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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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関連する実験動画

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

固体NMR結晶は,パラマグネティック制約を通過する.

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
まとめ

パラ磁性金属タンパク質の擬似接触シフト (PCS) を使用した固体NMRスペクトロスコーピー (SS-NMR) は,NMR結晶学を可能にします. この方法は,高精度でタンパク質構造と結晶の包装の両方を決定します.

科学分野:

  • バイオフィジックス 生物物理学
  • 構造生物学 構造生物学とは
  • 固体NMRスペクトロスコーピー 固体NMRスペクトロスコーピー

背景:

  • パラマグネット性金属タンパク質は,生物学的プロセスを理解する上で極めて重要です.
  • 固体NMR光譜法 (SS-NMR) は,タンパク質の構造を研究するための強力な技術です.
  • NMR結晶学は,NMRデータを結晶学原理と組み合わせています.

研究 の 目的:

  • 固体NMRにおける擬似接触シフト (PCS) の有用性を証明し,タンパク質構造を決定する.
  • 正確な結晶包装分析のためのSS-NMR-derived restraintsの適用を検証する.

主な方法:

  • SS-NMRを用いたパラ磁性金属タンパク質のマイクロ結晶粉末における擬似接触シフト (PCS) の測定.
  • PCSを他のSS-NMR実験制限装置と統合する.
  • 採取したデータを分析するために,NMR結晶学原理の適用.

主要な成果:

  • SS-NMRからPCSを用いたタンパク質分子構造の決定に成功した.
  • 研究された金属タンパク質の結晶包装の正確な解明.
  • PCSが価値ある長期的構造情報を提供することを実証する.

さらに関連する動画

Paramagnetic Relaxation Enhancement for Detecting and Characterizing Self-Associations of Intrinsically Disordered Proteins
07:24

Paramagnetic Relaxation Enhancement for Detecting and Characterizing Self-Associations of Intrinsically Disordered Proteins

Published on: September 23, 2021

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
08:55

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Published on: June 7, 2018

関連する実験動画

Last 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

Paramagnetic Relaxation Enhancement for Detecting and Characterizing Self-Associations of Intrinsically Disordered Proteins
07:24

Paramagnetic Relaxation Enhancement for Detecting and Characterizing Self-Associations of Intrinsically Disordered Proteins

Published on: September 23, 2021

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
08:55

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Published on: June 7, 2018

結論:

  • SS-NMRで測定されたPCSは,NMR結晶学のための効果的な抑制剤です.
  • このアプローチにより,タンパク質構造と結晶の包装を同時に決定できます.
  • SS-NMRを用いたNMR結晶学は,従来のX線結晶学を補完する方法を提供します.