Home About us Contact | |||
Advanced Photon Source (advance + photon_source)
Selected AbstractsUltra-small-angle X-ray scattering at the Advanced Photon SourceJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3 2009Jan Ilavsky The design and operation of a versatile ultra-small-angle X-ray scattering (USAXS) instrument at the Advanced Photon Source (APS) at Argonne National Laboratory are presented. The instrument is optimized for the high brilliance and low emittance of an APS undulator source. It has angular and energy resolutions of the order of 10,4, accurate and repeatable X-ray energy tunability over its operational energy range from 8 to 18,keV, and a dynamic intensity range of 108 to 109, depending on the configuration. It further offers quantitative primary calibration of X-ray scattering cross sections, a scattering vector range from 0.0001 to 1,Å,1, and stability and reliability over extended running periods. Its operational configurations include one-dimensional collimated (slit-smeared) USAXS, two-dimensional collimated USAXS and USAXS imaging. A robust data reduction and data analysis package, which was developed in parallel with the instrument, is available and supported at the APS. [source] Iron K -edge anomalous small-angle X-ray scattering at 15-ID-D at the Advanced Photon SourceJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2007Nigel Kirby Small-angle X-ray scattering (SAXS) is an ideal technique for characterizing inorganic nanoparticles in biological specimens large enough to be representative of tissues. As tissues consist of complex mixtures of structures, identifying particular structural features from single-wavelength scattering data can be problematic. Synchrotron SAXS can supply element-specific structural information in complex samples, using anomalous scattering close to absorption edges. Anomalous dispersion is a secondary effect that produces relatively subtle changes in scattering patterns. In order to utilize this effect for anomalous SAXS analysis, stringent control of instrument performance is required. This work outlines the development of high-quality data collection and processing strategies for Fe K -edge anomalous SAXS on the ChemMatCARS beamline at the Advanced Photon Source (APS), Chicago, with an emphasis on intensity normalization. The methods reported here were developed during a study of iron-loaded mammal tissues, but could equally well be applied to other complex specimens. [source] A twelve-analyzer detector system for high-resolution powder diffractionJOURNAL OF SYNCHROTRON RADIATION, Issue 5 2008Peter L. Lee A dedicated high-resolution high-throughput X-ray powder diffraction beamline has been constructed at the Advanced Photon Source (APS). In order to achieve the goals of both high resolution and high throughput in a powder instrument, a multi-analyzer detector system is required. The design and performance of the 12-analyzer detector system installed on the powder diffractometer at the 11-BM beamline of APS are presented. [source] Design and performance of an ultra-high-vacuum-compatible artificial channel-cut monochromatorJOURNAL OF SYNCHROTRON RADIATION, Issue 1 2008Suresh Narayanan The design and performance of a novel ultra-high-vacuum-compatible artificial channel-cut monochromator that has been commissioned at undulator beamline 8-ID-I at the Advanced Photon Source are presented. Details of the mechanical and optical design, control system implementation and performance of the new device are given. The monochromator was designed to meet the challenging stability and optical requirements of the X-ray photon correlation spectroscopy program hosted at this beamline. In particular, the device incorporates a novel in-vacuum sine-bar drive mechanism for the combined pitch motion of the two crystals and a flexure-based high-stiffness weak-link mechanism for fine-tuning the pitch and roll of the second crystal relative to the first crystal. The monochromator delivers an exceptionally uniform and stable beam and thereby improved brilliance preservation. [source] Observation of interference effects in coherent diffraction of nanocrystals under X-ray standing-wave illuminationJOURNAL OF SYNCHROTRON RADIATION, Issue 6 2007Piotr Gryko Coherent X-ray diffraction is a useful technique for understanding the structure of compact objects including those which can be represented as phase objects. X-rays are highly penetrating and have wavelengths very close to atomic spacing. In this work, gold nanocrystals (on a reflecting substrate) were imaged at the Advanced Photon Source and found to produce a novel double diffraction pattern. Simulations were carried out to explain the experimental diffraction pattern in terms of reflection of the incident beam from the substrate to produce a standing wave. The experimental data were then phased to produce a two-dimensional real-space image of the gold. It is expected that the standing-wave illumination may be a useful tool to aid the convergence of the phasing algorithms for nanocrystals. [source] Zr and Ba edge phenomena in the scintillation intensity of fluorozirconate-based glass-ceramic X-ray detectorsJOURNAL OF SYNCHROTRON RADIATION, Issue 3 2007Bastian Henke The energy-dependent scintillation intensity of Eu-doped fluorozirconate glass-ceramic X-ray detectors has been investigated in the energy range from 10 to 40,keV. The experiments were performed at the Advanced Photon Source, Argonne National Laboratory, USA. The glass ceramics are based on Eu-doped fluorozirconate glasses, which were additionally doped with chlorine to initiate the nucleation of BaCl2 nanocrystals therein. The X-ray excited scintillation is mainly due to the 5d,4f transition of Eu2+ embedded in the BaCl2 nanocrystals; Eu2+ in the glass does not luminesce. Upon appropriate annealing the nanocrystals grow and undergo a phase transition from a hexagonal to an orthorhombic phase of BaCl2. The scintillation intensity is investigated as a function of the X-ray energy, particle size and structure of the embedded nanocrystals. The scintillation intensity versus X-ray energy dependence shows that the intensity is inversely proportional to the photoelectric absorption of the material, i.e. the more photoelectric absorption the less scintillation. At 18 and 37.4,keV a significant decrease in the scintillation intensity can be observed; this energy corresponds to the K -edge of Zr and Ba, respectively. The glass matrix as well as the structure and size of the embedded nanocrystals have an influence on the scintillation properties of the glass ceramics. [source] On the design of ultrafast shutters for time-resolved synchrotron experimentsJOURNAL OF SYNCHROTRON RADIATION, Issue 1 2007Milan Gembicky A comprehensive treatment of the limitations and possibilities for single-pulse selection in synchrotron operating modes with ,150,ns bunch separation, as occurs in the standard operating mode at the Advanced Photon Source, is presented. It is shown that the strength of available materials and allowable kinetic energy build-up limit single-bunch selection for this separation to sample sizes of ,100,µm, and that for minimization of kinetic energy build-up it is preferable to increase the r.p.m. within physically acceptable limits rather than increase the disc radius to obtain a desirable peripheral speed. A slight modification of the equal-bunch spacing standard fill patterns is proposed that allows use of samples as large as 500,µm. The corresponding peripheral speed of the chopper wheel is ,600,m,s,1, which is within the limits of high-strength titanium alloys. For smaller samples, peripheral speeds are proportionally lower. Versatility can be achieved with interchangeable chopper wheels and the use of different orientations of the rotation axis relative to the X-ray beam, which opens the possibility of larger, rather than one-of-a-kind, production runs. [source] A sagittally focusing double-multilayer monochromator for ultrafast X-ray imaging applicationsJOURNAL OF SYNCHROTRON RADIATION, Issue 1 2007Jinyuan Liu The development of a sagittally focusing double-multilayer monochromator is reported, which produces a spatially extended wide-bandpass X-ray beam from an intense synchrotron bending-magnet source at the Advanced Photon Source, for ultrafast X-ray radiography and tomography applications. This monochromator consists of two W/B4C multilayers with a 25,Å period coated on Si single-crystal substrates. The second multilayer is mounted on a sagittally focusing bender, which can dynamically change the bending radius of the multilayer in order to condense and focus the beam to various points along the beamline. With this new apparatus, it becomes possible to adjust the X-ray beam size to best match the area detector size and the object size to facilitate more efficient data collection using ultrafast X-ray radiography and tomography. [source] Radiation driven collapse of protein crystalsJOURNAL OF SYNCHROTRON RADIATION, Issue 1 2006Sébastien Boutet During coherent X-ray diffraction measurements on crystals of ferritin at room temperature using monochromatic undulator radiation from the Advanced Photon Source, a sudden lattice contraction was observed following a characteristic latent period and ultimately leading to the collapse of the crystal. The progression of this collapse is analysed using a two-state Hendricks,Teller model. It reveals that 55% of the layers collapse by 1.6% before the crystal completely stops diffracting. [source] Quantitative high-pressure pair distribution function analysisJOURNAL OF SYNCHROTRON RADIATION, Issue 5 2005John B. Parise The collection of scattering data at high pressure and temperature is now relatively straightforward thanks to developments at high-brightness synchrotron radiation facilities. Reliable data from powders, that are suitable for structure determination and Rietveld refinement, are routinely collected up to about 30,GPa in either a large-volume high-pressure apparatus or diamond anvil cell. In those cases where the total elastic scattering is of interest, as it is in the case of nano-crystalline and glassy materials, technical developments, including the use of focused high-energy X-rays (>80,keV), are advantageous. Recently completed experiments on nano-crystalline materials at the 1-ID beamline at the Advanced Photon Source suggest that quantitative data, suitable for pair distribution function analysis, can be obtained. [source] Facilities for high-pressure research with the diamond anvil cell at GSECARSJOURNAL OF SYNCHROTRON RADIATION, Issue 5 2005Guoyin Shen An overview of facilities for high-pressure research with the diamond anvil cell (DAC) at the GeoSoilEnviroCARS (GSECARS) sector at the Advanced Photon Source (Argonne, Illinois) is presented. There are three operational experimental stations (13-ID-C, 13-ID-D and 13-BM-D) where DAC instrumentation is installed for various types of experiments at high pressure and extreme temperature conditions. A fourth station (13-BM-C) is under construction and will be operational in 2006. While most X-ray diffraction experiments have been undertaken with powder samples so far, there is a growing demand for single-crystal diffraction (SCD) at high pressure. As one of the principal components at GSECARS, SCD is currently under rapid development. Other relevant techniques have also been developed for obtaining complementary information from powder or single-crystal samples at high pressure. For example, an on-line Brillouin system is installed and operational at 13-BM-D for acoustic velocity and single-crystal elasticity determinations. In addition, various X-ray spectroscopy techniques (e.g. X-ray emission and X-ray Raman) are employed for measuring electronic and magnetic properties. Future developments are discussed with the DAC program at GSECARS. [source] An X-ray nanodiffraction technique for structural characterization of individual nanomaterialsJOURNAL OF SYNCHROTRON RADIATION, Issue 2 2005Y. Xiao An X-ray micro/nanodiffraction technique that allows structural characterization of individual nanomaterials has been developed at an insertion-device beamline of the Advanced Photon Source. Using the extremely high brightness of the third-generation synchrotron radiation source and advanced high-resolution high-energy zone-plate focusing optics, X-rays of energies from 6 to 12,keV have been focused into a spot smaller than 200,nm with a photon density gain of more than 50000 so that significant photon flux can be intercepted by a nanoscale material to generate a measurable diffraction signal for structural characterization. This paper describes the instrumentation of the technique and discusses the application of the technique to studies of tin oxide nanobelts. [source] High-resolution wide-angle X-ray scattering of protein solutions: effect of beam dose on protein integrityJOURNAL OF SYNCHROTRON RADIATION, Issue 5 2003Robert F. Fischetti Wide-angle X-ray scattering patterns from proteins in solution contain information relevant to the determination of protein fold. At relevant scattering angles, however, these data are weak, and the degree to which they might be used to categorize the fold of a protein is unknown. Preliminary work has been performed at the BioCAT insertion-device beamline at the Advanced Photon Source which demonstrates that one can collect X-ray scattering data from proteins in solution to spacings of at least 2.2,Å (q = 2.8,Å,1). These data are sensitive to protein conformational states, and are in good agreement with the scattering predicted by the program CRYSOL using the known three-dimensional atomic coordinates of the protein. An important issue in the exploitation of this technique as a tool for structural genomics is the extent to which the high intensity of X-rays available at third-generation synchrotron sources chemically or structurally damage proteins. Various data-collection protocols have been investigated demonstrating conditions under which structural degradation of even sensitive proteins can be minimized, making this technique a viable tool for protein fold categorization, the study of protein folding, unfolding, protein,ligand interactions and domain movement. [source] High-energy diffuse scattering on the 1-ID beamline at the Advanced Photon SourceJOURNAL OF SYNCHROTRON RADIATION, Issue 3 2003T. R. Welberry This paper reports on experiments in which high-energy (65.35,keV) X-rays were used to record the detailed diffuse diffraction patterns of a number of ceramic materials. The methodology has enabled a greater q -range to be explored (up to sin,/,,,,0.97) than is possible with laboratory-based experiments, with better q -space resolution and increased sensitivity, thus allowing previously unseen detail in diffraction patterns to be recorded. In all, 11 sections of data have been collected for Ca-CSZ, eight for Y-CSZ and six for wüstite. [source] Radiation damage of protein crystals at cryogenic temperatures between 40,K and 150,KJOURNAL OF SYNCHROTRON RADIATION, Issue 4 2002Tsu-Yi Teng X-ray radiation damage of lysozyme single crystals by an intense monochromatic beam from the Advanced Photon Source is studied at cryogenic temperatures between 40,K and 150,K. The results confirm that primary radiation damage is both linearly dependent on the X-ray dose and independent of temperature. The upper limit for the primary radiation damage observed in our previous study [Teng & Moffat (2000), J. Synchrotron Rad. 7, 313317] holds over the wider temperature range of this study. The X-ray diffraction quality of the data acquired at 40,K is superior to those at 100,K, apparently due to temperature dependence of secondary and tertiary radiation damage and to reduced thermal motion. [source] Measurement of the speed of X-raysJOURNAL OF SYNCHROTRON RADIATION, Issue 2 2002E. Zolotoyabko X-ray pulses from the Advanced Photon Source at Argonne National Laboratory were used to measure the speed of X-rays in the energy range between 21 and 60,keV. An LiNbO3 -based 0.58,GHz surface acoustic wave device served as a temporal analyzer in the stroboscopic time-resolved diffraction measurements. By synchronizing the surface acoustic wave excitation and periodic X-ray illumination of the LiNbO3 crystal, the temporal modifications in the LiNbO3 diffraction profiles could be followed and the time points of X-ray arrivals at the analyzer position for different analyzer to storage ring distances determined. The speed of the X-rays was determined as the ratio of measured spacings and corresponding delay time intervals. Within the experimental error bars, the obtained X-ray velocities converged to the tabulated constant for the speed of light in a vacuum. [source] The historical development of cryogenically cooled monochromators for third-generation synchrotron radiation sourcesJOURNAL OF SYNCHROTRON RADIATION, Issue 2 2000Donald H. Bilderback In the period of the late-1980s, before the construction of multi-GeV third-generation storage rings with their intense insertion-device sources, the perceived number one problem for X-ray instrumentation was proper cooling of the first optical element in the beamline. This article, first given as an acceptance speech for the Compton Award ceremony at the Advanced Photon Source, presents a somewhat historical and anecdotal overview of how cryogenically cooled monochromator optics have been developed to provide a monochromator cooling solution adequate for today's power levels. A series of workshops and international collaborations were the key components for the progress and final success of this development. [source] Design of a vacuum-compatible high-precision monochromatic beam-position monitor for use with synchrotron radiation from 5 to 25,keVJOURNAL OF SYNCHROTRON RADIATION, Issue 2 2000R. W. Alkire The Structural Biology Center beamline, 19ID, has been designed to take full advantage of the highly intense undulator radiation and very low source emittance available at the Advanced Photon Source. In order to keep the X-ray beam focused onto the pre-sample slits, a novel position-sensitive PIN diode array has been developed. The array consists of four PIN diodes positioned upstream of a 0.5,µm-thick metal foil placed in the X-ray beam. Using conventional difference-over-the-sum techniques, two-dimensional position information is obtained from the metal foil fluorescence. Because the full X-ray beam passes through the metal foil, the true beam center-of-mass is measured. The device is compact, inexpensive to construct, operates in a vacuum and has a working range of 8,mm × 10,mm that can be expanded with design modifications. Measured position sensitivity is 1,2,µm. Although optimized for use in the 5,25,keV energy range, the upper limit can be extended by changing metals or adjusting foil thickness. [source] A new high-speed beam chopper for time-resolved X-ray studiesJOURNAL OF SYNCHROTRON RADIATION, Issue 1 2000Armon McPherson A new high-speed X-ray beam chopper, which can be phase locked to the temporal structure of the Advanced Photon Source (APS) storage ring, has been developed and tested. The open window time of the chopper is 2450,ns, which corresponds to ,67% of the revolution time of the APS storage ring. By phase locking the rotation of the beam chopper to the storage-ring orbital frequency, any portion of the storage-ring fill pattern can be positioned within the beam-chopper transmission-time window. [source] Performance limits of direct cryogenically cooled silicon monochromators , experimental results at the APSJOURNAL OF SYNCHROTRON RADIATION, Issue 1 2000Wah-Keat Lee The successful use of cryogenically cooled silicon monochromators at third-generation synchrotron facilities is well documented. At the Advanced Photon Source (APS) it has been shown that, at 100,mA operation with the standard APS undulator A, the cryogenically cooled silicon monochromator performs very well with minimal (<2 arcsec) or no observable thermal distortions. However, to date there has not been any systematic experimental study on the performance limits of this approach. This paper presents experimental results on the performance limits of these directly cooled crystals. The results show that if the beam is limited to the size of the radiation central cone then, at the APS, the crystal will still perform well at twice the present 100,mA single 2.4,m-long 3.3,cm-period undulator heat load. However, the performance would degrade rapidly if a much larger incident white-beam size is utilized. [source] The Structure of Yttrialite and Its Identification Using Laboratory and Synchrotron-Based Powder X-Ray DiffractionJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2009William J. Heward A highly crystalline sample of the impurity stabilized phase y -Y2Si2O7, generally known as yttrialite, has been formed from the melt of a glass with a nominal composition of 62(SiO2),10(Al2O3),28(Y2O3) mol%. Powder X-ray diffraction patterns were collected using in-house instrumentation and the 11-BM diffractometer at the Advanced Photon Source, Argonne National Laboratory, Argonne, IL. Rietveld refinements were carried out on the patterns using two structural models. On patterns collected using in-house instrumentation the correct structure assignment was difficult to determine; however, the extremely high-quality data afforded by the 11-BM instrument showed conclusively that the sample was found to crystallize in the monoclinic system (SG=P21/m) with lattice parameters a=5.03032(6), b=8.06892(6), c=7.33620(6) Å, and ,=108.673(1). Furthermore, simulations have shown that it is likely that this structure model can be used to describe natural yttrialite or yttrialite that is formed at low temperatures, though the possibility that such materials are paracrystalline is also discussed. [source] Imaging of cochlear tissue with a grating interferometer and hard X-raysMICROSCOPY RESEARCH AND TECHNIQUE, Issue 12 2009Claus-Peter Richter Abstract This article addresses an important current development in medical and biological imaging: the possibility of imaging soft tissue at resolutions in the micron range using hard X-rays. Challenging environments, including the cochlea, require the imaging of soft tissue structure surrounded by bone. We demonstrate that cochlear soft tissue structures can be imaged with hard X-ray phase contrast. Furthermore, we show that only a thin slice of the tissue is required to introduce a large phase shift. It is likely that the phase contrast image of the soft tissue structures is sufficient to image the structures even if surrounded by bone. For the present set of experiments, structures with low-absorption contrast have been visualized using in-line phase contrast imaging and a grating interferometer. The experiments have been performed at the Advanced Photon Source at Argonne National Laboratories, a third generation source of synchrotron radiation. The source provides highly coherent X-ray radiation with high-photon flux (>1012 photons/s) at high-photon energies (5,70 keV). Radiographic and light microscopy images of the gerbil cochlear slice samples were compared. It has been determined that a 20-,m thick tissue slice induces a phase shift between 1/3, and 2/3,. Microsc. Res. Tech., 2009. © 2009 Wiley-Liss, Inc. [source] High pressure structure of Tb2Ti2O7 pyrochlore at cryogenic temperaturesPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 1 2007Ravhi S. Kumar Abstract The structure of Tb2Ti2O7 pyrochlore was investigated at high pressures up to 24 GPa at cryogenic temperatures down to 6.5 K using angular dispersive X-ray diffraction with synchrotron radiation at HPCAT, Advanced Photon Source. The cell parameters were obtained by performing full profile Rietveld refinements of the diffraction data. The equation of state is obtained at low temperatures by fitting the pressure-volume data to a second order Birch Murnaghan eqation and a bulk modulus value of 168(4) GPa is obtained. The results show persistance of the pyrochlore structure up to the maximum pressure studied in the experiment and further indicate that pressure induces solely magnetic ordering which do not involve crystal symmetry changes. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Excited-state molecular structures captured by X-ray transient absorption spectroscopy: a decade and beyondACTA CRYSTALLOGRAPHICA SECTION A, Issue 2 2010Lin X. Chen Transient molecular structures along chemical reaction pathways are important for predicting molecular reactivity, understanding reaction mechanisms, as well as controlling reaction pathways. During the past decade, X-ray transient absorption spectroscopy (XTA, or LITR-XAS, laser-initiated X-ray absorption spectroscopy), analogous to the commonly used optical transient absorption spectroscopy, has been developed. XTA uses a laser pulse to trigger a fundamental chemical process, and an X-ray pulse(s) to probe transient structures as a function of the time delay between the pump and probe pulses. Using X-ray pulses with high photon flux from synchrotron sources, transient electronic and molecular structures of metal complexes have been studied in disordered media from homogeneous solutions to heterogeneous solution,solid interfaces. Several examples from the studies at the Advanced Photon Source in Argonne National Laboratory are summarized, including excited-state metalloporphyrins, metal-to-ligand charge transfer (MLCT) states of transition metal complexes, and charge transfer states of metal complexes at the interface with semiconductor nanoparticles. Recent developments of the method are briefly described followed by a future prospective of XTA. It is envisioned that concurrent developments in X-ray free-electron lasers and synchrotron X-ray facilities as well as other table-top laser-driven femtosecond X-ray sources will make many breakthroughs and realise dreams of visualizing molecular movies and snapshots, which ultimately enable chemical reaction pathways to be controlled. [source] Single-crystal diffuse scattering studies on polymorphs of molecular crystals.ACTA CRYSTALLOGRAPHICA SECTION B, Issue 3 2009The drug benzocaine (ethyl 4-aminobenzoate), commonly used as a local anaesthetic, is a bimorphic solid at room temperature. Form (I) is monoclinic P21/c, while the metastable form (II) is orthorhombic P212121. Three-dimensional diffuse X-ray scattering data have been collected for the two forms on the 11-ID-B beamline at the Advanced Photon Source (APS). Both forms show strong and highly structured diffuse scattering. The data have been interpreted and analysed using Monte Carlo (MC) modelling on the basis that the scattering is purely thermal in origin and indicates the presence of highly correlated molecular motions. In both forms (I) and (II) broad diffuse streaks are observed in the 0kl section which indicate strong longitudinal displacement correlations between molecules in the ,031, directions, extending over distances of up to 50,Å. Streaks extending between Bragg peaks in the hk0 section normal to [100] correspond to correlated motions of chains of molecules extending along a that are linked by N,H...O=C hydrogen bonds and which occur together as coplanar ribbon pairs. The main difference between the two forms is in the dynamical behaviour of the ribbon pairs and in particular how they are able to slide relative to each other. While for form (I) a model involving harmonic springs is able to describe the motion satisfactorily, as simple excursions away from the average structure, there is evidence in form (II) of anharmonic effects that are precursors of a phase transition to a new low-temperature phase, form (III), that was subsequently found. [source] Crystallization and preliminary X-ray analysis of UDP- N -acetylenolpyruvylglucosamine reductase (MurB) from Staphylococcus aureusACTA CRYSTALLOGRAPHICA SECTION D, Issue 7 2001Melissa S. Harris UDP- N -acetylenolpyruvylglucosamine reductase (MurB) is an essential enzyme in the bacterial cell-wall biosynthetic pathway, making it a potential therapeutic target for novel antibiotics. Diffraction-quality crystals of both the native and Se-methionine-expressed MurB from Staphylococcus aureus have been prepared by sitting-drop vapour diffusion from solutions containing polyethylene glycol (PEG) 8000, ammonium sulfate, sodium cacodylate pH 6.5 and dimethyl sulfoxide (DMSO). Crystals belong to the cubic space group I213, with unit-cell parameters a = b = c = 178.99,Å. X-ray data from these crystals were collected at the Advanced Photon Source 17-ID beamline and were used to solve the MurB structure to 2.3,Å resolution. [source] Crystallization and preliminary X-ray analysis of Ebola VP35 interferon inhibitory domain mutant proteinsACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 6 2010Daisy W. Leung VP35 is one of seven structural proteins encoded by the Ebola viral genome and mediates viral replication, nucleocapsid formation and host immune suppression. The C-terminal interferon inhibitory domain (IID) of VP35 is critical for dsRNA binding and interferon inhibition. The wild-type VP35 IID structure revealed several conserved residues that are important for dsRNA binding and interferon antagonism. Here, the expression, purification and crystallization of recombinant Zaire Ebola VP35 IID mutants R312A, K319A/R322A and K339A in space groups P6122, P212121 and P21, respectively, are described. Diffraction data were collected using synchrotron sources at the Advanced Light Source and the Advanced Photon Source. [source] Cloning, expression, purification, crystallization and preliminary X-ray diffraction analysis of macrophage growth locus A (MglA) protein from Francisella tularensisACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 5 2010Priadarsini Subburaman Francisella tularensis, a potential bioweapon, causes a rare infectious disease called tularemia in humans and animals. The macrophage growth locus A (MglA) protein from F. tularensis associates with RNA polymerase to positively regulate the expression of multiple virulence factors that are required for its survival and replication within macrophages. The MglA protein was overproduced in Escherichia coli, purified and crystallized. The crystals diffracted to 7.5,Å resolution at the Advanced Photon Source, Argonne National Laboratory and belonged to the hexagonal space group P61 or P65, with unit-cell parameters a = b = 125, c = 54,Å. [source] Preliminary neutron and X-ray crystallographic studies of equine cyanomethemoglobinACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 4 2010A. Y. Kovalevsky Room-temperature and 100,K X-ray and room-temperature neutron diffraction data have been measured from equine cyanomethemoglobin to 1.7,Å resolution using a home source, to 1.6,Å resolution on NE-CAT at the Advanced Photon Source and to 2.0,Å resolution on the PCS at Los Alamos Neutron Science Center, respectively. The cyanomethemoglobin is in the R state and preliminary room-temperature electron and neutron scattering density maps clearly show the protonation states of potential Bohr groups. Interestingly, a water molecule that is in the vicinity of the heme group and coordinated to the distal histidine appears to be expelled from this site in the low-temperature structure. [source] Crystallization and preliminary X-ray diffraction of the DEAD-box protein Mss116p complexed with an RNA oligonucleotide and AMP-PNPACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 8 2009Mark Del Campo The Saccharomyces cerevisiae DEAD-box protein Mss116p is a general RNA chaperone which functions in mitochondrial group I and group II intron splicing, translation and RNA-end processing. For crystallization trials, full-length Mss116p and a C-terminally truncated protein (Mss116p/,598,664) were overproduced in Escherichia coli and purified to homogeneity. Mss116p exhibited low solubility in standard solutions (,1,mg,ml,1), but its solubility could be increased by adding 50,mMl -arginine plus 50,mMl -glutamate and 50% glycerol to achieve concentrations of ,10,mg,ml,1. Initial crystals were obtained by the microbatch method in the presence of a U10 RNA oligonucleotide and the ATP analog AMP-PNP and were then improved by using seeding and sitting-drop vapor diffusion. A cryocooled crystal of Mss116p/,598,664 in complex with AMP-PNP and U10 belonged to space group P21212, with unit-cell parameters a = 88.54, b = 126.52, c = 55.52,Å, and diffracted X-rays to beyond 1.9,Å resolution using synchrotron radiation from sector 21 at the Advanced Photon Source. [source] |