Pressure-frozen 1,2,3-trichloropropane

2006 ◽  
Vol 62 (6) ◽  
pp. 1071-1077 ◽  
Author(s):  
Marcin Podsiadło ◽  
Andrzej Katrusiak
Keyword(s):  
Molecular Conformation ◽  
Elevated Pressure ◽  
Aliphatic Chain ◽  
X Ray Diffraction ◽  
Molecular Arrangement ◽  
Intermolecular Contacts ◽  
Diamond Anvil ◽  
Van Der Waals Radii ◽  
Cl Atoms

The structure of 1,2,3-trichloropropane, ClCH2CHClCH2Cl, in-situ crystallized in a diamond–anvil cell, has been determined by single-crystal X-ray diffraction at 0.28 and 0.35 GPa. A melting point at 295 K and 0.22 GPa has been determined. The molecular conformation of aliphatic chain and terminal Cl atoms is approximately C 2 symmetric. Of the intermolecular contacts, the tightest are the Cl...Cl and then the Cl...H contacts, whereas the H...H distances are considerably longer than the sum of the van der Waals radii and leave narrow voids in the structure. The elevated pressure reduces the H...H separations but hardly affects the Cl...Cl distances. The crystal growth rates, compression and types of intermolecular interactions in the structures can be correlated with the directions of the Cl...Cl contacts, which can be considered the main motif responsible for the molecular arrangement in the structure.

In situ high-pressure crystallization and compression of halogen contacts in dichloromethane

2005 ◽  
Vol 61 (5) ◽  
pp. 595-600 ◽  
Author(s):  
Marcin Podsiadło ◽  
Kamil Dziubek ◽  
Andrzej Katrusiak
Keyword(s):  
Diamond Anvil Cell ◽  
Crystal Habit ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts ◽  
Diamond Anvil ◽  
Pressure Crystallization ◽  
Low Temperature Phase

The structure of dichloromethane, CH2Cl2, crystallized in situ in a diamond–anvil cell, has been determined by single-crystal X-ray diffraction at 1.33 and 1.63 GPa. The pressure-frozen crystal was determined to be orthorhombic, with the space group Pbcn, and isostructural with the low-temperature phase at 0.1 MPa. The CH2Cl2 molecules are located on one set of crystallographic twofold axes. The characteristics determined for the CH2Cl2 crystal (compression of the close intermolecular contacts, molecular association and the crystal habit of dichloromethane) suggest that the crystal cohesion forces are dominated by H...Cl interactions rather than by Cl...Cl attractions.

scholarly journals Crystal design by CH...N and N...N interactions: high-pressure structures of high-nitrogen-content azido-triazolopyridazines compounds

2020 ◽  
Vol 76 (6) ◽  
pp. 1136-1142
Author(s):  
Anna Olejniczak ◽  
Anna Katrusiak ◽  
Marcin Podsiadło ◽  
Andrzej Katrusiak
Keyword(s):  
High Pressure ◽  
Nitrogen Content ◽  
High Nitrogen Content ◽  
X Ray Diffraction ◽  
High Nitrogen ◽  
Methyl Derivative ◽  
Intermolecular Contacts ◽  
Diamond Anvil ◽  
Crystal Design

High-nitrogen-content compounds 6-azido-1,2,4-triazolo[4,3-b]pyridazine (C5H3N7) and its 3-methyl derivative (C6H5N7) have been in situ crystallized in a diamond-anvil cell and their structures determined by single-crystal X-ray diffraction. Under ambient and high-pressure conditions the crystallizations yield the same phases: the C5H3N7 anhydrate and C6H5N7 hydrated clathrate. In both the structures there are clearly distinguished regions of short CH...N and N...N intermolecular contacts, the latter involving exclusively the azide groups. High pressure initially increases the contents of water in the channel pores of the clathrate.

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.

In situ synchrotron X-ray diffraction with laser-heated diamond anvil cells study of Pt up to 95 GPa and 3150 K

RSC Advances ◽  
2015 ◽  
Vol 5 (19) ◽  
pp. 14603-14609 ◽  
Author(s):  
Xiaoli Huang ◽  
Fangfei Li ◽  
Qiang Zhou ◽  
Gang Wu ◽  
Yanping Huang ◽  
...  
Keyword(s):  
X Ray Diffraction ◽  
Diamond Anvil Cells ◽  
X Ray ◽  
Diamond Anvil ◽  
Laser Heated

In situ synchrotron X-ray diffraction with laser-heated diamond anvil cells study the EOS of Pt.

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.

Construction of laser-heated diamond anvil cell system for in situ x-ray diffraction study at SPring-8

2001 ◽  
Vol 72 (2) ◽  
pp. 1289 ◽  
Author(s):  
Tetsu Watanuki ◽  
Osamu Shimomura ◽  
Takehiko Yagi ◽  
Tadashi Kondo ◽  
Maiko Isshiki
Keyword(s):  
Diffraction Study ◽  
Diamond Anvil Cell ◽  
Cell System ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diamond Anvil ◽  
Laser Heated

scholarly journals Lab in a DAC – high-pressure crystal chemistry in a diamond-anvil cell

2019 ◽  
Vol 75 (6) ◽  
pp. 918-926 ◽  
Author(s):  
Andrzej Katrusiak
Keyword(s):  
High Pressure ◽  
Diamond Anvil Cell ◽  
Ambient Pressure ◽  
Elevated Pressure ◽  
Sample Volume ◽  
Chemical Research ◽  
New Era ◽  
New Information ◽  
Intermolecular Contacts ◽  
Diamond Anvil

The diamond-anvil cell (DAC) was invented 60 years ago, ushering in a new era for material sciences, extending research into the dimension of pressure. Most structural determinations and chemical research have been conducted at ambient pressure, i.e. the atmospheric pressure on Earth. However, modern experimental techniques are capable of generating pressure and temperature higher than those at the centre of Earth. Such extreme conditions can be used for obtaining unprecedented chemical compounds, but, most importantly, all fundamental phenomena can be viewed and understood from a broader perspective. This knowledge, in turn, is necessary for designing new generations of materials and applications, for example in the pharmaceutical industry or for obtaining super-hard materials. The high-pressure chambers in the DAC are already used for a considerable variety of experiments, such as chemical reactions, crystallizations, measurements of electric, dielectric and magnetic properties, transformations of biological materials as well as experiments on living tissue. Undoubtedly, more applications involving elevated pressure will follow. High-pressure methods become increasingly attractive, because they can reduce the sample volume and compress the intermolecular contacts to values unattainable by other methods, many times stronger than at low temperature. The compressed materials reveal new information about intermolecular interactions and new phases of single- and multi-component compounds can be obtained. At the same time, high-pressure techniques, and particularly those of X-ray diffraction using the DAC, have been considerably improved and many innovative developments implemented. Increasingly more equipment of in-house laboratories, as well as the instrumentation of beamlines at synchrotrons and thermal neutron sources are dedicated to high-pressure research.

Dimethyl-, Disilyl- and Digermylsulfide: Different Intermolecular Contacts in the Solid State

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts

The compounds (H3C)2S, (H3Si)2S and (H3Ge)2S have been crystallised in situ on a diffractometer and their crystal structures determined by low-temperature X-ray diffraction. The molecules are present as monomers in the crystals. The aggregation of the molecules through secondary intermolecular contacts in the crystal is different: (H3C)2S is weakly associated into dimers by S···S contacts, whereas (H3Si)2S and (H3Ge)2S form Si···S and Ge···S contacts in an ice-analogous aggregation motif. Important geometry parameters are (H3C)2S: C-S 1.794(av) Å , C-S-C 99.2(1)°; (H3Si)2S: Si- S 2.143(1) Å , Si-S-Si 98.4°; (H3Ge)2S Ge-S 2.223(2) and 2.230(2) Å , Ge-S-Ge 98.2(1)◦.

In situ synchrotron X-ray diffraction study of the formation of TaB2 from the elements in a laser heated diamond anvil cell

2010 ◽  
Vol 12 (12) ◽  
pp. 2059-2064 ◽  
Author(s):  
Björn Winkler ◽  
Erick A. Juarez-Arellano ◽  
Alexandra Friedrich ◽  
Lkhamsuren Bayarjargal ◽  
Florian Schröder ◽  
...  
Keyword(s):  
Diffraction Study ◽  
Diamond Anvil Cell ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diamond Anvil ◽  
Laser Heated
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