Low-temperature phase transition in glycine–glutaric acid co-crystals studied by single-crystal X-ray diffraction, Raman spectroscopy and differential scanning calorimetry

2012 ◽  
Vol 68 (3) ◽  
pp. 287-296 ◽  
Author(s):  
Boris A. Zakharov ◽  
Evgeniy A. Losev ◽  
Boris A. Kolesov ◽  
Valeri A. Drebushchak ◽  
Elena V. Boldyreva
Keyword(s):  
Phase Transition ◽  
Differential Scanning Calorimetry ◽  
Raman Spectroscopy ◽  
Single Crystal ◽  
Glutaric Acid ◽  
Group Symmetry ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

The occurrence of a first-order reversible phase transition in glycine–glutaric acid co-crystals at 220–230 K has been confirmed by three different techniques – single-crystal X-ray diffraction, polarized Raman spectroscopy and differential scanning calorimetry. The most interesting feature of this phase transition is that every second glutaric acid molecule changes its conformation, and this fact results in the space-group symmetry change from P21/c to P\bar 1. The topology of the hydrogen-bonded motifs remains almost the same and hydrogen bonds do not switch to other atoms, although the hydrogen bond lengths do change and some of the bonds become inequivalent.

The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]

2019 ◽  
Vol 75 (6) ◽  
pp. 1144-1151
Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
Room Temperature ◽  
Variable Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Hybrid Compound ◽  
Space Group ◽  
X Ray

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.

New crystal structures in the realm of 5,5′-azotetrazolates

2015 ◽  
Vol 70 (2) ◽  
pp. 125-134 ◽  
Author(s):  
Martin Lampl ◽  
Gerhard Laus ◽  
Doris E. Braun ◽  
Volker Kahlenberg ◽  
Klaus Wurst ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Single Crystal ◽  
Crystal Structures ◽  
Organic Cations ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Diffraction Patterns

AbstractThe preparation of six new 5,5′-azotetrazolates with organic cations is reported. Differential scanning calorimetry of all compounds showed exothermic decompositions. The crystal structures of the six 5,5′-azotetrazolates were determined by single-crystal X-ray diffraction analyses. The phase purities of the bulk samples were confirmed by Pawley fits of the experimental and calculated powder X-ray diffraction patterns.

Differential scanning calorimetry and X-ray diffraction studies of a series of synthetic β-D-galactosyl diacylglycerols

1991 ◽  
Vol 69 (12) ◽  
pp. 863-867 ◽  
Author(s):  
D. A. Mannock ◽  
R. N. McElhaney
Keyword(s):  
Phase Transition ◽  
Differential Scanning Calorimetry ◽  
Phase Behaviour ◽  
Lipid Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Phase Transition Temperatures ◽  
Bonding Properties ◽  
Lower Temperature

We have investigated the physical properties of a homologous series of synthetic, saturated 1,2-di-O-acyl-3-O-(β-D-galactopyranosyl)-sn-glycerols using calorimetry and X-ray diffraction. Unannealed aqueous dispersions of these compounds exhibit a lower temperature, moderately energetic, chain-melting (Lβ/Lα phase transition and a higher temperature, weakly energetic, bilayer/nonbilayer phase transition. On annealing below the Lβ/Lα phase transition, the Lβ phase converts to an LC phase, which may undergo a highly energetic LC/Lα or LC/HII phase transition at very high temperatures on reheating. The temperatures of these phase transitions are higher than those seen in the corresponding α- and β-D-glucosyl diacylglycerols. However, the Lβ/Lα and bilayer/nonbilayer phase transition temperatures of the β-D-galactosyl diacylglycerols are lower than those of the corresponding diacyl phosphatidylethanolamines. These observations are discussed in terms of the hydration and hydrogen bonding properties of their respective headgroups.Key words: differential scanning calorimetry, low-angle x-ray diffraction, glycolipids, galactolipids, lipid phase behaviour.

scholarly journals Phase Transition and Melt-Recrystallization Behavior of Poly(Butylene Adipate) Investigated by Simultaneous Measurements of Wide-Angle X-Ray Diffraction (WAXD) and Differential Scanning Calorimetry (DSC)

Polymers ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 75
Author(s):  
Mengfan Wang ◽  
Weiyu Cao
Keyword(s):  
Phase Transition ◽  
Differential Scanning Calorimetry ◽  
Heating Process ◽  
Wide Angle ◽  
Melt Crystallization ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Β Phase ◽  
Simultaneous Measurements

Simultaneous measurements of wide-angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC) were carried out to investigate the phase transition and melting behaviors of poly(butylene adipate) (PBA). Thermal expansion changes along the a and b axes of the β form unit cell are different from each other during the heating process. At the beginning of the β to αH (high-temperature α phase) phase transition, the β phase melts very fast, while the recrystallization of the αH phase is delayed and slowed. With the further increment of the temperature, the melting rate of the β phase slows down, while the recrystallization of the αH phase accelerates. The diffraction peak intensity ratios of the β(020):β(110) and αH(020):αH(110) diffraction peaks during the first heating process have similar value. However, the above value is different from the value of α(020):α(110) during the following melt-crystallization process. This difference comes from the different orientations of the crystal lattices of the α and αH(β) crystals to the substrate plane, which indicates that the αH phase inherits the orientation of the β phase during phase transition and the orientation of αH form crystals is different from the α form crystals that crystallized from the melt.

Characterization of New Cocrystals by Raman Spectroscopy, Powder X-ray Diffraction, Differential Scanning Calorimetry, and Transmission Raman Spectroscopy

2010 ◽  
Vol 10 (5) ◽  
pp. 2360-2371 ◽  
Author(s):  
M. A. Elbagerma ◽  
H. G. M. Edwards ◽  
T. Munshi ◽  
M. D. Hargreaves ◽  
Pavel Matousek ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Raman Spectroscopy ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Transmission Raman

High-temperature single-crystal X-ray diffraction study of tetragonal and cubic perovskite-type PbTiO3phases

2016 ◽  
Vol 72 (3) ◽  
pp. 381-388 ◽  
Author(s):  
Akira Yoshiasa ◽  
Tomotaka Nakatani ◽  
Akihiko Nakatsuka ◽  
Maki Okube ◽  
Kazumasa Sugiyama ◽  
...  
Keyword(s):  
Phase Transition ◽  
High Temperature ◽  
Single Crystal ◽  
Diffraction Study ◽  
Relative Displacement ◽  
High Temperature Phase ◽  
Cubic Phase ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
X Ray

A high-temperature single-crystal X-ray diffraction study of a synthetic PbTiO3perovskite was carried out over the wide temperature range 298–928 K. A transition from a tetragonal (P4mm) to a cubic (Pm \bar 3 m) phase has been revealed near 753 K. In the non-centrosymmetricP4mmsymmetry group, the difference in relative displacement between Pb and O along thec-axis is much larger than that between Ti and O. The Pb and Ti cations contribute sufficiently to polarization being shifted in the opposite direction compared with the shift of O atoms. Deviation from the linear changes in Debye–Waller factors and bonding distances in the tetragonal phases can be interpreted as a precursor phenomenon before the phase transition. Disturbance of the temperature factorUeqfor O is observed in the vicinity of the transition point, whileUeqvalues for Pb and Ti are continuously changing with increasing temperature. The O site includes the clear configurational disorder in the cubic phase. The polar local positional distortions remain in the cubic phase and are regarded as the cause of the paraelectricity. Estimated values of the Debye temperature ΘDfor Pb and Ti are 154 and 467 K in the tetragonal phase and decrease 22% in the high-temperature phase. Effective potentials for Pb and Ti change significantly and become soft after the phase transition.

scholarly journals Inorganic Anion Regulates the Phase Transition in Two Organic Cation Salts Containing [(4-Nitroanilinium)(18-crown-6)]+ Supramolecules

2017 ◽  
Author(s):  
Yuan Chen ◽  
Yang Liu ◽  
Binzu Gao ◽  
Chuli Zhu ◽  
Zunqi Liu
Keyword(s):  
Phase Transition ◽  
Phase Transitions ◽  
Variable Temperature ◽  
Structural Phase ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Space Group ◽  
X Ray

Two novel inorganic–organic hybrid supramolecular assemblies, namely, (4-HNA)(18-crown-6)(HSO4) (1) and (4-HNA)2(18-crown-6)2(PF6)2(CH3OH) (2) (4-HNA = 4-nitroanilinium), were synthesized and characterized by infrared spectroscopy, single X-ray diffraction, differential scanning calorimetry (DSC), and temperature-dependent dielectric measurements. The two compounds underwent reversible phase transitions at about 255 K and 265 K, respectively. These phase transitions were revealed and confirmed by the thermal anomalies in DSC measurements and abrupt dielectric anomalies during heating. The phase transition may have originated from the [(4-HNA)(18-crown-6)]+ supramolecular cation. The inorganic anions tuned the crystal packings and thus influenced the phase-transition points and types. The variable-temperature X-ray diffraction data for crystal 1 revealed the occurrence of a phase transition in the high-temperature phase with the space group of P21/c and in the low-temperature phase with the space group of P21/n. Crystal 2 exhibited the same space group P21/c at different temperatures. The results indicated that crystals 1 and 2 both underwent an iso-structural phase transition.

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