinación exitosa de la estructura molecular de la proteína utilizando PCS de SS-NMR.
  • Elucidación precisa del envasado cristalino de la metaloproteína estudiada.
  • Demostrar que los PCS proporcionan información estructural valiosa a largo plazo.

Conclusiones:

  • Los PCS medidos por SS-NMR son restricciones efectivas para la cristalografía de RMN.
  • Este enfoque permite la determinación simultánea de la estructura de la proteína y el empaque de cristales.
  • La cristalografía de RMN utilizando SS-NMR ofrece un método complementario a la cristalografía de rayos X tradicional.