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Related Concept Videos

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...
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
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...
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied first.
Applications Of NMR In Biology01:25

Applications Of NMR In Biology

Nuclear magnetic resonance (NMR) spectroscopy is a very valuable analytical technique for researchers. It has been used for more than 50 years as an analytical tool. F. Bloch and E. Purcell formulated NMR in 1946 and won the 1952 Nobel Prize in Physics  for their work. Biological macromolecules such as proteins, nucleic acids, lipids, and organic molecules including pharmaceutical compounds, can be studied using this versatile tool that exploits the magnetic properties of certain nuclei.
The...
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse.

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Related Experiment Video

Updated: Jun 11, 2026

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

Problems, artifacts and solutions in the INADEQUATE NMR experiment.

Alex D Bain1, Donald W Hughes, Christopher K Anand

  • 1Department of Chemistry and Chemical Biology, McMaster University, 1280 Main Street West, Hamilton, Ontario, Canada L8S 4M1. bain@mcmaster.ca

Magnetic Resonance in Chemistry : MRC
|July 1, 2010
PubMed
Summary

The INADEQUATE experiment offers detailed organic molecule analysis with modern equipment, requiring only milligrams of sample. This method reveals carbon skeleton structures and long-range connectivities, proving valuable for routine structure determination.

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Area of Science:

  • Organic Chemistry
  • Spectroscopy
  • Structural Elucidation

Background:

  • The INADEQUATE experiment provides detailed carbon skeleton information for organic molecules.
  • Traditionally, it required large sample amounts, limiting its routine use.
  • Modern advancements in spectrometers and probes have significantly reduced sample requirements.

Purpose of the Study:

  • To analyze the INADEQUATE experiment step-by-step for optimal sensitivity and artifact identification.
  • To demonstrate the experiment's utility on diverse organic molecules.
  • To highlight the value of a modified INADEQUATE experiment for long-range connectivity analysis.

Main Methods:

  • Step-by-step analysis of the INADEQUATE pulse sequence.
  • Application of the experiment to 1-octanol, 17alpha-ethynylestradiol, and beta-hydrastine.
  • Investigation of a modified INADEQUATE version tuned for small couplings and long delays.

Main Results:

  • Successful acquisition of structural data using only milligrams of sample.
  • Identification of factors contributing to sensitivity and potential artifacts.
  • Demonstration of two- and three-bond carbon correlations via double-quantum coherence.
  • Characterization of long-range connectivities using the modified experiment.

Conclusions:

  • The INADEQUATE experiment is now viable for routine organic structure determination.
  • Modern instrumentation makes the experiment sensitive and efficient.
  • The experiment, including its modified versions, provides crucial structural insights.