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相关概念视频

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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相关实验视频

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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

通过对磁束的固态NMR晶体学通过对磁束.

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
概括

固态NMR光谱学 (SS-NMR) 使用对磁性金属蛋白的伪接触转移 (PCS) 实现了NMR结晶学. 这种方法可以很准确地确定蛋白质结构和晶体包装.

科学领域:

  • 生物物理学的生物物理.
  • 结构生物学 结构生物学
  • 固态NMR光谱学 固态NMR光谱学

背景情况:

  • 偏磁性金属蛋白对于理解生物过程至关重要.
  • 固态NMR光谱 (SS-NMR) 是研究蛋白质结构的一种强大技术.
  • 核磁共振晶体学将核磁共振数据与晶体学原理相结合.

研究的目的:

  • 为了证明在固态NMR中伪接触移位 (PCS) 的实用性,以确定蛋白质结构.
  • 为了验证SS-NMR衍生限制的应用,以准确进行晶体包装分析.

主要方法:

  • 使用SS-NMR测量一个偏磁性金属蛋白的微晶粉中伪接触移位 (PCS).
  • 将PCS与其他SS-NMR实验限制装置集成.
  • 应用NMR结晶学原理来分析获得的数据.

主要成果:

  • 使用SS-NMR的PCS成功确定了蛋白质分子结构.
  • 准确阐明研究的金属蛋白的晶体包装.
  • 证明PCS提供了有价值的长期结构信息.

结论:

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Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
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  • 通过SS-NMR测量的PCS是NMR结晶学的有效限制.
  • 这种方法可以同时确定蛋白质结构和晶体包装.
  • 使用SS-NMR的NMR结晶学为传统的X射线结晶学提供了一种补充方法.