Ab initio structure determination of the low-temperature phase of succinonitrile from laboratory X-ray powder diffraction data-coping with potential poor powder quality using DFT ab initio methods

P. S. Whitfield, Y. Le Page, Ali Abouimrane, I. J. Davidson

Research output: Contribution to journalArticle

11 Citations (Scopus)

Abstract

Without experimental or predicted literature crystal structures for succinonitrile at low temperature, structure solution was attempted from powder diffraction data taken at 173 and 90 K from a solid sample. Its room-temperature plastic-crystal state makes production of a sample with good particle statistics and random orientation almost impossible. Combining constrained models, simulated annealing, and careful application of second-order spherical harmonic corrections nevertheless produced viable-looking structures at 90 and 173 K, yielding two distinct structure models with the same projection down c. VASP optimization of atom coordinates in the experimental cell agreed well with the 90 K model but poorly with the model derived from the 173 K data. The refined 90 K structure changed little on optimization and fitted all datasets from 85 to 225 K. Plots of cell data, torsion angles, and isotropic displacement parameters against temperature suggest possible phase transitions around 100, 120, and 180 K. Cell data at 90 K: monoclinic P21/a, a=9.0851 (5) Å, b=8.5617 (5) Å, c=5.8343 (3) Å, Β=79.295 (2) °, and Z=4. Succinonitrile has gauche conformation, in agreement with literature spectroscopy data.

Original languageEnglish
Pages (from-to)292-299
Number of pages8
JournalPowder Diffraction
Volume23
Issue number4
DOIs
Publication statusPublished - 2008
Externally publishedYes

Fingerprint

succinonitrile
Discrete Fourier transforms
Powders
X ray powder diffraction
diffraction
x rays
cells
Model structures
Simulated annealing
Torsional stress
Temperature
optimization
Conformations
simulated annealing
spherical harmonics
Crystal structure
Phase transitions
Statistics
Spectroscopy
Plastics

Keywords

  • DFT methods
  • Nonambient diffraction
  • Simulated annealing
  • Structure solution

ASJC Scopus subject areas

  • Materials Science(all)
  • Condensed Matter Physics
  • Instrumentation
  • Radiation

Cite this

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abstract = "Without experimental or predicted literature crystal structures for succinonitrile at low temperature, structure solution was attempted from powder diffraction data taken at 173 and 90 K from a solid sample. Its room-temperature plastic-crystal state makes production of a sample with good particle statistics and random orientation almost impossible. Combining constrained models, simulated annealing, and careful application of second-order spherical harmonic corrections nevertheless produced viable-looking structures at 90 and 173 K, yielding two distinct structure models with the same projection down c. VASP optimization of atom coordinates in the experimental cell agreed well with the 90 K model but poorly with the model derived from the 173 K data. The refined 90 K structure changed little on optimization and fitted all datasets from 85 to 225 K. Plots of cell data, torsion angles, and isotropic displacement parameters against temperature suggest possible phase transitions around 100, 120, and 180 K. Cell data at 90 K: monoclinic P21/a, a=9.0851 (5) {\AA}, b=8.5617 (5) {\AA}, c=5.8343 (3) {\AA}, Β=79.295 (2) °, and Z=4. Succinonitrile has gauche conformation, in agreement with literature spectroscopy data.",
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T1 - Ab initio structure determination of the low-temperature phase of succinonitrile from laboratory X-ray powder diffraction data-coping with potential poor powder quality using DFT ab initio methods

AU - Whitfield, P. S.

AU - Le Page, Y.

AU - Abouimrane, Ali

AU - Davidson, I. J.

PY - 2008

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N2 - Without experimental or predicted literature crystal structures for succinonitrile at low temperature, structure solution was attempted from powder diffraction data taken at 173 and 90 K from a solid sample. Its room-temperature plastic-crystal state makes production of a sample with good particle statistics and random orientation almost impossible. Combining constrained models, simulated annealing, and careful application of second-order spherical harmonic corrections nevertheless produced viable-looking structures at 90 and 173 K, yielding two distinct structure models with the same projection down c. VASP optimization of atom coordinates in the experimental cell agreed well with the 90 K model but poorly with the model derived from the 173 K data. The refined 90 K structure changed little on optimization and fitted all datasets from 85 to 225 K. Plots of cell data, torsion angles, and isotropic displacement parameters against temperature suggest possible phase transitions around 100, 120, and 180 K. Cell data at 90 K: monoclinic P21/a, a=9.0851 (5) Å, b=8.5617 (5) Å, c=5.8343 (3) Å, Β=79.295 (2) °, and Z=4. Succinonitrile has gauche conformation, in agreement with literature spectroscopy data.

AB - Without experimental or predicted literature crystal structures for succinonitrile at low temperature, structure solution was attempted from powder diffraction data taken at 173 and 90 K from a solid sample. Its room-temperature plastic-crystal state makes production of a sample with good particle statistics and random orientation almost impossible. Combining constrained models, simulated annealing, and careful application of second-order spherical harmonic corrections nevertheless produced viable-looking structures at 90 and 173 K, yielding two distinct structure models with the same projection down c. VASP optimization of atom coordinates in the experimental cell agreed well with the 90 K model but poorly with the model derived from the 173 K data. The refined 90 K structure changed little on optimization and fitted all datasets from 85 to 225 K. Plots of cell data, torsion angles, and isotropic displacement parameters against temperature suggest possible phase transitions around 100, 120, and 180 K. Cell data at 90 K: monoclinic P21/a, a=9.0851 (5) Å, b=8.5617 (5) Å, c=5.8343 (3) Å, Β=79.295 (2) °, and Z=4. Succinonitrile has gauche conformation, in agreement with literature spectroscopy data.

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KW - Simulated annealing

KW - Structure solution

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