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Structure solution and refinement from powder or single-crystal diffraction data? Pros and cons: An example of the high-pressure β′-polymorph of glycine

Published online by Cambridge University Press:  29 February 2012

Nickolay A. Tumanov,
Elena V. Boldyreva and
Hans Ahsbahs
Nickolay A. Tumanov
Affiliation:
Novosibirsk State University, Novosibirsk, Russian Federation and Institute of Solid State Chemistry and Mechanochemistry, Siberian Branch of the Russian Academy of Sciences (SB RAS), Novosibirsk, Russian Federation
Elena V. Boldyreva
Affiliation:
Novosibirsk State University, Novosibirsk, Russian Federation and Institute of Solid State Chemistry and Mechanochemistry, Siberian Branch of the Russian Academy of Sciences (SB RAS), Novosibirsk, Russian Federation
Hans Ahsbahs
Affiliation:
Philipps-Universität Marburg, Marburg, Germany
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Abstract

The structure of a high-pressure polymorph of glycine (the β′-polymorph formed reversibly at 0.8 GPa from the β-polymorph) was determined from high-resolution X-ray powder diffraction data collected in situ in a diamond anvil cell at nine pressure points up to 2.6 GPa. X-ray powder diffraction study gave a structural model of at least the same quality as that obtained from a single-crystal diffraction experiment. The difference between the powder-diffraction and the single-crystal models is related to the orientation of the NH3-tails and the structure of the hydrogen-bonds network. The phase transition between the β- and β′-polymorphs is reversible and preserves a single crystal intact. No transformations were observed between the β-, α-, and β′-polymorphs on compression and decompression, although the α- and β′-polymorphs belong to the same space group (P21/c). The instability of the β- and γ-forms with pressure can be predicted easily when considering the densities of their structures versus pressure. The direction of the transformation (i.e., which of the high-pressure polymorphs is formed) is determined by structural filiation between the parent and the high-pressure phases because of the kinetic control of the transformations.

Keywords

amino acidhigh pressurepolymorphstructure solution from powder diffraction datagrid search techniquesimulated annealing

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Type
Technical Articles
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Powder Diffraction , Volume 23 , Issue 4 , December 2008, pp. 307 - 316
Copyright
Copyright © Cambridge University Press 2008

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