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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

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The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
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¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

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At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
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Atomic Spectroscopy: Effects of Temperature01:27

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Atomization, converting samples into gas-phase atoms and ions, is essential for atomic spectroscopy. The flame temperature required for atomization affects the efficiency of the atomic spectroscopic methods by increasing the atomization efficiency and the relative population of the excited and ground states.
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Irradiation of a spin-active nucleus causes an increase or decrease in the signal intensity of neighboring nuclei that are not necessarily chemically bonded or involved in J-coupling. This phenomenon, called the nuclear Overhauser enhancement (NOE), results from through-space interactions between the nuclear spins. The NOE effect decreases with increasing internuclear distance and is generally not observed beyond 4 angstroms. In NOE, dipole-dipole interactions between neighboring spin-active...
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The Arrhenius equation,
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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.
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Subtle temperature-induced changes in small molecule conformer dynamics - observed and quantified by NOE

C R Jones1, M D Greenhalgh1, J R Bame1

  • 1School of Chemistry, University of Bristol Cantocks Close, Bristol, BS8 1TS, UK. Craig.Butts@bristol.ac.uk.

Chemical Communications (Cambridge, England)
|January 22, 2016
PubMed
Summary

Nuclear Overhauser Effect (NOE) distance measurements accurately track subtle changes in molecular conformer populations with temperature. This demonstrates NOE

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Area of Science:

  • Biophysical Chemistry
  • Structural Biology
  • Computational Chemistry

Background:

  • Understanding molecular dynamics and structural changes is crucial in chemistry and biology.
  • Nuclear Overhauser Effect (NOE) is a key technique for determining inter-atomic distances in molecules.
  • Precise NOE measurements are essential for accurate structural and dynamic information.

Purpose of the Study:

  • To evaluate the accuracy of NOE-distance measurements in detecting small changes in molecular conformer populations.
  • To assess the impact of temperature variations on conformer populations using NOE data.
  • To validate NOE-derived dynamics information against theoretical predictions.

Main Methods:

  • Utilizing Nuclear Overhauser Effect (NOE) spectroscopy to measure inter-atomic distances.
  • Analyzing NOE-distance data to quantify changes in conformer populations.
  • Comparing experimental results with Boltzmann distribution predictions.

Main Results:

  • NOE-distance relationships accurately monitored minute changes in conformer populations (<0.5%/10 °C).
  • Experimental findings showed excellent agreement with Boltzmann predictions.
  • The study confirmed the effectiveness of NOE measurements for dynamics and structural analysis.

Conclusions:

  • Accurate NOE-distance measurements provide high-quality structural and dynamics information for small molecules.
  • NOE is a powerful tool for monitoring subtle conformational changes influenced by environmental factors like temperature.
  • This technique enhances our ability to study molecular behavior at a fine-grained level.