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Determination of Crystal Structures01:29

Determination of Crystal Structures

In the late 1800s, the revelation that light extended beyond visible wavelengths led to the discovery of X-rays by Wilhelm Roentgen. Recognized as high-energy electromagnetic radiation with short wavelengths, X-rays prompted exploration into their interaction with crystals. Max von Laue proposed in 1912 that the periodic arrangement of atoms, ions, or molecules in crystals would cause them to diffract X-rays, a hypothesis confirmed through experiments with copper sulfate and zinc sulfide...
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Microcrystal Electron Diffraction of Small Molecules
09:48

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Published on: March 15, 2021

Crystal structure of indapamide determined from powered diffraction data.

M Smrkolj1, A Meden

  • 1Krka, Pharmaceutical Factory, Novo mesto, Slovenia. matej.smrkolj@krka.biz

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|February 8, 2007
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Summary

Indapamide, used for hypertension, exists as a non-stoichiometric hydrate with weakly bound water. Its crystal structure, solved from powder diffraction, explains water uptake and release without framework changes.

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Area of Science:

  • Crystallography
  • Materials Science
  • Pharmaceutical Science

Background:

  • Indapamide is a diuretic used to treat hypertension.
  • The European Pharmacopoeia allows up to 3 wt.% water in indapamide.
  • Previous analyses suggested indapamide forms a non-stoichiometric hydrate with weakly bound water.

Purpose of the Study:

  • To determine the unknown crystal structure of indapamide.
  • To confirm the hypothesis of indapamide existing as a non-stoichiometric hydrate.
  • To understand the hydration-dehydration behavior of indapamide.

Main Methods:

  • X-ray powder diffraction (XRPD) data analysis.
  • Structure solution and refinement from powder data.
  • Thermal analysis (TGA, DSC) and Dynamic Vapor Sorption (DVS) were used for characterization.

Main Results:

  • The crystal structure of indapamide was solved from laboratory XRPD data.
  • The structure confirmed the presence of water molecules in voids between indapamide molecules.
  • Weakly bound water molecules are reversibly incorporated/released without altering the main crystal framework.

Conclusions:

  • Indapamide exists as a non-stoichiometric hydrate.
  • The crystal structure explains the observed water content and its dependence on relative humidity.
  • Understanding hydration behavior is crucial for indapamide's pharmaceutical applications.