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A previously unknown cyclic alkanolamine and molecular ranking using the pair distribution function
Author(s) -
Gallo Gianpiero,
Terban Maxwell W.,
Moudrakovski Igor,
Huber Tatjana,
Etter Martin,
Ernst Martin,
Hinrichsen Bernd,
Dinnebier Robert E.
Publication year - 2021
Publication title -
acta crystallographica section b
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.604
H-Index - 33
ISSN - 2052-5206
DOI - 10.1107/s2052520621010088
Subject(s) - orthorhombic crystal system , chemistry , crystallography , powder diffraction , crystal structure , infrared spectroscopy , raman spectroscopy , rietveld refinement , computational chemistry , organic chemistry , physics , optics
A new six‐membered cyclic alkanolamine with chemical formula C 6 H 15 N 3 O 3 was synthesized by the reaction of glycolaldehyde with gaseous ammonia. The molecular structure, characterized by a hexagonal ring of alternating carbon and nitrogen atoms with three hydroxymethyl groups attached to the carbon atoms, could not be unambiguously determined by elemental analysis and 1 H/ 13 C/ 15 N NMR. The molecular structure and conformation were further determined using a combination of vibrational spectroscopy (IR and Raman) and real‐space pair distribution function (PDF) analysis. The crystal structure was determined ab initio from laboratory X‐ray powder diffraction (XRPD) with orthorhombic space group Ama 2 (No. 40) and unit‐cell parameters a = 12.1054 (2) Å, b = 13.5537 (2) Å and c = 5.20741 (8) Å. Consistent structure models could be obtained by symmetry‐independent PDF and PDF‐Rietveld co‐refinements. Independent local structure refinements indicate that the most likely deviations from the average structure consist of small tilting and translational distortions of hydrogen‐bonded molecular stacks. Thermal analysis (TG/DTA) and temperature‐dependent XRPD measurements were also performed to determine the thermal behavior.