scholarly journals The impact of pressure on β-Cyclodextrin·acetaminophen inclusion complexes

2014 ◽  
Vol 70 (a1) ◽  
pp. C264-C264 ◽  
Author(s):  
Sofiane Saouane ◽  
Wolfgang Morgenroth ◽  
Hanns-Peter Liermann ◽  
Carsten Paulmann ◽  
Francesca Fabbiani
Keyword(s):  
High Pressure ◽  
Inclusion Complex ◽  
Aqueous Solubility ◽  
Crystal Form ◽  
Model Systems ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
The Impact

Cyclodextrins (CDs) have attracted considerable interest as model systems in supramolecular host-guest chemistry. They are described as hollow truncated cones with a hydrophilic outer surface and a nonpolar inner cavity suitable for small molecules' encapsulation.[1] By virtue of their character, CDs are used as excipients to improve the aqueous solubility of active pharmaceutical ingredients (APIs). High-pressure crystallisation techniques have been established as a suitable tool for exploring the phenomenon of polymorphism and solvate formation of pharmaceutical compounds throughout numerous examples reported in the literature.[2] Thus, exploring the inclusion-complex formation and the polymorphic behaviour of CDs with APIs at high pressure would be an interesting extension of the technique. The present work describes the attempt of an in-situ crystallisation of β-CD·acetaminophen inclusion complex and compression studies of the known β-CD·acetaminophen complex[3] in different crystallisation media at pressures up to 1.0 GPa. A new high-pressure crystal form observed at 0.8 GPa as well as unexpected results are presented herein. The crystals have been characterised by means of polarised optical microscopy, Raman spectroscopy and single-crystal X-ray diffraction using both home and synchrotron sources.

scholarly journals Pressure-induced Jahn-Teller Switch in the Homoleptic Hybrid Perovskite [(CH3)2NH2]Cu(HCOO)3: Orbital Reordering by Unconventional Degrees of Freedom

2021 ◽  
Author(s):  
Rebecca Scatena ◽  
Michał Andrzejewski ◽  
Roger D Johnson ◽  
Piero Macchi
Keyword(s):  
Phase Transition ◽  
High Pressure ◽  
Coordination Polymer ◽  
Degrees Of Freedom ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hybrid Perovskite ◽  
Jahn Teller

Through in-situ, high-pressure x-ray diffraction experiments we have shown that the homoleptic perovskite-like coordination polymer [(CH3)2NH2]Cu(HCOO)3 undergoes a pressure-induced orbital reordering phase transition above 5.20 GPa. This transition is distinct...

PHASE TRANSITION IN LAYERED PEROVSKITE LIKE MANGANATE Ca3Mn2O7 UNDER HIGH PRESSURE

2001 ◽  
Vol 15 (18) ◽  
pp. 2491-2497 ◽  
Author(s):  
J. L. ZHU ◽  
L. C. CHEN ◽  
R. C. YU ◽  
F. Y. LI ◽  
J. LIU ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Diamond Anvil Cell ◽  
The Other ◽  
Layered Perovskite ◽  
X Ray Diffraction ◽  
Two Phase ◽  
X Ray ◽  
Diamond Anvil

In situ high pressure energy dispersive X-ray diffraction measurements on layered perovskite-like manganate Ca 3 Mn 2 O 7 under pressures up to 35 GPa have been performed by using diamond anvil cell with synchrotron radiation. The results show that the structure of layered perovskite-like manganate Ca 3 Mn 2 O 7 is unstable under pressure due to the easy compression of NaCl-type blocks. The structure of Ca 3 Mn 2 O 7 underwent two phase transitions under pressures in the range of 0~35 GPa. One was at about 1.3 GPa with the crystal structure changing from tetragonal to orthorhombic. The other was at about 9.5 GPa with the crystal structure changing from orthorhombic back to another tetragonal.

scholarly journals In situ observation of phase changes of a silica-supported cobalt catalyst for the Fischer–Tropsch process by the development of a synchrotron-compatible in situ/operando powder X-ray diffraction cell

2018 ◽  
Vol 25 (6) ◽  
pp. 1673-1682 ◽  
Author(s):  
Adam S. Hoffman ◽  
Joseph A. Singh ◽  
Stacey F. Bent ◽  
Simon R. Bare
Keyword(s):  
High Pressure ◽  
Elevated Pressure ◽  
Phase Changes ◽  
In Situ Observation ◽  
X Ray Diffraction ◽  
Fischer Tropsch ◽  
X Ray ◽  
And Performance ◽  
Co Nanoparticles

In situ characterization of catalysts gives direct insight into the working state of the material. Here, the design and performance characteristics of a universal in situ synchrotron-compatible X-ray diffraction cell capable of operation at high temperature and high pressure, 1373 K, and 35 bar, respectively, are reported. Its performance is demonstrated by characterizing a cobalt-based catalyst used in a prototypical high-pressure catalytic reaction, the Fischer–Tropsch synthesis, using X-ray diffraction. Cobalt nanoparticles supported on silica were studied in situ during Fischer–Tropsch catalysis using syngas, H2 and CO, at 723 K and 20 bar. Post reaction, the Co nanoparticles were carburized at elevated pressure, demonstrating an increased rate of carburization compared with atmospheric studies.

scholarly journals Lanthanoid Complexes Supported by Retro-Claisen Condensation Products of β-Triketonates

2018 ◽  
Author(s):  
Laura Abad Galán ◽  
Alexandre N. Sobolev ◽  
Eli Zysman-Colman ◽  
Mark Ogden ◽  
Massimiliano Massi
Keyword(s):  
Chelating Ligands ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Claisen Condensation ◽  
X Ray ◽  
Condensation Products ◽  
Complexation Reactions ◽  
The Impact ◽  
Low Solubility

<i>β</i>-Triketonates have been recently used as chelating ligands for lanthanoid ions, presenting unique structures varying from polynuclear assemblies to polymers. In an effort to overcome low solubility of the complexes of tribenzoylmethane, four <i>β</i>-triketones with higher lipophilicity were synthesised. Complexation reactions were performed for each of these molecules using different alkaline bases in alcoholic media. X-ray diffraction studies suggested that the ligands were undergoing decomposition under the reaction conditions. This is proposed to be caused by <i>in situ</i>retro-Claisen condensation reactions, consistent with two examples that have been reported previously. The lability of the lanthanoid cations in the presence of a varying set of potential ligands gave rise to structures where one, two, or three of the molecules involved in the retro-Claisen condensationreaction were linked to the lanthanoid centres. These results, along with measurements of ligand decomposition in the presence of base alone, suggest that using solvents of lower polarity will mimimise the impact of the retro-Claisen condensation in these complexes. <br>

scholarly journals In-situ high-pressure x-ray diffraction study of zinc ferrite nanoparticles

2016 ◽  
Vol 56 ◽  
pp. 68-72 ◽  
Author(s):  
S. Ferrari ◽  
R.S. Kumar ◽  
F. Grinblat ◽  
J.C. Aphesteguy ◽  
F.D. Saccone ◽  
...  
Keyword(s):  
High Pressure ◽  
Diffraction Study ◽  
Zinc Ferrite ◽  
Ferrite Nanoparticles ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals In Situ High-Pressure X-ray Diffraction and Raman Spectroscopy Study of Ti3C2Tx MXene

2018 ◽  
Vol 13 (1) ◽  
Author(s):  
Luxi Zhang ◽  
Weitao Su ◽  
Yanwei Huang ◽  
He Li ◽  
Li Fu ◽  
...  
Keyword(s):  
Raman Spectroscopy ◽  
High Pressure ◽  
Spectroscopy Study ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals The Viscosity and Atomic Structure of Volatile-Bearing Melilititic Melts at High Pressure and Temperature and the Transport of Deep Carbon

Minerals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 267 ◽  
Author(s):  
Vincenzo Stagno ◽  
Veronica Stopponi ◽  
Yoshio Kono ◽  
Annalisa D’Arco ◽  
Stefano Lupi ◽  
...  
Keyword(s):  
Experimental Data ◽  
High Pressure ◽  
Atomic Structure ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
High Pressure And Temperature ◽  
X Ray ◽  
Falling Sphere ◽  
Basaltic Melts

Understanding the viscosity of mantle-derived magmas is needed to model their migration mechanisms and ascent rate from the source rock to the surface. High pressure–temperature experimental data are now available on the viscosity of synthetic melts, pure carbonatitic to carbonate–silicate compositions, anhydrous basalts, dacites and rhyolites. However, the viscosity of volatile-bearing melilititic melts, among the most plausible carriers of deep carbon, has not been investigated. In this study, we experimentally determined the viscosity of synthetic liquids with ~31 and ~39 wt% SiO2, 1.60 and 1.42 wt% CO2 and 5.7 and 1 wt% H2O, respectively, at pressures from 1 to 4.7 GPa and temperatures between 1265 and 1755 °C, using the falling-sphere technique combined with in situ X-ray radiography. Our results show viscosities between 0.1044 and 2.1221 Pa·s, with a clear dependence on temperature and SiO2 content. The atomic structure of both melt compositions was also determined at high pressure and temperature, using in situ multi-angle energy-dispersive X-ray diffraction supported by ex situ microFTIR and microRaman spectroscopic measurements. Our results yield evidence that the T–T and T–O (T = Si,Al) interatomic distances of ultrabasic melts are higher than those for basaltic melts known from similar recent studies. Based on our experimental data, melilititic melts are expected to migrate at a rate ~from 2 to 57 km·yr−1 in the present-day or the Archaean mantle, respectively.

Sign in / Sign up

Export Citation Format

Share Document