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

Nikolay Tumanov, Elena V. Boldyreva, Hans Ahsbahs

Research output: Contribution to journalArticle

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 N H3 -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.

Original languageEnglish
Pages (from-to)307-316
Number of pages10
JournalPowder Diffraction
Volume23
Issue number4
DOIs
Publication statusPublished - 2008
Externally publishedYes

Fingerprint

glycine
Polymorphism
Powders
Glycine
Amino acids
Diffraction
Single crystals
single crystals
diffraction
pressure reduction
X ray powder diffraction
anvils
x rays
diamonds
Diamond
hydrogen bonds
high resolution
kinetics
Crystal orientation
cells

Keywords

  • Amino acid
  • Grid search technique
  • High pressure
  • Polymorph
  • Simulated annealing
  • Structure solution from powder diffraction data

Cite this

@article{4e0fbb036c604341bd41480048875e0f,
title = "Structure solution and refinement from powder or single-crystal diffraction data? Pros and cons: An example of the high-pressure Β′-polymorph of glycine",
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 N H3 -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 acid, Grid search technique, High pressure, Polymorph, Simulated annealing, Structure solution from powder diffraction data",
author = "Nikolay Tumanov and Boldyreva, {Elena V.} and Hans Ahsbahs",
year = "2008",
doi = "10.1154/1.2999248",
language = "English",
volume = "23",
pages = "307--316",
journal = "Powder Diffraction",
issn = "0885-7156",
publisher = "International Centre for Diffraction Data",
number = "4",

}

Structure solution and refinement from powder or single-crystal diffraction data? Pros and cons : An example of the high-pressure Β′-polymorph of glycine. / Tumanov, Nikolay; Boldyreva, Elena V.; Ahsbahs, Hans.

In: Powder Diffraction, Vol. 23, No. 4, 2008, p. 307-316.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Structure solution and refinement from powder or single-crystal diffraction data? Pros and cons

T2 - An example of the high-pressure Β′-polymorph of glycine

AU - Tumanov, Nikolay

AU - Boldyreva, Elena V.

AU - Ahsbahs, Hans

PY - 2008

Y1 - 2008

N2 - 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 N H3 -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.

AB - 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 N H3 -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.

KW - Amino acid

KW - Grid search technique

KW - High pressure

KW - Polymorph

KW - Simulated annealing

KW - Structure solution from powder diffraction data

UR - http://www.scopus.com/inward/record.url?scp=57249086407&partnerID=8YFLogxK

U2 - 10.1154/1.2999248

DO - 10.1154/1.2999248

M3 - Article

VL - 23

SP - 307

EP - 316

JO - Powder Diffraction

JF - Powder Diffraction

SN - 0885-7156

IS - 4

ER -