On the Determination of Single Crystal X-Ray Diffraction Patterns from Two-Crystal Spectrometer Rocking Curves

1938 ◽  
Vol 53 (2) ◽  
pp. 200-200
Author(s):  
Franklin Miller ◽  
Lyman G. Parratt
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
Crystal Spectrometer ◽  
X Ray ◽  
Diffraction Patterns

scholarly journals X-Ray Diffraction from Magnetically Oriented Microcrystal Suspension

2014 ◽  
Vol 70 (a1) ◽  
pp. C1136-C1136
Author(s):  
Kazuaki Aburaya ◽  
Chiaki Tsuboi ◽  
Fumiko Kimura ◽  
Kenji Matsumoto ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Single Crystal ◽  
Magnetic Circuit ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
Uv Curable ◽  
X Ray ◽  
Novel Method ◽  
Diffraction Patterns ◽  
Magnetic Field Generator

A three dimensionally magnetically oriented microcrystal array (3D-MOMA) is attractive to determination of a crystal structure as well as a molecular structure because it does not require a single crystal with sufficient size and quality for diffraction studies. We have developed a novel method to fabricate 3D-MOMA and determined several crystal structures using the 3D-MOMAs[1],[2]. However, the structure determination through MOMA requires a solidification treatment with UV curable monomer prior to X-ray diffraction experiment. We have developed a new X-ray diffractometer equipped with a magnetic field generator, which makes it possible to collect diffraction data without the solidification treatment. In this poster, we describe X-ray diffraction analyses of a magnetically oriented microcrystal suspension (MOMS) of L-alanine without the solidification treatment. A suspension of L-alanine microcrystals was poured in a glass capillary and rotated at a constant speed in a magnetic circuit attached in the X-ray diffractometer. Then, diffraction images were collected every 60 seconds. In the initial phase, the diffraction pattern showed a broad shape similar to that from a powder sample. As time goes on, diffraction patterns have gradually changed to single-crystal like patterns. After 2 hours, the shape of diffraction spots became as sharp as that of a single crystal. This observation shows that the microcrystals are oriented in the same direction. Owing to the improvement of the magnetic circuit and X-ray diffractometer, the quality of the diffraction has been greatly improved compared to that reported previously[3]. Further details of the analyses will be shown in the poster.

scholarly journals Crystal structure of the thortveitite-relatedMphase, (MnxZn1–x)2V2O7(0.75

2018 ◽  
Vol 74 (10) ◽  
pp. 1079-1087
Author(s):  
Kevin M. Knowles ◽  
Anjan Sil ◽  
Berthold Stöger ◽  
Matthias Weil
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Distorted Version ◽  
Triclinic Structure ◽  
Diffraction Patterns ◽  
Triclinic Unit Cell

The determination of the crystal structure of theMphase, (MnxZn1–x)2V2O7(0.75 <x< 0.913), in the pseudobinary Mn2V2O7–Zn2V2O7system forx≃ 0.8 shows that the previously published triclinic unit-cell parameters for this thortveitite-related phase do not describe a true lattice for this phase. Instead, single-crystal X-ray data and Rietveld refinement of synchrotron X-ray powder data show that theMphase has a different triclinic structure in the space groupP-1 withZ= 2. As prior work has suggested, the crystal structure can be described as a distorted version of the thortveitite crystal structure of β-Mn2V2O7. A twofold superstructure in diffraction patterns of crystals of theMphase used for single-crystal X-ray diffraction work arises from twinning by reticular pseudomerohedry. This superstructure can be described as a commensurate modulation of a pseudo-monoclinic basis structure closely related to the crystal structure of β-Mn2V2O7. In comparison with the distortions introduced when β-Mn2V2O7transforms at low temperature to α-Mn2V2O7, the distortions which give rise to theMphase from the β-Mn2V2O7prototype are noticeably less pronounced.

scholarly journals Born out of Fire and Ice: Polymorph Studies of the Antiviral Famciclovir

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Variable Temperature ◽  
Chemical Properties ◽  
Crystal Form ◽  
X Ray Diffraction ◽  
Crystal Forms ◽  
X Ray ◽  
Physical Chemical ◽  
Diffraction Patterns ◽  
Crystalline Forms

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.

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,

Plastic deformations in kyanites by tectonometamorphic processes: a single-crystal X-ray diffraction study

2009 ◽  
Vol 73 (3) ◽  
pp. 359-371 ◽  
Author(s):  
G. D. Gatta ◽  
N. Rotiroti ◽  
M. Zucali
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
Plastic Deformations ◽  
X Ray ◽  
Deformational History ◽  
Significant Difference ◽  
Elliptical Section ◽  
History Of ◽  
Diffraction Patterns ◽  
Two Stages

AbstractThe crystalch emistry and crystal structure of naturalky anite crystals from the Eclogitic Micaschists Complex of the Sesia-Lanzo Zone, Western Italian Alps, have been investigated by means of optical microscopy, wavelength dispersive X-ray microanalysis, and single-crystal X-ray diffraction. The association of kyanite + garnet + phengitic-mica + chloritoid suggests that the eclogite-facies stages occurred at P ≤ 2.1 GPa and T ≤ 650ºC. Kyanite grains are large (cm-sized) porphyroblasts grown dynamically during one of the deformational events related to the subduction of the Austroalpine continentalcr ust. Under the polarizing microscope, kyanite grains show almost homogeneous cores, whereas rims are sometimes symplectitic aggregates of quartz and kyanite, confirming at least two stages of growth most likely related to the multistage deformational history of these rocks. Chemical analysis shows that Fe3+ is the major substituting cation for Al3+, ranging between 0.038 and 0.067 a.p.f.u.The single-crystal X-ray diffraction investigation of the kyanites shows severely textured patterns on the (h0l)*-plane. Such evidence is not observed in the unwarped diffraction patterns on (0kl)* and (hk0)*. The most significant difference between the structuralp arameters refined in this study, with respect to those of previously published unstrained gem-quality crystals, concerns the displacement parameters. The anisotropic displacement ellipsoids of all the atomic sites are significantly larger than those previously described, and systematically oriented with the largest elliptical section almost perpendicular to [010]. The larger ellipsoids in the kyanite crystal investigated here reflect the displacement of the centre of gravity of the electron distribution, rather than an anomalous atomic thermal motion. The magnitude and orientation of the displacement parameters and the textured/strained diffraction pattern may be the result of two combined effects: (1) that the kyanite crystals are actually composed of several blocks; (2) the crystals are affected by a pervasive residual strain, as a result of tectonometamorphic plastic deformations and re-crystallization.

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 Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

scholarly journals Determination of the full deformation tensor by multi-Bragg fast scanning nano X-ray diffraction

2020 ◽  
Vol 53 (1) ◽  
pp. 99-106
Author(s):  
Andreas Johannes ◽  
Jura Rensberg ◽  
Tilman A. Grünewald ◽  
Philipp Schöppe ◽  
Maurizio Ritzer ◽  
...  
Keyword(s):  
Surface Tension ◽  
Single Crystal ◽  
Spatial Resolution ◽  
Deformation Tensor ◽  
X Ray Diffraction ◽  
Projected Area ◽  
Absolute Value ◽  
X Ray ◽  
Grown Single Crystal

This work showcases a method to map the full deformation tensor in a single micro-sized crystal. It is shown that measuring the position of two Bragg reflections in reciprocal space is sufficient to obtain the full deformation tensor, if the condition of incompressibility of the material is imposed. This method is used to reveal the surface tension induced deformation at the edges of an as-grown single-crystal VO2 microwire. All components of the deformation tensor of the microwire were measured down to an absolute value of 10−4 in an 8 × 14 µm projected area of the wire. With a beam-defined spatial resolution of 150 × 150 nm, the measurement time was merely 2.5 h.

scholarly journals Synthesis of the Modifications of Ca2SiO4 and the Determination of their Powder X-ray Diffraction Patterns

1963 ◽  
Vol 71 (806) ◽  
pp. 63-68 ◽  
Author(s):  
Goro YAMAGUCHI ◽  
Yoshio ONO ◽  
Shigeo KAWAMURA ◽  
Yoshiaki SODA
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns
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