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Structural Chemistry

, Volume 19, Issue 3, pp 517–525 | Cite as

Metergoline II: structure solution from powder diffraction data with preferred orientation and from microcrystal

  • Michal HušákEmail author
  • Alexandr Jegorov
  • Jiří Brus
  • Wouter van Beek
  • Philip Pattison
  • Mogens Christensen
  • Vincent Favre-Nicolin
  • Jaroslav Maixner
Original Research

Abstract

Metergoline is a dopamine agonist and serotonin antagonist used both in human and veterinary medicine. In addition to the previously known crystalline form, a new polymorph, which crystallizes from aqueous solution, was found. Since it was initially impossible to prepare a single crystal of quality suitable for single crystal X-ray diffraction measurements using a conventional laboratory source, the structure was solved from the powder diffraction data using synchrotron radiation. The structure determination also included solving the effects of preferred orientation. Characterization was simultaneously done by solid-state NMR spectroscopy. Finally, a small single crystal suitable for synchrotron diffraction was found after numerous tries. Crystal structure determination using this single crystal confirmed the powder-based solution. Comparison of information obtained by different experimental methods (powder diffraction, ssNMR, single crystal diffraction) was made.

Keywords

Crystal structure Metergoline Powder diffraction Preferred orientation 

Notes

Acknowledgments

This study was supported by the grant of the Czech Grant Agency (GAČR 203/07/0040), grant from the Grant Agency of the Academy of Sciences of the Czech Republic (IAA400500602) and by the research program MSM6046137302 of the Ministry of Education, Youth and Sports of the Czech Republic. We acknowledge the European Synchrotron Radiation Facility for provision of synchrotron radiation facilities and we would like to thank Denis Testemale for assistance in using beam line BM01B.

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Copyright information

© Springer Science+Business Media, LLC 2008

Authors and Affiliations

  • Michal Hušák
    • 1
    Email author
  • Alexandr Jegorov
    • 2
  • Jiří Brus
    • 3
  • Wouter van Beek
    • 4
    • 5
  • Philip Pattison
    • 4
    • 6
  • Mogens Christensen
    • 7
  • Vincent Favre-Nicolin
    • 8
    • 9
  • Jaroslav Maixner
    • 10
  1. 1.Department of Solid State ChemistryInstitute of Chemical Technology PraguePrague 6Czech Republic
  2. 2.IVAX Pharmaceuticals, Research and DevelopmentCeske BudejoviceCzech Republic
  3. 3.Institute of Macromolecular ChemistryCzech Academy of SciencesPrague 6Czech Republic
  4. 4.BM01B Beamline (Swiss-Norwegian), ESRFGrenoble CedexFrance
  5. 5.Dipartamento di Scienze e Tecnologie AvanzateUniversita` del Piemonte Orientale, and NanoSistemi ICAlessandriaItlay
  6. 6.Laboratoire de CristallographieEcole Polytechnique Federale de Lausanne, BSP – DorignyLausanneSwitzerland
  7. 7.Department of ChemistryAarhus UniversityAarhus CDenmark
  8. 8.Université Joseph FourierGrenoble Cedex 9France
  9. 9.CEA/DRFMC/SP2MGrenoble Cedex 9France
  10. 10.Central LaboratoriesInstitute of Chemical Technology PraguePrague 6Czech Republic

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