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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

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

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

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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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Updated: Apr 11, 2026

Controlling the Size, Shape and Stability of Supramolecular Polymers in Water
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Do Cyclodextrins Aggregate in Water? Insights from NMR Experiments.

Artur J M Valente, Rui A Carvalho, Olle Söderman1

  • 1§Division of Physical Chemistry, Department of Chemistry, Lund University, PO Box 124, S-221 00 Lund, Sweden.

Langmuir : the ACS Journal of Surfaces and Colloids
|May 29, 2015
PubMed
Summary

Nuclear Magnetic Resonance (NMR) techniques found no significant aggregation of cyclodextrins (α-, β-, and γ-) in aqueous solutions. Any aggregates present constitute less than 1% of the total cyclodextrin, suggesting minimal self-assembly in these conditions.

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Area of Science:

  • Supramolecular Chemistry
  • Physical Chemistry
  • Analytical Chemistry

Background:

  • Previous studies suggested cyclodextrins self-assemble into aggregates in aqueous solutions, influencing supramolecular mechanisms.
  • Cryo-Transmission Electron Microscopy (cryo-TEM) previously indicated aggregate sizes ranging from 90 nm to micrometers.
  • These findings were supported by measurements of viscosity and activity coefficients, interpreted as evidence of cyclodextrin self-aggregation.

Purpose of the Study:

  • To re-evaluate the aggregation of native cyclodextrins (α-, β-, and γ-) in aqueous solutions.
  • To investigate the presence and extent of cyclodextrin self-assembly using advanced NMR techniques.
  • To determine if self-aggregation is a significant factor in supramolecular mechanisms involving cyclodextrins.

Main Methods:

  • Utilized (1)H Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Employed NMR diffusometry to measure molecular diffusion.
  • Applied NMR relaxometry and proton peak intensity analysis to assess molecular dynamics and concentration.

Main Results:

  • No cyclodextrin aggregates were detected within the detection limits of the NMR experiments.
  • The fraction of cyclodextrins potentially involved in aggregation is less than 1%.
  • The presence of transient clusters with short lifetimes cannot be definitively excluded.

Conclusions:

  • NMR data indicate a negligible extent of cyclodextrin aggregation in aqueous solutions.
  • The self-aggregation of cyclodextrins is likely not a dominant factor in supramolecular mechanisms under the studied conditions.
  • Further investigation into transient, short-lived clusters may be warranted.