X-ray crystallographic structures of neuroprotective pyrimidine derivatives: (I) the mesylate salt of BW1003C87 and (II) sipatrigine base

Drugs based on 5-phenyl-2,4 diamino pyrimidine and 6-phenyl-1,2,4 triazine derivatives are well known for their effects on the central nervous system. The study presented here provides detailed crystal structures of two pyrimidine derivatives which have neuroprotective properties in models of both grey and white matter ischemia. Recently published studies suggest that the compounds lamotrigine (a triazine derivative), and the two pyrimidines BW1003C87 (I) and sipatrigine (II) mediate their primary in vivo mode of action by inhibiting voltage-gated Na+ channels. The X-ray crystal structures will contribute valuable data for applications involving binding and modelling studies of the biological actions of these drugs.

An Electron-Microscope X-Ray-Diffraction And Amino-Acid-Analysis Study Of The Opercular Filament Cuticle Calcareous Opercular Plate And Habitation Tube Of Pomatoceros Lamarckii Quatrefages (Polychaeta Serpulidae)

The structure, X-ray diffraction and amino acid compositions of the opercular filament cuticle, calcareous opercular plate and habitation tube of the polychaete serpulid, Pomatoceros lamarckii quatrefages, are reported. The opercular filament cuticle is made up of protein and chitin. The chitin is probably in the crystallographic α form. The structure and amino acid composition of the organic components of the opercular filament cuticle and calcareous opercular plate have similarities but are distinctly different from those of the calcareous habitation tube. The opercular plate and habitation tube are composed of different polymorphs of calcium carbonate, aragonite and calcite respectively. Comparisons are made with other chitin-protein systems, structural and calcified proteins.

An investigation into the subambient behavior of aqueous mannitol solutions using differential scanning calorimetry, cold stage microscopy, and X-ray diffractometry

The subambient behavior of aqueous mannitol solutions is of considerable relevance to the preparation of freeze dried formulations. In this investigation the properties of 3% w/v mannitol solutions were investigated using differential scanning calorimetry (DSC), cold stage microscopy (CSM), and X-ray diffraction (XRD) to identify the thermal transitions and structural transformations undergone by this system. It was found that on cooling from ambient the system formed ice at circa -20°C while a further exotherm was seen at approximately -30°C. Upon reheating an endotherm was seen at circa -30°C followed immediately by an exotherm at circa -25°C. Temperature cycling indicated that the thermal transitions observed upon reheating were not reversible. Modulated temperature DSC (MTDSC) indicated that the transitions observed upon reheating corresponded to a glass transition immediately followed by recrystallization, XRD data showed that recrystallization was into the ß form. Annealing at -35°C for 40 min prior to cooling and reheating resulted in a maximum enthalpy being observed for the reheating exotherm. It is concluded that on cooling 3% w/v aqueous mannitol solutions an amorphous phase is formed that subsequently recrystallises into the ß form. The study has also shown that DSC, CSM, and XRD are useful complementary techniques for the study of frozen systems

DFT and in situ EXAFS investigation of gold/ceria-zirconia low-temperature water gas shift catalysts: Identification of the nature of the active form of gold

A combined experimental and theoretical investigation of the nature of the active form of gold in oxide-supported gold catalysts for the water gas shift reaction has been performed. In situ extended X-ray absorption fine structure (EXAFS) and X-ray absorption near-edge structure (XANES) experiments have shown that in the fresh catalysts the gold is in the form of highly dispersed gold ions. However, under water gas shift reaction conditions, even at temperatures as low as 100 degrees C, the evidence from EXAFS and XANES is only 14 consistent with rapid, and essentially complete, reduction of the gold to form metallic clusters containing about 50 atoms. The presence of Au-Ce distances in the EXAFS spectra, and the fact that about 15% of the gold atoms can be reoxidized after exposure to air at 150 degrees C, is indicative of a close interaction between a fraction (ca. 15%) of the gold atoms and the oxide support. Density functional theory (DFT) calculations are entirely consistent with this model and suggest that an important aspect of the active and stable form of gold under water gas shift reaction conditions is the location of a partially oxidized gold (Audelta+) species at a cerium cation vacancy in the surface of the oxide support. It is found that even with a low loading gold catalysts (0.2%) the fraction of ionic gold under water gas shift conditions is below the limit of detection by XANES (<5%). It is concluded that under water gas shift reaction conditions the active form of gold comprises small metallic gold clusters in intimate contact with the oxide support.

Synchrotron X-ray diffraction study of the phase transformations in titanium alloys

High-resolution synchrotron X-ray diffraction was used to study the phase transformations in titanium alloys. Three titanium alloys were investigated: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo-0.08Si and beta21s. Both room and high temperature measurements were performed. The room temperature experiments were performed to study the structure of the alloys after different heat treatments, namely as received (AR), furnace cooling (FC), water quenching (WQ) and water quenching followed by ageing. The alpha, alpha', alpha'' and beta phases were observed in different combinations depending on the heat treatment conditions and the alloy studied. A multicomponent hexagonal close packed (hcp) alpha phase, with different c and the same a lattice parameters, was detected in Ti-6Al-4V after FC. High temperature synchrotron X-ray diffraction was used for 'in situ' study of the transformations on the sample surface at elevated temperatures. The results were used to trace the kinetics of surface oxidation and the concurrent phase transformations taking place under different conditions. The influence of the temperature and oxygen content on the lattice parameters of the alpha phase was derived and new data obtained on the coefficients of thermal expansion in the different directions of the hcp alpha phase, for Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo-0.08Si.

Flare X-ray Observations of AB Doradus: Evidence of Stellar Coronal Opacity

X-ray spectra of the late-type star AB Dor obtained with the XMM-Newton satellite are analyzed. AB Dor was particularly active during the observations. An emission measure reconstruction technique is employed to analyze flare and quiescent spectra, with emphasis on the Fe XVII 15 - 17 angstrom wavelength region. The Fe XVII 16.78 angstrom/ 15.01 angstrom line ratio increases significantly in the hotter flare plasma. This change in the ratio is opposite to the theoretical predictions and is attributed to the scattering of 15.01 angstrom line photons from the line of sight. The escape probability technique indicates an optical depth of approximate to 0.4 for the 15.01 angstrom line. During the flare, the electron density is 4.4(-1.6)(+2.7) x 10(10) cm(-3), and the fractional Fe abundance is 0.5 +/- 0.1 of the solar photospheric value Using these parameters, a path length of approximate to 8000 km is derived. There is no evidence of opacity in the quiescent X-ray spectrum of the star.

An investigation into the use of atomic datasets in simulations of the Ni-like gadolinium x-ray laser

The effect of differing the datasets used in the modelling of the Ni-like Gd x-ray laser (XRL) is examined through the 1.50 hydro-atomic code, EHYBRID. Two atomic datasets, including energy levels and radiative and collisional excitation rates, are used as input data for the code. It is found that the behaviour of the XRL is somewhat different than might be expected from superficial examination of the atomic data. The similarities in the gain profiles at low densities are found to have encouraging implications. in our attempts to model XRLs.

X-ray and extreme-ultraviolet emission from the coronae of Capella

The primary objective of this work is the analysis and interpretation of coronal observations of Capella obtained in 1999 September with the High Energy Transmission Grating Spectrometer on the Chandra X-ray Observatory and the Extreme Ultraviolet Explorer (EUVE). He-like lines of O (O vii) are used to derive a density of 1.7 x 10(10) cm(-3) for the coronae of the binary, consistent with the upper limits derived from Fe xxi, Ne ix and Mg xi line ratios. Previous estimates of the electron density based on Fe xxi should be considered as upper limits. We construct emission measure distributions and compare the theoretical and observed spectra to conclude that the coronal material has a temperature distribution that peaks around 4-6 MK, implying that the coronae of Capella were significantly cooler than in the previous years. In addition, we present an extended line list with over 100 features in the 5-24 Angstrom wavelength range, and find that the X-ray spectrum is very similar to that of a solar flare observed with SMM. The observed to theoretical Fe xvii 15.012-Angstrom line intensity reveals that opacity has no significant effect on the line flux. We derive an upper limit to the optical depth, which we combine with the electron density to derive an upper limit of 3000 km for the size of the Fe xvii emitting region. In the same context, we use the Si iv transition region lines of Capella from HST/Goddard High-Resolution Spectrometer observations to show that opacity can be significant at T = 10(5) K, and derive a path-length of approximate to 75 kin for the transition region. Both the coronal and transition region observations are consistent with very small emitting regions, which could be explained by small loops over the stellar surfaces.

Improved data for solar flare X-ray spectral analysis

The inclusion of collisional rates for He-like Fe and Ca ions is discussed with reference to the analysis of solar flare Fe XXV and Ca XIX line emission, particularly from the Yohkoh Bragg Crystal Spectrometer (BCS). The new data are a slight improvement on calculations presently used in the BCS analysis software in that the discrepancy in the Fe XXV y and z line intensities (observed larger than predicted) is reduced. Values of electron temperature from satellite-to-resonance line ratios are slightly reduced (by up to 1 MK) for a given observed ratio. The new atomic data will be incorporated in the Yohkoh BCS databases. The data should also be of interest for the analysis of high-resolution, non-solar spectra expected from the Constellation-X and Astro-E space missions. A comparison is made of a tokamak S XV spectrum with a synthetic spectrum using atomic data in the existing software and the agreement is found to be good, so validating these data for particularly high-n satellite wavelengths close to the S XV resonance line. An error in a data file used for analyzing BCS Fe XXVI spectra is corrected, so permitting analysis of these spectra.

Plasma-based studies with intense X-ray and particle beam sources

The construction of short pulse (

He-like x-ray line emission from laser irradiated sources

Photon yields for the 1s(2)-1s2p (He-alpha) transition of He- like ions have been measured for laser irradiated, thin foils of Ti, V and Fe. The laser pulses were of 0.527 mum wavelength and of either 80 or 300 ps duration. The data shows significant shot-to-shot variation but the Ti data is broadly consistent with previous results. In this work, we extend the previous results to include, new elements, longer pulse lengths and yields measured for emission from both surfaces of the foils. We compare our data to simulations using a hydrodynamic code and a collisional radiative model.