Quantitative Phase Analyses Through The Rietveld Method with X-Ray Powder Diffraction Data of Heat-Treated Carbamazepine Form III

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

Purification, Characterization, and Preliminary X-Ray Diffraction Analysis of a Lactose-Specific Lectin from Cymbosema roseum Seeds

The unique carbohydrate-binding property of lectins makes them invaluable tools in biomedical research. Here, we report the purification, partial primary structure, carbohydrate affinity characterization, crystallization, and preliminary X-ray diffraction analysis of a lactose-specific lectin from Cymbosema roseum seeds (CRLII). Isolation and purification of CRLII was performed by a single step using a Sepharose-4B-lactose affinity chromatography column. The carbohydrate affinity characterization was carried using assays for hemagglutination activity and inhibition. CRLII showed hemagglutinating activity toward rabbit erythrocytes. O-glycoproteins from mucine mucopolysaccharides showed the most potent inhibition capacity at a minimum concentration of 1.2 A mu g mL(-1). Protein sequencing by mass spectrometry was obtained by the digestion of CRLII with trypsin, Glu-C, and AspN. CRLII partial protein sequence exhibits 46% similarity with the ConA-like alpha chain precursor. Suitable protein crystals were obtained with the hanging-drop vapor-diffusion method with 8% ethylene glycol, 0.1 M Tris-HCl pH 8.5, and 11% PEG 8,000. The monoclinic crystals belong to space group P2(1) with unit cell parameters a = 49.4, b = 89.6, and c = 100.8 A....

Resonant x-ray diffraction as a tool to calculate mixed valence ratios: Application to Prussian Blue materials

An approach is proposed here to calculate mixed valence ratios in molecular compounds. Synchrotron x-ray powder diffraction experiments were conducted to determine the Fe(+3)/Fe(+2) ratio in Prussian Blue compounds, which were elected as an example of the use of this approach. As a result, a resonant x-ray diffraction measurement provided direct evidence that the vacant [Fe(CN)(6)] group was randomly absent from similar to 31% of the structure, which was indicated by structural differences caused by variations in the anomalous dispersion term. These findings are very important for a deeper understanding of the changes occurring in properties during in situ compositional variations. (c) 2008 American Institute of Physics.

Composition of the first coordination sphere of Ni2+ in concentrated aqueous NiBr2 solutions by x-ray diffraction

Two concentrated solutions of NiBr2 have been examined by x-ray diffraction. The Fourier transformed scattering data indicate inner complex formation between Ni2 + and Br- ions. Average numbers of bonded bromide ions per nickel atom have been determined for each solution and the reliability of the complexation numbers as well as of the other structural parameters has been critically examined. © 1985 American Institute of Physics.

X-ray diffraction investigation of Co(II) ions in borosilicate glasses

The radial distribution functions of cobalt glasses with 6%, 8%, and 14% CoO are compared with those of suitable cobalt-free borosilicate matrices leading to difference distribution curves representative of the cobalt structural arrangement. Analysis of the curves indicates that cobalt ions are surrounded by approximately four oxygen neighbors at the distance expected for fourfold coordination. © 1986 American Institute of Physics.

Small angle X-ray scattering study of structural changes in silica gel modified with organofunctional groups

Silica gel surfaces, organofunctionalized with 2-mercaptobenzimidazole, iminosalicylaldehyde and imidazole groups were examined using the small angle X-ray scattering technique (SAXS). From the scattering intensity data it was concluded that particles have a uniform size after the coupling reaction. The chemical treatment of the silica gel leads to an attachment of the organofunctional groups on the solid-pore interface of the silica with an increase of the mean size of the solid phase and some coalescence of the pores. © 1989.

Synthesis and X-ray studies of di-μ-cyanato-bis[{cyanato (N,N- dimethylethylenediamine)}copper(II)]

The compound di-μ-cyanato-bis[{cyanato(N,N-dimethylethylenediamine)} copper(II)] was synthesized, and studied by IR spectroscopy and X-ray diffraction. It is dimeric with bridging and terminal cyanate groups, and the copper atoms show a square-based pyramid coordination geometry. © 1990.

High temperature X-ray diffraction study of the U4O9 formation on UO2 sintered plates

The surface oxidation of UO2 sintered plates at 170-275 ° C was studied in situ by high temperature X-ray diffractometry. At very low oxygen concentration, UO2 is oxidized to U4O9, while at 300°C and argon-20 vol% oxygen it is oxidized up to U3O7. X-ray diffraction profiles of the UO2, U4O9 and U3O7 phases were well characterized during the transformations. The activation energy for the transformation of UO2 to U4O9, obtained from X-ray diffraction data, was found to be 117 ± 9 kJ/mol and 90 ± 14 kJ/mol for the β-(311) and α-(200) reflections, respectively. © 1991.

Pore structure characterization of kaolin, metakaolin, and their acid-treated products using small-angle X-ray scattering

Pore structure of dealuminated kaolin and metakaolin was studied by small-angle X-ray scattering (SAXS). Both parent kaolin and metakaolin have about 10% of the total pore volume provided by globular pores with 105 Å mean pore size. Their surface area is about 14 m2/g. Acid dealumination of kaolin causes an increase of its globular pore volume without an appreciable change in the mean pore size, its surface area increasing up to about 90 m2/g. Acid dealumination of metakaolin enhances the globular pore volume, although there is generation of slit-shaped pores with a narrow thickness distribution whose mean value is 14 Å. This interlayer spacing causes an increase in surface area of about 190 m2/g by SAXS. © 1994.

Niobium filtration of conventional and high-frequency x-ray generator beams for intraoral radiography. Effects on absorbed doses, image density and contrast, and photon spectra

We have studied the effects of niobium beam filtration on absorbed doses, on image density and contrast, and on photon spectra with conventional and high-frequency dental x-ray generators. Added niobium reduced entry and superficial absorbed doses in periapical radiography by 9% to 40% with film and digital image receptors, decreased the radiation necessary to produce a given image density on E-speed film and reduced image contrast on D- and E-speed films. As shown by increased half-value layers for aluminum, titanium, and copper and by pulse-height analyses of beam spectra, niobium increased average beam energy by 6% to 19%. Despite the benefits of adding niobium on patient dose reduction and on narrowing the beams' energy spectra, the beam can be overhardened. Adding niobium, therefore, strikes the best balance between radiation dose reduction and beam attenuation, with its risks of increased exposure times, motion blur, and diminished image contrast, when it is used at modest thicknesses (30 μm) and at lower kVp (70) settings. © 1995 Mosby-Year Book, Inc.

Doping of polyaniline and derivatives induced by X-ray radiation

Thin films of chemically synthesized polyaniline and poly(o-methoxyaniline) were exposed to ionizing X-ray radiation and characterized by radiation induced conductivity measurements, ultraviolet-visible spectroscopy, electron paramagnetic resonance, electrical conductivity and solubility measurements. Samples irradiated in vacuum or dry Oxygen atmosphere did not have their electronic spectra changed. However, under humid atmosphere the energy of the excitonic transition was decreased and accompanied by a great conductivity increase. The results indicate that doping of polyaniline can be induced by X-ray radiation which might be of great interest for applications on lithography and microelectronics.

Crystallization and X-ray diffraction data analysis of oxyhemoglobin-I from the catfish Liposarcus anisitsi (pisces)

Hemoglobin remains, despite the enormous amount of research involving this molecule, as a prototype for allosteric models and new conformations. Functional studies carried out on Hemoglobin-I from the South-American Catfish Liposarcus anisitsi [1] suggest the existence of conformational states beyond those already described for human hemoglobin, which could be confirmed crystallographically. The present work represents the initial steps towards that goal.

Crystallization and preliminary X-ray analysis of SIII-SPIII, a ahospholipase A2 isolated from the venom of Bothrops jararacussu

Large single crystals have been obtained of SIII-SPIII, a phospholipase A2 from the venom of Bothrops jararacussu. The crystals belong to the orthorhombic system space group C222, and diffract X-rays to a resolution of 1.9 Å. Preliminary analysis reveals the presence of one molecule in the crystallographic asymmetric unit. The crystal structure is currently being determined using molecular replacement techniques.

Synthesis and characterization of the mer-[RuCl3(NO)(dppb)] isomer. X-ray structures of fac-[RuCl3(NO)(dppm)], cis-[RuCl2(dppm)2] and mer-[RuCl3(NO)(dppb)] [dppm=1,2-Bis(diphenylphosphino)methane and dppb=1,4-Bis(diphenylphosphino)butane]

The fac-[RuCl3(NO)(dppm)] (1) and cis-[RuCl2(dppm)2] (2) complexes were obtained with co-crystallization in the solid state from the reaction of RuCl3(NO) with the diphosphine in dichloromethane. mer-[RuCl3(NO)(dppb)] (3) was obtained from [RuCl3(dppb)(H2O)] by bubbling NO for 30 min in the same solvent. The crystal and molecular structures of these three compounds have been determined from X-ray studies. © Elsevier Science Ltd.

fac-[RuCl3(no)(dppb)] (I) and mer-[RuCl3(NO)(diop)] (II) complexes: Syntheses, characterization and x-ray structures

The fac-[RuCl3(NO)(dppb)] complex I has been prepared from solution of the correspondent mer isomer in refluxing methanol (dppb = 1,4-bis(diphenylphosphino)butane). The mer-[RuCl3(NO)(diop)] (II) has been obtained from the mer-[RuCl3(diop)(H2O)] by bubbling NO for 1 h in dichloromethane (diop = 2S,3S-O-isopropylidene-2,3-dihydroxy-1,4-bis(diphenylphosphino)butane). The complexes have been characterized by microanalysis, cyclic voltammetry (CV), IR and 31P{1H} NMR spectroscopies. The crystal and molecular structures of these two compounds have been determined from X-ray studies. The mer-[RuCl3(NO)(dppb)] isomer III was characterized in solution by NMR spectra (31P{1H}, 1H{31P}, 31P-1H HETCORR, COSY 1H-1H, HMQC 1H-13C and HMBC 1H-13C). © 2002 Elsevier Science Ltd. All rights reserved.