scholarly journals In-situ X-ray diffraction snapshotting: Determination of the kinetics of a photodimerization within a single crystal

2014 ◽  
Vol 4 (1) ◽  
Author(s):  
Fei-Long Hu ◽  
Shu-Long Wang ◽  
Jian-Ping Lang ◽  
Brendan F. Abrahams
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Kinetics Of

Determination of the kinetics of crystallisation of gibbsite using time resolved in situ energy dispersive powder X-ray diffraction

2000 ◽  
Vol 10 (10) ◽  
pp. 2355-2357 ◽  
Author(s):  
Andrew M. Fogg ◽  
Stephen J. Price ◽  
Robin J. Francis ◽  
Stephen O'Brien ◽  
Dermot O'Hare
Keyword(s):  
Energy Dispersive ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Kinetics Of

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Synthesis of 4-(3-coumarinyl)-3-benzyl-4-thiazolin-2-one 4-methylbenzylidenehydrazone and determination of the isomeric structure by X-ray analysis

2003 ◽  
Vol 218 (12) ◽  
Author(s):  
Süheyla Özbey ◽  
Nilgün Karalı ◽  
Aysel Gürsoy
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Spectral Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Isomeric Structure ◽  
Elemental Analyses

AbstractIn this study 4-(3-coumarinyl)-3-benzyl-4-thi azolin-2-one 4-methylbenzylidenehydrazone 3 was synthesised. An independent proof of the thiazolylhydrazone structure of 3 was achieved by single crystal X-ray diffraction analysis. Elemental analyses and spectral data (IR,

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

Sign in / Sign up

Export Citation Format

Share Document