Journal
ACTA CRYSTALLOGRAPHICA SECTION C-STRUCTURAL CHEMISTRY
Volume 78, Issue -, Pages 332-+Publisher
INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S205322962200451X
Keywords
cocrystal; order-disorder phase transition; crystal structure; phase co-existence; hexamethylenetetramine; tridecanedioic acid
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Funding
- Conselho Nacional de Desenvolvimento Cienti PRIME [381033/2021-0, 432542/2018-3]
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The cocrystal hexamethylenetetramine-tridecanedioic acid was studied using single-crystal X-ray diffraction techniques at various temperatures during cooling and heating processes. Two crystalline phases were observed, separated by a temperature range of 290-340 K where phase co-existence occurred. Phase I was stable above 341 K and had an orthorhombic structure, while Phase II was stable below 290 K and had a monoclinic symmetry. The coexistence of phases was observed during both cooling and heating processes and appeared to be related to complex domain-growth dynamics within the crystal.
The cocrystal hexamethylenetetramine-tridecanedioic acid (1/1) (HMT-C13), C6H12N4 center dot C13H24O4, was investigated by single-crystal X-ray diffraction techniques at several temperatures during cooling and heating processes. Our results show the formation of two crystalline phases, separated by a large temperature phase co-existence between 290 and 340 K. Phase I, stable above 341 K, presents an orthorhombic structure described in the space group Bmmb, with one N-4(CH2)(6)center dot C13H22O4 adduct in its asymmetric unit. Phase II, stable below 290 K, presents a monoclinic symmetry described by the space group P2(1)/c, with two N-4(CH2)(6)center dot C13H22O4 adducts in its asymmetric unit. The phase co-existence is observed both upon cooling and heating, and seems to be related to a complex domain-growth dynamic within the crystal.
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