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Determination of two structures of the solvent 3-hydroxypropionitrile crystallized at low temperatures

Published online by Cambridge University Press:  01 March 2024

Pamela S. Whitfield Open the ORCID record for Pamela S. Whitfield [Opens in a new window] ,
Zouina Karkar  and
Yaser Abu-Lebdeh
Pamela S. Whitfield*
Affiliation:
Excelsus Structural Solutions (Swiss AG), Park Innovaare, Villigen, Switzerland National Research Council Canada, 1200 Montreal Road, Ottawa, Ontario, Canada K1A 0R6
Zouina Karkar
Affiliation:
National Research Council Canada, 1200 Montreal Road, Ottawa, Ontario, Canada K1A 0R6
Yaser Abu-Lebdeh
Affiliation:
National Research Council Canada, 1200 Montreal Road, Ottawa, Ontario, Canada K1A 0R6
*
a)Author to whom correspondence should be addressed. Electronic mail: whitfieldps1@gmail.com
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Abstract

The title compound, 3-hydroxypropionitrile, was crystallized repeatedly in situ inside a quartz capillary using a liquid nitrogen cryostream. The X-ray powder diffraction patterns obtained indicated the presence of two distinct crystalline phases. The cleanest datasets for each of the phases were used to solve the crystal structures via simulated annealing, followed by refinement and optimization via dispersion-corrected density functional theory (DFT) calculations, with a final Rietveld refinement against the experimental data. The two structures appear to correspond to those proposed in a 1960s literature vibrational spectroscopy paper, one being the more stable with a gauche molecular conformation and the second metastable phase more complex with mixed conformations. Dispersion-corrected DFT computation using lattice parameters for both phases obtained from a single 84 K dataset with co-existing phases shows the stable and metastable phases to differ in energy by less than 0.5 kJ mol−1. A comparison of experimental far infrared spectra published in the 1960s with those calculated from the proposed crystal structures provides some independent supporting evidence for the proposed structures.

Keywords

structure determinationorganic crystalsphase behaviornon-ambient diffraction
Type
Technical Article
Information
Powder Diffraction , Volume 39 , Issue 1 , March 2024 , pp. 1 - 11
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Copyright
Copyright © The Author(s), 2024. Published by Cambridge University Press on behalf of International Centre for Diffraction Data

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