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  4. Structural changes of hexamethylenetetramine and undecanedioic acid co-crystal (HMT-C11) as a function of the temperature
 
research article

Structural changes of hexamethylenetetramine and undecanedioic acid co-crystal (HMT-C11) as a function of the temperature

Pinheiro, C. B.
•
Gardon, M.
•
Chapuis, G.  
2003
Acta Crystallographica Section B-Structural Science

HMT-C11 belongs to the family of adducts formed by the cocrystallization of N-4(CH2)(6) molecules ( hexamethylenetetramine or HMT) and aliphatic dicarboxylic acids HOOC(CH2)(n-2)COOH with 5 less than or equal to n less than or equal to 13 (Cn). The adducts exhibit a layered structure in which the packing between HMT and Cn is determined by strong hydrogen bonds. The compounds in this family studied so far present thermotropic structural phase transitions and, depending on the chain length, disordered, twinned and modulated phases. The structure refinement of HMT-C11 based on X-ray diffraction experiments indicates three distinct phases from the melting point down to liquid nitrogen temperature: phase I is not crystalline; phase II is disordered ( stacking fault) and its average structure is described in space group Bmmb; phase III is partially disordered and its symmetry is P2(1)/c. The systematic study of the structure evolution of phase III upon cooling revealed that the disorder has a dynamic character (anharmonicity). The main structural change observed from 293 K down to 93 K is the increase of the tilting angle of the C11 chains relative to the layer plane and the rotation of the HMT molecules. Both HMT and C11 behave like rigid bodies in the temperature range investigated. The quality of the refinements leads to a conclusive model for the O-H...N hydrogen bonds linking HMT and C11.

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Type
research article
DOI
10.1107/S0108768103007754
Author(s)
Pinheiro, C. B.
Gardon, M.
Chapuis, G.  
Date Issued

2003

Published in
Acta Crystallographica Section B-Structural Science
Volume

59

Start page

416

End page

427

Subjects

neutron-diffraction

•

azelaic acid

•

sebacic acid

•

refinement

•

phase

Note

Times Cited: 0 Article English Cited References Count: 36 682jb Part 3

Editorial or Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
LCR  
Available on Infoscience
March 7, 2006
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/227347
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