Synchrotron X-ray powder diffraction data of atorvastatin

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Crystal Structure Determination of Mebendazole Form A Using High-Resolution Synchrotron X-Ray Powder Diffraction Data

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

X-ray diffraction data of tibolone Delta(4) isomer (isotibolone)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Crystal structure of propylthiouracil determined using high-resolution synchrotron X-ray powder diffraction

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Purification, partial characterization and preliminary X-ray diffraction analysis of a mannose-specific lectin from Cymbosema roseum seeds

A lectin from Cymbosema roseum seeds (CRL) was purified, characterized and crystallized. The best crystals grew in a month and were obtained by the vapour-diffusion method using a precipitant solution consisting of 0.1 M Tris-HCl pH 7.8, 8% (w/v) PEG 3350 and 0.2 M proline at a constant temperature of 293 K. A data set was collected to 1.77 angstrom resolution at a synchrotron-radiation source. CRL crystals are orthorhombic, belonging to space group P2(1)2(1)2(1). Crystallographic refinement and full amino-acid sequence determination are in progress.

Purification, crystallization and preliminary X-ray diffraction analysis of carboxyhaemoglobin-II from the fish Piaractus mesopotamicus (pacu)

Carboxyhaemoglobin-II isolated from the pacu (Piaractus mesopotamicus) has been crystallized and X-ray diffraction data were collected to 2.0 Angstrom resolution using synchrotron radiation. Crystals were characterized as belonging to the space group I23; preliminary structural analysis reveals the presence of one dimer in the asymmetric unit.

Influence of annealing on X-ray diffraction of natural alexandrite

In this work we present results of X-ray diffraction using powder method, on natural alexandrite samples from Minas Gerais State (Brazil), as a function of a sequence of annealing. From these measurements we determine lattice parameters before (a = 9.405 Angstrom, b = 5.471 Angstrom, c = 4.409 Angstrom) and after annealing, and its structure is confirmed as orthorhombic. Measurements done after an annealing of 15 minutes at 700 degreesC and for 5 hours at 1000 degreesC indicate the migration of atoms present in the sample through different phases, which were also identified by Microprobe Analysis (WDS). However we have verified that such migration does not modify the structure. X-ray diffraction measurements have been carried out in conjunction with optical absorption in the UV-Vis as a function of annealing. (C) 2002 International Centre for Diffraction Data.

Phase-locking of superimposed diffractive gratings in photoresists

The superposition of optical interference patterns in a photoresist film can produce a rich variety of diffractive structures. In particular, a periodic non-sinusoidal surface relief profile can be synthesized by adding the Fourier components (sinusoidal gratings) of the desired profile. In order to control the shape of the grooves it is very important an accurate adjustment of the relative spatial shift between the recorded sinusoidal components. We describe the implementation of an opto-electronic feedback loop to select and lock such spatial shift at any desired position, thus allowing the synthesis of structures varying from symmetrical to asymmetrical relief profiles in a continuous range. To demonstrate the feasibility of the technique, the Fourier synthesis of two spatial harmonics is accomplished. The superposed sinusoidal gratings were recorded in positive photoresist films using a holographic setup operating at the line lambda = 457.9 run of an argon-ion laser. A detailed description of the procedure as well as the resulting profiles recorded in the photoresist is presented. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Crystallization and preliminary X-ray diffraction analysis of prephenate dehydratase from Mycobacterium tuberculosis H37Rv

Tuberculosis remains the leading cause of mortality arising from a bacterial pathogen ( Mycobacterium tuberculosis). There is an urgent need for the development of new antimycobacterial agents. The aromatic amino-acid pathway is essential for the survival of this pathogen and represents a target for structure-based drug design. Accordingly, the M. tuberculosis prephenate dehydratase has been cloned, expressed, purified and crystallized by the hanging-drop vapour-diffusion method using PEG 400 as a precipitant. The crystal belongs to the orthorhombic space group I222 or I2(1)2(1)2(1), with unit-cell parameters a = 98.26, b = 133.22, c = 225.01 angstrom, and contains four molecules in the asymmetric unit. A complete data set was collected to 3.2 angstrom resolution using a synchrotron-radiation source.

Crystallization and preliminary X-ray diffraction analysis of XAC1151, a small heat-shock protein from Xanthomonas axonopodis pv. citri belonging to the alpha-crystallin family

The hspA gene (XAC1151) from Xanthomonas axonopodis pv. citri encodes a protein of 158 amino acids that belongs to the small heat-shock protein ( sHSP) family of proteins. These proteins function as molecular chaperones by preventing protein aggregation. The protein was crystallized using the sitting-drop vapour-diffusion method in the presence of ammonium phosphate. X-ray diffraction data were collected to 1.65 angstrom resolution using a synchrotron-radiation source. The crystal belongs to the rhombohedral space group R3, with unit-cell parameters a = b = 128.7, c = 55.3 angstrom. The crystal structure was solved by molecular-replacement methods. Structure refinement is in progress.

C-H center dot center dot center dot O and N-H center dot center dot center dot O hydrogen bonds in liquid amides investigated by Monte Carlo simulation

Monte Carlo simulations of liquid formamide, N-methylformamide (MF), and N,N-dimethylformamide (DMF) have been performed in the isothermal and isobaric ensemble at 298 K and 1 atm, aiming to investigate the C-H ... O and N-H ... O hydrogen bonds. The interaction energy was calculated using the classical 6-12 Lennard-Jones pairwise potential plus a Coulomb term on a rigid six-site molecular model with the potential parameters being optimized in this work. Theoretical values obtained for heat of vaporization and liquid densities are in good agreement with the experimental data. The radial distribution function [RDF, g(r)] obtained compare well with R-X diffraction data available. The RDF and molecular mechanics (MM2) minimization show that the C-H ... O interaction has a significant role in the structure of the three liquids. These results are supported by ab initio calculations. This Interaction is particularly important in the structure of MF. The intensity of the N-H ... O hydrogen bond is greater in the MF than formamide. This could explain some anomalous properties verified in MF. (C) 1997 John Wiley & Sons, Inc.

Grazing incidence X-ray diffraction and atomic force microscopy analysis of BaBi2Ta2O9 thin films

Thin films of BaBi2Ta2O9 (BBT) composition were prepared through the metal organic decomposition method. The crystallinity, phase formation, crystallite size and morphology of the thin films were measured as a function of the type of substrate, stoichiometry of solution and process variables such as thickness and temperature. The thin films were investigated by grazing incidence X-ray diffractometry and atomic force microscopy (AFM) techniques. For the sample without excess of bismuth, diffraction peaks other than that of the BBT phase were observed. A well crystallized BBT single phase was observed for films prepared from a solution with 10% excess of bismuth, deposited on Si/Pt substrate, with a thickness up to 150 nm and sintered at temperatures of 700 degreesC. The thin BBT phase films heat-treated at 600 degreesC presented a diffraction pattern characteristic of samples with lower degree of crystallinity whereas for the thin films heat-treated at 800 degreesC, we observed the presence of other phases than the BBT. For the thin film deposited on the Sin+ substrate, we observe that the peaks corresponding to the BBT phase are broader than that observed on the samples deposited on the Pt and Si/Pt substrates. No variation of average crystallite size was observed as the excess of Bi increased from 10 to 20%. AFM images for the samples showed that the increasing the amount of bismuth promotes grain growth. The average surface roughness measured was in the range of 16-22 nm showing that the bismuth amount had no or little effect on the roughness of films. (C) 2002 Elsevier B.V. B.V. All rights reserved.