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Updated: Jul 28, 2025

Microfluidic Pneumatic Cages: A Novel Approach for In-chip Crystal Trapping, Manipulation and Controlled Chemical Treatment
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Programmed Pore-Shape Fixing in a Soft Porous Molecular Crystal-Navigating the Phase Interconversion Landscape.

Alan C Eaby1, Leigh Loots1, Jeanice L Basson1

  • 1Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Matieland, 7602, Stellenbosch, South Africa.

Angewandte Chemie (International Ed. in English)
|June 3, 2023
PubMed
Summary
This summary is machine-generated.

Pore-shape fixing effects were observed in soft porous crystals of p-tert-butylcalix[4]arene (TBC4). Smaller TBC4 crystals exhibited fixed porous structures, unlike larger ones, demonstrating a particle size-dependent phenomenon.

Keywords:
AdsorptionHost-Guest SystemsIn Situ CrystallographyShape-Fixing EffectSoft Porous Crystal

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Area of Science:

  • Materials Chemistry
  • Supramolecular Chemistry
  • Crystallography

Background:

  • Pore-shape fixing effects (PSFEs) in soft porous crystals remain underexplored.
  • Dynamic van der Waals solids offer unique possibilities for structural manipulation.

Purpose of the Study:

  • To investigate and report the PSFE in the prototypical dynamic van der Waals solid p-tert-butylcalix[4]arene (TBC4).
  • To understand the molecular-level mechanisms governing guest-induced phase transformations in TBC4.

Main Methods:

  • Variable-pressure (VP) single-crystal and powder X-ray diffraction.
  • VP differential scanning calorimetry.
  • Volumetric sorption analysis and attenuated total reflectance Fourier-transform infrared spectroscopy.

Main Results:

  • Two distinct porous shape-fixed phases were programmed in TBC4 using CO2 pressure and temperature.
  • Phase interconversion was found to be particle size-dependent: smaller crystals showed fixed metastable phases, while larger crystals exhibited reversible transitions.
  • A comprehensive phase interconversion scheme for TBC4 was established.

Conclusions:

  • This study provides the first example of PSFE in a porous molecular crystal.
  • The findings highlight the potential for controlling porous crystal structures through external stimuli and particle size.
  • The established phase interconversion scheme allows for predictable navigation of TBC4's structural landscape.