A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole

Benmore, C. J.; Mou, Q.; Benmore, K. J.; Robinson, D. S.; Neuefeind, J.; Ilavsky, J.; Byrn, S. R.; Yarger, J. L.

doi:10.1016/j.tca.2016.10.004

A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole

Journal Article · Fri Oct 07 00:00:00 EDT 2016 · Thermochimica Acta

DOI:https://doi.org/10.1016/j.tca.2016.10.004· OSTI ID:1329117

Benmore, C. J. ^[1]; Mou, Q. ^[2]; Benmore, K. J. ^[3]; Robinson, D. S. ^[4]; Neuefeind, J. ^[5]; Ilavsky, J. ^[4]; Byrn, S. R. ^[6]; Yarger, J. L. ^[2]

Argonne National Lab. (ANL), Argonne, IL (United States); Arizona State Univ., Tempe, AZ (United States)
Arizona State Univ., Tempe, AZ (United States)
Univ. of Sheffield, Sheffield (United Kingdom)
Argonne National Lab. (ANL), Argonne, IL (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Purdue Univ., West Lafayette, IN (United States)

Small and wide angle high energy x-ray scattering experiments were performed upon cooling itraconazole from the melt to investigate the structural origin of the two transitions at ~74 °C and ~90 °C observed in DSC measurements. Slight changes to the main WAXS peak at Q = 1.33 ± 0.01 Å^–1 were observed at 90 °C and are found to be inter-molecular in nature, suggesting a liquid to isotropic transition. This finding was supported by complementary wide angle neutron scattering measurements. For temperatures at and below ~74 °C two strong rings appear in the 2D-SAXS pattern at Q = 0.24 ± 0.01 Å^–1 and 0.43 ± 0.01 Å^–1. The SAXS spectra were further deconvoluted into sharp and broad components. Lastly, a narrowing of the broad component is associated with only minor changes in the packing arrangements of the itraconazole molecules below ~90 °C, while the appearance of the sharp component below ~74 °C is attributed to the formation of a polydomain lamellar phase.

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1329117

Alternate ID(s):: OSTI ID: 1364641
OSTI ID: 22781970
OSTI ID: 1396821

Journal Information:: Thermochimica Acta, Journal Name: Thermochimica Acta Journal Issue: C Vol. 644; ISSN 0040-6031

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Vapor deposition of a nonmesogen prepares highly structured organic glasses Bishop, Camille; Thelen, Jacob L.; Gann, Eliot Proceedings of the National Academy of Sciences, Vol. 116, Issue 43 https://doi.org/10.1073/pnas.1908445116	journal	September 2019

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