TY - JOUR
T1 - Dynamics and disorder
T2 - on the stability of pyrazinamide polymorphs
AU - Hoser, Anna Agnieszka
AU - Rekis, Toms
AU - Madsen, Anders Østergaard
N1 - Funding Information:
The following funding is acknowledged: Lundbeckfonden (grant No. R324-2019-2018). AAH would like to acknowledge funding from Foundation for Polish Science, Homing/2016–1/3 grant, POIR.04.04.00-00-1DAE/16.
PY - 2022
Y1 - 2022
N2 - This article focuses on the structure and relative stability of four pyrazinamide polymorphs. New single crystal X-ray diffraction data collected for all forms at 10 14;K and 122 14;K are presented. By combining periodic ab initio DFT calculations with normal-mode refinement against X-ray diffraction data, both enthalpic and entropic contributions to the free energy of all polymorphs are calculated. On the basis of the estimated free energies, the stability order of the polymorphs as a function of temperature and the corresponding solid state phase transition temperatures are anticipated. It can be concluded that the α and γ forms have higher vibrational entropy than that of the β and δ forms and therefore they are significantly more stabilized at higher temperatures. Due to the entropy which arises from the disorder in γ form, it overcomes form α and is the most stable form at temperatures above ∼500 14;K. Our findings are in qualitative agreement with the experimental calorimetry results.
AB - This article focuses on the structure and relative stability of four pyrazinamide polymorphs. New single crystal X-ray diffraction data collected for all forms at 10 14;K and 122 14;K are presented. By combining periodic ab initio DFT calculations with normal-mode refinement against X-ray diffraction data, both enthalpic and entropic contributions to the free energy of all polymorphs are calculated. On the basis of the estimated free energies, the stability order of the polymorphs as a function of temperature and the corresponding solid state phase transition temperatures are anticipated. It can be concluded that the α and γ forms have higher vibrational entropy than that of the β and δ forms and therefore they are significantly more stabilized at higher temperatures. Due to the entropy which arises from the disorder in γ form, it overcomes form α and is the most stable form at temperatures above ∼500 14;K. Our findings are in qualitative agreement with the experimental calorimetry results.
KW - Enantiotropism
KW - Normal-mode refinement
KW - Periodic density functional theory
KW - Polymorphism
KW - Quantum crystallography
U2 - 10.1107/S2052520622004577
DO - 10.1107/S2052520622004577
M3 - Journal article
C2 - 35695115
AN - SCOPUS:85131852942
VL - 78
SP - 416
EP - 424
JO - Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
JF - Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
SN - 2052-5192
ER -