Solvent diffusion through a non-porous crystal ‘caught in the act’ and related single-crystal-to-single-crystal transformations in a cationic dinuclear Ag(i) complex

CrystEngComm ◽  
2015 ◽  
Vol 17 (46) ◽  
pp. 8957-8964 ◽  
Author(s):  
Jo Alen ◽  
Luc Van Meervelt ◽  
Wim Dehaen ◽  
Liliana Dobrzańska
Keyword(s):  
Diffusion Process ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Solvent Diffusion ◽  
Solvent Uptake ◽  
Porous Crystal

A few snapshots of a dynamic solvent diffusion process through a seemingly non-porous crystal of a dinuclear, cyclic Ag(i) complex were revealed. These indicate the complexity of the process, which involves not only relocation of the molecules in the crystal lattice, but also conformational adjustments of the metallocycles in response to solvent uptake/release.

scholarly journals Magnetically Oriented Powder Crystal to Indexing and Structure Determination

2014 ◽  
Vol 70 (a1) ◽  
pp. C1560-C1560
Author(s):  
Fumiko Kimura ◽  
Wataru Oshima ◽  
Hiroko Matsumoto ◽  
Hidehiro Uekusa ◽  
Kazuaki Aburaya ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Powder Diffraction ◽  
Diffraction Method ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Lattice Parameters

In pharmaceutical sciences, the crystal structure is of primary importance because it influences drug efficacy. Due to difficulties of growing a large single crystal suitable for the single crystal X-ray diffraction analysis, powder diffraction method is widely used. In powder method, two-dimensional diffraction information is projected onto one dimension, which impairs the accuracy of the resulting crystal structure. To overcome this problem, we recently proposed a novel method of fabricating a magnetically oriented microcrystal array (MOMA), a composite in which microcrystals are aligned three-dimensionally in a polymer matrix. The X-ray diffraction of the MOMA is equivalent to that of the corresponding large single crystal, enabling the determination of the crystal lattice parameters and crystal structure of the embedded microcrytals.[1-3] Because we make use of the diamagnetic anisotropy of crystal, those crystals that exhibit small magnetic anisotropy do not take sufficient three-dimensional alignment. However, even for these crystals that only align uniaxially, the determination of the crystal lattice parameters can be easily made compared with the determination by powder diffraction pattern. Once these parameters are determined, crystal structure can be determined by X-ray powder diffraction method. In this paper, we demonstrate possibility of the MOMA method to assist the structure analysis through X-ray powder and single crystal diffraction methods. We applied the MOMA method to various microcrystalline powders including L-alanine, 1,3,5-triphenyl benzene, and cellobiose. The obtained MOMAs exhibited well-resolved diffraction spots, and we succeeded in determination of the crystal lattice parameters and crystal structure analysis.

scholarly journals Phase transformations in cucurbituril host-guest complexes

2014 ◽  
Vol 70 (a1) ◽  
pp. C646-C646
Author(s):  
Oksana Danylyuk ◽  
Karolina Kedra-Krolik ◽  
Marta Worzakowska ◽  
Joanna Osypiuk-Tomasik ◽  
Vladimir Fedin
Keyword(s):  
Single Crystal ◽  
Crystal Lattice ◽  
Supramolecular Assembly ◽  
Water Molecules ◽  
Guest Molecules ◽  
X Ray ◽  
Host Guest Complex ◽  
Crystallographic Study ◽  
Partial Dehydration ◽  
Structure Changes

The retention of crystallinity upon desolvation of molecular crystals is not common, as the molecules are rigidly and densely packed in the crystals and the original framework usually collapses once solvent is removed from the structure. However, in rare cases the host framework remains substantially unaffected by solvent (guest) removal yielding structure with open channels or discrete lattice voids that can show permanent porosity. [1] Furthermore, sometimes happens, the desolvation process proceeds as single-crystal to single-crystal transformation resulting in distortion and sliding of the structure, changes in conformation, coordination modes and/or space group. Here we would like to present crystallographic study and thermal analysis on the dehydration process of the crystalline supramolecular complex between macrocyclic host cucurbit[6]uril and dopamine. In the solid state the 1:1 host-guest complex assembles into hexameric tubes with water-filled interior channels. Another set of water channels is created between three neighboring tubes in the crystal lattice. The crystals of such supramolecular assembly are not stable when out from mother solution and immediately start to loose water upon exposure to air. However, despite severe cracking the crystals dried in air maintained their integrity and still gave satisfactory diffraction pattern. The X-ray analysis showed significant decrease in the unit cell volume of the partially dehydrated crystals that corresponds to the liberation of some of the water molecules from the channels. Moreover, the reorganization of dopamine guest molecules has occurred in the crystal lattice as a response to the escape of water molecules from the structure. The partial dehydration and reorganization of the supramolecular framework proceeds via a single-crystal to single-crystal mechanism.

Characterization of Plastic Deformation Induced by Microscale Laser Shock Peening

2004 ◽  
Vol 71 (5) ◽  
pp. 713-723 ◽  
Author(s):  
Hongqiang Chen ◽  
Jeffrey W. Kysar ◽  
Y. Lawrence Yao
Keyword(s):  
Plastic Deformation ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Electron Backscatter Diffraction ◽  
Fem Analysis ◽  
Copper Sample ◽  
Laser Shock Peening ◽  
Lattice Rotation ◽  
Laser Shock ◽  
Shock Peening

Electron backscatter diffraction (EBSD) is used to investigate crystal lattice rotation caused by plastic deformation during high-strain rate laser shock peening in single crystal aluminum and copper sample on 110¯ and (001) surfaces. New experimental methodologies are employed which enable measurement of the in-plane lattice rotation under approximate plane-strain conditions. Crystal lattice rotation on and below the microscale laser shock peened sample surface was measured and compared with the simulation result obtained from FEM analysis, which account for single crystal plasticity. The lattice rotation measurements directly complement measurements of residual strain/stress with X-ray micro-diffraction using synchrotron light source and it also gives an indication of the extent of the plastic deformation induced by the microscale laser shock peening.

scholarly journals Preparation and Crystal Structure of Zinc Bis[orotate(1–)] Octahydrate

1993 ◽  
Vol 48 (7) ◽  
pp. 961-964 ◽  
Author(s):  
Otto Kumberger ◽  
Jürgen Riede ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Medical Treatment ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Structure Analysis ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

A discrete zinc bis[orotate(1—)] complex of the composition Zn(OrH)2·8 H2O has been isolated and characterized by a single-crystal X-ray structure analysis. The crystals are monoclinic, space group P21/c (No. 14), Z = 2, a = 10.884(2), b = 12.896(1), c = 6.954(1) Å, β = 98.27(1)°. The crystal lattice features hexaquo complexes of zinc, the Zn(H2O)62+ cations being associated with two hydrated OrH- ions only through hydrogen bonds. The results are relevant for applications of zinc orotates in medical treatment.

Boron Segregation and Out-diffusion in Single-Crystal Si 1-y C y

2003 ◽  
Vol 765 ◽  
Author(s):  
E. J. Stewart ◽  
J.C. Sturm
Keyword(s):  
Diffusion Process ◽  
Single Crystal ◽  
Carbon Diffusion ◽  
Subsequent Oxidation ◽  
Boron Segregation ◽  
Carbon Precipitation

AbstractBoron segregation and its effect on carbon diffusion is studied in single-crystal Si1-yCy. We find that boron segregates from silicon to Si0.996C0.004 at a level m=[B]SiC/[B]Si = 1.7 during a 2 hour, 850°Cannealin N2. After this anneal, if most of the carbon is then removed from the Si1-yCy layer (via an oxidation-enhanced out-diffusion process), most of the boron segregation is removed as well. This argues against immobile B-C defects as the predominant mechanism driving the segregation. Boron is shown to increase carbon diffusion during the N2 anneal, but also appears to enhance carbon precipitation during a subsequent oxidation.

Crystal Lattice Engineering during Laser-induced Single Crystal Growth

2018 ◽  
Author(s):  
Keith Veenhuizen ◽  
Courtney Au-Yeung ◽  
Dmytro Savytskyy ◽  
Sean McAnany ◽  
Daniel Nolan ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Single Crystal Growth
Sign in / Sign up

Export Citation Format

Share Document