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Related Concept Videos

X-ray Crystallography02:18

X-ray Crystallography

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The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
Diffraction
Diffraction is the change in the direction of travel experienced by an electromagnetic wave when it encounters a physical barrier whose dimensions are comparable to those of the wavelength of the light. X-rays are electromagnetic radiation with wavelengths about as long as the distance between neighboring...
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Crystal Growth: Principles of Crystallization01:25

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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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X-ray Diffraction of Biological Samples01:10

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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
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Polymer Classification: Crystallinity01:21

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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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Factors Affecting Dissolution: Polymorphism, Amorphism and Pseudopolymorphism01:21

Factors Affecting Dissolution: Polymorphism, Amorphism and Pseudopolymorphism

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Polymorphism refers to the existence of a drug substance in multiple crystalline forms, known as polymorphs. Recently, this term has been expanded to include solvates (forms containing a solvent), amorphous forms (non-crystalline forms), and desolvated solvates (forms from which the solvent has been removed).
Some polymorphic crystals possess lower aqueous solubility than their amorphous counterparts, leading to incomplete absorption. For instance, the oral suspension of Chloramphenicol, which...
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On-Chip Crystallization and Large-Scale Serial Diffraction at Room Temperature
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Polymorph evolution during crystal growth studied by 3D electron diffraction.

Edward T Broadhurst1, Hongyi Xu2, Max T B Clabbers2

  • 1EaStCHEM School of Chemistry and Centre for Science at Extreme Conditions, The University of Edinburgh, King's Buildings, West Mains Road, Edinburgh EH9 3FJ, UK.

Iucrj
|January 18, 2020
PubMed
Summary
This summary is machine-generated.

3D electron diffraction (3DED) revealed glycine polymorphs during crystallization. The study tracked the formation and transformation of beta, alpha, and gamma glycine polymorphs, highlighting kinetic control over thermodynamic stability.

Keywords:
3DEDcryoTEMcrystallizationelectron diffractionglycinepolymorphism

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Area of Science:

  • Crystallography
  • Materials Science
  • Chemical Engineering

Background:

  • Glycine exists in multiple polymorphic forms under ambient conditions.
  • Understanding polymorph evolution is crucial for controlling material properties.
  • Previous methods limited real-time analysis of rapid crystallization processes.

Purpose of the Study:

  • To investigate the polymorph evolution during glycine crystallization from aqueous solution.
  • To determine the structures of glycine polymorphs using 3D electron diffraction.
  • To elucidate the kinetic and thermodynamic factors governing glycine polymorph formation.

Main Methods:

  • Utilized 3D electron diffraction (3DED) for in-situ analysis.
  • Collected continuous rotation electron diffraction data from glycine crystals.
  • Analyzed diffraction data from crystals with thicknesses around 100 nm.

Main Results:

  • Observed the formation of beta, alpha, and gamma glycine polymorphs.
  • The beta polymorph formed within 3 minutes, transforming to alpha within 4 minutes.
  • Kinetics favored the alpha polymorph over the thermodynamically stable gamma polymorph.
  • Successfully determined structures of beta and alpha polymorphs from rapid data acquisition.

Conclusions:

  • 3D electron diffraction enables rapid structural determination of transient crystalline phases.
  • Kinetics play a significant role in determining the dominant glycine polymorph, overriding thermodynamic stability in early stages.
  • The study provides insights into the dynamic crystallization pathways of pharmaceutical compounds.