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Crystallization is a phase transformation process in which crystals are precipitated from a supersaturated solution or formed from other sources. During crystallization, atoms or molecules arrange themselves into a well-defined, rigid crystal lattice to minimize energy.
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Recrystallization is a purification technique used to separate impurities from solid compounds. In this technique, no chemical reactions occur. Instead, it exploits physical properties only, specifically, the solubility differences between the desired compound and impurities, either at a single temperature or at different temperatures, and under other selected conditions. The solid-solution equilibrium (solubility equilibrium) of each component in the solution represents a binary phase...
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Unlike ionic or small covalent molecules, polymers do not form crystalline solids due to the diffusion limitations of their long-chain structures. However, polymers contain microscopic crystalline domains separated by amorphous domains.
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Related Experiment Video

Updated: Aug 8, 2025

Optimizing the Growth of Endothiapepsin Crystals for Serial Crystallography Experiments
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Optimizing the Growth of Endothiapepsin Crystals for Serial Crystallography Experiments

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Advanced crystallisation methods for small organic molecules.

J P Metherall1, R C Carroll2, S J Coles2

  • 1Newcastle University, Chemistry - School of Natural Environmental Sciences, Newcastle upon Tyne, NE1 7RU, UK. j.metherall@newcastle.ac.uk.

Chemical Society Reviews
|March 1, 2023
PubMed
Summary
This summary is machine-generated.

Advanced crystallization techniques are crucial for analyzing small organic molecules using single crystal X-ray diffraction (SCXRD). This review explores novel methods like host-guest inclusion and high-throughput crystallization to overcome sample preparation challenges.

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Area of Science:

  • Materials Science
  • Crystallography
  • Organic Chemistry

Background:

  • Spectroscopic techniques are insufficient for full characterization of molecular materials.
  • Single crystal X-ray diffraction (SCXRD) provides atomic-level structural elucidation, including absolute stereochemistry.
  • Obtaining high-quality crystals for SCXRD is a major bottleneck in sample preparation.

Purpose of the Study:

  • To review advanced methods for crystallizing small organic molecules for SCXRD.
  • To highlight recent developments in crystalline material sample preparation.
  • To guide researchers in selecting appropriate techniques for analytical challenges.

Main Methods:

  • Summary of classical crystallization methods.
  • Inclusion complexation using "crystalline sponges" and tetraaryladamantane chaperones.
  • High-throughput crystallization using "under-oil" approaches like microbatch and ENaCt.

Main Results:

  • Detailed review of inclusion complexation and high-throughput crystallization techniques.
  • Presentation of representative examples for each advanced method.
  • Discussion of the advantages and limitations of each technique.

Conclusions:

  • Advanced crystallization methods are essential for overcoming SCXRD sample preparation challenges.
  • Inclusion complexation and high-throughput methods offer novel solutions for obtaining suitable crystals.
  • Selection of the appropriate technique depends on the specific analytical requirements.