WorldWideScience

Sample records for acid x-ray crystallography

  1. X-ray Crystallography Facility

    2000-01-01

    Edward Snell, a National Research Council research fellow at NASA's Marshall Space Flight Center (MSFC), prepares a protein crystal for analysis by x-ray crystallography as part of NASA's structural biology program. The small, individual crystals are bombarded with x-rays to produce diffraction patterns, a map of the intensity of the x-rays as they reflect through the crystal.

  2. X-ray crystallography

    2001-01-01

    X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

  3. X-ray lasers and crystallography

    Spence, John C. H.

    2014-01-01

    The development of X-ray lasers and their applications in crystallography is described. In the birth of this new field, IUCrJ is ideally positioned to present this research to both specialists in crystallography, and to the wider audience in structural biology.

  4. X-Ray Crystallography Reagent

    Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

    2003-01-01

    Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes per square centimeter at the interface. By placing the microcapsules in a high osmotic dewatering solution. the protein solution is gradually made saturated and then supersaturated. and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged. protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D smucture of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

  5. Early days of X-ray crystallography

    Authier, André

    2013-01-01

    This book relates the discovery itself, the early days of X-ray crystallography, and the way the news of the discovery spread round the world. It explains how the first crystal structures were determined, and recounts which were the early applications of X-ray crystallography. It also tells how the concept of space lattice has developed since ancient times, and how our understanding of the nature of light has changed over time. The contributions of the main actors of the story, prior to the discovery, at the time of the discovery and immediately afterwards, are described through their writings and are put into the context of the time, accompanied by brief biographical details.

  6. Structure determination by X-ray crystallography

    Ladd, M F C

    1977-01-01

    Crystallography may be described as the science of the structure of materi­ als, using this word in its widest sense, and its ramifications are apparent over a broad front of current scientific endeavor. It is not surprising, therefore, to find that most universities offer some aspects of crystallography in their undergraduate courses in the physical sciences. It is the principal aim of this book to present an introduction to structure determination by X-ray crystal­ lography that is appropriate mainly to both final-year undergraduate studies in crystallography, chemistry, and chemical physics, and introductory post­ graduate work in this area of crystallography. We believe that the book will be of interest in other disciplines, such as physics, metallurgy, biochemistry, and geology, where crystallography has an important part to play. In the space of one book, it is not possible either to cover all aspects of crystallography or to treat all the subject matter completely rigorously. In particular, certain ...

  7. Structure determination by X-ray crystallography

    Ladd, M F C

    1995-01-01

    X-ray crystallography provides us with the most accurate picture we can get of atomic and molecular structures in crystals. It provides a hard bedrock of structural results in chemistry and in mineralogy. In biology, where the structures are not fully crystalline, it can still provide valuable results and, indeed, the impact here has been revolutionary. It is still an immense field for young workers, and no doubt will provide yet more striking develop­ ments of a major character. It does, however, require a wide range of intellectual application, and a considerable ability in many fields. This book will provide much help. It is a very straightforward and thorough guide to every aspect of the subject. The authors are experienced both as research workers themselves and as teachers of standing, and this is shown in their clarity of exposition. There are plenty of iliustrations and worked examples to aid the student to obtain a real grasp of the subject.

  8. Neutron Nucleic Acid Crystallography.

    Chatake, Toshiyuki

    2016-01-01

    The hydration shells surrounding nucleic acids and hydrogen-bonding networks involving water molecules and nucleic acids are essential interactions for the structural stability and function of nucleic acids. Water molecules in the hydration shells influence various conformations of DNA and RNA by specific hydrogen-bonding networks, which often contribute to the chemical reactivity and molecular recognition of nucleic acids. However, X-ray crystallography could not provide a complete description of structural information with respect to hydrogen bonds. Indeed, X-ray crystallography is a powerful tool for determining the locations of water molecules, i.e., the location of the oxygen atom of H2O; however, it is very difficult to determine the orientation of the water molecules, i.e., the orientation of the two hydrogen atoms of H2O, because X-ray scattering from the hydrogen atom is very small.Neutron crystallography is a specialized tool for determining the positions of hydrogen atoms. Neutrons are not diffracted by electrons, but are diffracted by atomic nuclei; accordingly, neutron scattering lengths of hydrogen and its isotopes are comparable to those of non-hydrogen atoms. Therefore, neutron crystallography can determine both of the locations and orientations of water molecules. This chapter describes the current status of neutron nucleic acid crystallographic research as well as the basic principles of neutron diffraction experiments performed on nucleic acid crystals: materials, crystallization, diffraction experiments, and structure determination. PMID:26227050

  9. X-ray diffraction crystallography. Introduction, examples and solved problems

    Waseda, Yoshio; Shinoda, Kozo [Tohoku Univ., Sendai (Japan). Inst. of Multidisciplinary Research for Advanced Materials; Matsubara, Eiichiro [Kyoto Univ. (Japan). Dept. of Materials Science and Engineering

    2011-07-01

    X-ray diffraction crystallography for powder samples is a well-established and widely used method. It is applied to materials characterization to reveal the atomic scale structure of various substances in a variety of states. The book deals with fundamental properties of X-rays, geometry analysis of crystals, X-ray scattering and diffraction in polycrystalline samples and its application to the determination of the crystal structure. The reciprocal lattice and integrated diffraction intensity from crystals and symmetry analysis of crystals are explained. To learn the method of X-ray diffraction crystallography well and to be able to cope with the given subject, a certain number of exercises is presented in the book to calculate specific values for typical examples. This is particularly important for beginners in X-ray diffraction crystallography. One aim of this book is to offer guidance to solving the problems of 90 typical substances. For further convenience, 100 supplementary exercises are also provided with solutions. Some essential points with basic equations are summarized in each chapter, together with some relevant physical constants and the atomic scattering factors of the elements. (orig.)

  10. Polycapillary x-ray optics for macromolecular crystallography

    Polycapillary x-ray optics have found potential application in many different fields, including antiscatter and magnification in mammography, radiography, x-ray fluorescence, x-ray lithography, and x-ray diffraction techniques. In x-ray diffraction, an optic is used to collect divergent x-rays from a point source and redirect them into a quasi-parallel, or slightly focused beam. Monolithic polycapillary optics have been developed recently for macromolecular crystallography and have already shown considerable gains in diffracted beam intensity over pinhole collimation. Development is being pursued through a series of simulations and prototype optics. Many improvements have been made over the stage 1 prototype reported previously, which include better control over the manufacturing process, reducing the diameter of the output beam, and addition of a slight focusing at the output of the optic to further increase x-ray flux at the sample. The authors report the characteristics and performance of the stage 1 and stage 2 optics

  11. The 100th Anniversary of X-Ray Crystallography

    Kojić-Prodić, B.

    2013-07-01

    Full Text Available The important thing in science is not so much to obtain new facts as to discover new ways of thinking about them.W. L. BraggThe 100th anniversary of X-ray crystallography dates back to the first X-ray diffraction experiment on a crystal of copper sulphate pentahydrate. Max von Laue designed the theoretical background of the experiment, which was performed by German physicists W. Friedrich and P. Knipping in 1912. At that time, the mathematical formulation of the phenomenon and the fundamental concepts of crystallography were subjects of mineralogy. Altogether, they facilitated the development of methods for determination of the structure of matter at the atomic level. In 1913, father and son Bragg started to develop X-ray structure analysis for determination of crystal structures of simple molecules. Historic examples of structure determination starting from rock salt to complex, biologically important (macromolecules, such as globular proteins haemoglobin and myoglobin, DNA, vitamin B12 and the recent discovery of ribozyme, illustrate the development of X-ray structural analysis. The determination of 3D structures of these molecules by X-ray diffraction had opened new areas of scientific research, such as molecular biophysics, molecular genetics, structural molecular biology, bioinorganic chemistry, organometallic chemistry, and many others. The discovery and development of X-ray crystallography revolutionised our understanding of natural sciences – physics, chemistry, biology, and also science of materials. The scientific community recognised these fundamental achievements (including the discovery of X-rays by awarding twenty-eight Nobel prizes to thirty-nine men and two women. The explosive growth of science and technology in the 20th and 21st centuries had been founded on the detailed knowledge of the three-dimensional structure of molecules, which was the basis for explaining and predicting the physical, chemical, biological and

  12. A Compact X-Ray System for Macromolecular Crystallography

    Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Gibson, Walter; Joy, Marshall

    2000-01-01

    We describe the design and performance of a high flux x-ray system for a macromolecular crystallography that combines a microfocus x-ray generator (40 micrometer full width at half maximum spot size at a power level of 46.5 W) and a collimating polycapillary optic. The Cu Ka lpha x-ray flux produced by this optimized system through a 500,um diam orifice is 7.0 times greater than the x-ray flux previously reported by Gubarev et al. [M. Gubarev et al., J. Appl. Crystallogr. 33, 882 (2000)]. The x-ray flux from the microfocus system is also 2.6 times higher than that produced by a rotating anode generator equipped with a graded multilayer monochromator (green optic, Osmic Inc. CMF24-48-Cu6) and 40% less than that produced by a rotating anode generator with the newest design of graded multilayer monochromator (blue optic, Osmic, Inc. CMF12-38-Cu6). Both rotating anode generators operate at a power level of 5000 W, dissipating more than 100 times the power of our microfocus x-ray system. Diffraction data collected from small test crystals are of high quality. For example, 42 540 reflections collected at ambient temperature from a lysozyme crystal yielded R(sub sym)=5.0% for data extending to 1.70 A, and 4.8% for the complete set of data to 1.85 A. The amplitudes of the observed reflections were used to calculate difference electron density maps that revealed positions of structurally important ions and water molecules in the crystal of lysozyme using the phases calculated from the protein model.

  13. A Compact X-Ray System for Macromolecular Crystallography. 5

    Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Joy, Marshall

    2000-01-01

    We describe the design and performance of a high flux x-ray system for macromolecular crystallography that combines a microfocus x-ray generator (40 gm FWHM spot size at a power level of 46.5Watts) and a 5.5 mm focal distance polycapillary optic. The Cu K(sub alpha) X-ray flux produced by this optimized system is 7.0 times above the X-ray flux previously reported. The X-ray flux from the microfocus system is also 3.2 times higher than that produced by the rotating anode generator equipped with a long focal distance graded multilayer monochromator (Green optic; CMF24-48-Cu6) and 30% less than that produced by the rotating anode generator with the newest design of graded multilayer monochromator (Blue optic; CMF12-38-Cu6). Both rotating anode generators operate at a power level of 5000 Watts, dissipating more than 100 times the power of our microfocus x-ray system. Diffraction data collected from small test crystals are of high quality. For example, 42,540 reflections collected at ambient temperature from a lysozyme crystal yielded R(sub sym) 5.0% for the data extending to 1.7A, and 4.8% for the complete set of data to 1.85A. The amplitudes of the reflections were used to calculate difference electron density maps that revealed positions of structurally important ions and water molecules in the crystal of lysozyme using the phases calculated from the protein model.

  14. Sub-atomic resolution X-ray crystallography and neutron crystallography: promise, challenges and potential

    Matthew P. Blakeley

    2015-07-01

    Full Text Available The International Year of Crystallography saw the number of macromolecular structures deposited in the Protein Data Bank cross the 100000 mark, with more than 90000 of these provided by X-ray crystallography. The number of X-ray structures determined to sub-atomic resolution (i.e. ≤1 Å has passed 600 and this is likely to continue to grow rapidly with diffraction-limited synchrotron radiation sources such as MAX-IV (Sweden and Sirius (Brazil under construction. A dozen X-ray structures have been deposited to ultra-high resolution (i.e. ≤0.7 Å, for which precise electron density can be exploited to obtain charge density and provide information on the bonding character of catalytic or electron transfer sites. Although the development of neutron macromolecular crystallography over the years has been far less pronounced, and its application much less widespread, the availability of new and improved instrumentation, combined with dedicated deuteration facilities, are beginning to transform the field. Of the 83 macromolecular structures deposited with neutron diffraction data, more than half (49/83, 59% were released since 2010. Sub-mm3 crystals are now regularly being used for data collection, structures have been determined to atomic resolution for a few small proteins, and much larger unit-cell systems (cell edges >100 Å are being successfully studied. While some details relating to H-atom positions are tractable with X-ray crystallography at sub-atomic resolution, the mobility of certain H atoms precludes them from being located. In addition, highly polarized H atoms and protons (H+ remain invisible with X-rays. Moreover, the majority of X-ray structures are determined from cryo-cooled crystals at 100 K, and, although radiation damage can be strongly controlled, especially since the advent of shutterless fast detectors, and by using limited doses and crystal translation at micro-focus beams, radiation damage can still take place

  15. Contribution of X-ray crystallography in energy related problems

    Crystallography is concerned with the study of the structure of matter at the atomic level in condensed state. The great practical importance of scientific knowledge of the structure of solid is self evident when consideration is given to the definition of desired physical and chemical properties. The strength of steel girders, the corrosion of alloys, the plasticity of lime, the wearing properties of case hardness steel, the dielectric capacity of materials, the lubricating properties of long chain paraffin's or of graphite, the stretching of rubber and innumerable other practical phenomena of every day life depend upon ultimate structure of these materials. To understand function to control, manipulate and best utilize their properties, and to produce materials with properties meeting a desired set of specification it is essential to understand thoroughly both the characteristics and origin of each property. Origins of materials properties lie in a combination of natural laws with the detailed structure and composition of materials, i.e. the choice, location, bonding, etc. of every atom in the material object. Therefore, to understand their various properties, it is important to explore the structure property relationship in materials. X-ray crystallography is not only helping to develop new materials having desired properties, but also in improving existing materials. Radiation effects, electrolytes, superconductors and catalysts etc. are just a few examples of many areas where crystallography is helping. With the invent of new radiation sources like synchrotron and new detectors materials and techniques, this almost 80 years old discipline continues to capture the interest of solid state physicists and chemists alike. (author)

  16. X-ray detectors for soft X-ray macromolecular crystallography

    Full text: Modern protein crystallography ultimately makes use of the two-dimensional position - sensitive detectors such as Image Plates and CCD with scintillation convertors coupled with fiber optics for detection of X-Ray diffraction pictures taken from macromolecular crystals. These detectors have high efficiency for 1.5-1.0 A synchrotron radiation, special resolution ∼80-50 μm and large effective area (i.e. Σ 300 mm2 for large MAR Image Plate). Both of these types of detectors lack energy resolution. A major drawback of Image Plates is long read-out time (2.5-4 minutes). CCD based devices permit data collection in a real time, however at present they are much more expensive. One of the novel and very promising trends in protein crystallography is to use soft X-ray synchrotron radiation between 2.2 keV and 6 keV (5.6 to 2.5 A) and there is an urgent need to develop suitable detection system for these kinds of applications. It is to be two- dimensional positional sensitive detector with pitch of about 10 to 20 μm, high efficiency and real-time readout. An active area of the detector is to be at least 20 x 20 mm2. It seems to be the simplest solution to use conventional direct-illumination CCD detectors because absorption length of the 5 A radiation in silicon is about 3 μm. However they lack, for example, energy resolution and optimum solution of the problem has yet to come. (author)

  17. X-Ray Crystallography: One Century of Nobel Prizes

    Galli, Simona

    2014-01-01

    In 2012, the United Nations General Assembly declared 2014 the International Year of Crystallography. Throughout the year 2014 and beyond, all the crystallographic associations and societies active all over the world are organizing events to attract the wider public toward crystallography and the numerous topics to which it is deeply interlinked.…

  18. A Compact X-Ray System for Support of High Throughput Crystallography

    Ciszak, Ewa; Gubarev, Mikhail; Gibson, Walter M.; Joy, Marshall K.; Whitaker, Ann F. (Technical Monitor)

    2001-01-01

    Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

  19. Synthesis, spectroscopy, X-ray crystallography, and DFT computations of nanosized phosphazenes

    Shariatinia, Z.; Moghadam, E.J.; Maghsoudi, N.; Mousavi, H.S.M.; Dušek, Michal; Eigner, Václav

    2015-01-01

    Roč. 641, č. 5 (2015), s. 967-978. ISSN 0044-2313 Grant ostatní: AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : phosphazene * ultrasonic * nanoparticle * x-ray crystallography * DFT calculation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.160, year: 2014

  20. Structural investigation of bistrifluron using x-ray crystallography, NMR spectroscopy, and molecular modeling

    Moon, J K; Rhee, S K; Kim, G B; Yun, H S; Chung, B J; Lee, S S; Lim, Y H

    2002-01-01

    A new insecticide, bistrifluron acts as an inhibitor of insect development and interferes with the cuticle formation of insects. Since it shows low acute oral and dermal toxicities, it can be one of potent insecticides. Based on X-ray crystallography, NMR spectroscopy and molecular modeling, the structural studies of bistrifluron have been carried out.

  1. Apparatus and method for nanoflow liquid jet and serial femtosecond x-ray protein crystallography

    Bogan, Michael J.; Laksmono, Hartawan; Sierra, Raymond G.

    2016-03-01

    Techniques for nanoflow serial femtosecond x-ray protein crystallography include providing a sample fluid by mixing a plurality of a first target of interest with a carrier fluid and injecting the sample fluid into a vacuum chamber at a rate less than about 4 microliters per minute. In some embodiments, the carrier fluid has a viscosity greater than about 3 centipoise.

  2. First Results from a Microfocus X-Ray System for Macromolecular Crystallography

    Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Gibson, Walter; Joy, Marshall

    1999-01-01

    The design and performance of a 40 Watt laboratory crystallography system optimized for the structure determination of small protein crystals are described. This system combines a microfocus x-ray generator (40 microns FWHM spot size at a power level of 40 Watts) and a short focal length (F = 2.6 mm) polycapillary collimating optic, and produces a small diameter quasi-parallel x-ray beam. Measurements of x-ray flux, divergence and spectral purity of the resulting x-ray beam are presented. The x-ray flux in a 250 microns diameter aperture produced by the microfocus system is 14.7 times higher .than that from a 3.15 kW rotating anode generator equipped with graphite monochromator. Crystallography data taken with the microfocus system are presented, and indicate that the divergence and spectral purity of the x-ray are sufficient to refine the diffraction data using a standard crystallographic software. Significant additional improvements in flux and beam divergence are possible, and plans for achieving these coals are discussed.

  3. X-ray Crystallography in Open-Framework Materials.

    Bloch, Witold M; Champness, Neil R; Doonan, Christian J

    2015-10-26

    Open-framework materials, such as metal-organic frameworks (MOFs) and coordination polymers have been widely investigated for their gas adsorption and separation properties. However, recent studies have demonstrated that their highly crystalline structures can be used to periodically organize guest molecules and non-structural metal compounds either within their pore voids or by anchoring to their framework architecture. Accordingly, the open framework can act as a matrix for isolating and elucidating the structures of these moieties by X-ray diffraction. This concept has broad scope for development as an analytical tool where obtaining single crystals of a target molecule presents a significant challenge and it additionally offers potential for obtaining insights into chemically reactive species that can be stabilized within the pore network. However, the technique does have limitations and as yet a general experimental method has not been realized. Herein we focus on recent examples in which framework materials have been utilized as a scaffold for ordering molecules for analysis by diffraction methods and canvass areas for future exploration. PMID:26373458

  4. Visualization of X-ray Beam Using CdWO4 Crystal for Macromolecular Crystallography

    Kazimierz J. Gofron

    2011-12-01

    Full Text Available In synchrotron diffraction experiments, it is typically assumed that the X-ray beam at the sample position is uniform, stable and has dimensions that are controlled by the focus and slits settings. As might be expected, this process is much more complex. We present here an investigation of the properties of a synchrotron X-ray beam at the sample position. The X-ray beam is visualized with a single crystal scintillator that converts X-ray photons into visible light photons, which can be imaged using Structure Biology Center (SBC on-axis and off-axis microscope optics. The X-ray penetration is dependent on the composition of the scintillator (especially the effective Z, and X-ray energy. Several scintillators have been used to visualize X-ray beams. Here we compare CdWO4, PbWO4, Bi4Ge3O12, Y3Al5O12:Ce (YAG:Ce, and Gd2O2S:Tb (phosphor. We determined that scintillator crystals made of CdWO4 and similar high-Z materials are best suited for the energy range (7–20 keV and are most suitable for beam visualization for macromolecular crystallography applications. These scintillators show excellent absorption, optical, and mechanical properties.

  5. Synthesis, X-ray crystallography, spectroscopy, electrochemistry, thermal and kinetic study of uranyl Schiff base complexes

    Asadi, Z.; Golzard, F.; Eigner, Václav; Dušek, Michal

    2013-01-01

    Roč. 66, č. 20 (2013), s. 3629-3646. ISSN 0095-8972 R&D Projects: GA ČR(CZ) GAP204/11/0809 Institutional support: RVO:68378271 Keywords : X-ray crystallography * uranyl Schiff base complex * kinetics of thermal decomposition * cyclic voltammetry * kinetics and mechanism Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.224, year: 2013

  6. Time-resolved protein nano-crystallography using an X-ray free-electron laser

    We demonstrate the use of an X-ray free electron laser synchronized with an optical pump laser to obtain X-ray diffraction snapshots from the photo-activated states of large membrane protein complexes in the form of nano-crystals flowing in a liquid jet. Light-induced changes of Photosystem I-Ferredoxin co-crystals were observed at time delays of 5 to 10 μs after excitation. The result correlates with the microsecond kinetics of electron transfer from Photosystem I to ferredoxin. The undocking process that follows the electron transfer leads to large rearrangements in the crystals that will terminally lead to the disintegration of the crystals. We describe the experimental setup and obtain the first time resolved femtosecond serial X-ray crystallography results from an irreversible photo-chemical reaction at the Linac Coherent Light Source. This technique opens the door to time-resolved structural studies of reaction dynamics in biological systems. (authors)

  7. Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature

    Tsujino, Soichiro; Tomizaki, Takashi

    2016-01-01

    Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinning of the crystal within a levitating droplet ensured an efficient sampling of the reciprocal space. The datasets were processed with a program suite developed for serial femtosecond crystallography (SFX). The structure, which was solved by molecular replacement, was found to be identical to the structure obtained by the conventional oscillation method for up to a 1.8-Å resolution limit. In particular, the absence of protein crystal damage resulting from the acoustic levitation was carefully established. These results represent a key step towards a fully automated sample handling and measurement pipeline, which has promising prospects for a high acquisition rate and high sample efficiency for room temperature X-ray crystallography. PMID:27150272

  8. Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature.

    Tsujino, Soichiro; Tomizaki, Takashi

    2016-01-01

    Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinning of the crystal within a levitating droplet ensured an efficient sampling of the reciprocal space. The datasets were processed with a program suite developed for serial femtosecond crystallography (SFX). The structure, which was solved by molecular replacement, was found to be identical to the structure obtained by the conventional oscillation method for up to a 1.8-Å resolution limit. In particular, the absence of protein crystal damage resulting from the acoustic levitation was carefully established. These results represent a key step towards a fully automated sample handling and measurement pipeline, which has promising prospects for a high acquisition rate and high sample efficiency for room temperature X-ray crystallography. PMID:27150272

  9. A spherical drift chamber area detector for X-ray crystallography

    Bolon, C; Lanza, R; Quigley, G; Rich, A

    1979-01-01

    A multiwire proportional chamber system has been built as an area detector for use in X-ray crystallography with Cu K/sub alpha / radiation (1.54AA). The chamber, constructed by Charpak and collaborators at CERN, consists of a 10cm thick spherical interaction region with a radial electric field, a transition from spherical to plane geometry and a 50cm*50cm multiwire proportional chamber and subtends a 90 degrees opening angle. Two dimensional position information is obtained from orthogonal cathode planes using a high speed analog centroid finding technique. Data on spatial and energy resolution as a function of angle and depth of interaction in the spherical drift region using a collimated, pulsed, X-ray source are presented. Ionization loss as a function of drift distance and field and loss due to field shaping grids has also been measured. (6 refs).

  10. Dose, exposure time, and resolution in Serial X-ray Crystallography

    Starodub, D; Hembree, G; Howells, M; Shapiro, D; Chapman, H N; Fromme, P; Schmidt, K; Weierstall, U; Doak, R B; Spence, J C H

    2007-01-01

    The resolution of X-ray diffraction microscopy is limited by the maximum dose that can be delivered prior to sample damage. In the proposed Serial Crystallography method, the damage problem is addressed by distributing the total dose over many identical hydrated macromolecules running continuously in a single-file train across a continuous X-ray beam, and resolution is then limited only by the available molecular and X-ray fluxes and molecular alignment. Orientation of the diffracting molecules is achieved by laser alignment. We evaluate the incident X-ray fluence (energy/area) required to obtain a given resolution from (1) an analytical model, giving the count rate at the maximum scattering angle for a model protein, (2) explicit simulation of diffraction patterns for a GroEL-GroES protein complex, and (3) the frequency cut off of the transfer function following iterative solution of the phase problem, and reconstruction of an electron density map in the projection approximation. These calculations include c...

  11. Large area high-resolution CCD-based X-ray detector for macromolecular crystallography

    Pokric, M; Jorden, A R; Cox, M P; Marshall, A; Long, P G; Moon, K; Jerram, P A; Pool, P; Nave, C; Derbyshire, G E; Helliwell, J R

    2002-01-01

    An X-ray detector system for macromolecular crystallography based on a large area charge-coupled device (CCD) sensor has been developed as part of a large research and development programme for advanced X-ray sensor technology, funded by industry and the Particle Physics and Astronomy Research Council (PPARC) in the UK. The prototype detector consists of two large area three-sides buttable charge-coupled devices (CCD 46-62 EEV), where the single CCD area is 55.3 mmx41.5 mm. Overall detector imaging area is easily extendable to 85 mmx110 mm. The detector consists of an optically coupled X-ray sensitive phosphor, skewed fibre-optic studs and CCDs. The crystallographic measurement requirements at synchrotron sources are met through a high spatial resolution (2048x1536 pixel array), high dynamic range (approx 10 sup 5), a fast readout (approx 1 s), low noise (<10e sup -) and much reduced parallax error. Additionally, the prototype detector system has been optimised by increasing its efficiency at low X-ray ene...

  12. Three-dimensional theory of emittance in Compton scattering and x-ray protein crystallography

    A complete, three-dimensional theory of Compton scattering is described, which fully takes into account the effects of the electron beam emittance and energy spread upon the scattered x-ray spectral brightness. The radiation scattered by an electron subjected to an arbitrary electromagnetic field distribution in vacuum is first derived in the linear regime, and in the absence of radiative corrections; it is found that each vacuum eigenmode gives rise to a single Doppler-shifted classical dipole excitation. This formalism is then applied to Compton scattering in a three-dimensional laser focus, and yields a complete description of the influence of the electron beam phase-space topology on the x-ray spectral brightness; analytical expressions including the effects of emittance and energy spread are also obtained in the one-dimensional limit. Within this framework, the x-ray brightness generated by a 25 MeV electron beam is modeled, fully taking into account the beam emittance and energy spread, as well as the three-dimensional nature of the laser focus; its application to x-ray protein crystallography is outlined. Finally, coherence, harmonics, and radiative corrections are also briefly discussed

  13. Analysis of urinary stone composition in Eastern India by X-ray diffraction crystallography

    Tarun Jindal

    2014-01-01

    Full Text Available Background: Stones in the urinary system are common in our country. This study was done to assess the composition of the urinary stones in eastern part of India. Materials and Methods: A prospective study was done over a period of thirty months. A total of 90 stones were analyzed in this time period by using X-ray diffraction crystallography. Results: Of the 90 stones analyzed, 77 were renal stones, 12 were ureteric stones and one was a bladder stone. Six stones (all renal did not have properties to be represented by X-ray diffraction crystallography. The overall prevalence of the oxalate containing stones was 85.7% with calcium oxalate monohydrate (COM being the major constituent. Calcium oxalate dihydrate (COD was the next most common constituent. Struvite stones constituted 9.5% of the stones analyzed. Pure calcium phosphate stones were found in 4.7% of the cases. Conclusion: Our study reveals that the stone composition in the eastern part of India is different from that in other parts of the country. We have a comparatively lower prevalence of oxalate stones while a higher prevalence of phosphate and struvite stones.

  14. Automatic processing of macromolecular crystallography X-ray diffraction data at the ESRF.

    Monaco, Stéphanie; Gordon, Elspeth; Bowler, Matthew W; Delagenière, Solange; Guijarro, Matias; Spruce, Darren; Svensson, Olof; McSweeney, Sean M; McCarthy, Andrew A; Leonard, Gordon; Nanao, Max H

    2013-06-01

    The development of automated high-intensity macromolecular crystallography (MX) beamlines at synchrotron facilities has resulted in a remarkable increase in sample throughput. Developments in X-ray detector technology now mean that complete X-ray diffraction datasets can be collected in less than one minute. Such high-speed collection, and the volumes of data that it produces, often make it difficult for even the most experienced users to cope with the deluge. However, the careful reduction of data during experimental sessions is often necessary for the success of a particular project or as an aid in decision making for subsequent experiments. Automated data reduction pipelines provide a fast and reliable alternative to user-initiated processing at the beamline. In order to provide such a pipeline for the MX user community of the European Synchrotron Radiation Facility (ESRF), a system for the rapid automatic processing of MX diffraction data from single and multiple positions on a single or multiple crystals has been developed. Standard integration and data analysis programs have been incorporated into the ESRF data collection, storage and computing environment, with the final results stored and displayed in an intuitive manner in the ISPyB (information system for protein crystallography beamlines) database, from which they are also available for download. In some cases, experimental phase information can be automatically determined from the processed data. Here, the system is described in detail. PMID:23682196

  15. X-ray tests of microfocusing mono-capillary optic for protein crystallography

    Bilderback, D H

    2001-01-01

    A single, borosilicate-glass capillary was drawn into a 30.5 cm long elliptical shape. The inside diameter was 0.40 mm at the large base end and 0.13 mm at the tip. With 12 keV X-rays from the CHESS D1 bending magnet, the single-bounce capillary produced a focus of better than 18 mu m in diameter (FHWM) at a 3 cm distance from the capillary tip. A flux gain of 110 in the focus position was observed along with a total flux in the spot of 4x10 sup 1 sup 0 X-rays/s (conditions: 5.3 GeV, 182 mA, 1.5% bandwidth multilayer, 12 keV X-rays). A measurement of the far field focus ring diameter yielded a divergence of 3.8 mrad, in good agreement with the 4 mrad design of the optic for protein crystallography. Using a small 25 mu m square beam, we measured the local reflectivity to be greater than 95% and the inner slope errors of the capillary to average about +-150 mu rad, both from raw and elliptically shaped tubing. Our conclusion is that more perfect starting tubing (i.e. one with lower slope errors) is needed to ma...

  16. In meso in situ serial X-ray crystallography of soluble and membrane proteins

    Huang, Chia-Ying [Trinity College, Dublin (Ireland); Olieric, Vincent [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Ma, Pikyee [Trinity College, Dublin (Ireland); Panepucci, Ezequiel [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Diederichs, Kay [Universität Konstanz, M647, D-78457 Konstanz (Germany); Wang, Meitian, E-mail: meitian.wang@psi.ch [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Caffrey, Martin, E-mail: meitian.wang@psi.ch [Trinity College, Dublin (Ireland)

    2015-05-14

    A method for performing high-throughput in situ serial X-ray crystallography with soluble and membrane proteins in the lipid cubic phase is described. It works with microgram quantities of protein and lipid (and ligand when present) and is compatible with the most demanding sulfur SAD phasing. The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β{sub 2}-adrenoreceptor–G{sub s} protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at

  17. In meso in situ serial X-ray crystallography of soluble and membrane proteins

    A method for performing high-throughput in situ serial X-ray crystallography with soluble and membrane proteins in the lipid cubic phase is described. It works with microgram quantities of protein and lipid (and ligand when present) and is compatible with the most demanding sulfur SAD phasing. The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β2-adrenoreceptor–Gs protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular

  18. Development of a shutterless continuous rotation method using an X-ray CMOS detector for protein crystallography

    Hasegawa, Kazuya; Hirata, Kunio; Shimizu, Tetsuya; Shimizu, Nobutaka; Hikima, Takaaki; Baba, Seiki; Kumasaka, Takashi; Yamamoto, Masaki

    2009-01-01

    A new shutterless continuous rotation method using an X-ray complementary metal-oxide semiconductor (CMOS) detector has been developed for high-speed, precise data collection in protein crystallography. The principle of operation and the basic performance of the X-ray CMOS detector (Hamamatsu Photonics KK C10158DK) have been shown to be appropriate to the shutterless continuous rotation method. The data quality of the continuous rotation method is comparable to that of the conventional oscill...

  19. Synthesis, x-ray crystallography and leishmanicidal activity of benzimidazolinyl piperidine derivative

    Protozoan parasites of the Leishmania genus are the main cause of vector-borne disease leishmaniasis throughout the world. It is caused by at least 17 different species of protozoan Leishmania and transmitted by the bite of infected sand flies. Leishmaniasis could be fatal. Present drugs have limitations to cure it due to the development of drug resistance. Hence, to design an effective leishmanicidal agent would be of great interest. Benzimidazolinyl piperidine has served as potential target due to a vast range of biological activities. In the present study a new 4-(2-keto-1-benzimidazolinyl)piperidine derivative, 1-(2-(4-fluorophenyl)-2-oxoethyl)-4-(2-oxo-2,3-dihydro-1H-benzo(d)imidazol) piperidinium bromide has been synthesized and characterized by X-ray crystallography, 1D and 2D NMR spectroscopy. Evaluation by in vitro leishmanicidal assay showed good activity. (author)

  20. NATO Advanced Study Institute on Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays

    Jeffrey, George

    1988-01-01

    X-ray and neutron crystallography have played an increasingly impor­ tant role in the chemical and biochemical sciences over the past fifty years. The principal obstacles in this methodology, the phase problem and com­ puting, have been overcome. The former by the methods developed in the 1960's and just recognised by the 1985 Chemistry Nobel Prize award to Karle and Hauptman, the latter by the dramatic advances that have taken place in computer technology in the past twenty years. Within the last decade, two new radiation sources have been added to the crystallographer's tools. One is synchrotron X-rays and the other is spallation neutrons. Both have much more powerful fluxes than the pre­ vious sources and they are pulsed rather than continuos. New techniques are necessary to fully exploit the intense continuos radiation spectrum and its pulsed property. Both radiations are only available from particular National Laboratories on a guest-user basis for scientists outside these Na­ tional Laboratories. Hi...

  1. The need for a shared database infrastructure: combining X-ray crystallography and electron microscopy

    Advances in structural biology are opening greater opportunities for understanding biological structures from the cellular to the atomic level. Particularly promising are the links that can be established between the information provided by electron microscopy and the atomic structures derived from X-ray crystallography and nuclear magnetic resonance spectroscopy. Combining such different kinds of structural data can result in novel biological information on the interaction of biomolecules in large supramolecular assemblies. As a consequence, the need to develop new databases in the field of structural biology that allow for an integrated access to data from all the experimental techniques is becoming critical. Pilot studies performed in recent years have already established a solid background as far as the basic information that an integrated macromolecular structure database should contain, as well as the basic principles for integration. These efforts started in the context of the BioImage project, and resulted in a first complete database prototype that provided a versatile platform for the linking of atomic models of X-ray diffraction data with electron microscopy information. Analysis of the requirements needed to combine data at different levels of resolution have resulted in sets of specifications that make possible the integration of all these different types in the context of a web environment. The case of a structural study linking electron microscopy and X-ray data, which is already contained within the BioImage data base and in the Protein Data Bank, is used here to illustrate the current approach, while a general discussion highlights the urgent need for integrated databases. (orig.)

  2. X-ray Structure of Native Scorpion Toxin BmBKTx1 by Racemic Protein Crystallography Using Direct Methods

    Mandal, Kalyaneswar; Pentelute, Brad L.; Tereshko, Valentina; Kossiakoff, Anthony A.; Kent, Stephen B.H.; (UC)

    2009-04-08

    Racemic protein crystallography, enabled by total chemical synthesis, has allowed us to determine the X-ray structure of native scorpion toxin BmBKTx1; direct methods were used for phase determination. This is the first example of a protein racemate that crystallized in space group I41/a.

  3. NATURAL CYCLOPENTANOID CYANOHYDRIN GLYCOSIDES .13. STRUCTURE DETERMINATION OF NATURAL EPOXYCYCLOPENTANES BY X-RAY CRYSTALLOGRAPHY AND NMR-SPECTROSCOPY

    Olafsdottir, E. S.; Sorensen, A. M.; Cornett, Claus; Jaroszewski, J. W.

    1991-01-01

    nonannellated cyclopentane derivatives. The new glucosides were shown, by NMR spectroscopy (including NOE measurements), X-ray crystallography, and enzymatic hydrolysis to the corresponding cyanohydrins, to be (1R,2R,3R,4R)- and (1S,2S,3S,4S)-1-(beta-D-glucopyranosyloxy)-2,3-epoxy-4-hydroxycyclopenta ne-1...

  4. Life in the fast lane for protein crystallization and X-ray crystallography

    Pusey, Marc L.; Liu, Zhi-Jie; Tempel, Wolfram; Praissman, Jeremy; Lin, Dawei; Wang, Bi-Cheng; Gavira, Jose A.; Ng, Joseph D.

    2005-01-01

    The common goal for structural genomic centers and consortiums is to decipher as quickly as possible the three-dimensional structures for a multitude of recombinant proteins derived from known genomic sequences. Since X-ray crystallography is the foremost method to acquire atomic resolution for macromolecules, the limiting step is obtaining protein crystals that can be useful of structure determination. High-throughput methods have been developed in recent years to clone, express, purify, crystallize and determine the three-dimensional structure of a protein gene product rapidly using automated devices, commercialized kits and consolidated protocols. However, the average number of protein structures obtained for most structural genomic groups has been very low compared to the total number of proteins purified. As more entire genomic sequences are obtained for different organisms from the three kingdoms of life, only the proteins that can be crystallized and whose structures can be obtained easily are studied. Consequently, an astonishing number of genomic proteins remain unexamined. In the era of high-throughput processes, traditional methods in molecular biology, protein chemistry and crystallization are eclipsed by automation and pipeline practices. The necessity for high-rate production of protein crystals and structures has prevented the usage of more intellectual strategies and creative approaches in experimental executions. Fundamental principles and personal experiences in protein chemistry and crystallization are minimally exploited only to obtain "low-hanging fruit" protein structures. We review the practical aspects of today's high-throughput manipulations and discuss the challenges in fast pace protein crystallization and tools for crystallography. Structural genomic pipelines can be improved with information gained from low-throughput tactics that may help us reach the higher-bearing fruits. Examples of recent developments in this area are reported from

  5. Development of an X-ray HARP–FEA detector system for high-throughput protein crystallography

    A new detector system for protein crystallography based on an X-ray HARP–FEA is presented. A new detector system for protein crystallography is now being developed based on an X-ray HARP–FEA (high-gain avalanche rushing amorphous photoconductor–field emitter array), which consists of an amorphous selenium membrane and a matrix field emitter array. The combination of the membrane avalanche effect with a single driven FEA has several advantages over currently available area detectors, including higher sensitivity, higher spatial resolution and a higher frame rate. Preliminary evaluation of the detector has been carried out and its effectiveness has been confirmed. Next, diffraction images were measured with continuous rotation of a protein crystal, and the images were compared with those measured by the existing CCD detector; the system successfully obtained high-spatial-resolution images. Using shutterless measurement, the total measurement time can be reduced significantly, making the method appropriate for high-throughput protein crystallography. The X-ray HARP–FEA detector is an attractive candidate for the next generation of X-ray area detectors

  6. Alignment protocol for effective use of hard x-ray quad collimator for micro-crystallography

    Xu, S.; Nagarajan, V.; Sanishvili, R.; Fischetti, R. F.

    2011-09-01

    In October 2009, a quad, mini-beam collimator was implemented at GM/CA CAT that allowed users to select between a 5, 10, or 20 micron mini-beam or a 300 micron scatter guard for macromolecular crystallography. Initial alignment of each pinhole to the optical axis of each path through the mini-beam collimator is performed under an optical microscope using an alignment jig. Next, the pre-aligned collimator and its kinematic mount are moved to the beamline and attached to a pair of high precision translation stages attached to an on-axis-visualization system for viewing the protein crystal under investigation. The collimator is aligned to the beam axis by two angular and two translational motions. The pitch and yaw adjustments are typically only done during initial installation, and therefore are not motorized. The horizontal and vertical positions are adjusted remotely with high precision translational stages. Final alignment of the collimator is achieved using several endstation components, namely, a YAG crystal at the sample position to visualize the mini-beam, a CCD detector to record an X-ray background image, and a PIN diode to record the mini-beam intensity. The alignment protocol and its opto-mechanical instrumentation design will be discussed in detail.

  7. Watching proteins function with 150-ps time-resolved X-ray crystallography

    Anfinrud, Philip

    2007-03-01

    We have used time-resolved Laue crystallography to characterize ligand migration pathways and dynamics in wild-type and several mutant forms of myoglobin (Mb), a ligand-binding heme protein found in muscle tissue. In these pump-probe experiments, which were conducted on the ID09B time-resolved beamline at the European Synchrotron and Radiation Facility, a laser pulse photodissociates CO from an MbCO crystal and a suitably delayed X-ray pulse probes its structure via Laue diffraction. Single-site mutations in the vicinity of the heme pocket docking site were found to have a dramatic effect on ligand migration. To visualize this process, time-resolved electron density maps were stitched together into movies that unveil with <2-å spatial resolution and 150-ps time-resolution the correlated protein motions that accompany and/or mediate ligand migration. These studies help to illustrate at an atomic level relationships between protein structure, dynamics, and function.

  8. -2,4-Dichlorobenzoyl phosphoric triamides: Synthesis, spectroscopic and X-ray crystallography studies

    Khodayar Gholivand; Nasrin Oroujzadeh; Zahra Shariatinia

    2010-07-01

    New phosphoric triamides 1-9 were synthesized by the reaction of -2,4-dichlorobenzoyl phosphoramidic dichloride with various cyclic aliphatic amines and the products were characterized by 1H, 13C, 31P NMR, IR spectroscopy and elemental analysis. Surprisingly, the 1H NMR spectrum of 2 indicated long range 6 (P, H) coupling constant = 1.3, 1.4 Hz and those of molecules 3, 4, 6-8 display longrange 4 (H, H) coupling constants (1.8-1.9 Hz) for the coupling of aromatic protons in 2,4-dichlorophenyl rings. 1H NMR spectra indicated 3 (PNCH) for enantiotopic and diastereotopic benzylic CH2 protons in compounds 7 and 8. The spectroscopic data of newly synthesized compounds were compared with those related -benzoyl derivatives. The structures of compounds 5, 8 and 10 (2,4-Cl2-C6H3C(O)NHP(O)[NCH2CH(CH3)2]2) have been determined by X-ray crystallography. The structures form centrosymmetric dimers through intermolecular strong -P=O…H-N-hydrogen bonds. The dimers connect to each other via rather strong and weak C-H…O plus weak C-H…Cl H-bonds to produce a 1-D network for 5 while 3-D polymeric chains for 8 and 10.

  9. A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

    Jasper J. van Thor

    2015-01-01

    Full Text Available In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe” which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF, in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.

  10. Iterative Mass Spectrometry and X-Ray Crystallography to Study Ion-Trapping and Rearrangements by a Flexible Cluster

    Zhang, Kun; Kurmoo, Mohamedally; Wei, Lian-Qiang; Zeng, Ming-Hua

    2013-01-01

    An important aspect of chemical reactions involves understanding the intermediate steps from reactants to products. The iterative use of mass spectrometry and X-Ray crystallography is demonstrated to be a powerful combination in this respect. We have applied them in identifying molecular clusters in solution followed by their solid-state structural characterizations. We used a key ligand, 2-[(2-hydroxy-3-methoxy-benzylidene)-amino]-ethanesulfonate (L), which serves as chelating/bridging units...

  11. Volume-conserving trans-cis isomerization pathways in photoactive yellow protein visualized by picosecond X-ray crystallography

    Jung, Yang Ouk; Lee, Jae Hyuk; Kim, Joonghan; Schmidt, Marius; Moffat, Keith; Šrajer, Vukica; Ihee, Hyotcherl

    2013-03-01

    Trans-to-cis isomerization, the key reaction in photoactive proteins, usually cannot occur through the standard one-bond-flip mechanism. Owing to spatial constraints imposed by a protein environment, isomerization probably proceeds through a volume-conserving mechanism in which highly choreographed atomic motions are expected, the details of which have not yet been observed directly. Here we employ time-resolved X-ray crystallography to visualize structurally the isomerization of the p-coumaric acid chromophore in photoactive yellow protein with a time resolution of 100 ps and a spatial resolution of 1.6 Å. The structure of the earliest intermediate (IT) resembles a highly strained transition state in which the torsion angle is located halfway between the trans- and cis-isomers. The reaction trajectory of IT bifurcates into two structurally distinct cis intermediates via hula-twist and bicycle-pedal pathways. The bifurcating reaction pathways can be controlled by weakening the hydrogen bond between the chromophore and an adjacent residue through E46Q mutation, which switches off the bicycle-pedal pathway.

  12. Direct detection of x-rays for protein crystallography employing a thick, large area CCD

    Atac, Muzaffer; McKay, Timothy

    1999-01-01

    An apparatus and method for directly determining the crystalline structure of a protein crystal. The crystal is irradiated by a finely collimated x-ray beam. The interaction of the x-ray beam with the crystal produces scattered x-rays. These scattered x-rays are detected by means of a large area, thick CCD which is capable of measuring a significant number of scattered x-rays which impact its surface. The CCD is capable of detecting the position of impact of the scattered x-ray on the surface of the CCD and the quantity of scattered x-rays which impact the same cell or pixel. This data is then processed in real-time and the processed data is outputted to produce a image of the structure of the crystal. If this crystal is a protein the molecular structure of the protein can be determined from the data received.

  13. NSLS-II Biomedical beamlines for macromolecular crystallography, FMX and AMX, and for X-ray scattering, LIX: current developments

    We present the current status of development of the two macromolecular crystallography (MX) beamlines, FMX and AMX, and the X-ray scattering beamline LIX, at the National Synchrotron Light Source-II (NSLS-II) [1]. Together, FMX and AMX will cover a broad range of use cases from serial crystallography on micron sized crystals, to very large unit cell complexes, to rapid sample screening, e.g. for the always-hard-to-grow membrane proteins and for ligand binding studies. The LIX beamline will support a variety of X-ray scattering measurements for studies on proteins in solution, lipid membranes and biological tissues. We have performed Synchrotron Radiation Workshop (SRW) [2] and Shadow[3] simulations to help select optimal methods to modify the size of the beam easily and smoothly at both FMX and AMX. The very low emittance of the NSLS-II storage ring and the resulting low divergence of the X-ray beam, as well as the long optical path lengths in the photon delivery systems lead to stringent requirements e.g. for vibrational stability and mirror quality. We discuss beamline design considerations addressing these challenges, such as combining mirror optics with compound refractive lenses (CRLs).

  14. An Excel Spreadsheet for a One-Dimensional Fourier Map in X-ray Crystallography

    Clegg, William

    2004-01-01

    The teaching of crystal structure determination with single-crystal X-ray diffraction at undergraduate level faces numerous challenges. Single-crystal X-ray diffraction is used in a vast range of chemical research projects and forms the basis for a high proportion of structural results that are presented to high-school, undergraduate, and graduate…

  15. Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature

    Soichiro Tsujino; Takashi Tomizaki

    2016-01-01

    Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinn...

  16. Crystallography using synchrotron radiation X-ray. Application of Weissenberg and time resolved Laue methods to macromolecular structure analysis

    The three-dimensional structures of macromolecules under static and dynamic conditions are very important for the study of molecular biology. X-ray crystallography is the most powerful tool to obtain the three-dimensional structures of the macromolecules of especially large size, for which synchrotron radiation X-ray is used, The collection of diffraction data is the first, most important step for crystalline structure analysis. Efforts have been exerted to establish the data collection system using monochromatic synchrotron radiation X-ray (SRX). The diffraction intensity data collection system combined with a newly developed Weissenberg camera for macromolecules and an image plate (IP) using SRX has been established at the Photon Factory. Many important biological structures by high resolution have already come out with this data collection system, which is used also for the study on enzymatic reaction mechanism. A time resolved Laue camera has been designed, and the preliminary experiment has been carried out in the Photon Factory. These systems are reported. (K.I.)

  17. CCD[charge-coupled device]-based synchrotron x-ray detector for protein crystallography: Performance projected from an experiment

    The intense x radiation from a synchrotron source could, with a suitable detector, provide a complete set of diffraction images from a protein crystal before the crystal is damaged by radiation (2 to 3 min). An area detector consisting of a 40 mm dia. x-ray fluorescing phosphor, coupled with an image intensifier and lens to a CCD image sensor, was developed to determine the effectiveness of such a detector in protein crystallography. The detector was used in an experiment with a rotating anode x-ray generator. Diffraction patterns from a lysozyme crystal obtained with this detector are compared to those obtained with film. The two images appear to be virtually identical. The flux of 104 x-ray photons/s was observed on the detector at the rotating anode generator. At the 6-GeV synchrotron being designed at Argonne, the flux on an 80 x 80 mm2 detector is expected to be >109 photons/s. The projected design of such a synchrotron detector shows that a diffraction-peak count >106 could be obtained in ∼0.5 s. With an additional ∼0.5 s readout time of a 512 x 512 pixel CCD, the data acquisition time per frame would be ∼1 s so that ninety 10 diffraction images could be obtained, with approximately 1% precision, in less than 3 min

  18. Over-exposure from working with an X-ray crystallography set

    A service engineer was engaged in setting up and aligning a goniometer for use with a new X-ray generator and tube stand in the physics department of a university. The goniometer was of an old type, not matching with the shutter system of the tube shield. A piece of brass tubing 4cm in length was being used as a temporary enclosure for the useful X-ray beam, but the engineer realised after about four hours operation that the useful beam was not totally enclosed. A film badge worn by the engineer at waist level recorded a dose of less than 0.2rems, but the generator table had possibly shielded it. A later reconstruction of the incident produced an estimate of 2rems as the dose to the engineer's trunk surface. It was impossible to estimate the dose to his hands and wrists resulting from direct exposure to the X-ray beam, but the dose received must have been below 500 to 600rems, since no unusual skin effects have subsequently been detected. The incident demonstrates the need for adequate training, frequent monitoring especially when the useful beam is not totally enclosed, and an appreciation of the hazards involved when working with crystallographic equipment generating very intense X-ray beams. The combination of pieces of equipment made by different manufacturers requires particular care. Maintenance and alignment of modern crystallographic apparatus can also be hazardous to inexperienced operators. (U.K.)

  19. Synthesis, X-ray crystallography, and DFT calculations of a novel phosphoramide

    Shariatinia, Z.; Dušek, Michal; Eigner, Václav

    2014-01-01

    Roč. 640, č. 14 (2014), 2945-2955. ISSN 0044-2313 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : phosphoramide * x-ray structure * DFT Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.160, year: 2014

  20. Au 133 (SPh - t Bu) 52 Nanomolecules: X-ray Crystallography, Optical, Electrochemical, and Theoretical Analysis

    Dass, Amala; Theivendran, Shevanuja; Nimmala, Praneeth Reddy; Kumara, Chanaka; Jupally, Vijay Reddy; Fortunelli, Alessandro; Sementa, Luca; Barcaro, Giovanni; Zuo, Xiaobing; Noll, Bruce C.

    2015-04-15

    Crystal structure determination has revolutionized modern science in biology, chemistry, and physics. However, the difficulty in obtaining periodic crystal lattices which are needed for X-ray crystal analysis has hindered the determination of atomic structure in nanomaterials, known as the "nanostructure problem". Here, by using rigid and bulky ligands, we have overcome this limitation and successfully solved the X-ray crystallographic structure of the largest reported thiolated gold nanomolecule, Au133S52. The total composition, Au-133(SPh-tBu)(52), was verified using high resolution electrospray ionization mass spectrometry (ESI-MS). The experimental and simulated optical spectra show an emergent surface plasmon resonance that is more pronounced than in the slightly larger Au-144(SCH2CH2Ph)(60). Theoretical analysis indicates that the presence of rigid and bulky ligands is the key to the successful crystal formation.

  1. Radiation-damage-free quantum crystallography and resolution-enhanced x-ray imaging techniques using quantum multipath interference of thermal light

    Li, Zheng; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N; Shih, Yanhua

    2016-01-01

    Using higher order coherence of thermal light sources, we can achieve enhancement of resolution of standard x-ray imaging techniques, such as x-ray diffraction and phase contrast imaging. The cost of implementing such schemes is minimal comparing to the schemes using entangled two-photon pairs. The proposed diffractive quan- tum crystallography using multipath interference of thermal light can be eventually free of radiation damage, because the diffraction pattern could be formed by using low energy photons of optical wavelength. Thus it is promising to apply the proposed quantum crystallography scheme to nanocrystalline or non-crystalline samples that are too difficult to be crystallized.

  2. Hydrogen atoms can be located accurately and precisely by x-ray crystallography

    Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M.; Woźniak, Krzysztof; Jayatilaka, Dylan

    2016-01-01

    Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A–H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A–H bond lengths with those from neutron measurements for A–H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

  3. X-ray instrumentation for SR beamlines

    Kovalchuk, M V; Zheludeva, S I; Aleshko-Ozhevsky, O P; Arutynyan, E H; Kheiker, D M; Kreines, A Y; Lider, V V; Pashaev, E M; Shilina, N Y; Shishkov, V A

    2000-01-01

    The main possibilities and parameters of experimental X-ray stations are presented: 'Protein crystallography', 'X-ray structure analysis', 'High-precision X-ray optics', 'X-ray crystallography and material science', 'X-ray topography', 'Photoelectron X-ray standing wave' that are being installed at Kurchatov SR source by A.V. Shubnikov Institute of Crystallography.

  4. Azo coupling of 4-nitrophenyldiazonium chloride with aliphatic nucleophiles: an integrated organic synthesis and X-ray crystallography experiment

    This article describes an undergraduate experiment for the synthesis of p-nitrophenyldiazonium chloride and its coupling with acetylacetone and two enaminones, 4-phenylamino-pent-3-en-2-one and 4-amino-pent-3-en-2-one, in an adaptation of a previously reported synthetic protocol. The azo dyes 4-(E)-phenylamino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one and 4-(E)-amino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one were obtained, and the solid state structure of this latter azo compound was characterized by single crystal X-ray diffraction studies. This two-week integrated laboratory approach involves simple synthetic experiments and microwave chemistry in the organic laboratory plus crystallography analysis, suitable for novice students on undergraduate experimental chemistry courses. (author)

  5. FIST - a suite of X-ray powder crystallography programs for use with a HP-65 calculator

    Programs for X-ray powder crystallography are defined for use with a Hewlett Packard HP-65 (programmable) pocket calculator. These include the prediction of all Bragg reflections for defined P-, F-, I-cubic, tetragonal, hexagonal and orthorhombic cells; the calculation of the position of a specific Bragg reflection from defined unit cells with all symmetries except triclinic; interconversion of theta, 2theta, sin2theta and d, as well as the calculation of the Nelson-Riley function; the computation of crystal densities; the interconversion of rhombohedral and hexagonal unit cells, lsub(c) determinations for graphite, the calculation of a and c for boron carbide; and Miller index transformations between various unit cells. (author)

  6. Structure description ambiguity depending upon which edition of International Tables for (X-ray) Crystallography is used

    Parthe, E.; Gelato, L.M.; Chabot, B.

    1988-11-01

    The editorial policy of certain scientific journals where crystal structure data are published does not expressly specify that all three fractional coordinates of the atoms in the asymmetric unit have to be given for all Wyckoff sites. Owing to the differences between the 1952 edition and the 1983 edition of International Tables for (X-ray) Crystallography - in the way the xyz triplets of certain Wyckoff sites are formulated and also the interchange of Wyckoff letters assigned to the sites - failure to give all three atom coordinates may lead to ambiguities. It is shown that for seven monoclinic space groups (setting with unique axis c), three tetragonal and one cubic space groups (all with origin choice 2, i.e. symmetry centre at the origin) the shortened description may lead to different atom arrangements depending upon which edition of the International Tables is used.

  7. Structure description ambiguity depending upon which edition of International Tables for (X-ray) Crystallography is used

    The editorial policy of certain scientific journals where crystal structure data are published does not expressly specify that all three fractional coordinates of the atoms in the asymmetric unit have to be given for all Wyckoff sites. Owing to the differences between the 1952 edition and the 1983 edition of International Tables for (X-ray) Crystallography - in the way the xyz triplets of certain Wyckoff sites are formulated and also the interchange of Wyckoff letters assigned to the sites - failure to give all three atom coordinates may lead to ambiguities. It is shown that for seven monoclinic space groups (setting with unique axis c), three tetragonal and one cubic space groups (all with origin choice 2, i.e. symmetry centre at the origin) the shortened description may lead to different atom arrangements depending upon which edition of the International Tables is used. (orig.)

  8. Microwave assisted synthesis, X-ray crystallography and DFT calculations of selected aromatic thiosemicarbazones

    Serda, Maciej; Małecki, Jan G.; Mrozek-Wilczkiewicz, Anna; Musioł, Robert; Polański, Jarosław

    2013-04-01

    Series of four benzaldehyde thiosemicarbazones has been synthesized under microwave irradiation and characterized structurally by means of infrared and NMR spectroscopies and mass spectrometry. Their crystal structures were determined by single crystal X-ray analysis followed by DFT calculations. Partial charges on the molecular surface and dipole moments of the structures were calculated. Crystal structures are stabilized by intramolecular hydrogen bonding and stacking interactions. Studied compounds are interesting as antiproliferative and antifungal agents acting through interactions with iron. Thus presented results may be useful in design new more active or specific structures.

  9. A damage-free structural determination of the highly X-ray irradiation-sensitive active site of bovine heart cytochrome c oxidase by the femtosecond X-ray laser crystallography using SACLA

    A peroxide-like ligand in the O2 reduction site of the fully oxidized bovine heart cytochrome c oxidase (CcO) as isolated blocks the proton pump activity of CcO. High resolution structural determination of the ligand-bound O2 reduction site was essentially impossible because of the high sensitivity of the bound ligand to X-ray irradiation. The present high resolution and damage-free determination of the site by the femtosecond X-ray crystallographic analysis using SACLA, an X-ray free electron laser facility, has provided various insights for the mechanism of proton pump. Furthermore, the successful determination by femtosecond level X-ray irradiation assures that X-ray structural changes during the physiological processes driven by proteins are able to be followed with the time resolution sufficiently high for following any physiologically relevant process in the protein. The concept of Picobiology, for which the present newly developed time-resolved X-ray structural technique together with a recently established time-resolved infrared spectroscopy are prerequisite, is introduced for showing the importance of the femtosecond X-ray laser crystallography for understanding of Life Process. (author)

  10. Domain Movements upon Activation of Phenylalanine Hydroxylase Characterized by Crystallography and Chromatography-Coupled Small-Angle X-ray Scattering.

    Meisburger, Steve P; Taylor, Alexander B; Khan, Crystal A; Zhang, Shengnan; Fitzpatrick, Paul F; Ando, Nozomi

    2016-05-25

    Mammalian phenylalanine hydroxylase (PheH) is an allosteric enzyme that catalyzes the first step in the catabolism of the amino acid phenylalanine. Following allosteric activation by high phenylalanine levels, the enzyme catalyzes the pterin-dependent conversion of phenylalanine to tyrosine. Inability to control elevated phenylalanine levels in the blood leads to increased risk of mental disabilities commonly associated with the inherited metabolic disorder, phenylketonuria. Although extensively studied, structural changes associated with allosteric activation in mammalian PheH have been elusive. Here, we examine the complex allosteric mechanisms of rat PheH using X-ray crystallography, isothermal titration calorimetry (ITC), and small-angle X-ray scattering (SAXS). We describe crystal structures of the preactivated state of the PheH tetramer depicting the regulatory domains docked against the catalytic domains and preventing substrate binding. Using SAXS, we further describe the domain movements involved in allosteric activation of PheH in solution and present the first demonstration of chromatography-coupled SAXS with Evolving Factor Analysis (EFA), a powerful method for separating scattering components in a model-independent way. Together, these results support a model for allostery in PheH in which phenylalanine stabilizes the dimerization of the regulatory domains and exposes the active site for substrate binding and other structural changes needed for activity. PMID:27145334

  11. Syntheses, spectroscopic study and X-ray crystallography of some new phosphoramidates and lanthanide(III) complexes of N-(4-nitrobenzoyl)-N',N''-bis(morpholino)phosphoric triamide

    Gholivand, K.; Mostaanzadeh, H.; Kovaľ, Tomáš; Dušek, Michal; Erben, M.F.; Stoeckli-Evans, H.; Della Védova, C.O.

    2010-01-01

    Roč. 66, Part 4 (2010), s. 441-450. ISSN 0108-7681 Grant ostatní: AVČR(CZ) Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : phosphoramidates * lanthanide(III) complexes * NMR * IR spectroscopy * x-ray crystallography Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.829, year: 2010

  12. Structural Elucidation of Dendritic Host-Guest Complexes by X-ray Crystallography and Molecular Dynamics Simulations

    Chang, T; Pieterse, K.; Broeren, M.A.C.; Kooijman, H.; Spek, A.L.; Hilbers, M.F.; Meijer, E. W.

    2007-01-01

    The multiple monovalent binding of adamantyl-urea poly(propyleneimine) dendrimers with carboxylic acid-urea guests was investigated using molecular dynamics simulations and Xray crystallography to better understand the structure and behavior of the dynamic multivalent complex in solution. The results from the two methods are consistent and suggest a preferred molecular picture of this complicated aggregate of multiple components. The guest molecules can bind to the dendrimer in a variety of w...

  13. Kissing G domains of MnmE monitored by X-ray crystallography and pulse electron paramagnetic resonance spectroscopy.

    Simon Meyer

    2009-10-01

    Full Text Available MnmE, which is involved in the modification of the wobble position of certain tRNAs, belongs to the expanding class of G proteins activated by nucleotide-dependent dimerization (GADs. Previous models suggested the protein to be a multidomain protein whose G domains contact each other in a nucleotide dependent manner. Here we employ a combined approach of X-ray crystallography and pulse electron paramagnetic resonance (EPR spectroscopy to show that large domain movements are coupled to the G protein cycle of MnmE. The X-ray structures show MnmE to be a constitutive homodimer where the highly mobile G domains face each other in various orientations but are not in close contact as suggested by the GDP-AlF(x structure of the isolated domains. Distance measurements by pulse double electron-electron resonance (DEER spectroscopy show that the G domains adopt an open conformation in the nucleotide free/GDP-bound and an open/closed two-state equilibrium in the GTP-bound state, with maximal distance variations of 18 A. With GDP and AlF(x, which mimic the transition state of the phosphoryl transfer reaction, only the closed conformation is observed. Dimerization of the active sites with GDP-AlF(x requires the presence of specific monovalent cations, thus reflecting the requirements for the GTPase reaction of MnmE. Our results directly demonstrate the nature of the conformational changes MnmE was previously suggested to undergo during its GTPase cycle. They show the nucleotide-dependent dynamic movements of the G domains around two swivel positions relative to the rest of the protein, and they are of crucial importance for understanding the mechanistic principles of this GAD.

  14. Inhibition of d-xylose isomerase by polyols: atomic details by joint X-ray/neutron crystallography

    A joint X-ray/neutron structure of d-xylose isomerase in complex with the inhibitor sorbitol was determined at room temperature at an acidic pH of 5.9. Protonation of the O5 O atom of the sugar was directly observed in the nuclear density maps. Under acidic conditions sorbitol gains a water-mediated interaction with the enzyme active site, which may explain the increased potency of the inhibitor at low pH. d-Xylose isomerase (XI) converts the aldo-sugars xylose and glucose to their keto analogs xylulose and fructose, but is strongly inhibited by the polyols xylitol and sorbitol, especially at acidic pH. In order to understand the atomic details of polyol binding to the XI active site, a 2.0 Å resolution room-temperature joint X-ray/neutron structure of XI in complex with Ni2+ cofactors and sorbitol inhibitor at pH 5.9 and a room-temperature X-ray structure of XI containing Mg2+ ions and xylitol at the physiological pH of 7.7 were obtained. The protonation of oxygen O5 of the inhibitor, which was found to be deprotonated and negatively charged in previous structures of XI complexed with linear glucose and xylulose, was directly observed. The Ni2+ ions occupying the catalytic metal site (M2) were found at two locations, while Mg2+ in M2 is very mobile and has a high B factor. Under acidic conditions sorbitol gains a water-mediated interaction that connects its O1 hydroxyl to Asp257. This contact is not found in structures at basic pH. The new interaction that is formed may improve the binding of the inhibitor, providing an explanation for the increased affinity of the polyols for XI at low pH

  15. Inhibition of d-xylose isomerase by polyols: atomic details by joint X-ray/neutron crystallography

    Kovalevsky, Andrey, E-mail: ayk@lanl.gov [Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States); Hanson, B. Leif [University of Toledo, 2801 West Bancroft Street, Toledo, OH 43606 (United States); Mason, Sax A. [Institut Laue–Langevin, 6 Rue Jules Horowitz, 38042 Grenoble (France); Forsyth, V. Trevor [Institut Laue–Langevin, 6 Rue Jules Horowitz, 38042 Grenoble (France); Keele University, Staffordshire (United Kingdom); Fisher, Zoe [Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States); Mustyakimov, Marat [Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States); Oak Ridge National Laboratory, PO Box 2008, MS 6475, Oak Ridge, TN 37831 (United States); Blakeley, Matthew P. [Institut Laue–Langevin, 6 Rue Jules Horowitz, 38042 Grenoble (France); Keen, David A. [Harwell Science and Innovation Campus, Didcot, Oxon OX11 0QX (United Kingdom); Langan, Paul [Oak Ridge National Laboratory, PO Box 2008, MS 6475, Oak Ridge, TN 37831 (United States); Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States)

    2012-09-01

    A joint X-ray/neutron structure of d-xylose isomerase in complex with the inhibitor sorbitol was determined at room temperature at an acidic pH of 5.9. Protonation of the O5 O atom of the sugar was directly observed in the nuclear density maps. Under acidic conditions sorbitol gains a water-mediated interaction with the enzyme active site, which may explain the increased potency of the inhibitor at low pH. d-Xylose isomerase (XI) converts the aldo-sugars xylose and glucose to their keto analogs xylulose and fructose, but is strongly inhibited by the polyols xylitol and sorbitol, especially at acidic pH. In order to understand the atomic details of polyol binding to the XI active site, a 2.0 Å resolution room-temperature joint X-ray/neutron structure of XI in complex with Ni{sup 2+} cofactors and sorbitol inhibitor at pH 5.9 and a room-temperature X-ray structure of XI containing Mg{sup 2+} ions and xylitol at the physiological pH of 7.7 were obtained. The protonation of oxygen O5 of the inhibitor, which was found to be deprotonated and negatively charged in previous structures of XI complexed with linear glucose and xylulose, was directly observed. The Ni{sup 2+} ions occupying the catalytic metal site (M2) were found at two locations, while Mg{sup 2+} in M2 is very mobile and has a high B factor. Under acidic conditions sorbitol gains a water-mediated interaction that connects its O1 hydroxyl to Asp257. This contact is not found in structures at basic pH. The new interaction that is formed may improve the binding of the inhibitor, providing an explanation for the increased affinity of the polyols for XI at low pH.

  16. Structural Properties of Human CaMKII Ca2+ /Calmodulin-Dependent Protein Kinase II using X-ray Crystallography

    Cao, Yumeng Melody; McSpadden, Ethan; Kuriyan, John; Department of Molecular; Cell Biology; Department of Chemistry Team

    To this day, human memory storage remains a mystery as we can at most describe the process vaguely on a cellular level. Switch-like properties of Calcium/Calmodulin-Dependent Protein Kinase II make it a leading candidate in understanding the molecular basis of human memory. The protein crystal was placed in the beam of a synchrotron source and the x-ray crystallography data was collected as reflections on a diffraction pattern that undergo Fourier transform to obtain the electron density. We observed two drastic differences from our solved structure at 2.75Å to a similar construct of the mouse CaMKII association domain. Firstly, our structure is a 6-fold symmetric dodecamer, whereas the previously published construct was a 7-fold symmetric tetradecamer. This suggests the association domain of human CaMKII is a dynamic structure that is triggered subunit exchange process. Secondly, in our structure the N-terminal tag is docked as an additional beta-strand on an uncapped beta-sheet present in each association domain protomer. This is concrete evidence of the involvement of the polypeptide docking site in the molecular mechanism underlining subunit exchange. In the future, we would like to selectively inhibit the exchange process while not disrupting the other functionalities of CaMKII.

  17. Iterative mass spectrometry and X-ray crystallography to study ion-trapping and rearrangements by a flexible cluster.

    Zhang, Kun; Kurmoo, Mohamedally; Wei, Lian-Qiang; Zeng, Ming-Hua

    2013-01-01

    An important aspect of chemical reactions involves understanding the intermediate steps from reactants to products. The iterative use of mass spectrometry and X-Ray crystallography is demonstrated to be a powerful combination in this respect. We have applied them in identifying molecular clusters in solution followed by their solid-state structural characterizations. We used a key ligand, 2-[(2-hydroxy-3-methoxy-benzylidene)-amino]-ethanesulfonate (L), which serves as chelating/bridging units to stabilize the precursor [Li₄Ni₆(OH)₂(L)₆(CH₃CN)₆](ClO₄)₂·4CH₃CN. The results of subsequent reactions witness a cascade of processes involving fragmentation, inner bridging ligand substitution (OH⁻ to OCH₃⁻), changing modes of binding (chelate to monodentate) of the key ligand, ion-trapping and exchange (Li⁺, Na⁺ and Ca²⁺) and their site preferences, coordinating and non-coordinating solvents (CH₃CN to CH₃OH, H₂O and EtOH) replacement. The flexibility of the Ni₃OL₃ species in solution permits the formation of six derivatives. The complimentary techniques open a broader prospect for cluster design and applications. PMID:24343303

  18. Probing the Role of Divalent Metal Ions in a Bacterial Psychrophilic Metalloprotease: Binding Studies of an Enzyme in the Crystalline State by X-Ray Crystallography

    Ravaud, Stephanie; Gouet, Patrice; Haser, Richard; Aghajari, Nushin

    2003-01-01

    The psychrophilic alkaline metalloprotease (PAP) produced by a Pseudomonas bacterium isolated in Antarctica belongs to the clan of metzincins, for which a zinc ion is essential for catalytic activity. Binding studies in the crystalline state have been performed by X-ray crystallography in order to improve the understanding of the role of the zinc and calcium ions bound to this protease. Cocrystallization and soaking experiments with EDTA in a concentration range from 1 to 85 mM have resulted ...

  19. X-ray instrumentation for SR beamlines

    Kovalchuk, M.V.; Shilin, Yu.N.; Zheludeva, S.I. E-mail: zheludeva@ns.crys.ras.ru; Aleshko-Ozhevsky, O.P.; Arutynyan, E.H.; Kheiker, D.M.; Kreines, A.Ya.; Lider, V.V.; Pashaev, E.M.; Shilina, N.Yu.; Shishkov, V.A

    2000-06-21

    The main possibilities and parameters of experimental X-ray stations are presented: 'Protein crystallography', 'X-ray structure analysis', 'High-precision X-ray optics', 'X-ray crystallography and material science', 'X-ray topography', 'Photoelectron X-ray standing wave' that are being installed at Kurchatov SR source by A.V. Shubnikov Institute of Crystallography.

  20. X-ray crystal structure of N-6 adenine deoxyribose nucleic acid methyltransferase from Streptococcus pneumoniae

    Tran, Phidung Hong

    X-ray diffraction by using resonant anomalous scattering has become a popular tool for solving crystal structures in the last ten years with the expanded availability of tunable synchrotron radiation for protein crystallography. Mercury atoms were used for phasing. The crystal structure of N-6 deoxyribose nucleic acid methyltransferase from Streptoccocus pneumoniae (DpnM) was solved by using the Multiple Anomalous Diffraction technique. The crystal structure reveals the formation of mercaptide between the mercury ion and the thiol group on the cysteine amino acid in a hydrophobic environment. The crystal structure contains the bound ligand, S- adenosyl-l-methionine on the surface of the concave opening. The direction of the β-strands on the beta sheets are identical to other solved methyltransferases. The highly conserved motifs, DPPY and the FxGxG, are found to be important in ligand binding and possibly in methyl group transfer. The structure has a concave cleft with an opening on the order of 30 Å that can accommodate a DNA duplex. By molecular modelling coupled to sequence alignment, two other highly conserved residues Arg21 and Gly19 are found to be important in catalysis.

  1. Determination of plutonium in nitric acid solutions using energy dispersive L X-ray fluorescence with a low power X-ray generator

    This work presents the development of an in-line energy dispersive L X-ray fluorescence spectrometer set-up, with a low power X-ray generator and a secondary target, for the determination of plutonium concentration in nitric acid solutions. The intensity of the L X-rays from the internal conversion and gamma rays emitted by the daughter nuclei from plutonium is minimized and corrected, in order to eliminate the interferences with the L X-ray fluorescence spectrum. The matrix effects are then corrected by the Compton peak method. A calibration plot for plutonium solutions within the range 0.1–20 g L−1 is given

  2. Room-temperature serial crystallography using a kinetically optimized microfluidic device for protein crystallization and on-chip X-ray diffraction

    Michael Heymann

    2014-09-01

    Full Text Available An emulsion-based serial crystallographic technology has been developed, in which nanolitre-sized droplets of protein solution are encapsulated in oil and stabilized by surfactant. Once the first crystal in a drop is nucleated, the small volume generates a negative feedback mechanism that lowers the supersaturation. This mechanism is exploited to produce one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room-temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different unoriented crystals. As proof of concept, the structure of glucose isomerase was solved to 2.1 Å, demonstrating the feasibility of high-throughput serial X-ray crystallography using synchrotron radiation.

  3. Complementarity of neutron and ultrahigh resolution synchrotron X-ray protein crystallography studies: Results with concanavalin A at cryo and room temperature

    The complementarity of synchrotron derived ultrahigh resolution X-ray and neutron protein crystallography is explored via an ensemble of part lectin concanavalin A crystal structures. Thus a resume of the study of a cryo 0.94 A and a neutron (+X-ray) protein crystal 2.4 A structure in room temperature is made and these are then compared in their efficiency to determine the positions of the bound solvent atoms i.e. as hydrogens and deuteriums. First results are also presented of comparisons of two ultrahigh resolution protein crystal structures, the 0.94 A and the new 0.92 A structure. Thus the variability is in the multiple occupancies of side chains. Overall, one can see that a 'complete' structure definition, with today's experimental capabilities, is possible and can include structure ensemble variations. (author)

  4. Shoot-and-Trap: Use of specific X-ray damage to study structural protein dynamics by temperature-control led cryo-crystallography

    Colletier, J.P.; Sanson, B.; Weik, M. [Univ Grenoble 1, Lab Biophys Mol, F-38027 Grenoble (France); Bourgeois, D. [CEA-CNRS-Univ Grenoble 1, Inst Biol Struct Jean Pierre Ebel, Commissariat Energie Atom, Lab Cristallogenese etCristallog Prot, F-38027 Grenoble (France); Fournier, D. [CNRS, Inst Pharmacol et Biol Struct, Grp Biotechnol Prot, F-31077 Toulouse (France); Bourgeois, D. [European Synchrotron Radiat Facil, F-38000 Grenoble (France); Silman, I. [Weizmann Inst Sci, Dept Neurobiol, IL-76100 Rehovot (Israel); Sussman, J.L. [Weizmann Inst Sci, Dept Struct Biol, IL-76100 Rehovot (Israel)

    2008-07-01

    Although X-ray crystallography is the most widely used method for macromolecular structure determination, it does not provide dynamical information, and either experimental tricks or complementary experiments must be used to overcome the inherently static nature of crystallographic structures. Here we used specific X-ray damage during temperature-controlled crystallographic experiments at a third-generation synchrotron source to trigger and monitor (Shoot-and-Trap) structural changes putatively involved in an enzymatic reaction. In particular, a non-hydrolyzable substrate analogue of acetylcholinesterase, the 'off-switch' at cholinergic synapses, was radio-cleaved within the buried enzymatic active site. Subsequent product clearance, observed at 150 K but not at 100 K, indicated exit from the active site possibly via a 'backdoor'. The simple strategy described here is, in principle, applicable to any enzyme whose structure in complex with a substrate analogue is available and, therefore, could serve as a standard procedure in kinetic crystallography studies. (authors)

  5. Clear as Crystal: The Story of the Braggs--How X-Ray Crystallography Has Contributed to Science

    George, Robert; Patterson, John

    2014-01-01

    Here is a brief history of the work of two of Australia's most famous scientists, Sir William Bragg and his son Sir Lawrence Bragg. Jointly awarded the Nobel Prize in 1915 for their groundbreaking research into the use of X-rays to study the chemical structure and function of molecules, they have contributed to our heritage and to science at…

  6. Single-Crystal Raman Spectroscopy and X-ray Crystallography at Beamline X26-C of the NSLS

    Three-dimensional structures derived from X-ray diffraction of protein crystals provide a wealth of information. Features and interactions important for the function of macromolecules can be deduced and catalytic mechanisms postulated. Still, many questions can remain, for example regarding metal oxidation states and the interpretation of 'mystery density', i.e. ambiguous or unknown features within the electron density maps, especially at ∼2 (angstrom) resolutions typical of most macromolecular structures. Beamline X26-C at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), provides researchers with the opportunity to not only determine the atomic structure of their samples but also to explore the electronic and vibrational characteristics of the sample before, during and after X-ray diffraction data collection. When samples are maintained under cryo-conditions, an opportunity to promote and follow photochemical reactions in situ as a function of X-ray exposure is also provided. Plans are in place to further expand the capabilities at beamline X26-C and to develop beamlines at NSLS-II, currently under construction at BNL, which will provide users access to a wide array of complementary spectroscopic methods in addition to high-quality X-ray diffraction data.

  7. Au133(SPh-tBu)52 Nanomolecules: X-ray Crystallography, Optical, Electrochemical, and Theoretical Analysis

    Dass, Amala; Theivendran, Shevanuja; Nimmala, Praneeth Reddy; Kumara, Chanaka; Jupally, Vijay Reddy; Fortunelli, Alessandro; Sementa, Luca; Barcaro, Giovanni; Zuo, Xiaobing; Noll, Bruce C.

    2015-04-15

    Crystal structure determination has revolutionized modern science in biology, chemistry, and physics. However, the difficulty in obtaining periodic crystal lattices which are needed for X-ray crystal analysis has hindered the determination of atomic structure in nanomaterials, known as the “nanostructure problem”. Here, by using rigid and bulky ligands, we have overcome this limitation and successfully solved the X-ray crystallographic structure of the largest reported thiolated gold nanomolecule, Au133S52. The total composition, Au133(SPh-tBu)52, was verified using high resolution electrospray ionization mass spectrometry (ESI-MS). The experimental and simulated optical spectra show an emergent surface plasmon resonance that is more pronounced than in the slightly larger Au144(SCH2CH2Ph)60. Theoretical analysis indicates that the presence of rigid and bulky ligands is the key to the successful crystal formation.

  8. Testing of gadolinium oxy-sulphide phosphors for use in CCD-based X-ray detectors for macromolecular crystallography

    Pokric, M

    2002-01-01

    The resolution and detective quantum efficiency of CCD-based detectors used for X-ray diffraction is primarily affected by the layer of phosphor that converts incident X-ray photons into visible photons. The optimum thickness of this phosphor layer is strongly dependent on the fraction of absorbed incident X-ray photons and required spatial resolution. A range of terbium doped gadolinium oxy-sulphide (Gd sub 2 O sub 2 S : Tb) phosphor samples, provided by Applied Scintillation Technologies, have been evaluated for spatial resolution, light output and uniformity. The phosphor samples varied in coating weight (10-25 mg/cm sup 2), grain size (2.5, 4, 10 mu m), and applied coating (no coating, reflectors and absorbers). In addition, a non-uniform layer was introduced to some samples in order to provide an inherent diffusion layer. The experimental results showed that the introduction of a reflector increases the point spread function (PSF) and increases light yield up to 30%, while an absorber reduces the PSF tai...

  9. Determination of plutonium in nitric acid solutions using energy dispersive L X-ray fluorescence with a low power X-ray generator

    Py, J. [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France); Groetz, J.-E., E-mail: jegroetz@univ-fcomte.fr [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Hubinois, J.-C.; Cardona, D. [Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France)

    2015-04-21

    This work presents the development of an in-line energy dispersive L X-ray fluorescence spectrometer set-up, with a low power X-ray generator and a secondary target, for the determination of plutonium concentration in nitric acid solutions. The intensity of the L X-rays from the internal conversion and gamma rays emitted by the daughter nuclei from plutonium is minimized and corrected, in order to eliminate the interferences with the L X-ray fluorescence spectrum. The matrix effects are then corrected by the Compton peak method. A calibration plot for plutonium solutions within the range 0.1–20 g L{sup −1} is given.

  10. Isolation and Characterization, Including by X-ray Crystallography, of Contact and Solvent-Separated Ion Pairs of Silenyl Lithium Species.

    Pinchuk, Daniel; Mathew, Jomon; Kaushansky, Alexander; Bravo-Zhivotovskii, Dmitry; Apeloig, Yitzhak

    2016-08-22

    Reaction of bromoacylsilane 1 (pink solution) with tBu2 MeSiLi (3.5 equiv) in a 4:1 hexane:THF solvent mixture at -78 °C to room temperature yields the solvent separated ion pair (SSIP) of silenyl lithium E-[(tBuMe2 Si)(tBu2 MeSi)C=Si(SiMetBu2 )](-) [Li⋅4THF](+) 2 a (green-blue solution). Removal of the solvent and addition of benzene converts 2 a into the corresponding contact ion pair (CIP) 2 b (violet-red solution) with two THF molecules bonded to the lithium atom. The 2 a⇌2 b interconversion is reversible upon THF⇌ benzene solvent change. Both 2 a and 2 b were characterized by X-ray crystallography, NMR and UV/Vis spectroscopy, and theoretical calculations. The degree of dissociation of the Si-Li bond has a large effect on the visible spectrum (and thus color) and on the silenylic (29) Si NMR chemical shift, but a small effect on the molecular structure. This is the first report of the X-ray molecular structure of both the SSIP and the CIP of any R2 E=E'RM species (E=C, Si; E'=C, Si; M=metal). PMID:27466152

  11. Toward resolving the catalytic mechanism of dihydrofolate reductase using neutron and ultrahigh-resolution X-ray crystallography [Neutron and ultrahigh resolution X-ray crystallography reveals water as the proton donor in the catalytic mechanism of dihydrofolate reductase

    Dihydrofolate reductase (DHFR) catalyzes the NADPH-dependent reduction of dihydrofolate (DHF) to tetrahydrofolate (THF). An important step in the mechanism involves proton donation to the N5 atom of DHF. The inability to determine the protonation states of active site residues and substrate has led to the lack of consensus on a catalytic mechanism. To resolve this ambiguity, we conducted neutron and ultrahigh resolution X-ray crystallographic studies of the pseudo-Michaelis ternary complex of DHFR with folate and NADP+ from E. coli. The neutron data were collected to 2.0 Å resolution using a 3.6 mm3 crystal with the quasi-Laue technique, and the structure reveals that the N3 atom of folate is protonated while Asp27 is negatively charged. Previous mechanisms have proposed a keto-to-enol tautomerization of the substrate to facilitate protonation of the N5 atom. The structure supports the existence of the keto tautomer due to protonation of the N3 atom, suggesting tautomerization is unnecessary for catalysis. In the 1.05 Å resolution X-ray structure of the ternary complex, conformational disorder of the Met20 side chain is coupled to electron density for a partially occupied water within hydrogen-bonding distance of the N5 atom of folate; this suggests direct protonation of substrate by solvent. We propose a catalytic mechanism for DHFR that involves stabilization of the keto tautomer of the substrate, elevation of the pKa of the N5 atom of DHF by Asp27, and protonation of N5 by water whose access to the active site is gated by fluctuation of the Met20 side chain even though the Met-20 loop is closed

  12. Low-Z polymer sample supports for fixed-target serial femtosecond X-ray crystallography

    Feld, Geoffrey K. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); National Institute of Environmental Health Science, Research Triangle Park, NC (United States); Heymann, Michael [Brandeis Univ., Waltham, MA (United States); Univ. of Hamburg and DESY, Hamburg (Germany); Benner, W. Henry [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Pardini, Tommaso [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Tsai, Ching -Ju [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Boutet, Sebastien [SLAC National Accelerator Lab., Menlo Park, CA (United States); Coleman, Matthew A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hunter, Mark S. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); SLAC National Accelerator Lab., Menlo Park, CA (United States); Li, Xiaodan [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Messerschmidt, Marc [SLAC National Accelerator Lab., Menlo Park, CA (United States); BioXFEL Science and Technology Center, Buffalo, NY (United States); Opathalage, Achini [Brandeis Univ., Waltham, MA (United States); Pedrini, Bill [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Williams, Garth J. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Krantz, Bryan A. [Univ. of California, Berkeley, CA (United States); Fraden, Seth [Brandeis Univ., Waltham, MA (United States); Hau-Riege, Stefan [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Evans, James E. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Segelke, Brent W. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Frank, Matthias [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2015-06-27

    X-ray free-electron lasers (XFELs) offer a new avenue to the structural probing of complex materials, including biomolecules. Delivery of precious sample to the XFEL beam is a key consideration, as the sample of interest must be serially replaced after each destructive pulse. The fixed-target approach to sample delivery involves depositing samples on a thin-film support and subsequent serial introduction via a translating stage. Some classes of biological materials, including two-dimensional protein crystals, must be introduced on fixed-target supports, as they require a flat surface to prevent sample wrinkling. A series of wafer and transmission electron microscopy (TEM)-style grid supports constructed of low-Z plastic have been custom-designed and produced. Aluminium TEM grid holders were engineered, capable of delivering up to 20 different conventional or plastic TEM grids using fixed-target stages available at the Linac Coherent Light Source (LCLS). As proof-of-principle, X-ray diffraction has been demonstrated from two-dimensional crystals of bacteriorhodopsin and three-dimensional crystals of anthrax toxin protective antigen mounted on these supports at the LCLS. In conclusion, the benefits and limitations of these low-Z fixed-target supports are discussed; it is the authors' belief that they represent a viable and efficient alternative to previously reported fixed-target supports for conducting diffraction studies with XFELs.

  13. Elucidation of Lipid Binding Sites on Lung Surfactant Protein A Using X-ray Crystallography, Mutagenesis, and Molecular Dynamics Simulations.

    Goh, Boon Chong; Wu, Huixing; Rynkiewicz, Michael J; Schulten, Klaus; Seaton, Barbara A; McCormack, Francis X

    2016-07-01

    Surfactant protein A (SP-A) is a collagenous C-type lectin (collectin) that is critical for pulmonary defense against inhaled microorganisms. Bifunctional avidity of SP-A for pathogen-associated molecular patterns (PAMPs) such as lipid A and for dipalmitoylphosphatidylcholine (DPPC), the major component of surfactant membranes lining the air-liquid interface of the lung, ensures that the protein is poised for first-line interactions with inhaled pathogens. To improve our understanding of the motifs that are required for interactions with microbes and surfactant structures, we explored the role of the tyrosine-rich binding surface on the carbohydrate recognition domain of SP-A in the interaction with DPPC and lipid A using crystallography, site-directed mutagenesis, and molecular dynamics simulations. Critical binding features for DPPC binding include a three-walled tyrosine cage that binds the choline headgroup through cation-π interactions and a positively charged cluster that binds the phosphoryl group. This basic cluster is also critical for binding of lipid A, a bacterial PAMP and target for SP-A. Molecular dynamics simulations further predict that SP-A binds lipid A more tightly than DPPC. These results suggest that the differential binding properties of SP-A favor transfer of the protein from surfactant DPPC to pathogen membranes containing appropriate lipid PAMPs to effect key host defense functions. PMID:27324153

  14. Combination of X-ray crystallography, SAXS and DEER to obtain the structure of the FnIII-3, 4 domains of integrin α6β4

    Alonso-García, Noelia [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); García-Rubio, Inés [ETH Zürich, Vladimir-Prelog-Weg 2, CH-8093 Zürich (Switzerland); Academia General Militar, Carretera de Huesca s/n, 50090 Zaragoza (Spain); Manso, José A. [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); Buey, Rubén M. [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); Urien, Hector [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); Sonnenberg, Arnoud [Netherlands Cancer Institute, Plesmanlaan 121, 1066 CX Amsterdam (Netherlands); Jeschke, Gunnar [ETH Zürich, Vladimir-Prelog-Weg 2, CH-8093 Zürich (Switzerland); Pereda, José M. de, E-mail: pereda@usal.es [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain)

    2015-04-01

    The structure of the FnIII-3, 4 region of integrin β4 was solved using a hybrid approach that combines crystallographic structures, SAXS, DEER and molecular modelling. The structure helps in understanding how integrin β4 might bind to other hemidesmosomal proteins and mediate signalling. Integrin α6β4 is a major component of hemidesmosomes that mediate the stable anchorage of epithelial cells to the underlying basement membrane. Integrin α6β4 has also been implicated in cell proliferation and migration and in carcinoma progression. The third and fourth fibronectin type III domains (FnIII-3, 4) of integrin β4 mediate binding to the hemidesmosomal proteins BPAG1e and BPAG2, and participate in signalling. Here, it is demonstrated that X-ray crystallography, small-angle X-ray scattering and double electron–electron resonance (DEER) complement each other to solve the structure of the FnIII-3, 4 region. The crystal structures of the individual FnIII-3 and FnIII-4 domains were solved and the relative arrangement of the FnIII domains was elucidated by combining DEER with site-directed spin labelling. Multiple structures of the interdomain linker were modelled by Monte Carlo methods complying with DEER constraints, and the final structures were selected against experimental scattering data. FnIII-3, 4 has a compact and cambered flat structure with an evolutionary conserved surface that is likely to correspond to a protein-interaction site. Finally, this hybrid method is of general application for the study of other macromolecules and complexes.

  15. New insight into the dynamic properties and the active site architecture of H-Ras p21 revealed by X-ray crystallography at very high resolution

    Klink Björn U

    2010-10-01

    Full Text Available Abstract Background In kinetic crystallography, the usually static method of X-ray diffraction is expanded to allow time-resolved analysis of conformational rearrangements in protein structures. To achieve this, reactions have to be triggered within the protein crystals of interest, and optical spectroscopy can be used to monitor the reaction state. For this approach, a modified form of H-Ras p21 was designed which allows reaction initiation and fluorescence readout of the initiated GTPase reaction within the crystalline state. Rearrangements within the crystallized protein due to the progressing reaction and associated heterogeneity in the protein conformations have to be considered in the subsequent refinement processes. Results X-ray diffraction experiments on H-Ras p21 in different states along the reaction pathway provide detailed information about the kinetics and mechanism of the GTPase reaction. In addition, a very high data quality of up to 1.0 Å resolution allowed distinguishing two discrete subconformations of H-Ras p21, expanding the knowledge about the intrinsic flexibility of Ras-like proteins, which is important for their function. In a complex of H-Ras•GppNHp (guanosine-5'-(β,γ-imido-triphosphate, a second Mg2+ ion was found to be coordinated to the γ-phosphate group of GppNHp, which positions the hydrolytically active water molecule very close to the attacked γ-phosphorous atom. Conclusion For the structural analysis of very high-resolution data we have used a new 'two-chain-isotropic-refinement' strategy. This refinement provides an alternative and easy to interpret strategy to reflect the conformational variability within crystal structures of biological macromolecules. The presented fluorescent form of H-Ras p21 will be advantageous for fluorescence studies on H-Ras p21 in which the use of fluorescent nucleotides is not feasible.

  16. Characteristic Ligand-Induced Crystal Forms of HIV-1 Protease Complexes: A Novel Discovery of X-Ray Crystallography

    Mixtures of saquinavir (SQV) and ritonavir (RTV) were cocrystallized with HIV-1 protease (PR) in an attempt to compare their relative potencies using a crystallographic approach and factors responsible for the respective crystal forms obtained were examined. The mixture ratio of the SQV/RTV was in the range of 1:1 to 1:50 with increasing concentration of dimethyl sulphoxide (DMSO) used. Two crystal forms of PR complexes were obtained. At concentrations of 0.8 and 1.2 % DMSO using 1:1 and 1:15 ratios of SQV/RTV, the crystal form was monoclinic while increasing the concentration of DMSO to 3.2 and 5.0% using 1:15 and 1:50 ratios of SQV/RTV, the orthorhombic crystal form was obtained. The high resolution X-ray crystal structures of the PR/ inhibitor complexes reveal that crystal forms with respective space groups are dependent on the occupancy of either SQV or RTV in the active site of the PR. The occupancy of either of the PR inhibitors in the active site of PR has interestingly demonstrated unique cooperativity effects in crystallization of protein-ligand complexes. The crystal forms obtained were also related to the concentration of DMSO and ammonium sulphate in crystallization, and storage conditions of purified PR. Surprisingly, the relative occupancies of these inhibitors in the active site suggested a competition between the two inhibitors which were not inhibition constants related. Analysis of the structures in both crystal forms show no difference in DMSO content but at higher concentration of DMSO (3.2 - 5.0%) in the orthorhombic crystal forms, there were protein-sulphate interactions which were absent in the monoclinic forms with lower concentration (0.8 - 1.2%) of DMSO. This work has clearly demonstrated that there is cooperativity in crystallization and the conditions of crystallization influence specific intermolecular contacts in crystal packing (crystal form). (author)

  17. SPECTROSCOPY STUDIES, X-RAY CRYSTALLOGRAPHY, AND ANTITUMOR EVALUATION OF THE BEHAVIOR OF REACTIONS OF BISDIMEDONE DERIVATIVES WITH MALONONITRILE OR WITH BENZYLIDENEMALONONITILE IN ETHANOLIC PIPERIDINE

    Fatima Al-Omran

    2014-03-01

    Full Text Available A simple, environmentally acceptable, a one-pot method, which is efficient, inexpensive, and rapid, afforded excellent yields of the 4H-chromeme derivatives 5 and 6 from a three-component reaction of dimedone, arylaldehdes 2a-b, and malononitrile and a two-component reaction of bisdimedones 3a-b and malononitrile, respectively. Refluxing ethanolic piperidine was used as the catalyst for the 10-min reactions. A one-pot reaction of benzylidenemalononitrile, instead of malononitrile, with bisdimedones 3a-b, using the aforementioned reaction, also provided the 4H-chromene derivative 5 in excellent yield. The structures of the newly synthesized compounds were elucidated by elemental analyses, X-ray crystallography, and a variety of spectroscopic methods, including proton and carbon nuclear magnetic resonance spectroscopy (1H-NMR and 13C-NMR, respectively, correlation spectroscopy (COSY, heteronuclear single quantum coherence spectroscopy (HSQC, heteronuclear multiple-bond correlation spectroscopy (HMBC, and mass spectrometry (MS. The inhibitory effects of the 4H-chromeme derivatives 5 and 6 on the in vitro growth of human tumor cell and normal cell lines were greater than that of the reference drug doxorubicin.

  18. Study of humic acids by small-angle X-ray and neutron scattering

    Humic acids are an important component of natural ecological system and represent a polydisperse complex of natural biopolymers with molecular masses from several to hundreds kilodaltons. They are both a source of organic compounds and a protector against anthropogenic pollutions of biosphere. The aim of the report is to underline some possibilities of small-angle X-ray and neutron scattering to study HA and their fractions. (author)

  19. Interaction of the replication terminator protein (RTP) with DNA probed by NMR spectroscopy and x-ray crystallography

    Full text: The arrest of replication forks during the termination of DNA replication in Bacillus subtilis is dependent upon the binding of the 30 kDa replication terminator protein (RTP) to its cognate Ter binding site. Two adjacently bound dimers of RTP form a termination complex that can prevent the progression of a replication fork approaching from one direction, but not the other. The crystal structure of free RTP has previously been solved, but the precise orientation with which it binds to Ter sites remains unknown. This information is important for understanding the molecular mechanism of replication fork arrest. We have used NMR spectroscopy to observe 1H-15N correlations arising from 15N-labelled RTP mutant, and to track their perturbations upon the addition of DNA. This showed that 60% of the amino acid residues are affected by the DNA interaction, and also that the complex is symmetrical. Assignment of the 1H-15N correlations was achieved using a suite of triple resonance NMR experiments with 15N,13C,2H enriched protein recorded at 800 MHz and using TROSY pulse sequences. This revealed that α3-helices are involved in the binding interaction, and that the 'wings' of RTP may not be contributing to binding. Crystals of the complex have been grown from the NMR sample, and data collected to 3.1 Angstroms is anticipated to provide further molecular detail

  20. Mapping the topographic epitope landscape on the urokinase plasminogen activator receptor (uPAR by surface plasmon resonance and X-ray crystallography

    Baoyu Zhao

    2015-12-01

    Full Text Available The urokinase-type plasminogen activator receptor (uPAR or CD87 is a glycolipid-anchored membrane protein often expressed in the microenvironment of invasive solid cancers and high levels are generally associated with poor patient prognosis (Kriegbaum et al., 2011 [1]. uPAR is organized as a dynamic modular protein structure composed of three homologous Ly6/uPAR domains (LU.This internally flexible protein structure of uPAR enables an allosteric regulation of the interactions with its two principal ligands: the serine protease urokinase-type plasminogen activator (uPA and the provisional matrix protein vitronectin (Vn (Mertens et al., 2012; Gårdsvoll et al., 2011; Madsen et al., 2007 [2–4]. The data presented here relates to the non-covalent trapping of one of these biologically relevant uPAR-conformations by a novel class of monoclonal antibodies (Zhao et al., 2015 [5] and to the general mapping of the topographic epitope landscape on uPAR. The methods required to achieve these data include: (1 recombinant expression and purification of a uPAR-hybrid protein trapped in the desired conformation [patent; WO 2013/020898 A12013]; (2 developing monoclonal antibodies with unique specificities using this protein as antigen; (3 mapping the functional epitope on uPAR for these mAbs by surface plasmon resonance with a complete library of purified single-site uPAR mutants (Zhao et al., 2015; Gårdsvoll et al., 2006 [5,6]; and finally (4 solving the three-dimensional structures for one of these mAbs by X-ray crystallography alone and in complex with uPAR [deposited in the PDB database as 4QTH and 4QTI, respectively].

  1. Mapping the topographic epitope landscape on the urokinase plasminogen activator receptor (uPAR) by surface plasmon resonance and X-ray crystallography.

    Zhao, Baoyu; Gandhi, Sonu; Yuan, Cai; Luo, Zhipu; Li, Rui; Gårdsvoll, Henrik; de Lorenzi, Valentina; Sidenius, Nicolai; Huang, Mingdong; Ploug, Michael

    2015-12-01

    The urokinase-type plasminogen activator receptor (uPAR or CD87) is a glycolipid-anchored membrane protein often expressed in the microenvironment of invasive solid cancers and high levels are generally associated with poor patient prognosis (Kriegbaum et al., 2011 [1]). uPAR is organized as a dynamic modular protein structure composed of three homologous Ly6/uPAR domains (LU).This internally flexible protein structure of uPAR enables an allosteric regulation of the interactions with its two principal ligands: the serine protease urokinase-type plasminogen activator (uPA) and the provisional matrix protein vitronectin (Vn) (Mertens et al., 2012; Gårdsvoll et al., 2011; Madsen et al., 2007 [2-4]). The data presented here relates to the non-covalent trapping of one of these biologically relevant uPAR-conformations by a novel class of monoclonal antibodies (Zhao et al., 2015 [5]) and to the general mapping of the topographic epitope landscape on uPAR. The methods required to achieve these data include: (1) recombinant expression and purification of a uPAR-hybrid protein trapped in the desired conformation [patent; WO 2013/020898 A12013]; (2) developing monoclonal antibodies with unique specificities using this protein as antigen; (3) mapping the functional epitope on uPAR for these mAbs by surface plasmon resonance with a complete library of purified single-site uPAR mutants (Zhao et al., 2015; Gårdsvoll et al., 2006 [5,6]); and finally (4) solving the three-dimensional structures for one of these mAbs by X-ray crystallography alone and in complex with uPAR [deposited in the PDB database as 4QTH and 4QTI, respectively]. PMID:26504891

  2. [Diffuse x-ray wide-angle scattering of polyglutamic acid in solution].

    Fedorov, B A; Becker, M; Damaschun, G; Damaschun, H; Gedicke, C; Zirwer, D

    1977-01-01

    The diffuse wide angle x-ray scattering (WAXS) of polyglutamic acid (PGA) in solution was studied using an x-ray diffractometer with small aperture of the primary beam. The scattering curve was recorded at an angular interval from (article: see text). The experimental scattering intensity of PGA with alpha-helical CD spectrum showed a maximum at 14.4 nm-1. Unordered PGA in solution yielded no maximum at this scattering angle. The studies have proved that the scattering theory can be applied to globular proteins in solution as well as to chain molecules in solution in this angular interval. The differences between the calculated scattering curves and the experimental curves indicate minor movements of the side chains of PGA in solutions and slight structuring of the solvent at the surface of the polypeptide chain. PMID:25547

  3. Structures of Plutonium(IV) and Uranium(VI) with N,N-Dialkyl Amides from Crystallography, X-ray Absorption Spectra, and Theoretical Calculations.

    Acher, Eléonor; Hacene Cherkaski, Yanis; Dumas, Thomas; Tamain, Christelle; Guillaumont, Dominique; Boubals, Nathalie; Javierre, Guilhem; Hennig, Christoph; Solari, Pier Lorenzo; Charbonnel, Marie-Christine

    2016-06-01

    The structures of plutonium(IV) and uranium(VI) ions with a series of N,N-dialkyl amides ligands with linear and branched alkyl chains were elucidated from single-crystal X-ray diffraction (XRD), extended X-ray absorption fine structure (EXAFS), and theoretical calculations. In the field of nuclear fuel reprocessing, N,N-dialkyl amides are alternative organic ligands to achieve the separation of uranium(VI) and plutonium(IV) from highly concentrated nitric acid solution. EXAFS analysis combined with XRD shows that the coordination structure of U(VI) is identical in the solution and in the solid state and is independent of the alkyl chain: two amide ligands and four bidentate nitrate ions coordinate the uranyl ion. With linear alkyl chain amides, Pu(IV) also adopt identical structures in the solid state and in solution with two amides and four bidentate nitrate ions. With branched alkyl chain amides, the coordination structure of Pu(IV) was more difficult to establish unambiguously from EXAFS. Density functional theory (DFT) calculations were consequently performed on a series of structures with different coordination modes. Structural parameters and Debye-Waller factors derived from the DFT calculations were used to compute EXAFS spectra without using fitting parameters. By using this methodology, it was possible to show that the branched alkyl chain amides form partly outer-sphere complexes with protonated ligands hydrogen bonded to nitrate ions. PMID:27171842

  4. X-rays and some applications

    This book is one of the specialized books issued by the Arab Atomic Energy Agency about the key technologies of interest to Arab researchers . The book contains 10 chapters as follows: the nature of X-ray, methods of production and measurement of X-rays, X-ray and materials, X-ray crystallography, X-ray and chemistry, X-ray and physics, biological effects of X-ray, radiography in the field of medicine and biology, X-ray in the field of industry, other applications in agriculture, imaging artifacts and paintings and geology.

  5. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

    Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D. [National Security Technologies, LLC, Livermore, California 94550 (United States); Wu, M.; Loisel, G. P. [Sandia National Laboratories, Albuquerque, New Mexico 87123 (United States)

    2014-11-15

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  6. Measuring the X-ray Resolving Power of Bent Potassium Acid Phthalate Diffraction Crystals

    Haugh, M. J. [NSTec; Wu, M. [SNL; Jacoby, K. D. [NSTec; Loisel, G. P. [SNL

    2014-11-01

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories (SNL) in Albuquerque, NM. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a dual goniometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  7. Site-specific Incorporation of 3-Iodo-L-tyrosine into Proteins and Single-wavelength Anomalous Dispersion Phasing with Soft X-ray in Protein Crystallography

    Murayama, Kazutaka; Sakamoto, Kensaku

    Iodine is a good anomalous scatter for radiations from in-house X-ray generators (Cu/CrKα). Non-natural amino acid, 3-iodo-L-tyrosine, is able to be site-specifically incorporated into proteins with amber suppresser tRNA and mutated TyrRS from M. jannaschii in the E. coli expression system. To determine the crystal structure of acetyl transferase from T. thermophilus, iodotyrosine-containing proteins were prepared and crystallized. Structure determination was successfully conducted with the protein variant with iodotyrosine at position 111. Anomalous signals from iodotyrosine with Cu/CrKα radiations were both sufficient to calculate clear electron density map. In the crystal structure, iodotyrosine did not significantly disturb the native structure.

  8. Structure of Langmuir-Blodgett films of fatty acid salts from electron, x-ray, and neutron diffraction data

    The data on the structure of Langmuir-Blodgett films of fatty acid salts obtained by the methods of electron diffraction structure analysis are compared with the corresponding results of X-ray and neutron reflectivity measurements

  9. X-ray microtomography of hydrochloric acid propagation in carbonate rocks

    Acid treatments are used in the oil and gas industry, to increase the permeability of the carbonate reservoirs by creating preferential channels, called wormholes. Channels formation is strongly influenced by acid type and injection rate. The aim of this study is to evaluate some characteristics of the microporous system of carbonate rocks, before and after acidizing. For that purpose X-ray high-resolution microtomography was used. The results show that this technique can be used as a reliable method to analyze microstructural characteristics of the wormholes. - Highlights: • Wormholes are flow channels, which are created when acid is injected in rocks. • Wormhole morphology classification is a function of the acid injection rate. • Microtomography evaluates porous media as well as the wormholes structures formed

  10. Oil-free hyaluronic acid matrix for serial femtosecond crystallography

    Sugahara, Michihiro; Song, Changyong; Suzuki, Mamoru; Masuda, Tetsuya; Inoue, Shigeyuki; Nakane, Takanori; Yumoto, Fumiaki; Nango, Eriko; Tanaka, Rie; Tono, Kensuke; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Yabashi, Makina; Nureki, Osamu; Numata, Keiji; Iwata, So

    2016-04-01

    The grease matrix was originally introduced as a microcrystal-carrier for serial femtosecond crystallography and has been expanded to applications for various types of proteins, including membrane proteins. However, the grease-based matrix has limited application for oil-sensitive proteins. Here we introduce a grease-free, water-based hyaluronic acid matrix. Applications for proteinase K and lysozyme proteins were able to produce electron density maps at 2.3-Å resolution.

  11. Oil-free hyaluronic acid matrix for serial femtosecond crystallography

    Michihiro Sugahara; Changyong Song; Mamoru Suzuki; Tetsuya Masuda; Shigeyuki Inoue; Takanori Nakane; Fumiaki Yumoto; Eriko Nango; Rie Tanaka; Kensuke Tono; Yasumasa Joti; Takashi Kameshima; Takaki Hatsui; Makina Yabashi; Osamu Nureki

    2016-01-01

    The grease matrix was originally introduced as a microcrystal-carrier for serial femtosecond crystallography and has been expanded to applications for various types of proteins, including membrane proteins. However, the grease-based matrix has limited application for oil-sensitive proteins. Here we introduce a grease-free, water-based hyaluronic acid matrix. Applications for proteinase K and lysozyme proteins were able to produce electron density maps at 2.3-Å resolution.

  12. Destruction of formic acid by soft X-rays in star-forming regions

    Boechat-Roberty, H M; Santos, A C F

    2005-01-01

    Formic acid is much more abundant in the solid state, both in interstellar ices and cometary ices, than in the interstellar gas (ice/gas ~ 10^{4}) and this point remains a puzzle. The goal of this work is to experimentally study ionization and photodissociation processes of HCOOH (formic acid), a glycine precursor molecule. The measurements were taken at the Brazilian Synchrotron Light Laboratory (LNLS), employing soft X-ray photons from toroidal grating monochromator TGM) beamline (200 - 310 eV). Mass spectra were obtained using photoelectron photoion coincidence (PEPICO) method. Kinetic energy distributions and abundances for each ionic fragment have been obtained from the analysis of the corresponding peak shapes in the mass spectra. Photoionization and photodissociation cross sections were also determined. Due to the large photodissociation cross section of HCOOH it is possible that in PDRs regions, just after molecules evaporation from the grain surface, formic acid molecules are almost totally destroyed...

  13. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    Balaev, V. V.; Lashkov, A. A., E-mail: alashkov83@gmail.com; Gabdoulkhakov, A. G.; Seregina, T. A.; Dontsova, M. V.; Mikhailov, A. M. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2015-03-15

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis (YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability (R{sub work} = 16.2, R{sub free} = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh.

  14. Exploring the Mechanism of β-Lactam Ring Protonation in the Class A β-lactamase Acylation Mechanism Using Neutron and X-ray Crystallography

    Vandavasi, Venu Gopal; Weiss, Kevin L.; Cooper, Jonathan B.; Erskine, Peter T.; Tomanicek, Stephen J.; Ostermann, Andreas; Schrader, Tobias E.; Ginell, Stephan L.; Coates, Leighton

    2016-01-14

    The catalytic mechanism of class A beta-lactamases is often debated due in part to the large number of amino acids that interact with bound beta-lactam substrates. The role and function of the conserved residue Lys 73 in the catalytic mechanism of class A type beta-lactamase enzymes is still not well understood after decades of scientific research. To better elucidate the functions of this vital residue, we used both neutron and high-resolution X-ray diffraction to examine both the structures of the ligand free protein and the acyl-enzyme complex of perdeuterated E166A Toho-1 beta-lactamase with the antibiotic cefotaxime. The E166A mutant lacks a critical glutamate residue that has a key role in the deacylation step of the catalytic mechanism, allowing the acyl-enzyme adduct to be captured for study. In our ligand free structures, Lys 73 is present in a single conformation, however in all of our acyl-enzyme structures, Lys 73 is present in two different conformations, in which one conformer is closer to Ser 70 while the other conformer is positioned closer to Ser 130, which supports the existence of a possible pathway by which proton transfer from Lys 73 to Ser 130 can occur. This and further clarifications of the role of Lys 73 in the acylation mechanism may facilitate the design of inhibitors that capitalize on the enzymes native machinery.

  15. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis (YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability (Rwork = 16.2, Rfree = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh

  16. Resonant x-ray reflectivity from a bromine-labeled fatty acid Langmuir monolayer

    Resonant x-ray reflectivity exploits the energy dependence of atomic scattering factors to locate resonant atoms within the electron density distribution of thin films. We apply the technique to a monolayer of bromo-stearic acid at the air/water interface. The data collection protocol employed cycles through several energies in the vicinity of the bromine K absorption edge and verifies that the energy dependencies observed are indeed resonant effects. The analysis specifies the location of the Br atom with sub-angstrom precision and must consider both the real and imaginary parts of the changes in the scattering factor to be consistent with the known structure and stoichiometry of this test case

  17. The interaction of protein and polysilicic acid: an x-ray and neutron reflection study

    The objective of this study was to begin to emulate biomineralisation processes whereby an ordered network of silica, directed by an organic template, is constructed. Two preparative routes were applied. In the first method a protein-silica interaction was induced by near-matching the isoelectric point of a thin protein film (bovine milk beta-casein or beta-lactoglobulin) to that of a polysilicic acid sub-phase in order to form a composite material at the air-water interface. The film conformation adopted at the interface was then studied by reflectivity using neutrons and X-rays as a function of film compression and pH. The second method involved a self-assembly process, illustrated here by an attempt to include either hen egg-white lysozyme, bovine milk beta-casein or beta-lactoglobulin into a highly ordered silicate film grown at the air-water interface

  18. Osmium(III) analogues of KP1019: Electrochemical and chemical synthesis, spectroscopic characterization, x-ray crystallography, hydrolytic stability, and antiproliferative activity

    Kuhn, Paul-Steffen

    2014-10-20

    A one-electron reduction of osmium(IV) complexes trans-[OsIVCl4(Hazole)2], where Hazole = 1H-pyrazole ([1]0), 2H-indazole ([2]0), 1H-imidazole ([3]0), and 1H-benzimidazole ([4]0), afforded a series of eight new complexes as osmium analogues of KP1019, a lead anticancer drug in clinical trials, with the general formula (cation)[trans-OsIIICl4(Hazole)2], where cation = H2pz+ (H2pz[1]), H2ind+ (H2ind[2]), H2im+ (H2im[3]), Ph4P+ (Ph4P[3]), nBu4N+ (nBu4N[3]), H2bzim+ (H2bzim[4]), Ph4P+ (Ph4P[4]), and nBu4N+ (nBu4N[4]). All complexes were characterized by elemental analysis, 1H NMR spectroscopy, electrospray ionization mass spectrometry, UV-vis spectroscopy, cyclic voltammetry, while H2pz[1], H2ind[2], and nBu4[3], in addition, by X-ray diffraction. The reduced species [1]- and [4]- are stable in aqueous media in the absence of air oxygen and do not react with small biomolecules such as amino acids and the nucleotide 5′-dGMP. Cell culture experiments in five different human cancer cell lines (HeLa, A549, FemX, MDA-MB-453, and LS-174) and one noncancerous cell line (MRC-5) were performed, and the results were discussed and compared to those for KP1019 and cisplatin. Benzannulation in complexes with similar structure enhances antitumor activity by several orders of magnitude, implicating different mechanisms of action of the tested compounds. In particular, complexes H2ind[2] and H2bzim[4] exhibited significant antiproliferative activity in vitro when compared to H2pz[1] and H2im[3]. (Chemical Equation Presented).

  19. Electron Crystallography of Aquaporins

    Andrews, Simeon; Reichow, Steve L; Gonen, Tamir

    2008-01-01

    Aquaporins are a family of ubiquitous membrane proteins that form a pore for the permeation of water. Both electron and X-ray crystallography played major roles in determining the atomic structures of a number of aquaporins. This review focuses on electron crystallography, and its contribution to the field of aquaporin biology. We briefly discuss electron crystallography and the two-dimensional crystallization process. We describe features of aquaporins common to both electron and X-ray cryst...

  20. X-ray Excited Optical Fluorescence and Diffraction Imaging of Reactivity and Crystallinity in a Zeolite Crystal: Crystallography and Molecular Spectroscopy in One.

    Ristanović, Zoran; Hofmann, Jan P; Richard, Marie-Ingrid; Jiang, Tao; Chahine, Gilbert A; Schülli, Tobias U; Meirer, Florian; Weckhuysen, Bert M

    2016-06-20

    Structure-activity relationships in heterogeneous catalysis are challenging to be measured on a single-particle level. For the first time, one X-ray beam is used to determine the crystallographic structure and reactivity of a single zeolite crystal. The method generates μm-resolved X-ray diffraction (μ-XRD) and X-ray excited optical fluorescence (μ-XEOF) maps of the crystallinity and Brønsted reactivity of a zeolite crystal previously reacted with a styrene probe molecule. The local gradients in chemical reactivity (derived from μ-XEOF) were correlated with local crystallinity and framework Al content, determined by μ-XRD. Two distinctly different types of fluorescent species formed selectively, depending on the local zeolite crystallinity. The results illustrate the potential of this approach to resolve the crystallographic structure of a porous material and its reactivity in one experiment via X-ray induced fluorescence of organic molecules formed at the reactive centers. PMID:27145171

  1. Characterization of amino acid adlayers on InAs surfaces using X-ray photoelectron spectroscopy

    Removal of surface oxide layers and the prevention of their reformation is an essential step in the use of III-V semiconductor technologies. Highlighted here are data exploring the use of amino acid (AA) self-assembled monolayers (SAMs) to block the pre-growth of oxides on indium arsenide surfaces. Three different AAs were used: lysine, aspartic acid, and cysteine. The adlayers were characterized by atomic force microscopy (AFM), Raman, and angle resolved X-ray photoelectron spectroscopy (ARXPS). AFM data suggest that the AA functional groups affect the packing and orientation of the molecules on the surfaces, reinforced by contact angle data. Raman data provide proof that the type of functional group alters the intensity of the unscreened LO phonon, resulting in an electrostatic stabilization, in the case of lysine, which lends to the case of electrostatic interactions blocking oxide formation. ARXPS demonstrated that the degree of oxide blocking is dependent upon the type of functional group and further verifies inferences made from the Raman spectra. The degree of monolayer formation is also determined from this data. It is concluded that AA's can be useful means for blocking oxide growth on InAs (1 0 0) surfaces, which also provides insights into how protein and peptide side chains might interact with such surfaces.

  2. X-ray-induced photo-chemistry and X-ray absorption spectroscopy of biological samples

    George, Graham N.; Pickering, Ingrid J.; Pushie, M. Jake; Nienaber, Kurt; Hackett, Mark J.; Ascone, Isabella; Hedman, Britt; Hodgson, Keith O.; Aitken, Jade B.; Levina, Aviva; Glover, Christopher; Lay, Peter A.

    2012-01-01

    X-ray-induced photo-chemistry of metal sites within biological molecules is a concern for X-ray absorption spectroscopy, X-ray crystallography and other techniques in which samples are illuminated with X-rays. The effects of X-ray-induced photo-chemistry are reviewed and the methods used to mitigate these in X-ray absorption spectroscopy are outlined.

  3. Study of the earth's deep interior and crystallography. X-ray and neutron diffraction experiments under high pressures

    History of the study of the Earth's deep interior was reviewed. In order to understand Earth's deep interior from the view point of materials science, X-ray diffraction under high pressure and high temperature played very important role. Use of synchrotron radiation dramatically advanced this experimental technique and it is now possible to make precise X-ray study under the P-T conditions corresponding even to the center of the Earth. In order to clarify the behavior of light elements such as hydrogen, however, studies using neutron diffraction are also required. A new neutron beam line dedicated for high-pressure science is constructed at J-PARC and is now ready for use. (author)

  4. Azo coupling of 4-nitrophenyldiazonium chloride with aliphatic nucleophiles: an integrated organic synthesis and X-ray crystallography experiment; Acoplamento de cloreto de 4-nitrofenildiazonio com nucleofilos alifaticos: experimento integrado de sintese organica e cristalografia de raios X

    Cunha, Silvio; Marques, Monique F.; Rocha, Valeria, E-mail: silviodc@ufba.br [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Instituto de Quimica; Lariucci, Carlito; Vencato, Ivo [Universidade Federal de Goiania (UFG), GO (Brazil). Instituto de Fisica

    2013-11-01

    This article describes an undergraduate experiment for the synthesis of p-nitrophenyldiazonium chloride and its coupling with acetylacetone and two enaminones, 4-phenylamino-pent-3-en-2-one and 4-amino-pent-3-en-2-one, in an adaptation of a previously reported synthetic protocol. The azo dyes 4-(E)-phenylamino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one and 4-(E)-amino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one were obtained, and the solid state structure of this latter azo compound was characterized by single crystal X-ray diffraction studies. This two-week integrated laboratory approach involves simple synthetic experiments and microwave chemistry in the organic laboratory plus crystallography analysis, suitable for novice students on undergraduate experimental chemistry courses. (author)

  5. X-ray Crystallography, DFT Calculations and Molecular Docking of Indole-Arylpiperazine Derivatives as α1A-Adrenoceptor Antagonists

    Wei Xu; Jun-Jun Huang; Bin-Hao Shao; Xing-Jie Xu; Ren-Wang Jiang; Mu Yuan

    2015-01-01

    Indole-arylpiperazine derivatives have exhibited good selectivity for the α1A-adrenoceptor, but the structure-activity-binding mechanism relationship remains unclear. In the current study, three compounds (1, 2 and 3) were investigated through single-crystal X-ray diffraction analysis, density functional theory (DFT) calculations and molecular docking using a homology model of the α1A receptor. Compounds 1 and 3 form H-bonds networks to stabilize their three-dimensional structures, while C–H...

  6. Synthesis, X-ray crystallography, spectroscopic (FT-IR, 1H &13C NMR and UV), computational (DFT/B3LYP) and enzymes inhibitory studies of 7-hydroximinocholest-5-en-3-ol acetate

    Ahmad, Faheem; Parveen, Mehtab; Alam, Mahboob; Azaz, Shaista; Malla, Ali Mohammed; Alam, Mohammad Jane; Lee, Dong-Ung; Ahmad, Shabbir

    2016-07-01

    The present study reports the synthesis of 7-Hydroximinocholest-5-en-3-ol acetate (syn. 3β-acetoxycholest-5-en-7-one oxime; in general, steroidal oxime). The identity of steroidal molecule was confirmed by NMR, FT-IR, MS, CHN microanalysis and X-ray crystallography. DFT calculations on the titled molecule have been performed. The molecular structure and spectra interpreted by Gaussian hybrid computational analysis theory (B3LYP) are found to be in good correlation with the experimental data obtained from the various spectrophotometric techniques. The vibrational bands appearing in the FTIR are assigned with great accuracy using harmonic frequencies along with intensities and animated modes. Molecular properties like HOMO-LUMO analysis, chemical reactivity descriptors, MEP mapping, dipole moment and natural atomic charges have been presented at the same level of theory. Moreover, the Hirshfeld analysis was carried out to ascertain the secondary interactions and associated 2D fingerprint plots. The percentages of various interactions are pictorialized by fingerprint plots of Hirshfeld surface. Steroidal oxime exhibited promising inhibitory activity against acetylcholinesterase (AChE) as compared to the reference drug, tacrine. Molecular docking was performed to introduce steroidal molecules into the X-ray crystal structures of acetylcholinesterase at the active site to find out the probable binding mode. The results of molecular docking admitted that steroidal oxime may exhibit enzyme inhibitor activity.

  7. X-ray investigation of gene-engineered human insulin crystallized from a solution containing polysialic acid

    Timofeev, V. I.; Chuprov-Netochin, R. N.; Samigina, V. R.; Bezuglov, V. V.; Miroshnikov, K. A.; Kuranova, I. P.

    2010-01-01

    Attempts to crystallize the noncovalent complex of recombinant human insulin with polysialic acid were carried out under normal and microgravity conditions. Both crystal types belonged to the same space group, I213, with unit-cell parameters a = b = c = 77.365 Å, α = β = γ = 90.00°. The reported space group and unit-cell parameters are almost identical to those of cubic insulin reported in the PDB. The results of X-ray studies confirmed that the crystals obtained were cubic insulin crystals and that they contained no polysialic acid or its fragments. Electron-density maps were calculated using X-ray diffraction sets from earth-grown and microgravity-grown crystals and the three-dimensional structure of the insulin molecule was determined and refined. The conformation and secondary-structural elements of the insulin molecule in different crystal forms were compared. PMID:20208155

  8. Intergrown new zeolite beta polymorphs with interconnected 12-ring channels solved by combining electron crystallography and single-crystal X-ray diffraction

    Yu, Zhengbao

    2012-10-09

    Two new polymorphs of zeolite beta, denoted as SU-78A and SU-78B, were synthesized by employing dicyclohexylammonium hydroxides as organic structure-directing agents. The structure was solved by combining transmission electron microscopy and single-crystal X-ray diffraction. SU-78 is an intergrowth of SU-78A and SU-78B and contains interconnected 12-ring channels in three directions. The two polymorphs are built from the same building layer, similar to that for the zeolite beta family. The layer stacking in SU-78, however, is different from those in zeolite beta polymorph A, B, and C, showing new zeolite framework topologies. SU-78 is thermally stable up to 600 °C. © 2012 American Chemical Society.

  9. Titration of a Solid Acid Monitored by X-Ray Diffraction

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

    An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

  10. Structural investigation of (2E)-2-(ethoxycarbonyl)-3-[(4-methoxyphenyl)amino]prop-2-enoic acid: X-ray crystal structure, spectroscopy and DFT

    Venkatesan, Perumal; Rajakannan, Venkatachalam; Venkataramanan, Natarajan S.; Ilangovan, Andivelu; Sundius, Tom; Thamotharan, Subbiah

    2016-09-01

    The title compound, (2E)-2-(ethoxycarbonyl)-3-[(4-methoxyphenyl)amino]prop-2-enoic acid is characterized by means of X-ray crystallography, spectroscopic methods and quantum chemical calculations. The title compound crystallizes in centrosymmetric space group P21/c. Moreover, the crystal structure is primarily stabilized through intramolecular Nsbnd H⋯O and Osbnd H⋯O and intermolecular Nsbnd H⋯O and Csbnd H⋯O interactions along with carbonyl⋯carbonyl and Csbnd H⋯C contacts. These intermolecular interactions are analysed and quantified by using Hirshfeld surface analysis, PIXEL energy, NBO, AIM and DFT calculations. The overall lattice energies of the title and parent compounds suggest that the title compound is stabilized by a 4.5 kcal mol-1 higher energy than the parent compound. The additional stabilization force comes from the methoxy substitution on the title molecule, which is evident since the methoxy group is involved in the intermolecular Csbnd H⋯O interaction as an acceptor. The vibrational modes of the interacting groups are investigated using both experimental and theoretical FT-IR and FT-Raman spectra. The experimental and theoretical UV-Vis spectra agree well. The time dependent DFT spectra show that the ligand-to-ligand charge transfer is responsible for the intense absorbance of the compound.

  11. Novel protein-inhibitor interactions in site 3 of Ca(2+)-bound S100B as discovered by X-ray crystallography.

    Cavalier, Michael C; Melville, Zephan; Aligholizadeh, Ehson; Raman, E Prabhu; Yu, Wenbo; Fang, Lei; Alasady, Milad; Pierce, Adam D; Wilder, Paul T; MacKerell, Alexander D; Weber, David J

    2016-06-01

    Structure-based drug discovery is under way to identify and develop small-molecule S100B inhibitors (SBiXs). Such inhibitors have therapeutic potential for treating malignant melanoma, since high levels of S100B downregulate wild-type p53 tumor suppressor function in this cancer. Computational and X-ray crystallographic studies of two S100B-SBiX complexes are described, and both compounds (apomorphine hydrochloride and ethidium bromide) occupy an area of the S100B hydrophobic cleft which is termed site 3. These data also reveal novel protein-inhibitor interactions which can be used in future drug-design studies to improve SBiX affinity and specificity. Of particular interest, apomorphine hydrochloride showed S100B-dependent killing in melanoma cell assays, although the efficacy exceeds its affinity for S100B and implicates possible off-target contributions. Because there are no structural data available for compounds occupying site 3 alone, these studies contribute towards the structure-based approach to targeting S100B by including interactions with residues in site 3 of S100B. PMID:27303795

  12. X-ray Crystallography, DFT Calculations and Molecular Docking of Indole-Arylpiperazine Derivatives as α1A-Adrenoceptor Antagonists.

    Xu, Wei; Huang, Jun-Jun; Shao, Bin-Hao; Xu, Xing-Jie; Jiang, Ren-Wang; Yuan, Mu

    2015-01-01

    Indole-arylpiperazine derivatives have exhibited good selectivity for the α1A-adrenoceptor, but the structure-activity-binding mechanism relationship remains unclear. In the current study, three compounds (1, 2 and 3) were investigated through single-crystal X-ray diffraction analysis, density functional theory (DFT) calculations and molecular docking using a homology model of the α1A receptor. Compounds 1 and 3 form H-bonds networks to stabilize their three-dimensional structures, while C-H···π interactions play a significant role in the packing of 2. Based on DFT-optimized conformations, the HOMO-LUMO energy gaps and molecular electrostatic potential (MEP) were theoretically calculated at the B3LYP/6-311G (d, p) level of theory. Chemical reactivity increases in the order of 3 < 2 < 1, and the maximum positive region of the MEP maps is mainly localized over the NH group. The binding mechanisms of ligand-α1A-adrenoceptor complexes were illustrated by molecular docking. Binding to Gln177 of the second extracellular loop region via hydrogen bonds is likely to be essential for α1A-selective antagonists. The present work sheds light on the studies of structure-activity-binding mechanism and aids in the design of α1A antagonists with high selectivity. PMID:26528963

  13. X-ray Crystallography, DFT Calculations and Molecular Docking of Indole-Arylpiperazine Derivatives as α1A-Adrenoceptor Antagonists

    Wei Xu

    2015-10-01

    Full Text Available Indole-arylpiperazine derivatives have exhibited good selectivity for the α1A-adrenoceptor, but the structure-activity-binding mechanism relationship remains unclear. In the current study, three compounds (1, 2 and 3 were investigated through single-crystal X-ray diffraction analysis, density functional theory (DFT calculations and molecular docking using a homology model of the α1A receptor. Compounds 1 and 3 form H-bonds networks to stabilize their three-dimensional structures, while C–H···π interactions play a significant role in the packing of 2. Based on DFT-optimized conformations, the HOMO-LUMO energy gaps and molecular electrostatic potential (MEP were theoretically calculated at the B3LYP/6-311G (d, p level of theory. Chemical reactivity increases in the order of 3 < 2 < 1, and the maximum positive region of the MEP maps is mainly localized over the NH group. The binding mechanisms of ligand-α1A-adrenoceptor complexes were illustrated by molecular docking. Binding to Gln177 of the second extracellular loop region via hydrogen bonds is likely to be essential for α1A-selective antagonists. The present work sheds light on the studies of structure-activity-binding mechanism and aids in the design of α1A antagonists with high selectivity.

  14. Nucleic acid fragmentation on the millisecond timescale using a conventional X-ray rotating anode source: application to protein–DNA footprinting

    Henn, Arnon; Halfon, Jacob; Kela, Itai; Orion, Itzhak; Sagi, Irit

    2001-01-01

    Nucleic acid fragmentation (footprinting) by ·OH radicals is used often as a tool to probe nucleic acid structure and nucleic acid–protein interactions. This method has proven valuable because it provides structural information with single base pair resolution. Recent developments in the field introduced the ‘synchrotron X-ray footprinting’ method, which uses a high-flux X-ray source to produce single base pair fragmentation of nucleic acid in tens of milliseconds. We developed a complementar...

  15. Isolation and x-ray structure of deoxycholic acid from the sponge Ircinia sp.

    Singh, K.S.; Kaminsky, W.

    GX [4d]. Acknowledgments - We are grateful to the Council of Scientific and Industrial Research (CSIR) and the Ministry of Earth Sciences (MoES), India for financial support as well as to the National Science Foundation, USA, grant 0840520... for providing funding for the X-ray equipment. We thank Deepak N. Naik for carrying out antimicrobial screening and Uday Mandrekar for sample collection. References [1] Singh KS, Kaminsky WH, Rodrigues C, Naik CG. (2009) Structural studies and antimicrobial...

  16. Use of X-ray and gamma-induced mutants of lactic acid bacteria in the manufacture of dairy products

    With the aid of X-ray and gamma irradiation were got mutants of lactic acid bacteria, which steadily retain acquired properties. Use of proteolytically active mutant strains in the production of armianski and sovetski cheeses shortened the time of their ripening and increased their quality. Gamma-mutant strain L. lactis 1621/I-M with high phenolstability was received and antibiotic activity with respect to some representatives of pathogenic microflora of the bowels. Use of this mutant in starters for sour milk products will raise their therapeutic effect against intestinal diseases. Deep morphological changes are taking place in lactic acid bacteria under the influence of ionizing radiation. (orig.)

  17. X-Ray Characterisation of Various Aluminium Phases in the Medicinal Herb Bacopa Monnieri Affected by Simulated Acid Rain

    Mallick, B.

    2012-01-01

    In the present investigation various aluminium-based new phases formed due to substitution of sulphur via simulated acid rain in Bacopa monnieri have been analyzed using X-ray diffraction (XRD) technique. So far there is no report on the effects of acid rain on the B. monnieri herb and its vital properties like memory-boosting mechanism. Therefore, in the present study, an attempt has been made to analyze the various aluminium phase (salt) formations due to the substitution of sulphur via sim...

  18. X-Ray Absorption Fine Structure Investigation of Copper(II) Mixed Ligand Complexes with Pyridinedicarboxylic Acid as Primary Ligand

    Dar, D. Ah.; Gaur, A.; Soni, B.; Shrivastava, B. D.; Prasad, J.; Srivastava, K.; Jha, S. N.; Bhattacharyya, D.

    2015-05-01

    The X-ray absorption fine structure (XAFS) spectra at the K-edge of the copper complexes Cu(PDC)(Mim)3 H2O ( 1) and Cu(PDC)2(EA)2H2O ( 2) (where PDC - Pyridine-2,3-dicarboxylic acid, Mim - 2-methylimidazole, and EA - ethyl acetate) have been investigated. The experimental extended X-ray absorption fine structure data of complex 1 have been analyzed by fitting the theoretical model generated from its own crystallographic data. The crystallographic data for complex 2 are not available. It has been found by comparing the intensity of the pre-edge peaks and X-ray absorption near edge structure features of complexes 1 and 2 that both complexes possess square pyramidal geometry around the copper centers and thus complex 2 is analogous to complex 1. Hence, the theoretical model generated for complex 1 has been fitted to the experimental EXAFS data of complex 2 to determine the structural parameters of complex 2. The coordination geometry of both complexes has been depicted. Further, the chemical shifts have been used to determine the oxidation state as well as to estimate the effective nuclear charge on the copper atom.

  19. Structure of HI-6*sarin-acetylcholinesterase determined by X-ray crystallography and molecular dynamics simulation: reactivator mechanism and design.

    Fredrik Ekström

    Full Text Available Organophosphonates such as isopropyl metylphosphonofluoridate (sarin are extremely toxic as they phosphonylate the catalytic serine residue of acetylcholinesterase (AChE, an enzyme essential to humans and other species. Design of effective AChE reactivators as antidotes to various organophosphonates requires information on how the reactivators interact with the phosphonylated AChEs. However, such information has not been available hitherto because of three main challenges. First, reactivators are generally flexible in order to change from the ground state to the transition state for reactivation; this flexibility discourages determination of crystal structures of AChE in complex with effective reactivators that are intrinsically disordered. Second, reactivation occurs upon binding of a reactivator to the phosphonylated AChE. Third, the phosphorous conjugate can develop resistance to reactivation. We have identified crystallographic conditions that led to the determination of a crystal structure of the sarin(nonaged-conjugated mouse AChE in complex with [(E-[1-[(4-carbamoylpyridin-1-ium-1-ylmethoxymethyl]pyridin-2-ylidene]methyl]-oxoazanium dichloride (HI-6 at a resolution of 2.2 A. In this structure, the carboxyamino-pyridinium ring of HI-6 is sandwiched by Tyr124 and Trp286, however, the oxime-pyridinium ring is disordered. By combining crystallography with microsecond molecular dynamics simulation, we determined the oxime-pyridinium ring structure, which shows that the oxime group of HI-6 can form a hydrogen-bond network to the sarin isopropyl ether oxygen, and a water molecule is able to form a hydrogen bond to the catalytic histidine residue and subsequently deprotonates the oxime for reactivation. These results offer insights into the reactivation mechanism of HI-6 and design of better reactivators.

  20. Fourier-transform Ghost Imaging with Hard X-rays

    Hong YU; Lu, Ronghua; Han, Shensheng; Xie, Honglan; Du, Guohao; Xiao, Tiqiao; Zhu, Daming

    2016-01-01

    Knowledge gained through X-ray crystallography fostered structural determination of materials and greatly facilitated the development of modern science and technology in the past century. Atomic details of sample structures is achievable by X-ray crystallography, however, it is only applied to crystalline structures. Imaging techniques based on X-ray coherent diffraction or zone plates are capable of resolving the internal structure of non-crystalline materials at nanoscales, but it is still ...

  1. Synthesis and X-ray Crystallography of [Mg(H2O)6][AnO2(C2H5COO)3]2 (An = U, Np, or Pu).

    Serezhkin, Viktor N; Grigoriev, Mikhail S; Abdulmyanov, Aleksey R; Fedoseev, Aleksandr M; Savchenkov, Anton V; Serezhkina, Larisa B

    2016-08-01

    Synthesis and X-ray crystallography of single crystals of [Mg(H2O)6][AnO2(C2H5COO)3]2, where An = U (I), Np (II), or Pu (III), are reported. Compounds I-III are isostructural and crystallize in the trigonal crystal system. The structures of I-III are built of hydrated magnesium cations [Mg(H2O)6](2+) and mononuclear [AnO2(C2H5COO)3](-) complexes, which belong to the AB(01)3 crystallochemical group of uranyl complexes (A = AnO2(2+), B(01) = C2H5COO(-)). Peculiarities of intermolecular interactions in the structures of [Mg(H2O)6][UO2(L)3]2 complexes depending on the carboxylate ion L (acetate, propionate, or n-butyrate) are investigated using the method of molecular Voronoi-Dirichlet polyhedra. Actinide contraction in the series of U(VI)-Np(VI)-Pu(VI) in compounds I-III is reflected in a decrease in the mean An═O bond lengths and in the volume and sphericity degree of Voronoi-Dirichlet polyhedra of An atoms. PMID:27404584

  2. Repair of x-ray-induced deoxyribonucleic acid single-strand breaks in xth mutants of Escherichia coli.

    Seeberg, E; Steinum, A L

    1980-01-01

    An exonuclease III-deficient strain of Escherichia coli K-12, BW2001 (xthA11), was unable to perform rapid repair of X-ray-induced deoxyribonucleic acid single-strand breaks and appeared to have a defect in the priming of the 3'-termini necessary for initiation of repair synthesis at the breaks. This defect cannot be explained solely by the lack of exonuclease III activity, because other xth mutants tested, including a deletion mutant, repaired radiation-induced strand breaks at close to the ...

  3. X-ray investigation of gene-engineered human insulin crystallized from a solution containing polysialic acid

    Crystals of insulin have been grown from a solution containing insulin and polysialic acid and the three-dimensional structure of insulin in these crystals has been solved at 1.6 Å resolution. Attempts to crystallize the noncovalent complex of recombinant human insulin with polysialic acid were carried out under normal and microgravity conditions. Both crystal types belonged to the same space group, I213, with unit-cell parameters a = b = c = 77.365 Å, α = β = γ = 90.00°. The reported space group and unit-cell parameters are almost identical to those of cubic insulin reported in the PDB. The results of X-ray studies confirmed that the crystals obtained were cubic insulin crystals and that they contained no polysialic acid or its fragments. Electron-density maps were calculated using X-ray diffraction sets from earth-grown and microgravity-grown crystals and the three-dimensional structure of the insulin molecule was determined and refined. The conformation and secondary-structural elements of the insulin molecule in different crystal forms were compared

  4. Dominating IgE-binding epitope of Bet v 1, the major allergen of birch pollen, characterized by X-ray crystallography and site-directed mutagenesis

    Spangfort, Michael D; Mirza, Osman; Ipsen, Henrik;

    2003-01-01

    surface area of Bet v 1 and is clearly conformational. A synthetic peptide representing a sequential motif in the epitope (11 of 16 residues) did not inhibit the binding of mAb BV16 to Bet v 1, illustrating limitations in the use of peptides for B cell epitope characterization. The single amino acid...

  5. Particle-induced x-ray emission: Instrumentation, calibration, and application to contact lens solutions and fulvic acid solutions

    An expression was derived describing the profile of the proton beam at the PIXE target position. The expression was used to predict the profile for several experimental configurations. The profile was experimentally measured. The PIXE system was calibrated using solutions and commercial foils. Experimental data was adjusted for all absorbers and interferences, and a quadratic relationship was determined relating calibration factor and atomic number for each series of X-ray transitions. Calibration factors were determined for all elements above aluminum, for both a pinhole filter and a 14-mil mylar filter. A group of contact lens solutions was analyzed using PIXE, ICP, and ISE. A digestion method was developed for removal. of chloride ion. Cluster analysis was used to classify the data. A commercial humic acid was separated into three fractions. The fulvic acid was characterized, and separations of metal-fulvic acid complexes from metal ions in solution were attempted using ultrafiltration

  6. Particle-induced x-ray emission: Instrumentation, calibration, and application to contact lens solutions and fulvic acid solutions

    Jenson, D.D.

    1989-01-01

    An expression was derived describing the profile of the proton beam at the PIXE target position. The expression was used to predict the profile for several experimental configurations. The profile was experimentally measured. The PIXE system was calibrated using solutions and commercial foils. Experimental data was adjusted for all absorbers and interferences, and a quadratic relationship was determined relating calibration factor and atomic number for each series of X-ray transitions. Calibration factors were determined for all elements above aluminum, for both a pinhole filter and a 14-mil mylar filter. A group of contact lens solutions was analyzed using PIXE, ICP, and ISE. A digestion method was developed for removal. of chloride ion. Cluster analysis was used to classify the data. A commercial humic acid was separated into three fractions. The fulvic acid was characterized, and separations of metal-fulvic acid complexes from metal ions in solution were attempted using ultrafiltration.

  7. Understanding nucleic acid structural changes by comparing wide-angle x-ray scattering (WAXS) experiments to molecular dynamics simulations

    Pabit, Suzette A.; Katz, Andrea M.; Tolokh, Igor S.; Drozdetski, Aleksander; Baker, Nathan; Onufriev, Alexey V.; Pollack, Lois

    2016-05-01

    Wide-angle x-ray scattering (WAXS) is emerging as a powerful tool for increasing the resolution of solution structure measurements of biomolecules. Compared to its better known complement, small angle x-ray scattering (SAXS), WAXS targets higher scattering angles and can enhance structural studies of molecules by accessing finer details of solution structures. Although the extension from SAXS to WAXS is easy to implement experimentally, the computational tools required to fully harness the power of WAXS are still under development. Currently, WAXS is employed to study structural changes and ligand binding in proteins; however, the methods are not as fully developed for nucleic acids. Here, we show how WAXS can qualitatively characterize nucleic acid structures as well as the small but significant structural changes driven by the addition of multivalent ions. We show the potential of WAXS to test all-atom molecular dynamics (MD) simulations and to provide insight into understanding how the trivalent ion cobalt(III) hexammine (CoHex) affects the structure of RNA and DNA helices. We find that MD simulations capture the RNA structural change that occurs due to addition of CoHex.

  8. Insights into regioselective metabolism of mefenamic acid by cytochrome P450 BM3 mutants through crystallography, docking, molecular dynamics, and free energy calculations

    Capoferri, Luigi; Leth, Rasmus; Ter Haar, Ernst; Mohanty, Arun K; Grootenhuis, Peter D J; Vottero, Eduardo; Commandeur, Jan M N; Vermeulen, Nico P E; Jørgensen, Flemming Steen; Olsen, Lars; Geerke, Daan P

    2016-01-01

    active-site mutations such as V87I were reported to invert regioselectivity in NSAID hydroxylation. In this work, we combine crystallography and molecular simulation to study the effect of single mutations on binding and regioselective metabolism of mefenamic acid by M11 mutants. The heme domain of the...... protein mutant M11 was expressed, purified, and crystallized, and its X-ray structure was used as template for modeling. A multistep approach was used that combines molecular docking, molecular dynamics (MD) simulation, and binding free-energy calculations to address protein flexibility. In this way...... mefenamic acid by M11 and its mutants by including protein flexibility and dynamics in free-energy computation. In addition, we could obtain structural insights into the change in regioselectivity of mefenamic acid hydroxylation due to single active-site mutations. Our findings confirm that use of MD and...

  9. Acid-β-glycerophosphatase reaction products in the central nervous system mitochondria following x-ray irradiation

    A survey of the literature to date on the enzyme histochemistry of intracellular organelles has not yielded any reference to the presence of acid phosphatase reaction products in the mammalian mitochondria of the central nervous system. A combination of Gomori's acid phosphatase method, however, with standard electron microscopy has disclosed the presence of enzyme reaction products in the mitochondria of the central nervous system of rats from 2 hr to 22 weeks after x-ray irradiation, as well as in a cerebral biopsy performed on a patient affected by Huntington's chorea. No enzyme reaction products, on the other hand, were observed in serial sections that had been incubated in substrates either containing sodium fluoride or lacking in β-glycerophosphate. The abnormal mitochondrial enzyme reaction (chemical lesion) is considered to be the consequence of the pathologic process affecting the ultrastructural-chemical organization of the organelle

  10. X-ray Photoelectron Spectroscopy of the Passive Surface of Nickel-Carbon Electrocatalysts after Polarisation in Sulfuric Acid

    Thin films of nickel-carbon prepared by d.c. magnetron sputter deposition have previously been shown to exhibit passivity against corrosion as well as electrocatalytic activity towards the hydrogen oxidation reaction of the low-temperature acidic fuel cell. Pure nickel dissolves rapidly under such conditions. X-ray photoelectron spectroscopy (XPS) of Ni-C films containing between 13 and 64 at.% Ni, and polarized at +0.15 V(SHE) in 1.5 M H2SO4 at room temperature demonstrates that this passivity is not due to oxide formation, but rather to the presence of the carbon component. XPS identifies the Ni component as being in the metallic state, both before and after polarization in acid. The carbon component comprises a range of phases, with a graphitic or graphenic component being responsible for passivation

  11. Fast and simple method for determination of fatty acid methyl esters (FAME) in biodiesel blends using X-ray spectrometry.

    Sitko, Rafal; Zawisza, Beata; Kowalewska, Zofia; Kocot, Karina; Polowniak, Marzena

    2011-09-30

    The determination of fatty acid methyl esters (FAME) in diesel fuel blends is an important aspect of production and blending process as well as quality control of distribution operations. In this study, energy-dispersive X-ray fluorescence spectrometer (EDXRF) is used for the first time for determination of FAME in biodiesel blends. The principle of the method is based on intensity difference of X-ray radiation scattered from hydrocarbons and from FAME. The experiment shows that coherent and incoherent radiation, commonly applied for evaluation of the average atomic number of the sample with light matrix, cannot be applied for FAME determination. However, the application of scattered continuous radiation gives excellent correlation between FAME concentration and intensity of scattered radiation. The best results are obtained if continuum is collected in the range of energy between 10.5 and 15.0 keV for rhodium X-ray tube, operated at 35 kV. Linear relationship between the FAME concentration and the inverse of scattered continuous radiation is obtained with the correlation coefficients of 0.999. Standard deviation of measurement is ca. 0.46% (v/v) of FAME and detection limit is 1.2% (v/v) for 600 s counting time and 50% dead-time loss using Si-PIN detector. The investigation shows that crucial issue in determination of FAME in biodiesel blends using EDXRF spectrometer is the precision of measurements resulting from the counting statistics. Therefore, much better results (0.20% (v/v) standard deviation and 0.52% (v/v) detection limit) can be expected if higher intensity of primary radiation is applied and X-ray spectrum is collected by silicon drift detector of high input count rate. For concentration of FAME from 10 to 100% (v/v), the differences between reference method (Fourier transform infrared spectrometry) and the proposed method usually do not exceed 1% (v/v) of FAME. The proposed method is fast, simple and enables FAME determination in wide range of

  12. Speciation of sulfur in humic and fulvic acids using X-ray absorption near-edge structure (XANES) spectroscopy

    Morra, Matthew J.; Fendorf, Scott E.; Brown, Paul D.

    1997-02-01

    Sulfur species in soils and sediments have previously been determined indirectly using destructive techniques. A direct and more accurate method for S speciation would improve our understanding of S biogeochemistry. X-ray absorption near edge structure (XANES) spectroscopy was performed on purified humic and fulvic acids from terrestrial and aquatic environments. This methodology allows direct determination of S species using the relationship that exists with the energy required for core electron transitions and in some cases, correlation with additional spectral features. Soil, peat, and aquatic humic acids were dominated by sulfonates with an oxidation state of +5, but also contained ester-bonded sulfates with an oxidation state of +6. Leonardite humic acid contained ester-bonded sulfate and an unidentified S compound with an oxidation state of +4.0. In contrast, high-valent S in soil, peat, and aquatic fulvic acids was exclusively in the form of sulfonic acids. Reduced S species were also present in both humic and fulvic acids. XANES is a valuable method for the speciation of S in humic materials and of potential use in S speciation of unfractionated soils.

  13. Speciation of sulfur in humic and fulvic acids using X-ray Absorption Near-Edge Structures (XANES) spectroscopy

    Morra, M.J.; Fendorf, S.E.; Brown, P.D. [Univ. of Idaho, Moscow, ID (United States)

    1997-02-01

    Sulfur species in soils and sediments have previously been determined indirectly using destructive techniques. A direct and more accurate method for S speciation would improve our understanding of S biogeochemistry. X-ray absorption near edge structure (XANES) spectroscopy was performed on purified humic and fulvic acids from terrestrial and aquatic environments. This methodology allows direct determination of S species using the relationship that exists with the energy required for core electron transitions and in some cases, correlation with additional spectral features. Soil, peat, and aquatic humic acids were dominated by sulfonates with an oxidation state of +5, but also contained ester-bonded sulfates with an oxidation state of +6. Leonardite humic acid contained ester-bonded sulfate and an unidentified S compound with an oxidation state of +4.0. In contrast, high-valent S in soil, peat, and aquatic fulvic acids was exclusively in the form of sulfonic acids. Reduced S species were also present in both humic and fulvic acids. XANES is a valuable method for the speciation of S in humic materials and of potential use in S speciation of unfractionated soils. 27 refs., 4 figs., 3 tabs.

  14. Rigid body essential X-ray crystallography

    Bjerrum, Esben Jannik; Biggin, Philip C

    2008-01-01

    The ligand-binding domain (LBD) from the ionotropic glutamate receptor subtype 2 (GluR2) has been shown to adopt a range of ligand-dependent conformational states. These states have been described in terms of the rotation required to fit subdomain (lobe) 2 following superposition of subdomain (lo...

  15. X-ray crystallography - principles of safety

    This is a 13 minute videotape which provides an introduction to the principles of safety, with the emphasis throughout on the need for each individual to cultivate safe working habits. The nature of the hazard is explained, and there are sections on: design of equipment; safe working practice; monitoring; warning signs and administrative controls. The use of interlocks is demonstrated, with examples of: mechanical, electrical and combination types, and individual partial and total enclosures are shown. (author)

  16. X-ray diffraction

    We have been interested in structural elucidation by x-ray diffraction of compounds of biological interest. Understanding exactly how atoms are arranged in three-dimensional arrays as molecules can help explain the relationship between structure and functions. The species investigated may vary in size and shape; our recent studies included such diverse substances as antischistosomal drugs, a complex of cadmium with nucleic acid base, nitrate salts of adenine, and proteins

  17. Joint x-ray

    X-ray - joint; Arthrography; Arthrogram ... x-ray technologist will help you position the joint to be x-rayed on the table. Once in place, pictures are taken. The joint may be moved into other positions for more ...

  18. X-Ray Characterisation of Various Aluminium Phases in the Medicinal Herb Bacopa Monnieri Affected by Simulated Acid Rain

    B. Mallick

    2012-07-01

    Full Text Available In the present investigation various aluminium-based new phases formed due to substitution of sulphur via simulated acid rain in Bacopa monnieri have been analyzed using X-ray diffraction (XRD technique. So far there is no report on the effects of acid rain on the B. monnieri herb and its vital properties like memory-boosting mechanism. Therefore, in the present study, an attempt has been made to analyze the various aluminium phase (salt formations due to the substitution of sulphur via simulated acid rain (SiAR in B. Monnieri because of its toxicological importance. The new phases like AlH(SO42 and Al2S3 along with usual Al2O3:H2O, MgO, FeAl2(PO42(OH2:8H2O, (K2Ca(SO42:H2O, have been observed in B. monnieri when treated with sulphuric-simulated acid rain (S-SiAR of two different pH (3.39 and 5.45 for 20 weeks. These Al-based new salts formed in the above medicinal herb due to the induction of S-SiAR may cause Alzheimer’s disease and induce other abnormities.

  19. [Computed X-ray tomography in predicting the efficacy of oral cholelithiasis with bile acids].

    Fu, X B

    1993-02-01

    The efficacy of oral cholelitholytic therapy with chenodeoxycholic acid (CDCA) and ursodeoxycholic acid (UDCA) in 137 patients with gallstones was compared with their CT patterns. The best dissolving results were obtained from patients with the stones in isodense and faint category (OCG). Besides, gallstones, which showed no obvious filling defect on OCG but distinct echo and shadow on B-type ultrasonography, were also insoluble. PMID:8391902

  20. Accurate small and wide angle x-ray scattering profiles from atomic models of proteins and nucleic acids

    Nguyen, Hung T.; Pabit, Suzette A.; Meisburger, Steve P.; Pollack, Lois; Case, David A.

    2014-12-01

    A new method is introduced to compute X-ray solution scattering profiles from atomic models of macromolecules. The three-dimensional version of the Reference Interaction Site Model (RISM) from liquid-state statistical mechanics is employed to compute the solvent distribution around the solute, including both water and ions. X-ray scattering profiles are computed from this distribution together with the solute geometry. We describe an efficient procedure for performing this calculation employing a Lebedev grid for the angular averaging. The intensity profiles (which involve no adjustable parameters) match experiment and molecular dynamics simulations up to wide angle for two proteins (lysozyme and myoglobin) in water, as well as the small-angle profiles for a dozen biomolecules taken from the BioIsis.net database. The RISM model is especially well-suited for studies of nucleic acids in salt solution. Use of fiber-diffraction models for the structure of duplex DNA in solution yields close agreement with the observed scattering profiles in both the small and wide angle scattering (SAXS and WAXS) regimes. In addition, computed profiles of anomalous SAXS signals (for Rb+ and Sr2+) emphasize the ionic contribution to scattering and are in reasonable agreement with experiment. In cases where an absolute calibration of the experimental data at q = 0 is available, one can extract a count of the excess number of waters and ions; computed values depend on the closure that is assumed in the solution of the Ornstein-Zernike equations, with results from the Kovalenko-Hirata closure being closest to experiment for the cases studied here.

  1. Conjugated linoleic acid inhibiting DNA repair damaged by x-ray

    Non-homologous end-joining is the most effective repair of DNA double strand break. Epidermal growth factor receptor activates DSB repairs. Integration of EGFR inhibitors with radiation or chemotherapy were used in lung cancer treatment. Radiosensitivity effect of conjugated linoleic acid on tumor cells and reduced metastasis are reported

  2. Chest x-ray

    Chest radiography; Serial chest x-ray; X-ray - chest ... You stand in front of the x-ray machine. You will be told to hold your breath when the x-ray is taken. Two images are usually taken. You will ...

  3. MALDI-FTMS for the characterization of ultraviolet and X-ray damage to nucleic acid constituents

    Both low energy (far-ultraviolet) and high energy (X-ray) radiation can cause DNA damage by inducing strand breaks, base modifications, and sugar alternations. These changes may lead to mutations and ultimately cell death if they cannot be biologically repaired. It is therefore necessary to characterize both the identities (at the isomeric level) and the abundances of the radiation-induced products to probe the nature of DNA damage in these cases. Matrix-assisted laser desorption/ionization Fourier transform mass spectroscopy (MALDI-FTMS) is well-suited for the direct detection and characterization of radiation-induced damage to nucleic acid constituents, including oligonucleotides. This technique eliminates the need to hydrolyze and derivatize the samples prior to mass analysis, thereby reducing the possibility of modifying the sample after irradiation. The accurate mass measurement and ion trapping capabilities of FTMS permit the detailed examination of the structures of these products. Reverse phase liquid chromatography (HPLC) is used to purify irradiated samples prior to mass analysis to quantitate the dose dependent formation of products after they have been identified by mass spectrometry

  4. Thoracic spine x-ray

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... care provider's office. You will lie on the x-ray table in different positions. If the x-ray ...

  5. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

  6. Chest X-Ray

    Full Text Available ... the most commonly performed x-ray exams and use a very small dose of ionizing radiation to ... to your health. While a chest x-ray use a tiny dose of ionizing radiation, the benefit ...

  7. Dental x-rays

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film ... dentist's office. There are many types of dental x-rays. Some are: Bitewing Periapical Palatal (also called occlusal) ...

  8. X-ray (image)

    X-rays are a form of ionizing radiation that can penetrate the body to form an image on ... will be shades of gray depending on density. X-rays can provide information about obstructions, tumors, and other ...

  9. X-ray apparatus

    A diagnostic x-ray device, readily convertible between conventional radiographic and tomographic operating modes, is described. An improved drive system interconnects and drives the x-ray source and the imaging device through coordinated movements for tomography

  10. Crystallization and preliminary X-ray diffraction analysis of the sialic acid-binding domain (VP8*) of porcine rotavirus strain CRW-8

    Scott, Stacy A. [Institute for Glycomics, Griffith University (Gold Coast Campus) PMB 50, Gold Coast Mail Centre, Queensland 9726 (Australia); Holloway, Gavan; Coulson, Barbara S. [Department of Microbiology and Immunology, The University of Melbourne, Victoria 3010 (Australia); Szyczew, Alex J.; Kiefel, Milton J.; Itzstein, Mark von; Blanchard, Helen, E-mail: h.blanchard@griffith.edu.au [Institute for Glycomics, Griffith University (Gold Coast Campus) PMB 50, Gold Coast Mail Centre, Queensland 9726 (Australia)

    2005-06-01

    The sialic acid-binding domain (VP8*) component of the porcine CRW-8 rotavirus spike protein has been overexpressed in E. coli, purified and co-crystallized with an N-acetylneuraminic acid derivative. X-ray diffraction data have been collected to 2.3 Å, which has enabled determination of the structure by molecular replacement. Rotavirus recognition and attachment to host cells involves interaction with the spike protein VP4 that projects outwards from the surface of the virus particle. An integral component of these spikes is the VP8* domain, which is implicated in the direct recognition and binding of sialic acid-containing cell-surface carbohydrates and facilitates subsequent invasion by the virus. The expression, purification, crystallization and preliminary X-ray diffraction analysis of VP8* from porcine CRW-8 rotavirus is reported. Diffraction data have been collected to 2.3 Å resolution, enabling the determination of the VP8* structure by molecular replacement.

  11. X-Rays

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of your ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat and ...

  12. Chest X-Ray

    Full Text Available ... by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, ... you about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed ...

  13. X-Ray Imaging

    ... Brain Surgery Imaging Clinical Trials Basics Patient Information X-Ray Imaging Print This Page X-ray imaging is perhaps the most familiar type of imaging. Images produced by X-rays are due to the different absorption rates of ...

  14. The role of the arachidonic acid cascade in the species-specific X-ray-induced inflammation of the rabbit eye

    To identify the mediator(s) of the apparently species-specific X-ray-induced inflammation of the rabbit eye, inhibitors of the synthesis and/or release of known or putative mediators of ocular inflammation were administered prior to irradiation. The X-ray-induced ocular inflammation, particularly the rise in intraocular pressure, was found to be inhibited by intravenous pretreatment of rabbits with flurbiprofen, indomethacin, or imidazole (1, 10, and 100 mg/kg i.v., respectively), or by combined intravitreal and topical administration of flurbiprofen. Systemic, intravitreal, and/or topical pretreatment with prednisolone or disodium cromoglycate or the retrobulbar injection of ethyl alcohol or capsaicin failed to block the inflammatory response, whereas vitamin E apparently exerted some protective effect. These findings show that the X-ray-induced inflammation of the rabbit eye is mediated, at least in part, by prostaglandins (PGs) and/or related autacoids. In addition, these results suggest that the unique sensitivity of the rabbit eye to X-ray-induced inflammation is due either to the presence in this species of a unique or uniquely effective triggering mechanism for the release of PG precursors or to the greater sensitivity of this species to the ocular inflammatory effects of PGs. Thus the rabbit eye may provide a unique model for studying some aspects of arachidonic acid release or ocular PG effects, but extreme caution must be exercised in generalizing such findings to other species

  15. The role of the arachidonic acid cascade in the species-specific X-ray-induced inflammation of the rabbit eye

    Bito, L.Z.; Klein, E.M.

    1982-05-01

    To identify the mediator(s) of the apparently species-specific X-ray-induced inflammation of the rabbit eye, inhibitors of the synthesis and/or release of known or putative mediators of ocular inflammation were administered prior to irradiation. The X-ray-induced ocular inflammation, particularly the rise in intraocular pressure, was found to be inhibited by intravenous pretreatment of rabbits with flurbiprofen, indomethacin, or imidazole (1, 10, and 100 mg/kg i.v., respectively), or by combined intravitreal and topical administration of flurbiprofen. Systemic, intravitreal, and/or topical pretreatment with prednisolone or disodium cromoglycate or the retrobulbar injection of ethyl alcohol or capsaicin failed to block the inflammatory response, whereas vitamin E apparently exerted some protective effect. These findings show that the X-ray-induced inflammation of the rabbit eye is mediated, at least in part, by prostaglandins (PGs) and/or related autacoids. In addition, these results suggest that the unique sensitivity of the rabbit eye to X-ray-induced inflammation is due either to the presence in this species of a unique or uniquely effective triggering mechanism for the release of PG precursors or to the greater sensitivity of this species to the ocular inflammatory effects of PGs. Thus the rabbit eye may provide a unique model for studying some aspects of arachidonic acid release or ocular PG effects, but extreme caution must be exercised in generalizing such findings to other species.

  16. Extended X-ray absorption fine structure data analysis of copper (II) hydroxamic acid mixed ligand complexes

    The X-ray absorption spectra of copper mixed ligand complexes, having hydroxamic acid as one of the ligands, have been recorded at the K-edge of copper at BL-8 Dispersive EXAFS beamline at the 2.5 GeV INDUS-2 Synchrotron, RRCAT, Indore, India. For the analysis of EXAFS data, crystallographic data of the complex or of its analog is required, which is not available. Hence, for the analysis of EXAFS data, theoretical EXAFS data of the studied complexes have been generated using the EXAFS equation employing computer software program Mathcad. Firstly, the experimental data has been processed using the computer program Athena to obtain the normalized absorption versus energy data. From the experimental EXAFS data, the phase shift parameter (an energy independent constant 5) has been computed using Lytle, Sayers and Stern's (LSS) method. The backscattering amplitude has been taken from the available theoretical tabulations and other parameters have been taken from crystallographic data of the copper metal. Fourier transforms of both the experimental and theoretical data have been computed, and the two Fourier transforms are found to agree with each other for all the complexes. The position of the first peak in the Fourier transform gives the value of the first shell bond length, which is shorter than the actual bond length as a result of energy dependence of the phase factor (δ(k)) in the sine function of the EXAFS equation. Since, the Fourier transform method and LSS method both are uncorrected for phase and other parameters of the EXAFS equation, the present method gives phase uncorrected bond length of the first coordination shell.

  17. Preconcentration of submicrogram amounts of metals from natural water for X-ray energy spectrometric determination using pyrrolidinecarbodithioic acid

    A method was developed for the routine determination of several trace metals in natural waters by X-ray energy spectrometry following precipitation with pyrrolidinecarbodithioate. Preoxidation with persulfate eliminates interferences by organic matter. By optimizing carrier ion selection and measurement conditions, one may determine dithioate-reactive elements with Z less than or equal to 50 by means of their K X-rays, and some with Z greater than or equal to 80 by means of their L X-rays. Determinations are feasible for several elements at concentrations down to 250 ng L-1, or below. Recoveries are generally greater than 90%, although some exceptions are noted. Reproducibility with real samples averaged about 25% relative standard deviation for five representative elements at concentrations above 250 ng L-1. 24 references, 5 figures, 4 tables

  18. Liquid structure of acetic acid-water and trifluoroacetic acid-water mixtures studied by large-angle X-ray scattering and NMR.

    Takamuku, Toshiyuki; Kyoshoin, Yasuhiro; Noguchi, Hiroshi; Kusano, Shoji; Yamaguchi, Toshio

    2007-08-01

    The structures of acetic acid (AA), trifluoroacetic acid (TFA), and their aqueous mixtures over the entire range of acid mole fraction xA have been investigated by using large-angle X-ray scattering (LAXS) and NMR techniques. The results from the LAXS experiments have shown that acetic acid molecules mainly form a chain structure via hydrogen bonding in the pure liquid. In acetic acid-water mixtures hydrogen bonds of acetic acid-water and water-water gradually increase with decreasing xA, while the chain structure of acetic acid molecules is moderately ruptured. Hydrogen bonds among water molecules are remarkably formed in acetic acid-water mixtures at xATFA molecules form not a chain structure but cyclic dimers through hydrogen bonding in the pure liquid. In TFA-water mixtures O...O hydrogen bonds among water molecules gradually increase when xA decreases, and hydrogen bonds among water molecules are significantly formed in the mixtures at xATFA molecules are considerably dissociated to hydrogen ions and trifluoroacetate in the mixtures. 1H, 13C, and 19F NMR chemical shifts of acetic acid and TFA molecules for acetic acid-water and TFA-water mixtures have indicated strong relationships between a structural change of the mixtures and the acid mole fraction. On the basis of both LAXS and NMR results, the structural changes of acetic acid-water and TFA-water mixtures with decreasing acid mole fraction and the effects of fluorination of the methyl group on the structure are discussed at the molecular level. PMID:17628099

  19. X-Ray Polarimetry

    Kaaret, Philip

    2014-01-01

    We review the basic principles of X-ray polarimetry and current detector technologies based on the photoelectric effect, Bragg reflection, and Compton scattering. Recent technological advances in high-spatial-resolution gas-filled X-ray detectors have enabled efficient polarimeters exploiting the photoelectric effect that hold great scientific promise for X-ray polarimetry in the 2-10 keV band. Advances in the fabrication of multilayer optics have made feasible the construction of broad-band ...

  20. Femtosecond X-ray protein nanocrystallography

    Chapman, Henry N. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Univ. of Hamburg (Germany); Barty, Anton [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; White, Thomas A. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Aquila, Andrew [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Schulz, Joachim [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; DePonte, Daniel P. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Martin, Andrew V. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Coppola, Nicola [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Liang, Mengning [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Caleman, Carl [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Gumprecht, Lars [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Stern, Stephan [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Nass, Karol [Univ. of Hamburg (Germany); Fromme, Petra [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Hunter, Mark S. [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Grotjohann, Ingo [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Fromme, Raimund [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Kirian, Richard A. [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Weierstall, Uwe [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Doak, R. Bruce [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Schmidt, Kevin E. [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Wang, Xiaoyu [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Spence, John C. H. [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Schlichting, Ilme [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Epp, Sascha W. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Rolles, Daniel [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Rudenko, Artem [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Foucar, Lutz [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Rudek, Benedikt [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Erk, Benjamin [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Schmidt, Carlo [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Hömke, André [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Strüder, Lothar [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Society Semiconductor Lab., Munich (Germany); Ullrich, Joachim [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Krasniqi, Faton [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Lomb, Lukas [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Shoeman, Robert L. [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Bott, Mario [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Barends, Thomas R. M. [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Kuhnel, Kai-Uwe [Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Schroter, Claus-Dieter [Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Hartmann, Robert [PNSensor GmbH, Munich (Germany); Holl, Peter [PNSensor GmbH, Munich (Germany); Reich, Christian [PNSensor GmbH, Munich (Germany); Soltau, Heike [PNSensor GmbH, Munich (Germany); Kimmel, Nils [Max Planck Society Semiconductor Lab., Munich (Germany); Weidenspointner, Georg [Max Planck Society Semiconductor Lab., Munich (Germany); Max Planck Inst. fur Extraterrestrische Physik, Garching (Germany); Pietschner, Daniel [Max Planck Society Semiconductor Lab., Munich (Germany); Hauser, Günter [Max Planck Society Semiconductor Lab., Munich (Germany); Herrmann, Sven [Max Planck Society Semiconductor Lab., Munich (Germany); Schaller, Gerhard [Max Planck Society Semiconductor Lab., Munich (Germany); Schopper, Florian [Max Planck Society Semiconductor Lab., Munich (Germany); Andritschke, Robert [Max Planck Society Semiconductor Lab., Munich (Germany); Boutet, Sébastien [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Krzywinski, Jacek [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Bostedt, Christoph [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Messerschmidt, Marc [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Bozek, John D. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Williams, Garth J. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Bogan, Michael J. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Hampton, Christina Y. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Sierra, Raymond G. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Starodub, Dmitri [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Gorke, Hubert [Forschungszentrum Julich (Germany); Hau-Riege, Stefan P. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Frank, Matthias [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Maia, Filipe R. N. C. [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Hajdu, Janos [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Timneanu, Nicusor [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Seibert, M. Marvin [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Andreasson, Jakob [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Rocker, Andrea [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Jönsson, Olof [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Svenda, Martin [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Holton, James M. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Marchesini, Stefano [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Neutze, Richard [Univ. of Gothenburg (Sweden). Dept. of Chemistry, Biochemistry and Biophysics; Schorb, Sebastian [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Rupp, Daniela [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Adolph, Marcus [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Gorkhover, Tais [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Andersson, Inger [Swedish Univ. of Agricultural Sciences, Uppsala Biomedical Centre, Uppsala, (Sweden). Dept. of Molecular Biology; Barthelmess, Miriam [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Bajt, Saša [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Hirsemann, Helmut [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Potdevin, Guillaume [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Graafsma, Heinz [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Nilsson, Björn [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science

    2011-02-03

    X-ray crystallography provides the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. In conventional measurements, the necessary increase in X-ray dose to record data from crystals that are too small leads to extensive damage before a diffraction signal can be recorded. It is particularly challenging to obtain large, well-diffracting crystals of membrane proteins, for which fewer than 300 unique structures have been determined despite their importance in all living cells. Here we present a method for structure determination where single-crystal X-ray diffraction ‘snapshots’ are collected from a fully hydrated stream of nanocrystals using femtosecond pulses from a hard-X-ray free-electron laser, the Linac Coherent Light Source. We prove this concept with nanocrystals of photosystem I, one of the largest membrane protein complexes. More than 3,000,000 diffraction patterns were collected in this study, and a three-dimensional data set was assembled from individual photosystem I nanocrystals (~200 nm to 2 μm in size). We mitigate the problem of radiation damage in crystallography by using pulses briefer than the timescale of most damage processes. This offers a new approach to structure determination of macromolecules that do not yield crystals of sufficient size for studies using conventional radiation sources or are particularly sensitive to radiation damage.

  1. X-ray interferometers

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  2. X-ray - skeleton

    A skeletal x-ray is an imaging test used to look at the bones. It is used to detect fractures , tumors, or ... in the health care provider's office by an x-ray technologist. You will lie on a table or ...

  3. Extremity x-ray

    An extremity x-ray is an image of the hands, wrist, feet, ankle, leg, thigh, forearm humerus or upper arm, hip, shoulder ... term "extremity" often refers to a human limb. X-rays are a form of radiation that passes through ...

  4. Dental x-rays

    ... addition, many dentists are taking x-rays using digital technology. The image runs through a computer. The amount of radiation given off during the procedure is less than traditional methods. Other types of dental x-rays can create a 3-D picture ...

  5. X-ray diffraction study of Penicillium Vitale catalase in the complex with aminotriazole

    The three-dimensional structure of the enzyme catalase from Penicillium vitale in a complex with the inhibitor aminotriazole was solved and refined by protein X-ray crystallography methods. An analysis of the three-dimensional structure of the complex showed that the inhibition of the enzyme occurs as a result of the covalent binding of aminotriazole to the amino-acid residue His64 in the active site of the enzyme. An investigation of the three-dimensional structure of the complex resulted in the amino-acid residues being more precisely identified. The binding sites of saccharide residues and calcium ions in the protein molecule were found.

  6. X-ray structure of 1D-coordination polymer of copperII bearing 1,4-pyrazine-2,3-dicarboxylic acid and 2-aminopyrimidine

    Mirzaei Masoud; Eshtiagh-Hosseini Hossein; Hassanpoor Azam; Barba Victor

    2012-01-01

    The new 1D-coordination polymer of CuII ion, {(2- apymH)2[Cu(pyzdc)2] .6H2O}n, (2-apym = 2-aminopyrimidine, pyzdcH2 = 1,4- pyrazine-2,3-dicarboxylic acid), was synthesized based on proton transfer mechanism and characterized by elemental analysis, infrared spectroscopy, and single crystal X-ray diffraction. The coordination polymer consists of infinite anionic chains of [Cu(pyzdc)2]2- anion bridged crossing double chain running along a-axis and discrete (2-apymH)+ fragment. The CuII ion...

  7. Bone X-Ray (Radiography)

    Full Text Available ... Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive medical ...

  8. Bone X-Ray (Radiography)

    Full Text Available ... Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose ... limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is ...

  9. Bone X-Ray (Radiography)

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  10. Lumbosacral spine x-ray

    X-ray - lumbosacral spine; X-ray - lower spine ... The test is done in a hospital x-ray department or your health care provider's office by an x-ray technician. You will be asked to lie on the x-ray table ...

  11. Bone X-Ray (Radiography)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  12. Abdomen X-Ray (Radiography)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a very ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  13. Crystallization and preliminary X-ray diffraction analysis of a Lys49-phospholipase A2 complexed with caffeic acid, a molecule with inhibitory properties against snake venoms

    Piratoxin I, a noncatalytic and myotoxic Lys49-phospholipase A2 from B. pirajai venom, was cocrystallized with the inhibitor caffeic acid and a data set was collected to a resolution of 1.65 Å. The electron-density map unambiguously indicated that three inhibitor molecules interact with the C-terminus of the protein. Phospholipases A2 (PLA2s) are one of the main components of bothropic venoms; in addition to their phospholipid hydrolysis action, they are involved in a wide spectrum of pharmacological activities, including neurotoxicity, myotoxicity and cardiotoxicity. Caffeic acid is an inhibitor that is present in several plants and is employed for the treatment of ophidian envenomations in the folk medicine of many developing countries; as bothropic snake bites are not efficiently neutralized by conventional serum therapy, it may be useful as an antivenom. In this work, the cocrystallization and preliminary X-ray diffraction analysis of the Lys49-PLA2 piratoxin I from Bothrops pirajai venom in the presence of the inhibitor caffeic acid (CA) are reported. The crystals diffracted X-rays to 1.65 Å resolution and the structure was solved by molecular-replacement techniques. The electron-density map unambiguously indicated the presence of three CA molecules that interact with the C-terminus of the protein. This is the first time a ligand has been observed bound to this region and is in agreement with various experiments previously reported in the literature

  14. Crystallization and preliminary X-ray crystallographic analysis of UDP-glucuronic acid:flavonol-3-O-glucuronosyltransferase (VvGT5) from the grapevine Vitis vinifera

    The UDP-glucuronic acid:flavonol-3-O-glucuronosyltransferase (VvGT5) from the grapevine V. vinifera was purified and crystallized. The best crystal diffracted X-rays to 2.2 Å resolution and belonged to space group P6122. Grapevine (Vitis vinifera) glycosyltransferase 5 (VvGT5) is a UDP-glucuronic acid:flavonol-3-O-glucuronosyltransferase that catalyses the 3-O-specific glucuronosylation of flavonols using UDP-glucuronic acid as a sugar donor to produce flavonol 3-O-glucosides, which are important bioactive phytochemicals. Recombinant VvGT5 expressed in Escherichia coli cells was purified and crystallized by the sitting-drop vapour-diffusion method. A full set of X-ray diffraction data was collected to 2.2 Å Bragg spacing from a single crystal using a synchrotron-radiation source. The crystal was hexagonal, belonging to space group P6122, with unit-cell parameters a = b = 102.70, c = 535.92 Å. The initial phases were determined by the molecular-replacement method

  15. Small-angle X-ray-scattering investigation and structural-model study of the fatty-acid synthetase from pig liver

    The structure of the fatty acid synthetase from pig liver was studied on models based upon structural and functional properties selected from pertinent results available from numerous investigations carried out with fatty acid synthetase from this and other sources. When comparing small-angle X-ray-scattering curves calculated with these models and curves obtained from small-angle X-ray-scattering experiments carried out with the pig-liver enzyme, we tried to select a model which would lead to an acceptable correlation between the calculated and the experimental curves and at the same time fulfil the known structural and the functional requirements. The comparison of the curves was started with a model of low complexity. The observed discrepancy, together with arguments from the structural and the functional properties, helped decide which is the next most reasonable model to be considered. This procedure was repeated for five models of increasing complexity. In the model which led to the best fit the multienzyme complex is composed of two halves in an asymmetric conformation including hollow spaces. This highly anisotropic model would imply that the two halves change their conformation each time a synthetic cycle is completed and that the growing fatty acid is handed over from one half to the other. (orig.)

  16. X-ray apparatus

    A patient support system for X-ray equipment in arteriographic studies of the heart is described in detail. The support system has been designed to overcome many of the practical problems encountered in using previous types of arteriographic X-ray equipment. The support system is capable of horizontal movement and, by a series of shafts attached to the main support system, the X-ray source and image intensifier or detector may be rotated through the same angle. The system is highly flexible and details are given of several possible operational modes. (U.K.)

  17. X-ray lasers

    Elton, Raymond C

    2012-01-01

    The first in its field, this book is both an introduction to x-ray lasers and a how-to guide for specialists. It provides new entrants and others interested in the field with a comprehensive overview and describes useful examples of analysis and experiments as background and guidance for researchers undertaking new laser designs. In one succinct volume, X-Ray Lasers collects the knowledge and experience gained in two decades of x-ray laser development and conveys the exciting challenges and possibilities still to come._Add on for longer version of blurb_M>The reader is first introduced

  18. X-Ray Diffraction.

    Smith, D. K.; Smith, K. L.

    1980-01-01

    Reviews applications in research and analytical characterization of compounds and materials in the field of X-ray diffraction, emphasizing new developments in applications and instrumentation in both single crystal and powder diffraction. Cites 414 references. (CS)

  19. Medical X-Rays

    ... The Conference of Radiation Control Program Directors (CRCPD) publishes Suggested State Regulations for the Control of Radiation , ... eSubmitter Guidance for Industry and Food and Drug Administration Staff - Assembler's Guide to Diagnostic X-Ray Equipment ...

  20. Chest X-Ray

    Full Text Available ... also be useful to help diagnose and monitor treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  1. Chest X-Ray

    Full Text Available ... However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs any risk. ...

  2. Chest X-Ray

    Full Text Available ... chest x-ray is used to evaluate the lungs, heart and chest wall and may be used ... diagnose and monitor treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A ...

  3. Chest X-Ray

    Full Text Available ... Angioplasty & vascular stenting Video: Arthrography Video: Contrast Material Radiology and You Take our survey About this Site ... radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey ...

  4. Chest X-Ray

    Full Text Available ... of ionizing radiation, the benefit of an accurate diagnosis far outweighs any risk. For more information about chest x-rays, visit Radiology Info dot org. Thank you for your time! ...

  5. Chest X-Ray

    Full Text Available ... Site Index A-Z Spotlight June is Men's Health Month Recently posted: Focused Ultrasound for Uterine Fibroids ... to consider the likelihood of benefit to your health. While a chest x-ray use a tiny ...

  6. X-ray tubes

    An improved form of x-ray tube is described which consists of a rotatable anode disc and an electron beam source enclosed in an envelope. The beam of electrons strikes the edge of the anode disc at an acute angle, producing x-rays which are transmitted through a window in the envelope. To improve performance and life of the anode disc it is additionally reciprocated back and forth along its axis of rotation. Dimensions are specified. (U.K.)

  7. Bone X-Ray (Radiography)

    Full Text Available ... around or in bones. top of page How should I prepare? Most bone x-rays require no ... might interfere with the x-ray images. Women should always inform their physician and x-ray technologist ...

  8. Bone X-Ray (Radiography)

    Full Text Available ... drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  9. Bone X-Ray (Radiography)

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ...

  10. Surface Structure and Chemical Switching of Thioctic Acid Adsorbed on Au(111) as Observed Using Near-Edge X-ray Absorption Fine Structure

    Meulenberg, R W; van Buuren, T; Vance, A L; Terminello, L J; Willey, T M; Bostedt, C; Fadley, C S

    2004-01-06

    Thioctic acid (alpha-lipoic acid) is a molecule with a large disulfide-containing base, a short alkyl-chain with four CH{sub 2} units, and a carboxyl termination. Self-assembled monolayer (SAM) films of thioctic acid adsorbed on Au(111) have been investigated with near-edge x-ray absorption fine structure (NEXAFS) spectroscopy and x-ray photoelectron spectroscopy (XPS) to determine film quality, bonding and morphology. Using standard preparation protocols for SAMs, that is, dissolving thioctic acid in ethanol and exposing gold to the solution, results in poor films. These films are highly disordered, contain a mixture of carboxyl and carboxylate terminations, have more than monolayer coverage, and exhibit unbound disulfide. Conversely, forming films by dissolving 1 mmol thioctic acid into 5% acetic acid in ethanol (as previously reported with carboxyl-terminated alkyl-thiols) forms ordered monolayers with small amounts of unbound sulfur. NEXAFS indicates tilted over endgroups with the carboxyl group normal on average 38{sup o} from the surface normal. Slight dichroism in other features indicates alkyl chains statistically more upright than prostrate on the surface. Reflection-absorption Fourier transform infrared (RA-FTIR) spectra indicate hydrogen bonding between neighboring molecules. In such well-formed monolayers, a stark reorientation occurs upon deprotonation of the endgroup by rinsing in a KOH solution. The carboxylate plane normal is now about 66{sup o} from sample normal, a much more upright orientation. Data indicate this reorientation may also cause a more upright orientation to the alkyl portion of the molecules.

  11. X-ray laser

    X-ray is among the most important research tools today, and has given priceless contributions to all disciplines within the natural sciences. State of the art in this field is called XFEL, X-ray Free Electron Laser, which may be 10 thousand million times stronger than the x-rays at the European Synchrotron Radiation Facility in Grenoble. In addition XFEL has properties that allow the study of processes which previously would have been impossible. Of special interest are depictions on atomic- and molecular level by the use of x-ray holographic methods, and being able to study chemical reactions in nature's own timescale, the femtosecond. Conclusion: The construction of x-ray lasers is a natural development in a scientific field which has an enormous influence on the surrounding society. While the discovery of x-ray was an important breakthrough in itself, new applications appear one after the other: Medical depiction, dissemination, diffraction, DNA and protein structures, synchrotron radiation and tomography. There is reason to believe that XFEL implies a technological leap as big as the synchrotrons some decades ago. As we are now talking about studies of femtosecond and direct depiction of chemical reactions, it is obvious that we are dealing with a revolution to come, with extensive consequences, both scientifically and culturally. (EW)

  12. Crystallization and preliminary X-ray crystallographic studies of a Lys49-phospholipase A2 homologue from Bothrops pirajai venom complexed with rosmarinic acid

    PrTX-I, a noncatalytic and myotoxic Lys49-phospholipase A2 from B. pirajai venom, was cocrystallized with the inhibitor rosmarinic acid from C. verbenacea. The crystals diffracted X-rays to 1.8 Å resolution and the structure was solved, indicating a remarkable electronic density for the ligand at the entrance to the hydrophobic channel. PrTX-I, a noncatalytic and myotoxic Lys49-phospholipase A2 from Bothrops pirajai venom, was crystallized in the presence of the inhibitor rosmarinic acid (RA). This is the active compound in the methanolic extract of Cordia verbenacea, a plant that is largely used in Brazilian folk medicine. The crystals diffracted X-rays to 1.8 Å resolution and the structure was solved by molecular-replacement techniques, showing electron density that corresponds to RA molecules at the entrance to the hydrophobic channel. The crystals belong to space group P212121, indicating conformational changes in the structure after ligand binding: the crystals of all apo Lys49-phospholipase A2 structures belong to space group P3121, while the crystals of complexed structures belong to space groups P21 or P212121

  13. Advances and problems in protein crystallography

    Řezáčová, Pavlína

    2009-01-01

    Roč. 16, 2a (2009), k7-k8. ISSN 1211-5894. [Struktura - Colloquium of Czech and Slovak Crystallographic Association. 22.06.2009-25.06.2009, Hluboká nad Vltavou] Institutional research plan: CEZ:AV0Z40550506 Keywords : protein crystallography * X-ray crystallography * structural biology Subject RIV: CC - Organic Chemistry

  14. Single molecule imaging with longer x-ray laser pulses

    Martin, Andrew V.; Corso, Justine K.; Caleman, Carl; Timneanu, Nicusor; Quiney, Harry M.

    2015-01-01

    During the last five years, serial femtosecond crystallography using x-ray laser pulses has developed into a powerful technique for determining the atomic structures of protein molecules from micrometer and sub-micrometer sized crystals. One of the key reasons for this success is the "self-gating" pulse effect, whereby the x-ray laser pulses do not need to outrun all radiation damage processes. Instead, x-ray induced damage terminates the Bragg diffraction prior to the pulse completing its pa...

  15. Incoherent x-ray scattering in single molecule imaging

    Slowik, Jan Malte; Dixit, Gopal; Jurek, Zoltan; Santra, Robin

    2014-01-01

    Imaging of the structure of single proteins or other biomolecules with atomic resolution would be enormously beneficial to structural biology. X-ray free-electron lasers generate highly intense and ultrashort x-ray pulses, providing a route towards imaging of single molecules with atomic resolution. The information on molecular structure is encoded in the coherent x-ray scattering signal. In contrast to crystallography there are no Bragg reflections in single molecule imaging, which means the coherent scattering is not enhanced. Consequently, a background signal from incoherent scattering deteriorates the quality of the coherent scattering signal. This background signal cannot be easily eliminated because the spectrum of incoherently scattered photons cannot be resolved by usual scattering detectors. We present an ab initio study of incoherent x-ray scattering from individual carbon atoms, including the electronic radiation damage caused by a highly intense x-ray pulse. We find that the coherent scattering pa...

  16. X-ray structure of 1D-coordination polymer of copperII bearing 1,4-pyrazine-2,3-dicarboxylic acid and 2-aminopyrimidine

    Mirzaei Masoud

    2012-01-01

    Full Text Available The new 1D-coordination polymer of CuII ion, {(2- apymH2[Cu(pyzdc2] .6H2O}n, (2-apym = 2-aminopyrimidine, pyzdcH2 = 1,4- pyrazine-2,3-dicarboxylic acid, was synthesized based on proton transfer mechanism and characterized by elemental analysis, infrared spectroscopy, and single crystal X-ray diffraction. The coordination polymer consists of infinite anionic chains of [Cu(pyzdc2]2- anion bridged crossing double chain running along a-axis and discrete (2-apymH+ fragment. The CuII ion is located on inversion centre in the basal plane of an elongated octahedron and two oxygen atoms from adjacent (pyzdc2-ligands occupy axial position. The interaction between oxygen atoms of water molecules along with the dicarboxylic acid play an important role in the overall supramolecular assembly.

  17. X-ray nanotomography

    Sasov, Alexander

    2004-10-01

    A compact laboratory x-ray "nano-CT" scanner has been created for 3D non-invasive imaging with 150-200 nanometers 3D spatial resolution, using advanced x-ray technologies and specific physical phenomena for signal detection. This spatial resolution in volume terms is 3 orders better than can be achieved in synchrotron tomography, 5 orders better then in existing laboratory micro-CT instruments and 10-12 orders better in comparison to clinical CT. The instrument employs an x-ray source with a 300-400nm x-ray spot size and uses small-angle scattering to attain a detail detectability of 150-200nm. An object manipulator allows positioning and rotation with an accuracy of 150nm. The x-ray detector is based on an intensified CCD with single-photon sensitivity. A typical acquisition cycle for 3D reconstruction of the full object volume takes from 10 to 60 minutes, with the collection of several hundred angular views. Subsequent volumetric reconstruction produces results as a set of cross sections with isotropic voxel size down to 140 x 140 x 140nm, or as a 3D-model, which can be virtually manipulated and measured. This unique spatial resolution in non-invasive investigations gives previously unattainable 3D images in several application areas, such as composite materials, paper and wood microstructure, biomedical applications and others.

  18. X-ray Pulsars

    Walter, Roland

    2016-01-01

    X-ray pulsars shine thanks to the conversion of the gravitational energy of accreted material to X-ray radiation. The accretion rate is modulated by geometrical and hydrodynamical effects in the stellar wind of the pulsar companions and/or by instabilities in accretion discs. Wind driven flows are highly unstable close to neutron stars and responsible for X-ray variability by factors $10^3$ on time scale of hours. Disk driven flows feature slower state transitions and quasi periodic oscillations related to orbital motion and precession or resonance. On shorter time scales, and closer to the surface of the neutron star, X-ray variability is dominated by the interactions of the accreting flow with the spinning magnetosphere. When the pulsar magnetic field is large, the flow is confined in a relatively narrow accretion column, whose geometrical properties drive the observed X-ray emission. In low magnetized systems, an increasing accretion rate allows the ignition of powerful explosive thermonuclear burning at t...

  19. X-ray astronomy

    This book contains the lectures, and the most important seminars held at the NATO meeting on X-Ray astronomy in Erice, July 1979. The meeting was an opportune forum to discuss the results of the first 8-months of operation of the X-ray satellite, HEAO-2 (Einstein Observatory) which was launched at the end of 1978. Besides surveying these results, the meeting covered extragalactic astronomy, including the relevant observations obtained in other portions of the electromagnetic spectrum (ultra-violet, optical, infrared and radio). The discussion on galactic X-ray sources essentially covered classical binaries, globular clusters and bursters and its significance to extragalactic sources and to high energy astrophysics was borne in mind. (orig.)

  20. Survey analysis and chemical characterization of solid inhomogeneous samples using a general homogenization procedure including acid digestion, drying, grinding and briquetting together with X-ray fluorescence.

    Sahlin, Eskil; Magnusson, Bertil

    2012-08-15

    A survey analysis and chemical characterization methodology for inhomogeneous solid waste samples of relatively large samples (typically up to 100g) using X-ray fluorescence following a general homogenization procedure is presented. By using a combination of acid digestion and grinding various materials can be homogenized e.g. pure metals, alloys, salts, ores, plastics, organics. In the homogenization step, solid material is fully or partly digested in a mixture of nitric acid and hydrochloric acid in an open vessel. The resulting mixture is then dried, grinded, and finally pressed to a wax briquette. The briquette is analyzed using wave-length dispersive X-ray fluorescence with fundamental parameters evaluation. The recovery of 55 elements were tested by preparing samples with known compositions using different alloys, pure metals or elements, oxides, salts and solutions of dissolved compounds. It was found that the methodology was applicable to 49 elements including Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Te, Cs, Ba, La, Ce, Ta, W, Re, Ir, Pt, Au, Tl, Pb, Bi, and Th, that all had recoveries >0.8. 6 elements were lost by volatilization, including Br, I, Os, and Hg that were completely lost, and S and Ge that were partly lost. Since all lanthanides are chemically similar to La and Ce, all actinides are chemically similar to Th, and Hf is chemically similar to Zr, it is likely that the method is applicable to 77 elements. By using an internal standard such as strontium, added as strontium nitrate, samples containing relatively high concentrations of elements not measured by XRF (hydrogen to fluorine), e.g. samples containing plastics, can be analyzed. PMID:22841048

  1. Powder X-ray diffraction study af alkali alanates

    Cao, Thao; Mosegaard Arnbjerg, Lene; Jensen, Torben René

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...

  2. CRL X-RAY TUBE

    Kolchevsky, N. N.; Petrov, P. V.

    2015-01-01

    A novel types of X-ray tubes with refractive lenses are proposed. CRL-R X-ray tube consists of Compound Refractive Lens- CRL and Reflection X-ray tube. CRL acts as X-ray window. CRL-T X-ray consists of CRL and Transmission X-ray tube. CRL acts as target for electron beam. CRL refractive lens acts as filter, collimator, waveguide and focusing lens. Properties and construction of the CRL X-ray tube are discussed.

  3. X-ray astronomical spectroscopy

    Holt, Stephen S.

    1987-01-01

    The contributions of the Goddard group to the history of X-ray astronomy are numerous and varied. One role that the group has continued to play involves the pursuit of techniques for the measurement and interpretation of the X-ray spectra of cosmic sources. The latest development is the selection of the X-ray microcalorimeter for the Advanced X-ray Astrophysics Facility (AXAF) study payload. This technology is likely to revolutionize the study of cosmic X-ray spectra.

  4. The structure investigations of dehydroacetic acid and 1,8-diaminonaphthalene condensation product by NMR, MS, and X-ray measurements

    Kołodziej, B.; Morawiak, M.; Kamieński, B.; Schilf, W.

    2016-05-01

    A new unexpected product of condensation reaction of 1,8-diaminonaphthalene (DAN) and carbonyl compound (here: dehydroacetic acid (dha)) was synthesized. Discussion about the molecular structure of possible products of this reaction was done on the base of NMR studies. The structure of the titled product in both DMSO solution and in the solid state was resolved by analysis of its spectral data (X-ray structure analysis, multinuclear NMR in solution and solid state spectra) and MS measurements. The presented studies provided clear evidence that the titled product exists in diluted DMSO solution as the mixture of two kinetic free ionic species whereas in concentrated DMSO solution as well as in the solid state this system forms associated ionic pairs bonded together by hydrogen bonds.

  5. Leaf-cutting ants toxicity of limonexic acid and degraded limonoids from Raulinoa echinata: X-ray structure of epoxy-fraxinellone

    Phytochemical survey of roots extracts of the South Brazilian endemic plant Raulinoa echinata Cowan, Rutaceae led to the isolation of known degraded limonoids: fraxinellone, fraxinellonone and epoxy-fraxinellone. The latter was previously isolated also from the stems, but the relative configuration could not be solved by NMR experiments. This paper deals with the X-ray diffraction analysis of epoxy-fraxinellone and its toxicity to leaf-cutting ants, describes the isolation of fraxinellonone and fraxinellone for the first time in Raulinoa. Epoxy-fraxinellone showed no toxicity to the leaf-cutting ants (Atta sexdens rubropilosa). The limonoid limonexic acid, isolated from stems, presented high toxicity to the leaf-cutting ants, diminishing considerably their longevity. (author)

  6. Expression, purification, crystallization and preliminary X-ray diffraction analysis of the VP8* sialic acid-binding domain of porcine rotavirus strain OSU

    Porcine rotavirus strain OSU VP8* domain has been expressed, purified and crystallized. X-ray diffraction data from different crystal forms of the VP8* domain have been collected to 2.65 and 2.2 Å resolution, respectively. The rotavirus outer capsid spike protein VP4 is utilized in the process of rotavirus attachment to and membrane penetration of host cells. VP4 is cleaved by trypsin into two domains: VP8* and VP5*. The VP8* domain is implicated in initial interaction with sialic acid-containing cell-surface carbohydrates and triggers subsequent virus invasion. The VP8* domain from porcine OSU rotavirus was cloned and expressed in Escherichia coli. Different crystal forms (orthorhombic P212121 and tetragonal P41212) were harvested from two distinct crystallization conditions. Diffraction data have been collected to 2.65 and 2.2 Å resolution and the VP8*65–224 structure was determined by molecular replacement

  7. Leaf-cutting ants toxicity of limonexic acid and degraded limonoids from Raulinoa echinata: X-ray structure of epoxy-fraxinellone

    Biavatti, Maique W.; Westerlon, Rosangela [Universidade do Vale do Itajai, SC (Brazil). Programa de Pos-Graduacao em Ciencias Farmaceuticas]. E-mail: maique@univali.br; Vieira, Paulo C.; Silva, M. Fatima G.F. da; Fernandes, Joao B. [Sao Carlos Univ., SP (Brazil). Dept. de Quimica; Penaflor, M. Fernanda G.V.; Bueno, Odair C. [UNESP, Rio Claro, SP (Brazil). Centro de Estudos de Insetos Sociais; Ellena, Javier [Sao Paulo Univ., Sao Carlos, SP (Brazil). Inst. de Fisica

    2005-11-15

    Phytochemical survey of roots extracts of the South Brazilian endemic plant Raulinoa echinata Cowan, Rutaceae led to the isolation of known degraded limonoids: fraxinellone, fraxinellonone and epoxy-fraxinellone. The latter was previously isolated also from the stems, but the relative configuration could not be solved by NMR experiments. This paper deals with the X-ray diffraction analysis of epoxy-fraxinellone and its toxicity to leaf-cutting ants, describes the isolation of fraxinellonone and fraxinellone for the first time in Raulinoa. Epoxy-fraxinellone showed no toxicity to the leaf-cutting ants (Atta sexdens rubropilosa). The limonoid limonexic acid, isolated from stems, presented high toxicity to the leaf-cutting ants, diminishing considerably their longevity. (author)

  8. Phosphole complexes of Gold(I) halides: Comparison of solution and solid-state structures by a combination of solution and CP/MAS 31P NMR spectroscopy and x-ray crystallography

    A series of complexes of 1-phenyldibenzophosphole (DBP), 1-phenyl-3,4,-dimethylphosphole (DMPP), and triphenylphosphine of the type LnAuX (n = 1, L = DBP, DMPP, Ph3P, X = Cl, Br, I; n = 3, L = DBP, X = Cl, Br, I; n = 3, L = Ph3P, X = Cl; n = 4, L = DBP, DMPP, X = PF6) have been prepared and characterized. The structures of (DBP)AuCl (1), (DBP)3AuCl (2), and (DMPP)AuCl (3) have been determined from three-dimensional x-ray data collected by counter methods. Crystal structure of the complexes is reported. The CP/MAS 31P(1H) NMR spectrum of complex 1 shows two resonances in a 1:1 intensity ratio, and the CP/MAS 31P(1H) NMR spectrum of complex 3 shows three resonances in a 1:1:1 intensity ratio for reasons that are not yet understood. Though the three phospholes are crystallographically inequivalent (d(AuP) = 2.359 (1), 2.382 (1), and 2.374 (2) angstrom) the molecule has effective Cs symmetry as evidenced by the observation of two 31P resonances in a 2:1 intensity ratio in its CP/MAS 31P(1H) NMR spectrum. Variable-temperature 31P(1H) NMR spectra obtained on solutions of LAuCl + L in various ratios were analyzed to determine the nature of the species present in solution and to gain information regarding their relative stabilities as a function of the nature of the phosphine. 79 refs., 8 figs., 9 tabs

  9. X-ray apparatus

    The invention discloses an X-ray apparatus that can be used for tomography with the aid of a computer. With this apparatus plus computer, it is possible to quickly achieve the required edge values whereby the influence of the movement is diminished

  10. Chest X-Ray

    Full Text Available ... Pediatric Ultrasound Video: Angioplasty & vascular stenting Video: Arthrography Radiology and You About this Site RadiologyInfo.org is ... radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey ...

  11. Medical x-ray

    This book describes the fundamental subject about medical radiography. It is a multidisciplinary field that requires cross professional input from scientists, engineers and medical doctors. However, it is presented in simple language to suit different levels of readers from x-ray operators and radiographers to physists, general practitioners and radiology specialists.The book is written in accordance to the requirements of the standard syllabus approved by the Ministry of Health Malaysia for the training of medical x-ray operator and general practitioners. In general, the content is not only designed to provide relevant and essential subject for related professionals in medical radiological services such as x-ray operator, radiographer and radiologists, but also to address those in associated radiological services including nurses, medical technologists and physicists.The book is organized and arranged sequentially into 3 parts for easy reference: Radiation safety; X-ray equipment and associated facilities; Radiography practices. With proper grasping of all these parts, the radiological services could be provided with confident and the highest professional standard. Thus, medical imaging with highest quality that can provide useful diagnostic information at minimum doses and at cost effective could be assured

  12. Chest X-Ray

    Full Text Available ... this Site RadiologyInfo.org is produced by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript ... Recently posted: Focused Ultrasound for Uterine Fibroids Dementia Video: General Ultrasound Video: Pediatric Nuclear Medicine Radiology and ...

  13. Chest X-Ray

    Full Text Available ... this Site RadiologyInfo.org is produced by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript ... time! Spotlight Recently posted: Pediatric MRI Intravascular Ultrasound Video: Chest CT Video:Thyroid Ultrasound Video: Head CT ...

  14. Quantitative Imaging of Single, Unstained Viruses with Coherent X-rays

    Song, Changyong; Mancuso, Adrian; Amirbekian, Bagrat; Peng, Li; Sun, Ren; Shah, Sanket S; Zhou, Z Hong; Ishikawa, Tetsuya; Miao, Jianwei

    2008-01-01

    Since Perutz, Kendrew and colleagues unveiled the structure of hemoglobin and myoglobin based on X-ray diffraction analysis in the 1950s, X-ray crystallography has become the primary methodology used to determine the 3D structure of macromolecules. However, biological specimens such as cells, organelles, viruses and many important macromolecules are difficult or impossible to crystallize, and hence their structures are not accessible by crystallography. Here we report, for the first time, the recording and reconstruction of X-ray diffraction patterns from single, unstained viruses. The structure of the viral capsid inside a virion was visualized. This work opens the door for quantitative X-ray imaging of a broad range of specimens from protein machineries, viruses and organelles to whole cells. Moreover, our experiment is directly transferable to the use of X-ray free electron lasers, and represents a major experimental milestone towards the X-ray imaging of single macromolecules.

  15. Pyroelectric x-ray detectors and x-ray pyrometers

    This paper discusses pyroelectric detectors which are very promising x-ray detectors for intense pulsed x-ray/γ-ray measurements and can be used as x-ray pyrometers. They are fast, passive, and inherently flat in spectral response for low energy x-rays. The authors report tests of LiTaO3, Sr.5Ba.5Nb2O6 and LiNbO3 detectors at Nova laser with 1 ns low energy x-rays and at Zapp Z-pinch machine with 100 ns x-rays. The temporal and spectral responses are discussed

  16. Pyroelectric x-ray detectors and x-ray pyrometers

    Pyroelectric detectors are very promising x-ray detectors for intense pulsed x-ray/γ-ray measurements and can be used as x-ray pyrometers. They are fast, passive, and inherently flat in spectral response for low-energy x rays. We report our tests of LiTaO3 detectors at Nova laser with 1-ns low-energy x rays and at Zapp Z-pinch machine with 100-ns x rays. The temporal and spectral responses are discussed

  17. Fourier-transform Ghost Imaging with Hard X-rays

    Yu, Hong; Han, Shensheng; Xie, Honglan; Du, Guohao; Xiao, Tiqiao; Zhu, Daming

    2016-01-01

    Knowledge gained through X-ray crystallography fostered structural determination of materials and greatly facilitated the development of modern science and technology in the past century. Atomic details of sample structures is achievable by X-ray crystallography, however, it is only applied to crystalline structures. Imaging techniques based on X-ray coherent diffraction or zone plates are capable of resolving the internal structure of non-crystalline materials at nanoscales, but it is still a challenge to achieve atomic resolution. Here we demonstrate a novel lensless Fourier-transform ghost imaging method with pseudo-thermal hard X-rays by measuring the second-order intensity correlation function of the light. We show that high resolution Fourier-transform diffraction pattern of a complex structure can be achieved at Fresnel region, and the amplitude and phase distributions of a sample in spatial domain can be retrieved successfully. The method of lensless X-ray Fourier-transform ghost imaging extends X-ray...

  18. Effect of a Routine Synchrotron X-Ray Microtomography Scan on the Amino Acid Content of the Murchison CM Chondrite

    Friedrich, J. M.; Glavin, D. P.; Rivers, M. L.; Dworkin, J. P.

    2015-07-01

    We conducted experiments to examine if exposure to synchrotron radiation during a typical µCT scan causes detectable changes in the amino acid content of a carbonaceous chondrite. We found a µCT scan caused no change in the amino acid content.

  19. Characterization of D-glucaric acid using NMR, x-ray crystal structure, and MM3 molecular modeling analyses

    D-glucaric acid was characterized in solution by comparing NMR spectra from the isotopically unlabeled molecule with those from D-glucaric acid labeled with deuterium or carbon-13 atoms. The NMR studies provided unequivocal assignments for all carbon atoms and non-hydroxyl protons of the molecule. ...

  20. Coherent convergent-beam time-resolved X-ray diffraction

    Spence, John C. H.; Zatsepin, Nadia A.; Li, Chufeng

    2014-01-01

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic ...

  1. X ray Production. Chapter 5

    The differential absorption of X rays in tissues and organs, owing to their atomic composition, is the basis for the various imaging methods used in diagnostic radiology. The principles in the production of X rays have remained the same since their discovery. However, much refinement has gone into the design of X ray tubes to achieve the performance required for today’s radiological examinations. In this chapter, an outline of the principles of X ray production and a characterization of the radiation output of X ray tubes will be given. The basic processes producing X rays are dealt with in Section 1.4

  2. X-ray crystallographic, FT-IR and NMR studies as well as anticancer and antibacterial activity of the salt formed between ionophore antibiotic Lasalocid acid and amines

    Huczyński, Adam; Rutkowski, Jacek; Wietrzyk, Joanna; Stefańska, Joanna; Maj, Ewa; Ratajczak-Sitarz, Małgorzata; Katrusiak, Andrzej; Brzezinski, Bogumil; Bartl, Franz

    2013-01-01

    Two new complexes of the ionophore antibiotic Lasalocid acid (LAS) with phenylamine (PhA) and butylamine (BuA) were synthesized and their molecular structures were studied using single crystal X-ray diffraction and spectroscopic methods. In the solid state both amines are protonated and all NH3+ protons are hydrogen bonded to etheric, hydroxyl and carboxylic oxygen atoms of the LAS anion. In chloroform solutions the structure observed in the crystal of LAS-BuA complex is preserved and an equilibrium between the LAS-PhA complex and dissociated Lasalocid acid and phenylamine is observed. In vitro antimicrobial tests of the complexes showed a significant activity towards some strains of Gram-positive bacteria. For the first time Lasalocid acid and its complexes with amines were tested in vitro for cytotoxic activity against human cancer cell lines: A-549 (lung), MCF-7 (breast), HT-29 (colon) and mouse cancer cell line P-388 (leukemia). We found that LAS and its complexes are strong cytotoxic agents towards all tested cell lines. The cytostatic activity of the compounds studied is greater than that of cisplatin, indicating that Lasalocid and its complexes are promising candidates for new anticancer drugs.

  3. X-ray microtomography

    In this paper the authors describe the application of a new high-resolution X-ray tomographic microscope to the study of porous media. The microscope was designed to exploit the properties of a synchrotron X-ray source to perform three dimensional tomography on millimeter sized objects with micron resolution and has been used in materials science studies with both synchrotron and conventional and synchrotron sources will be compared. In this work the authors have applied the microscope to measure the three dimensional structure of fused bead packs and berea sandstones with micron resolution and have performed preliminary studies of flow in these media with the microscope operated in a digital subtraction radiography mode. Computer graphics techniques have been applied to the data to visually display the structure of the pore body system. Tomographic imaging after flow experiments should detect the structure of the oil-water interface in the pore network and this work is ongoing

  4. X-ray generators

    Volume 4 provides a comparative survey on generators for stationary applications as available on the German market. It provides decision-making tools, physical characteristics, suggestions for radiation protection and for safe appliance operation as well as a concept for inspections all of which have been developed jointly by physicians of various specialities, physicists, engineers, business men, hospital experts and medicotechnical X-ray staff on the basis of a well-tried working concept. The systematic representation of correlations relevant to decision-making processes is based on a profile of technico-physical characteristics (standard product information) which was established by way of interdisciplinary dialog and which will enable any hospital or clinic to easily equip its X-ray department in an economic and purposeful way. The information on device data, device descriptions and market survey furnish the data tested by the manufacturers without guarantee and subject to correction. (orig./HP)

  5. X-ray lithography

    An invention relating to the development of photo-resists used in X-ray lithography is described. A COP resist which has been exposed to X-ray radiation, is developed with methyl ethyl ketone (MEK) developer and an ethanol solvent. The resist is first developed in a strong developing solution and then with a weaker developer whose concentration is slightly above that required to obtain complete development. Preferably the resist is exposed so as to obtain about a fifty per cent developed thickness and the developing is carried out in steps, the first with a concentration of 5:1.8 (MEK to ethanol) for five seconds, the second using concentrations of 5:1.8 and 5:2.7 for ten seconds and the third with a concentration of 5:2.7 for five seconds. (author)

  6. Bone X-Ray (Radiography)

    Full Text Available ... foot. top of page What are some common uses of the procedure? A bone x-ray is ... care is taken during x-ray examinations to use the lowest radiation dose possible while producing the ...

  7. Bone X-Ray (Radiography)

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and ...

  8. Dental X-ray apparatus

    Intra-oral dental X-ray apparatus for panoramic radiography is described in detail. It comprises a tubular target carrier supporting at its distal end a target with an inclined forward face. Image definition is improved by positioning in the path of the X-rays a window of X-ray transmitting ceramic material, e.g. 90% oxide of Be, or Al, 7% Si02. The target carrier forms a probe which can be positioned in the patient's mouth. X-rays are directed forwardly and laterally of the target to an X-ray film positioned externally. The probe is provided with a detachable sleeve having V-form arms of X-ray opaque material which serve to depress the tongue out of the radiation path and also shield the roof of the mouth and other regions of the head from the X-ray pattern. A cylindrical lead shield defines the X-ray beam angle. (author)

  9. Bone X-Ray (Radiography)

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ...

  10. Soft X-ray Imaging

    Seely, John

    1999-05-20

    The contents of this report cover the following: (1) design of the soft x-ray telescope; (2) fabrication and characterization of the soft x-ray telescope; and (3) experimental implementation at the OMEGA laser facility.

  11. Bone X-Ray (Radiography)

    Full Text Available ... and x-rays. A Word About Minimizing Radiation Exposure Special care is taken during x-ray examinations ... patient's body not being imaged receive minimal radiation exposure. top of page What are the limitations of ...

  12. Bone X-Ray (Radiography)

    Full Text Available ... images for evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ...

  13. Bone X-Ray (Radiography)

    Full Text Available ... fracture. guide orthopedic surgery, such as spine repair/fusion, joint replacement and fracture reductions. look for injury, ... and Media Arthritis X-ray, Interventional Radiology and Nuclear Medicine Radiation Safety Images related to X-ray ( ...

  14. Bone X-Ray (Radiography)

    Full Text Available ... As a result, bones appear white on the x-ray, soft tissue shows up in shades of gray and air appears black. Until recently, x-ray images were maintained on large film sheets (much ...

  15. Panoramic Dental X-Ray

    ... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a ... a large photographic negative). Today, most images are digital files that are stored electronically. These stored images ...

  16. Bone X-Ray (Radiography)

    Full Text Available ... that helps physicians diagnose and treat medical conditions. Imaging with x-rays involves exposing a part of ... oldest and most frequently used form of medical imaging. A bone x-ray makes images of any ...

  17. Bone X-Ray (Radiography)

    Full Text Available ... wrist, arm, elbow, shoulder, spine, pelvis, hip, thigh, knee, leg (shin), ankle or foot. top of page ... the patient standing upright, as in cases of knee x-rays. A portable x-ray machine is ...

  18. The Microwave-assisted Preparation and X-Ray Structure of 3-Bromocarbazole-N-Acetic Acid

    2001-01-01

    The rapid synthesis of 3-bromocarbazole-N-acetic acid was performed using microwave irradiation. Under the optimal conditions the yield was 85.6 %. The crystal structure showed that the carboxylic groups form bifurcated hydrogen bonds and the hydroxyl oxygen atoms serve as proton donors and also acceptor. Each carboxylic group was involved in four hydrogen bonds. The packing of crystal was dominated by links of these hydrogen bonds.

  19. Crystallization and preliminary X-ray diffraction studies of the abscisic acid receptor PYL3 and its complex with pyrabactin

    Crystals of the abscisic acid receptor PYL3 and of the PYL3–pyrabactin complex were obtained and optimized in order to obtain high-quality diffraction data. Diffraction data sets were collected and processed to 2.5 and 1.83 Å resolution, respectively. Abscisic acid (ABA) modulates many developmental processes and responses to environmental stress. Recently, a family of pyrabactin resistance-like proteins (PYLs) in Arabidopsis thaliana were identified to be abscisic acid receptors. Although the 14 PYLs members share a similar sequence identity, they exhibit different responses toward pyrabactin. Apo-PYL3 is a dimer; however, its oligomeric state changes greatly on the addition of pyrabactin. Moreover, pyrabactin binds dimeric PYL3 in a nonproductive mode which prevents receptor activation and inhibition of PP2Cs. Here, the expression, purification and crystallization of apo-PYL3 and of PYL3 complexed with pyrabactin are reported. Diffraction data were optimized to 2.5 Å resolution for apo-PYL3 and to 1.83 Å resolution for PYL3–pyrabactin. The crystals of apo-PYL3 and PYL3–pyrabactin belonged to space groups P41212 and P212121, respectively

  20. Characterization of the Adsorption of Nucleic Acid Bases onto Ferrihydrite via Fourier Transform Infrared and Surface-Enhanced Raman Spectroscopy and X-ray Diffractometry.

    Canhisares-Filho, José E; Carneiro, Cristine E A; de Santana, Henrique; Urbano, Alexandre; da Costa, Antonio C S; Zaia, Cássia T B V; Zaia, Dimas A M

    2015-09-01

    Minerals could have played an important role in concentration, protection, and polymerization of biomolecules. Although iron is the fourth most abundant element in Earth's crust, there are few works in the literature that describe the use of iron oxide-hydroxide in prebiotic chemistry experiments. In the present work, the interaction of adenine, thymine, and uracil with ferrihydrite was studied under conditions that resemble those of prebiotic Earth. At acidic pH, anions in artificial seawater decreased the pH at the point of zero charge (pHpzc) of ferrihydrite; and at basic pH, cations increased the pHpzc. The adsorption of nucleic acid bases onto ferrihydrite followed the order adenine > uracil > thymine. Adenine adsorption peaked at neutral pH; however, for thymine and uracil, adsorption increased with increasing pH. Electrostatic interactions did not appear to play an important role on the adsorption of nucleic acid bases onto ferrihydrite. Adenine adsorption onto ferrihydrite was higher in distilled water compared to artificial seawater. After ferrihydrite was mixed with artificial seawaters or nucleic acid bases, X-ray diffractograms and Fourier transform infrared spectra did not show any change. Surface-enhanced Raman spectroscopy showed that the interaction of adenine with ferrihydrite was not pH-dependent. In contrast, the interactions of thymine and uracil with ferrihydrite were pH-dependent such that, at basic pH, thymine and uracil lay flat on the surface of ferrihydrite, and at acidic pH, thymine and uracil were perpendicular to the surface. Ferrihydrite adsorbed much more adenine than thymine; thus adenine would have been better protected against degradation by hydrolysis or UV radiation on prebiotic Earth. PMID:26393397

  1. Active X-ray Optics

    Hudec, René; Inneman, A.; Pina, L.; Černá, D.; Tichý, V.

    Bellingham: SPIE, 2013 - (Juha, L.; Bajt, S.; London, R.; Hudec, R.; Pína, L.), 877718/1-877718/7. (Proceedings of SPIE. 8777). ISBN 9780819495792. [Damage to VUV, EUV, and X-ray Optics IV; and EUV and X-ray Optics: Synergy between Laboratory and Space III. Praha (CZ), 15.04.2013-18.04.2013] Institutional support: RVO:67985815 Keywords : X-ray optics * active optics * active X-ray optics Subject RIV: BN - Astronomy, Celestial Mechanics, Astrophysics

  2. Expression, purification, crystallization and preliminary X-ray analysis of a novel N-substituted branched-chain l-amino-acid dioxygenase from Burkholderia ambifaria AMMD

    Diffraction data were collected to a limiting resolution of 2.4 Å from a crystal of selenomethionyl-labelled SadA, an l-amino-acid dioxygenase. Ferrous ion- and α-ketoglutarate-dependent dioxygenase from Burkholderia ambifaria AMMD (SadA) catalyzes the C3-hydroxylation of N-substituted branched-chain l-amino acids, especially N-succinyl-l-leucine, coupled to the conversion of α-ketoglutarate to succinate and CO2. SadA was expressed in Escherichia coli, purified and crystallized using the sitting-drop vapour-diffusion method at 293 K. Crystals of selenomethionine-substituted SadA were obtained using a reservoir solution containing PEG 3000 as the precipitant at pH 9.5 and diffracted X-rays to 2.4 Å resolution. The crystal belonged to space group P212121, with unit-cell parameters a = 49.3, b = 70.9, c = 148.2 Å. The calculated Matthews coefficient (VM = 2.1 Å3 Da−1, 41% solvent content) suggested that the crystal contains two molecules per asymmetric unit

  3. Cation profiling of passive films on stainless steel formed in sulphuric and acetic acid by deconvolution of angle-resolved X-ray photoelectron spectra

    An approach for determining depth gradients of metal-ion concentrations in passive films on stainless steel using angle-resolved X-ray photoelectron spectroscopy (ARXPS) is described. The iterative method, which is based on analyses of the oxidised metal peaks, provides increased precision and hence allows faster ARXPS measurements to be carried out. The method was used to determine the concentration depth profiles for molybdenum, iron and chromium in passive films on 316L/EN 1.4432 stainless steel samples oxidised in 0.5 M H2SO4 and acetic acid diluted with 0.02 M Na2B4O7 · 10H2O and 1 M H2O, respectively. The molybdenum concentration in the film is pin-pointed to the oxide/metal interface and the films also contained an iron-ion-enriched surface layer and a chromium-ion-dominated middle layer. Although films of similar composition and thickness (i.e., about 2 nm) were formed in the two electrolytes, the corrosion currents were found to be three orders of magnitude larger in the acetic acid solution. The differences in the layer composition, found for the two electrolytes as well as different oxidation conditions, can be explained based on the oxidation potentials of the metals and the dissolution rates of the different metal ions.

  4. Comparative crystallization and preliminary X-ray diffraction studies of locked nucleic acid and RNA stems of a tenascin C-binding aptamer

    Locked nucleic acid (LNA) nucleotides are RNA analogues with a useful additional conformational constraint; the current investigation will provide the first crystallographic view of an all-LNA duplex. The pharmacokinetic properties of an aptamer against the tumour-marker protein tenascin-C have recently been successfully improved by the introduction of locked nucleic acids (LNAs) into the terminal stem of the aptamer. Since it is believed that this post-SELEX optimization is likely to provide a more general route to enhance the in vitro and in vivo stability of aptamers, elucidation of the structural basis of this improvement was embarked upon. Here, the crystallographic and X-ray diffraction data of the isolated aptamer stem encompassed in a six-base-pair duplex both with and without the LNA modification are presented. The obtained all-LNA crystals belong to space group P41212 or P43212, with unit-cell parameters a = b = 52.80, c = 62.83 Å; the all-RNA crystals belong to space group R32, with unit-cell parameters a = b = 45.21, c = 186.97 Å, γ = 120.00°

  5. Crystallization and preliminary X-ray diffraction analysis of a fatty-acid metabolism regulatory protein, FadR, from Bacillus halodurans

    Trigonal crystals of FadR from B. halodurans have been obtained. X-ray data were collected to 2.05 Å resolution using synchrotron radiation. FadR is an acyl-CoA-dependent transcription factor which regulates genes encoding proteins involved in fatty-acid degradation and synthesis in order to maintain lipid homeostasis. FadR from the alkaliphilic bacterium Bacillus halodurans was cloned and overexpressed in Escherichia coli. The FadR (Bh3102) protein from B. halodurans is composed of 195 amino-acid residues with a molecular mass of 22 378 Da. Crystals were obtained by the sitting-drop vapour-diffusion method and diffracted to 2.05 Å resolution. FadR was crystallized at 296 K using polyethylene glycol 3350 as a precipitant. The crystal belonged to the apparent trigonal space group P3221, with unit-cell parameters a = b = 56.34, c = 199.73 Å. The Matthews coefficient and solvent content were estimated to be 2.0 Å3 Da−1 and 39.8%, respectively, assuming that the asymmetric unit contained two molecules of FadR, which was subsequently confirmed by molecular-replacement calculations

  6. Purification, crystallization and preliminary X-ray diffraction analysis of a hydroxycinnamoyl-CoA shikimate/quinate hydroxycinnamoyltransferase (HCT) from Coffea canephora involved in chlorogenic acid biosynthesis

    A hydroxycinnamoyl-CoA shikimate/quinate hydroxycinnamoyltransferase involved in chlorogenic acid biosynthesis in C. canephora was crystallized using the vapour-diffusion method. A diffraction data set was collected to 3.0 Å resolution on the microfocus beamline (ID23-2) at ESRF and a structure solution was obtained using molecular replacement. Chlorogenic acids (CGAs) are a group of soluble phenolic compounds that are produced by a variety of plants, including Coffea canephora (robusta coffee). The last step in CGA biosynthesis is generally catalysed by a specific hydroxycinnamoyl-CoA quinate hydroxycinnamoyltransferase (HQT), but it can also be catalysed by the more widely distributed hydroxycinnamoyl-CoA shikimate/quinate hydroxycinnamoyltransferase (HCT). Here, the cloning and overexpression of HCT from C. canephora in Escherichia coli as well as its purification and crystallization are presented. Crystals were obtained by the sitting-drop technique at 293 K and X-ray diffraction data were collected on the microfocus beamline ID23-2 at the ESRF. The HCT crystals diffracted to better than 3.0 Å resolution, belonged to space group P42212 with unit-cell parameters a = b = 116.1, c = 158.9 Å and contained two molecules in the asymmetric unit. The structure was solved by molecular replacement and is currently under refinement. Such structural data are needed to decipher the molecular basis of the substrate specifities of this key enzyme, which belongs to the large plant acyl-CoA-dependent BAHD acyltransferase superfamily

  7. Novel 2-oxoimidazolidine-4-carboxylic acid derivatives as Hepatitis C virus NS3-4A serine protease inhibitors: synthesis, activity, and X-ray crystal structure of an enzyme inhibitor complex

    Arasappan, Ashok; Njoroge, F. George; Parekh, Tejal N.; Yang, Xiaozheng; Pichardo, John; Butkiewicz, Nancy; Prongay, Andrew; Yao, Nanhua; Girijavallabhan, Viyyoor (SPRI)

    2008-06-30

    Synthesis and HCV NS3 serine protease inhibitory activity of some novel 2-oxoimidazolidine-4-carboxylic acid derivatives are reported. Inhibitors derived from this new P2 core exhibited activity in the low {micro}M range. X-ray structure of an inhibitor, 15c bound to the protease is presented.

  8. Bone X-Ray (Radiography)

    Full Text Available ... lies. A drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... that is extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  9. Bone X-Ray (Radiography)

    Full Text Available ... x-rays. top of page What does the equipment look like? The equipment typically used for bone x-rays consists of ... and joint abnormalities, such as arthritis. X-ray equipment is relatively inexpensive and widely available in emergency ...

  10. Tunable X-ray source

    Boyce, James R.

    2011-02-08

    A method for the production of X-ray bunches tunable in both time and energy level by generating multiple photon, X-ray, beams through the use of Thomson scattering. The method of the present invention simultaneously produces two X-ray pulses that are tunable in energy and/or time.

  11. X-Ray Exam: Ankle

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Ankle KidsHealth > For Parents > X-Ray Exam: Ankle Print A A A Text Size ... español Radiografía: tobillo What It Is An ankle X-ray is a safe and painless test that uses ...

  12. X-Ray Exam: Finger

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Finger KidsHealth > For Parents > X-Ray Exam: Finger Print A A A Text Size ... español Radiografía: dedo What It Is A finger X-ray is a safe and painless test that uses ...

  13. X-Ray Exam: Wrist

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Wrist KidsHealth > For Parents > X-Ray Exam: Wrist Print A A A Text Size ... español Radiografía: muñeca What It Is A wrist X-ray is a safe and painless test that uses ...

  14. X-Ray Exam: Hip

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Hip KidsHealth > For Parents > X-Ray Exam: Hip Print A A A Text Size ... español Radiografía: cadera What It Is A hip X-ray is a safe and painless test that uses ...

  15. X-Ray Exam: Forearm

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Forearm KidsHealth > For Parents > X-Ray Exam: Forearm Print A A A Text Size ... español Radiografía: brazo What It Is A forearm X-ray is a safe and painless test that uses ...

  16. X-Ray Exam: Pelvis

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Pelvis KidsHealth > For Parents > X-Ray Exam: Pelvis Print A A A Text Size ... español Radiografía: pelvis What It Is A pelvis X-ray is a safe and painless test that uses ...

  17. X-Ray Exam: Foot

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Foot KidsHealth > For Parents > X-Ray Exam: Foot Print A A A Text Size ... español Radiografía: pie What It Is A foot X-ray is a safe and painless test that uses ...

  18. Bone X-Ray (Radiography)

    Full Text Available ... The x-ray tube is connected to a flexible arm that is extended over the patient while an x-ray film holder or image recording plate is placed beneath the patient. top of page How does the procedure work? X-rays are a form of radiation like ...

  19. Production and X-ray crystallographic analysis of fully deuterated human carbonic anhydrase II

    This article reports the production, crystallization and X-ray structure determination of perdeuterated human carbonic anhydrase (HCA II). The refined structure is shown to be highly isomorphous with hydrogenated HCA II, especially with regard to the active site architecture and solvent network. Human carbonic anhydrase II (HCA II) is a zinc metalloenzyme that catalyzes the reversible hydration and dehydration of carbon dioxide and bicarbonate, respectively. The rate-limiting step in catalysis is the intramolecular transfer of a proton between the zinc-bound solvent (H2O/OH−) and the proton-shuttling residue His64. This distance (∼7.5 Å) is spanned by a well defined active-site solvent network stabilized by amino-acid side chains (Tyr7, Asn62, Asn67, Thr199 and Thr200). Despite the availability of high-resolution (∼1.0 Å) X-ray crystal structures of HCA II, there is currently no definitive information available on the positions and orientations of the H atoms of the solvent network or active-site amino acids and their ionization states. In preparation for neutron diffraction studies to elucidate this hydrogen-bonding network, perdeuterated HCA II has been expressed, purified, crystallized and its X-ray structure determined to 1.5 Å resolution. The refined structure is highly isomorphous with hydrogenated HCA II, especially with regard to the active-site architecture and solvent network. This work demonstrates the suitability of these crystals for neutron macromolecular crystallography

  20. Insights into Equilibrium Dynamics of Proteins from Comparison of NMR and X-Ray Data with Computational Predictions

    Yang, Lee-Wei; Eyal, Eran; Chennubhotla, Chakra; Jee, JunGoo; Gronenborn, Angela M.; Bahar, Ivet

    2007-01-01

    For a representative set of 64 nonhomologous proteins, each containing a structure solved by NMR and X-ray crystallography, we analyzed the variations in atomic coordinates between NMR models, the temperature (B) factors measured by X-ray crystallography, and the fluctuation dynamics predicted by the Gaussian network model (GNM). The NMR and X-ray data exhibited a correlation of 0.49. The GNM results, on the other hand, yielded a correlation of 0.59 with X-ray data and a distinctively better ...

  1. Crystallization and preliminary X-ray diffraction analysis of ω-amino acid:pyruvate transaminase from Chromobacterium violaceum

    An ω-amino acid:pyruvate transaminase from C. violaceum has been purified and crystallized in two crystal forms. The structure has been solved using molecular replacement. The enzyme ω-transaminase catalyses the conversion of chiral ω-amines to ketones. The recombinant enzyme from Chromobacterium violaceum has been purified to homogeneity. The enzyme was crystallized from PEG 4000 using the microbatch method. Data were collected to 1.7 Å resolution from a crystal belonging to the triclinic space group P1, with unit-cell parameters a = 58.9, b = 61.9, c = 63.9 Å, α = 71.9, β = 87.0, γ = 74.6°. Data were also collected to 1.95 Å from a second triclinic crystal form. The structure has been solved using the molecular-replacement method

  2. X-ray diffraction

    The seventh edition of Philips' Review of literature on X-ray diffraction begins with a list of conference proceedings on the subject, organised by the Philips' organisation at regular intervals in various European countries. This is followed by a list of bulletins. The bibliography is divided according to the equipment (cameras, diffractometers, monochromators) and its applications. The applications are subdivided into sections for high/low temperature and pressure, effects due to the equipment, small angle scattering and a part for stress, texture and phase analyses of metals and quantitative analysis of minerals

  3. X-ray detector

    The multicell X-ray or gamma detector is used in computer tomography. To achieve good spatial resolution, the electrode plates are narrowly spaced in each cell and are designed identical over the whole length of the detector group. The uniform spacing and precise check of the angles between the electrodes and accurate control of the dimensions of the whole detector structure are achieved by depositing, in the fabrication process, a viscous, resin type material (e.g., epoxy resin) or glue at selected points between the electrodes and insulators. (ORU)

  4. High-resolution X-ray study of the effects of deuteration on crystal growth and the crystal structure of proteinase K

    A high-resolution X-ray crystallographic study of the effects of solvent deuteration on the crystallization of proteinase K shows negligibly small degradations of the crystals owing to solvent deuteration and small structural differences between nondeuterated and deuterated crystals of proteinase K. Deuteration of macromolecules is an important technique in neutron protein crystallography. Solvent deuteration of protein crystals is carried out by replacing water (H2O) with heavy water (D2O) prior to neutron diffraction experiments in order to diminish background noise. The effects of solvent deuteration on the crystallization of proteinase K (PK) with polyethylene glycol as a precipitant were investigated using high-resolution X-ray crystallography. In previous studies, eight NO3− anions were included in the PK crystal unit cell grown in NaNO3 solution. In this study, however, the PK crystal structure did not contain NO3− anions; consequently, distortions of amino acids arising from the presence of NO3− anions were avoided in the present crystal structures. High-resolution (1.1 Å) X-ray diffraction studies showed that the degradation of PK crystals induced by solvent deuteration was so small that this degradation would be negligible for the purpose of neutron protein crystallography experiments at medium resolution. Comparison of the nonhydrogen structures of nondeuterated and deuterated crystal structures demonstrated very small structural differences. Moreover, a positive correlation between the root-mean-squared differences and B factors indicated that no systematic difference existed

  5. In situ SERS and X-ray photoelectron spectroscopy studies on the pH-dependant adsorption of anthraquinone-2-carboxylic acid on silver electrode

    Li, Dan; Jia, Shaojie; Fodjo, Essy Kouadio; Xu, Hu; Wang, Yuhong; Deng, Wei

    2016-03-01

    In this study, in situ surface-enhanced Raman scattering (SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS) are used to investigate the redox reaction and adsorption behavior of anthraquinone-2-carboxylic acid (AQ-2-COOH) on an Ag electrode at different pH values. The obtained results indicate that AQ-2-COOH is adsorbed tilted on the Ag electrode through O-atom of ring carbonyl in a potential range from -0.3 to -0.5 V vs. SCE, but the orientation turns to more tilted orientation with both O-atom of the ring carbonyl and carboxylate group in positive potential region for pH 6.0 and 7.4. However, at pH 10.0, the orientation adopts tilted conformation constantly on the Ag electrode with both O-atom of the anthraquinone ring and carboxylate group in the potential range from -0.3 to -0.5 V vs. SCE or at positive potentials. Moreover, the adsorption behavior of AQ-2-COOH has been further confirmed by AR-XPS on the Ag surface. Proposed reasons for the observed changes in orientation are presented.

  6. Expression, purification, crystallization and preliminary X-ray diffraction analysis of the VP8* sialic acid-binding domain of porcine rotavirus strain OSU

    Zhang, Yang-De, E-mail: zhangyd1960@yahoo.com.cn; Li, Hao [National Hepatobiliary and Enteric Surgery Research Center of The Ministry of Health, Xiangya Hospital, Central South University, Hunan Province (China); Liu, Hui; Pan, Yi-Feng [Biochemistry Laboratory, Institution of Biomedical Engineering, Central South University, Hunan Province (China); National Hepatobiliary and Enteric Surgery Research Center of The Ministry of Health, Xiangya Hospital, Central South University, Hunan Province (China)

    2007-02-01

    Porcine rotavirus strain OSU VP8* domain has been expressed, purified and crystallized. X-ray diffraction data from different crystal forms of the VP8* domain have been collected to 2.65 and 2.2 Å resolution, respectively. The rotavirus outer capsid spike protein VP4 is utilized in the process of rotavirus attachment to and membrane penetration of host cells. VP4 is cleaved by trypsin into two domains: VP8* and VP5*. The VP8* domain is implicated in initial interaction with sialic acid-containing cell-surface carbohydrates and triggers subsequent virus invasion. The VP8* domain from porcine OSU rotavirus was cloned and expressed in Escherichia coli. Different crystal forms (orthorhombic P2{sub 1}2{sub 1}2{sub 1} and tetragonal P4{sub 1}2{sub 1}2) were harvested from two distinct crystallization conditions. Diffraction data have been collected to 2.65 and 2.2 Å resolution and the VP8*{sub 65–224} structure was determined by molecular replacement.

  7. In Vitro assessment of dentin erosion after immersion in acidic beverages: surface profile analysis and energy-dispersive X-ray fluorescence spectrometry study.

    Caneppele, Taciana Marco Ferraz; Jeronymo, Raffaela Di Iorio; Di Nicoló, Rebeca; de Araújo, Maria Amélia Máximo; Soares, Luís Eduardo Silva

    2012-01-01

    The aim of this study was to investigate the effects of some acidic drinks on dentin erosion, using methods of surface profile (SP) analysis and energy-dispersive X-ray fluorescence spectrometry (EDXRF). One hundred standardized dentin slabs obtained from bovine incisor roots were used. Dentin slabs measuring 5x5 mm were ground flat, polished and half of each specimen surface was protected with nail polish. For 60 min, the dentin surfaces were immersed in 50 mL of 5 different drinks (Gatorade®, Del Valle Mais orange juice®, Coca-Cola®, Red Bull® and white wine), 20 blocks in each drink. The pH of each beverage was measured. After the erosive challenge, the nail polish was removed and SP was analyzed. The mineral concentration of dentin surfaces was determined by means of EDXRF. Data were analyzed statistically by ANOVA and Tukey's test (α=0.05). SP analysis showed that Red-Bull had the highest erosive potential (pcontent between the reference surface and eroded surface. In conclusion, this study demonstrated that all studied beverages promoted erosion on root dentin and Red Bull had the highest erosive potential. There was no correlation between pH of beverages and their erosive potential and only the P content changed after erosive challenge. PMID:23207852

  8. Nanoflow electrospinning serial femtosecond crystallography

    A low flow rate liquid microjet method for delivery of hydrated protein crystals to X-ray lasers is presented. Linac Coherent Light Source data demonstrates serial femtosecond protein crystallography with micrograms, a reduction of sample consumption by orders of magnitude. An electrospun liquid microjet has been developed that delivers protein microcrystal suspensions at flow rates of 0.14–3.1 µl min−1 to perform serial femtosecond crystallography (SFX) studies with X-ray lasers. Thermolysin microcrystals flowed at 0.17 µl min−1 and diffracted to beyond 4 Å resolution, producing 14 000 indexable diffraction patterns, or four per second, from 140 µg of protein. Nanoflow electrospinning extends SFX to biological samples that necessitate minimal sample consumption

  9. Quantum effets in nonresonant X-ray scattering

    Slowik, Jan Malte

    2015-11-15

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  10. Quantum effets in nonresonant X-ray scattering

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  11. Serial femtosecond X-ray diffraction of 30S ribosomal subunit microcrystals in liquid suspension at ambient temperature using an X-ray free-electron laser

    Serial femtosecond X-ray (SFX) diffraction extending beyond 6 Å resolution using T. thermophilus 30S ribosomal subunit crystals is reported. High-resolution ribosome structures determined by X-ray crystallography have provided important insights into the mechanism of translation. Such studies have thus far relied on large ribosome crystals kept at cryogenic temperatures to reduce radiation damage. Here, the application of serial femtosecond X-ray crystallography (SFX) using an X-ray free-electron laser (XFEL) to obtain diffraction data from ribosome microcrystals in liquid suspension at ambient temperature is described. 30S ribosomal subunit microcrystals diffracted to beyond 6 Å resolution, demonstrating the feasibility of using SFX for ribosome structural studies. The ability to collect diffraction data at near-physiological temperatures promises to provide fundamental insights into the structural dynamics of the ribosome and its functional complexes

  12. Nanoflow electrospinning serial femtosecond crystallography.

    Sierra, Raymond G; Laksmono, Hartawan; Kern, Jan; Tran, Rosalie; Hattne, Johan; Alonso-Mori, Roberto; Lassalle-Kaiser, Benedikt; Glöckner, Carina; Hellmich, Julia; Schafer, Donald W; Echols, Nathaniel; Gildea, Richard J; Grosse-Kunstleve, Ralf W; Sellberg, Jonas; McQueen, Trevor A; Fry, Alan R; Messerschmidt, Marc M; Miahnahri, Alan; Seibert, M Marvin; Hampton, Christina Y; Starodub, Dmitri; Loh, N Duane; Sokaras, Dimosthenis; Weng, Tsu-Chien; Zwart, Petrus H; Glatzel, Pieter; Milathianaki, Despina; White, William E; Adams, Paul D; Williams, Garth J; Boutet, Sébastien; Zouni, Athina; Messinger, Johannes; Sauter, Nicholas K; Bergmann, Uwe; Yano, Junko; Yachandra, Vittal K; Bogan, Michael J

    2012-11-01

    An electrospun liquid microjet has been developed that delivers protein microcrystal suspensions at flow rates of 0.14-3.1 µl min(-1) to perform serial femtosecond crystallography (SFX) studies with X-ray lasers. Thermolysin microcrystals flowed at 0.17 µl min(-1) and diffracted to beyond 4 Å resolution, producing 14,000 indexable diffraction patterns, or four per second, from 140 µg of protein. Nanoflow electrospinning extends SFX to biological samples that necessitate minimal sample consumption. PMID:23090408

  13. X-ray crystallographic studies on C-phycocyanins from cyanobacteria from different habitats: marine and freshwater

    Satyanarayana, L.; Suresh, C. G.; Patel, Anamika; Mishra, Sandhya; Ghosh, Pushpito Kumar

    2005-01-01

    The protein C-phycocyanin, involved in photosynthesis, has been purified from three cyanobacterial species: Spirulina, Phormidium and Lyngbya. These three proteins have been crystallized and characterized using X-ray crystallography.

  14. X-ray lithography sources

    Synchrotron from dipole magnets in electron storage rings has emerged as a useful source of x-rays for lithography. To meet the need for these sources numerous groups around the world have embarked on projects to design and construct storage rings for x-ray lithography. Both conventional electromagnets as well as superconducting (SC) dipoles have been incorporated into the various designs. An overview of the worldwide effort to produce commercial x-ray sources will be presented. To better illustrate the elements involved in these sources a closer examination of the Superconducting X-ray Lithography Source Project (SXLS) at BNL will be presented. 11 refs., 1 fig., 5 tabs

  15. X-ray Absorption Spectroscopy

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

    This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

  16. X-ray Fluorescence Sectioning

    Cong, Wenxiang

    2012-01-01

    In this paper, we propose an x-ray fluorescence imaging system for elemental analysis. The key idea is what we call "x-ray fluorescence sectioning". Specifically, a slit collimator in front of an x-ray tube is used to shape x-rays into a fan-beam to illuminate a planar section of an object. Then, relevant elements such as gold nanoparticles on the fan-beam plane are excited to generate x-ray fluorescence signals. One or more 2D spectral detectors are placed to face the fan-beam plane and directly measure x-ray fluorescence data. Detector elements are so collimated that each element only sees a unique area element on the fan-beam plane and records the x-ray fluorescence signal accordingly. The measured 2D x-ray fluorescence data can be refined in reference to the attenuation characteristics of the object and the divergence of the beam for accurate elemental mapping. This x-ray fluorescence sectioning system promises fast fluorescence tomographic imaging without a complex inverse procedure. The design can be ad...

  17. Image reconstruction in serial femtosecond nanocrystallography using x-ray free-electron lasers

    Chen, Joe P. J.; Kirian, Richard A.; Beyerlein, Kenneth R.; Bean, Richard J.; Morgan, Andrew J.; Yefanov, Oleksandr M.; Arnal, Romain D.; Wojtas, David H.; Bones, Phil J.; Chapman, Henry N.; Spence, John C. H.; Millane, Rick P.

    2015-09-01

    Serial femtosecond nanocrystallography (SFX) is a form of x-ray coherent diffraction imaging that utilises a stream of tiny nanocrystals of the biological assembly under study, in contrast to the larger crystals used in conventional x-ray crystallography using conventional x-ray synchrotron x-ray sources. Nanocrystallography utilises the extremely brief and intense x-ray pulses that are obtained from an x-ray free-electron laser (XFEL). A key advantage is that some biological macromolecules, such as membrane proteins for example, do not easily form large crystals, but spontaneously form nanocrystals. There is therefore an opportunity for structure determination for biological molecules that are inaccessible using conventional x-ray crystallography. Nanocrystallography introduces a number of interesting image reconstruction problems. Weak diffraction patterns are recorded from hundreds of thousands of nancocrystals in unknown orientations, and these data have to be assembled and merged into a 3D intensity dataset. The diffracted intensities can also be affected by the surface structure of the crystals that can contain incomplete unit cells. Furthermore, the small crystal size means that there is potentially access to diffraction information between the crystalline Bragg peaks. With this information, phase retrieval is possible without resorting to the collection of additional experimental data as is necessary in conventional protein crystallography. We report recent work on the diffraction characteristics of nanocrystals and the resulting reconstruction algorithms.

  18. Radioisotope x-ray analysis

    Radioisotope x-ray fluorescence and x-ray preferential absorption (XRA) techniques are used extensively for the analysis of materials, covering such diverse applications as analysis of alloys, coal, environmental samples, paper, waste materials, and metalliferous mineral ores and products. Many of these analyses are undertaken in the harsh environment of industrial plants and in the field. Some are continuous on-line analyses of material being processed in industry, where instantaneous analysis information is required for the control of rapidly changing processes. Radioisotope x-ray analysis systems are often tailored to a specific but limited range of applications. They are simpler and often considerably less expensive than analysis systems based on x-ray tubes. These systems are preferred to x-ray tube techniques when simplicity, ruggedness, reliability, and cost of equipment are important; when minimum size, weight, and power consumption are necessary; when a very constant and predictable x-ray output is required; when the use of high-energy x-rays is advantageous; and when short x-ray path lengths are required to minimize the absorption of low-energy x-rays in air. This chapter reviews radioisotope XRF, preferential absorption, and scattering techniques. Some of the basic analysis equations are given. The characteristics of radioisotope sources and x-ray detectors are described, and then the x-ray analytical techniques are presented. The choice of radioisotope technique for a specific application is discussed. This is followed by a summary of applications of these techniques, with a more detailed account given of some of the applications, particularly those of considerable industrial importance. 79 refs., 28 figs., 7 tabs

  19. Interferometric phase detection at x-ray energies via Fano resonance control

    Heeg, K P; Schumacher, D; Wille, H -C; Röhlsberger, R; Pfeifer, T; Evers, J

    2014-01-01

    Modern x-ray light sources promise access to structure and dynamics of matter in largely unexplored spectral regions. However, the desired information is encoded in the light intensity and phase, whereas detectors register only the intensity. This phase problem is ubiquitous in crystallography and imaging, and impedes the exploration of quantum effects at x-ray energies. Here, we demonstrate phase-sensitive measurements characterizing the quantum state of a nuclear two-level system at hard x-ray energies. The nuclei are initially prepared in a superposition state. Subsequently, the relative phase of this superposition is interferometrically reconstructed from the emitted x-rays. Our results form a first step towards x-ray quantum state tomography, and provide new avenues for structure determination and precision metrology via x-ray Fano interference.

  20. Interferometric phase detection at x-ray energies via Fano resonance control.

    Heeg, K P; Ott, C; Schumacher, D; Wille, H-C; Röhlsberger, R; Pfeifer, T; Evers, J

    2015-05-22

    Modern x-ray light sources promise access to structure and dynamics of matter in largely unexplored spectral regions. However, the desired information is encoded in the light intensity and phase, whereas detectors register only the intensity. This phase problem is ubiquitous in crystallography and imaging and impedes the exploration of quantum effects at x-ray energies. Here, we demonstrate phase-sensitive measurements characterizing the quantum state of a nuclear two-level system at hard x-ray energies. The nuclei are initially prepared in a superposition state. Subsequently, the relative phase of this superposition is interferometrically reconstructed from the emitted x rays. Our results form a first step towards x-ray quantum state tomography and provide new avenues for structure determination and precision metrology via x-ray Fano interference. PMID:26047250

  1. Multimodal particle size distribution or fractal surface of acrylic acid copolymer nanoparticles: A small-angle X-ray scattering study using direct Fourier and indirect maximum entropy methods

    Mueller, J.J.; Hansen, S; Lukowski, G.; Gast, K.

    1995-01-01

    Acrylic acid copolymers are potential carriers for drug delivery. The surface, surface rugosity and the absolute dimension of the particles are parameters that determine the binding of drugs or detergents, diffusion phenomena at the surface and the distribution of the carrier within the human body. The particle-size distribution and surface rugosity of the particles have been investigated by small-angle X-ray scattering and dynamic light scattering. Direct Fourier transform as well as a new s...

  2. Bone X-Ray (Radiography)

    Full Text Available Toggle navigation Test/Treatment Patient Type Screening/Wellness Disease/Condition Safety En Español More Info Images/Videos News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose of ionizing ...

  3. X-ray Dynamic Defectoscopy

    Vavřík, Daniel; Visschers, J.; Jakůbek, J.; Ponchut, C.

    Orosei : IMC S.r.l., 2001. s. 47. [International Workshop on Radiation Imaging Detectors /3./. 23.09.2001-27.09.2001, Orosei] R&D Projects: GA ČR GA106/00/D064 Institutional research plan: CEZ:MSM 210000018 Keywords : X-ray Defectoscopy * Damage * X-ray Detectors Subject RIV: JL - Materials Fatigue, Friction Mechanics

  4. X-ray diagnostic equipment

    An X-ray tube is connected to several different image processing devices in X-ray diagnostic equipment. Only a single organ selector is allocated to it, for which the picture parameters for each image processing device are selected. The choice of the correct combination of picture parameters is made by means of a selector switch. (DG)

  5. X-ray tube arrangement

    An x-ray tube is described incorporating an elongated target/ anode over which the electron beam is deflected and from which x-rays are emitted. Improved methods of monitoring and controlling the amplitude of the beam deflection are presented. (U.K.)

  6. Bone X-Ray (Radiography)

    Full Text Available ... frequently compared to current x-ray images for diagnosis and disease management. top of page How is the procedure performed? The technologist, an individual specially trained to perform radiology examinations, positions the patient on the x-ray ...

  7. Bone X-Ray (Radiography)

    Full Text Available ... clothing that might interfere with the x-ray images. Women should always inform their physician and x-ray ... small burst of radiation that passes through the body, recording an image on photographic film or a special detector. Different ...

  8. X-ray photoelectron spectroscopy

    The methods and results of X-ray photoelectron spectroscopy in the study of plasmons, alloys and gold compounds are discussed. After a comprehensive introduction, seven papers by the author, previously published elsewhere, are reprinted and these cover a wide range of the uses of X-ray photoelectron spectroscopy. (W.D.L.)

  9. Determination of X-ray flux using silicon pin diodes

    Accurate measurement of photon flux from an X-ray source is a parameter required to calculate the dose absorbed by a sample. The development of a model for determining the photon flux incident on pin diodes, and experiments to test this model, are described for incident energies between 4 and 18 keV used in macromolecular crystallography. Accurate measurement of photon flux from an X-ray source, a parameter required to calculate the dose absorbed by the sample, is not yet routinely available at macromolecular crystallography beamlines. The development of a model for determining the photon flux incident on pin diodes is described here, and has been tested on the macromolecular crystallography beamlines at both the Swiss Light Source, Villigen, Switzerland, and the Advanced Light Source, Berkeley, USA, at energies between 4 and 18 keV. These experiments have shown that a simple model based on energy deposition in silicon is sufficient for determining the flux incident on high-quality silicon pin diodes. The derivation and validation of this model is presented, and a web-based tool for the use of the macromolecular crystallography and wider synchrotron community is introduced

  10. Fulvic acid sorption on muscovite mica as a function of pH and time using in situ X-ray reflectivity.

    Lee, Sang Soo; Fenter, Paul; Park, Changyong; Nagy, Kathryn L

    2008-08-01

    Interfacial structures of the basal surface of muscovite mica in 100 mg kg (-1) Elliott Soil Fulvic Acid II solutions were investigated using in situ X-ray reflectivity. Molecular-scale variations in the thickness and internal structure of the fulvic acid (FA) film were observed and quantified as a function of pH (2-12) and reaction time (3-500 h at pH 3.7). At pH density profile of the FA layer sorbed on the muscovite surface was composed of one near-surface peak followed by a broad peak that diminished in electron density with distance from the surface. The presence of the near-surface peak is attributed to condensation of FA molecules during sorption. The apparent thickness of the FA layer decreased from 12.3 to 7.2 to 6.4 A as pH increased from 2 to 3.7 to 6, respectively. At pH > or =8.5, a distinct interfacial structure was observed, consisting of sharper peaks similar to those previously observed for muscovite in the absence of FA. These peaks are most likely composed of smaller aqueous species, such as H 2O molecules, metal ion impurities from FA, and Na (+) from NaOH. The FA sorbed on the muscovite surface at pH 3.7 maintained a relatively constant thickness after 3 hours. However, the electron density of the near-surface FA peak increased by about 24% from 3 to 12 hours, and remained relatively constant from 12 to 500 hours. The electron density of the more distant part of the sorbed FA layer increased slightly after 12-50 hours of reaction but then decreased, and the broad peak flattened by 500 hours. Internal structural changes are possibly due to the slow sorption rate of FA molecules, or a fractionation effect, i.e., continuous subsitution of smaller FA molecules by larger FA molecules. PMID:18616301

  11. Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

    A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis

  12. Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

    Van Benschoten, Andrew H. [University of California San Francisco, San Francisco, CA 94158 (United States); Afonine, Pavel V. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Terwilliger, Thomas C.; Wall, Michael E. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Jackson, Colin J. [Australian National University, Canberra, ACT 2601 (Australia); Sauter, Nicholas K. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Adams, Paul D. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); University of California Berkeley, Berkeley, CA 94720 (United States); Urzhumtsev, Alexandre [Institut de Génétique et de Biologie Moléculaire et Cellulaire, CNRS–INSERM–UdS, 1 Rue Laurent Fries, BP 10142, 67404 Illkirch (France); Université de Lorraine, BP 239, 54506 Vandoeuvre-les-Nancy (France); Fraser, James S., E-mail: james.fraser@ucsf.edu [University of California San Francisco, San Francisco, CA 94158 (United States)

    2015-07-28

    A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis.

  13. X-ray diffraction and inelastic neutron scattering study of 1:1 tetramethylpyrazine chloranilic acid complex: temperature, isotope, and pressure effects.

    Prager, M; Pietraszko, A; Sobczyk, L; Pawlukojć, A; Grech, E; Seydel, T; Wischnewski, A; Zamponi, M

    2006-11-21

    The x-ray diffraction studies of the title complex were carried out at room temperature and 14 K for H/D (in hydrogen bridge) isotopomers. At 82 K a phase transition takes place leading to a doubling of unit cells and alternation of the hydrogen bond lengths linking tetramethylpyrazine (TMP) and chloranilic acid molecules. A marked H/D isotope effect on these lengths was found at room temperature. The elongation is much smaller at 14 K. The infrared isotopic ratio for O-H(D)...N bands equals to 1.33. The four tunnel splittings of methyl librational ground states of the protonated complex required by the structure are determined at a temperature T=4.2 K up to pressures P=4.7 kbars by high resolution neutron spectroscopy. The tunnel mode at 20.6 microeV at ambient pressure shifts smoothly to 12.2 microeV at P=3.4 kbars. This is attributed to an increase of the strength of the rotational potential proportional to r(-5.6). The three other tunnel peaks show no or weak shifts only. The increasing interaction with diminishing intermolecular distances is assumed to be compensated by a charge transfer between the constituents of deltae/e approximately 0.02 kbar(-1). The phase transition observed between 3.4 and 4.7 kbars leads to increased symmetry with only two more intense tunneling bands. In the isotopomer with deuterated hydrogen bonds and P=1 bar all tunnel intensities become equal in consistency with the low temperature crystal structure. The effect of charge transfer is confirmed by a weakening of rotational potentials for those methyl groups whose tunnel splittings were independent of pressure. Density functional theory calculations for the model TMP.(HF)2 complex and fully ionized molecule TMP+ point out that the intramolecular rotational potential of methyl groups is weaker in the charged species. They do not allow for the unequivocal conclusions about the role of the intermolecular charge transfer effect on the torsional frequencies. PMID:17129141

  14. X-ray photoelectron spectroscopy of oxygen-containing layers formed by a linear potential scan on stepped gold (111) films in aqueous 1 M sulphuric acid

    Rodriguez Nieto, Felipe J. [Instituto de Investigaciones Fisicoquimica Teoricas y Aplicadas INIFTA, Universidad Nacional de La Plata, Consejo Nacional de Investigaciones Cientificas y Tecnicas Sucursal 4, Casilla de Correo 16, (1900) La Plata (Argentina); Member of Comision de Investigaciones Cientificas de la Provincia de Buenos Aires (Argentina)], E-mail: rodrini@inifta.unlp.edu.ar; Fachini, Esteban; Cabrera, Carlos R. [Department of Chemistry, University of Puerto Rico, Rio Piedras Campus, P.O. Box 23346, San Juan, 00931-3346 (Puerto Rico); Arvia, Alejandro J. [Instituto de Investigaciones Fisicoquimica Teoricas y Aplicadas INIFTA, Universidad Nacional de La Plata, Consejo Nacional de Investigaciones Cientificas y Tecnicas Sucursal 4, Casilla de Correo 16, (1900) La Plata (Argentina)

    2009-01-01

    X-ray photoelectron spectroscopy (XPS) data of oxygen-containing layers (O-layers) made on stepped gold (111) film electrodes from aqueous 1 M sulphuric acid by single linear potential scans at 0.10 V s{sup -1} and 298 K are reported. The potential scan covered from the open circuit potential to anodic switching potential E{sub as} = 2.50 V versus normal hydrogen electrode (NHE) and holding times at E{sub as} in the range 30-300 s. The anodic charge density q{sub a} determined from the oxidation and reduction voltammetric scan is in the range 0.20 {<=} q{sub a} {<=} 2.5 mC cm{sup -2}. For the potential E = 0.5 V, in the absence of O-layers, the S 2p core level spectrum indicates the presence of sulphate/bisulphate adsorbates. For E{sub as} > 1.3 V, the O 1s core level spectrum involves the contribution from water, OH- and O-species. These spectra are deconvoluted utilising either three or four Gaussian contributions with values of peaked binding energy and full width at half-maximum height (FWMH) in good agreement with expectations. The envelope of these XPS O 1s signals after correction for the contribution of sulphate/bisulphate adsorbates and adventitious carbon approaches the XPS signal that has been reported for the core level spectrum in the O 1s region of oxidised gold surfaces produced by laser pulses at different molecular oxygen pressures. The O/OH concentration ratio in the O-layer increases with E{sub as} ageing time t{sub ag} and cathodic charge density q{sub c}. The hydrous nature of the O-layer, evaluated through the analysis of the core level spectra in the O 1s region, decreases as E{sub as} and t{sub ag} are increased. Results are interesting to unravel the composition and structure of electrochemically grown O-layers at the surface of the gold substrate, and the influence of the history of these O-layers on the respective XPS features.

  15. The design of macromolecular crystallography diffraction experiments

    Thoughts about the decisions made in designing macromolecular X-ray crystallography experiments at synchrotron beamlines are presented. The measurement of X-ray diffraction data from macromolecular crystals for the purpose of structure determination is the convergence of two processes: the preparation of diffraction-quality crystal samples on the one hand and the construction and optimization of an X-ray beamline and end station on the other. Like sample preparation, a macromolecular crystallography beamline is geared to obtaining the best possible diffraction measurements from crystals provided by the synchrotron user. This paper describes the thoughts behind an experiment that fully exploits both the sample and the beamline and how these map into everyday decisions that users can and should make when visiting a beamline with their most precious crystals

  16. Semiconductor X-ray detectors

    Lowe, Barrie Glyn

    2014-01-01

    Identifying and measuring the elemental x-rays released when materials are examined with particles (electrons, protons, alpha particles, etc.) or photons (x-rays and gamma rays) is still considered to be the primary analytical technique for routine and non-destructive materials analysis. The Lithium Drifted Silicon (Si(Li)) X-Ray Detector, with its good resolution and peak to background, pioneered this type of analysis on electron microscopes, x-ray fluorescence instruments, and radioactive source- and accelerator-based excitation systems. Although rapid progress in Silicon Drift Detectors (SDDs), Charge Coupled Devices (CCDs), and Compound Semiconductor Detectors, including renewed interest in alternative materials such as CdZnTe and diamond, has made the Si(Li) X-Ray Detector nearly obsolete, the device serves as a useful benchmark and still is used in special instances where its large, sensitive depth is essential. Semiconductor X-Ray Detectors focuses on the history and development of Si(Li) X-Ray Detect...

  17. X-ray quasars and the X-ray background

    The Einstein X-ray observations of a sample of 202 radio-and optically-selected quasars due to Ku, Helfand and Lucy and to Zamorani et al. are analysed. Correlations between X-ray, optical and radio luminosities are examined. The contribution of radio-loud quasars to the 2-keV X-ray background is estimated using high-frequency radio-source counts, and the contribution due to radio-quiet, optically bright quasars using optical counts. It is shown that radio-loud quasars and radio-quiet optically bright quasars together contribute approximately 15 per cent of the observed 2-keV X-ray background. The contribution of optically faint radio-quiet quasars is uncertain, but may be limited to a maximum of approximately 30 per cent if recent indications of a flattening in optical counts at faint magnitudes are correct. (author)

  18. Accurate macromolecular structures using minimal measurements from X-ray free-electron lasers

    Hattne, Johan; Echols, Nathaniel; Tran, Rosalie; Kern, Jan; Gildea, Richard J.; Brewster, Aaron S.; Alonso-Mori, Roberto; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Lampe, Alyssa; Han, Guangye; Gul, Sheraz

    2014-01-01

    X-ray free-electron laser (XFEL) sources enable the use of crystallography to solve three-dimensional macromolecular structures under native conditions and free from radiation damage. Results to date, however, have been limited by the challenge of deriving accurate Bragg intensities from a heterogeneous population of microcrystals, while at the same time modeling the X-ray spectrum and detector geometry. Here we present a computational approach designed to extract statistically...

  19. X-ray diffraction apparatus

    The invention provides an x-ray diffraction apparatus permitting the rotation of the divergence sit in conjunction with the rotation of the x-ray irradiated specimen, whereby the dimensions of the x-ray irradiated portion of the specimen remain substantially constant during the rotation of the specimen. In a preferred embodiment, the divergence slit is connected to a structural element linked with a second structural element connected to the specimen such that the divergence slit rotates at a lower angular speed than the specimen

  20. X-ray crystal interferometers

    Various configurations of the X-ray crystal interferometer are reviewed. The interferometer applications considered include metrology, the measurement of fundamental physical constants, the study of weakly absorbing phase objects, time-resolved diagnostics, the determination of hard X-ray beam parameters, and the characterization of structural defects in the context of developing an X-ray Michelson interferometer. The three-crystal Laue interferometer (LLL-interferometer), its design, and the experimental opportunities it offers are given particular attention. (instruments and methods of investigation)

  1. Preparation, crystallization and preliminary X-ray diffraction analysis of two intestinal fatty-acid binding proteins in the presence of 11-(dansylamino)undecanoic acid

    Intestinal fatty-acid binding proteins from human and rat have been crystallized in complex with the fluorescent probe 11-(dansylamino)undecanoic acid. Diffraction data for the crystals were collected to 1.8 Å resolution (human) and 1.6 Å resolution (rat). Fatty-acid binding proteins (FABPs) are abundantly expressed proteins that bind a range of lipophilic molecules. They have been implicated in the import and intracellular distribution of their ligands and have been linked with metabolic and inflammatory responses in the cells in which they are expressed. Despite their high sequence identity, human intestinal FABP (hIFABP) and rat intestinal FABP (rIFABP) bind some ligands with different affinities. In order to address the structural basis of this differential binding, diffraction-quality crystals have been obtained of hIFABP and rIFABP in complex with the fluorescent fatty-acid analogue 11-(dansylamino)undecanoic acid

  2. Bone X-Ray (Radiography)

    Full Text Available ... x-ray machine produces a small burst of radiation that passes through the body, recording an image on photographic film or a special detector. Different parts of the body absorb the x- ...

  3. Bone X-Ray (Radiography)

    Full Text Available ... an image on photographic film or a special detector. Different parts of the body absorb the x-rays in varying degrees. Dense bone absorbs much of the radiation while soft tissue, such as muscle, fat and ...

  4. Duodenal X-ray diagnostics

    The publication provides an overview of duodenal X-ray diagnostics with the aid of barium meals in 1362 patients. The introducing paragraphs deal with the topographic anatomy of the region and the methodics of X-ray investigation. The chapter entitled ''processes at the duodenum itself'' describes mainly ulcers, diverticula, congenital anomalies, tumors and inflammations. The neighbourhood processes comprise in the first place diseases having their origin at the pancreas and bile ducts. As a conclusion, endoscopic rectograde cholangio-pancreaticography and percutaneous transhepatic cholangiography are pointed out as advanced X-ray investigation methods. In the annex of X-ray images some of the described phenomena are shown in exemplary manner. (orig./MG)

  5. Bone X-Ray (Radiography)

    Full Text Available ... is commonly used to diagnose fractured bones or joint dislocation. Bone x-rays are the fastest and ... to view and assess bone fractures, injuries and joint abnormalities. This exam requires little to no special ...

  6. Bone X-Ray (Radiography)

    Full Text Available ... like a photographic negative). Today, most images are digital files that are stored electronically. These stored images ... and places the x-ray film holder or digital recording plate under the table in the area ...

  7. Bone X-Ray (Radiography)

    Full Text Available ... the patient lies. A drawer under the table holds the x-ray film or image recording plate . ... when feasible to protect from radiation. You must hold very still and may be asked to keep ...

  8. Bone X-Ray (Radiography)

    Full Text Available ... technologist, an individual specially trained to perform radiology examinations, positions the patient on the x-ray table ... bone is forming), for comparison purposes. When the examination is complete, you may be asked to wait ...

  9. Picosecond x-ray science

    The report discusses the exciting times for short pulse X-rays and the current users of the technology in the United States. Tracking nuclear motions with X-rays transcends scientific disciplines and includes Biology, Materials Science, Condensed Matter and Chemistry. 1 picosecond accesses many phenomena previously hidden at 100ps. Synchrotron advantage over laser plasma and LCLS is that it's easily tunable. There is a large and diverse user community of this technology that is growing rapidly. A working group is being formed to implement 'fast track' Phases 1 and 2 which includes tunable, polarized, monochromatic, focused X-rays; variable pulse length (1 to 100ps) and 1 kHz, 109 X-rays/s with 1% bandwidth. ERL would be a major advance for ultrafast time-resolved studies.

  10. X-ray microtomographic scanners

    Syryamkin, V. I., E-mail: klestov-simon@mail.ru; Klestov, S. A., E-mail: klestov-simon@mail.ru [National Research Tomsk State University, Tomsk, 634050 (Russian Federation)

    2015-11-17

    The article studies the operating procedures of an X-ray microtomographic scanner and the module of reconstruction and analysis 3D-image of a test sample in particular. An algorithm for 3D-image reconstruction based on image shadow projections and mathematical methods of the processing are described. Chapter 1 describes the basic principles of X-ray tomography and general procedures of the device developed. Chapters 2 and 3 are devoted to the problem of resources saving by the system during the X-ray tomography procedure, which is achieved by preprocessing of the initial shadow projections. Preprocessing includes background noise removing from the images, which reduces the amount of shadow projections in general and increases the efficiency of the group shadow projections compression. In conclusion, the main applications of X-ray tomography are presented.

  11. Bone X-Ray (Radiography)

    Full Text Available ... or in bones. top of page How should I prepare? Most bone x-rays require no special ... to 10 minutes. top of page What will I experience during and after the procedure? A bone ...

  12. Bone X-Ray (Radiography)

    Full Text Available ... the body absorb the x-rays in varying degrees. Dense bone absorbs much of the radiation while ... is further reviewed by committees from the American College of Radiology (ACR) and the Radiological Society of ...

  13. Dental X-ray apparatus

    Intra-oral dental X-ray apparatus for panoramic dental radiography is described in detail. It comprises an electron gun having an elongated tubular target carrier extending into the patient's mouth. The carrier supports an inclined target for direction of an X-ray pattern towards a film positioned externally of the patient's mouth. Image definition is improved by a focusing anode which focuses the electron beam into a sharp spot (0.05 to 0.10 mm diameter) on the target. The potential on the focusing anode is adjustable to vary the size of the spot. An X-ray transmitting ceramic (oxides of Be, Al and Si) window is positioned adjacent to the front face of the target. The electron beam can be magnetically deflected to change the X-ray beam direction. (author)

  14. Bone X-Ray (Radiography)

    Full Text Available ... very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures that ... around joints, and in evaluating the hips of children with congenital problems. top of page This page ...

  15. Bone X-Ray (Radiography)

    Full Text Available ... can be taken to the patient in a hospital bed or the emergency room. The x-ray ... and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern ...

  16. Bone X-Ray (Radiography)

    Full Text Available ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and ... in the typical diagnostic range for this exam. Risks There is always a slight chance of cancer ...

  17. Bone X-Ray (Radiography)

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... in a known abnormality can be monitored over time. Follow-up examinations are sometimes the best way ...

  18. X-ray thickness gauge

    New design of X-ray gauge of rolled product thickness is suggested. It is supplied with self-compensation unit, removing the error, caused by changes of half-cycles of supply voltage of radiation source

  19. Bone X-Ray (Radiography)

    Full Text Available ... during x-ray examinations to use the lowest radiation dose possible while producing the best images for evaluation. National and international radiology protection organizations continually review and update the technique standards ...

  20. Bone X-Ray (Radiography)

    Full Text Available ... Leave jewelry at home and wear loose, comfortable clothing. You may be asked to wear a gown. ... appliances, eye glasses and any metal objects or clothing that might interfere with the x-ray images. ...

  1. Bone X-Ray (Radiography)

    Full Text Available ... a large photographic negative). Today, most images are digital files that are stored electronically. These stored images ... and places the x-ray film holder or digital recording plate under the table in the area ...

  2. Bone X-Ray (Radiography)

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... examination may also be necessary so that any change in a known abnormality can be monitored over ...

  3. Bone X-Ray (Radiography)

    Full Text Available ... replacement and fracture reductions. look for injury, infection, arthritis , abnormal bone growths and bony changes seen in ... injuries, including fractures, and joint abnormalities, such as arthritis. X-ray equipment is relatively inexpensive and widely ...

  4. Bone X-Ray (Radiography)

    Full Text Available ... the lowest radiation dose possible while producing the best images for evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern x-ray systems ...

  5. Bone X-Ray (Radiography)

    Full Text Available ... pregnant. Many imaging tests are not performed during pregnancy so as not to expose the fetus to ... See the Safety page for more information about pregnancy and x-rays. top of page What does ...

  6. Bone X-Ray (Radiography)

    Full Text Available ... the patient in a hospital bed or the emergency room. The x-ray tube is connected to ... equipment is relatively inexpensive and widely available in emergency rooms, physician offices, ambulatory care centers, nursing homes ...

  7. Bone X-Ray (Radiography)

    Full Text Available ... the baby. See the Safety page for more information about pregnancy and x-rays. top of page ... procedure varies. See the Safety page for more information about radiation dose. Women should always inform their ...

  8. X-Ray Assembler Data

    U.S. Department of Health & Human Services — Federal regulations require that an assembler who installs one or more certified components of a diagnostic x-ray system submit a report of assembly. This database...

  9. X-ray fluorescence holography

    Hayashi, K; Takahashi, Y

    2003-01-01

    X-ray fluorescence holography (XFH) is a new structural analysis method of determining a 3D atomic arrangement around fluorescing atoms. We developed an XFH apparatus using advanced X-ray techniques and succeeded in obtaining high-quality hologram data. Furthermore, we introduced applications to the structural analysis of a thin film and the environment around dopants and, discussed the quantitative analysis of local lattice distortion. (author)

  10. Accelerator x-ray sources

    Talman, Richard

    2007-01-01

    This first book to cover in-depth the generation of x-rays in particle accelerators focuses on electron beams produced by means of the novel Energy Recovery Linac (ERL) technology. The resulting highly brilliant x-rays are at the centre of this monograph, which continues where other books on the market stop. Written primarily for general, high energy and radiation physicists, the systematic treatment adopted by the work makes it equally suitable as an advanced textbook for young researchers.

  11. Electromechanical x-ray generator

    Watson, Scott A; Platts, David; Sorensen, Eric B

    2016-05-03

    An electro-mechanical x-ray generator configured to obtain high-energy operation with favorable energy-weight scaling. The electro-mechanical x-ray generator may include a pair of capacitor plates. The capacitor plates may be charged to a predefined voltage and may be separated to generate higher voltages on the order of hundreds of kV in the AK gap. The high voltage may be generated in a vacuum tube.

  12. X-ray laser; Roentgenlaser

    Samuelsen, Emil J.; Breiby, Dag W.

    2009-07-01

    X-ray is among the most important research tools today, and has given priceless contributions to all disciplines within the natural sciences. State of the art in this field is called XFEL, X-ray Free Electron Laser, which may be 10 thousand million times stronger than the x-rays at the European Synchrotron Radiation Facility in Grenoble. In addition XFEL has properties that allow the study of processes which previously would have been impossible. Of special interest are depictions on atomic- and molecular level by the use of x-ray holographic methods, and being able to study chemical reactions in nature's own timescale, the femtosecond. Conclusion: The construction of x-ray lasers is a natural development in a scientific field which has an enormous influence on the surrounding society. While the discovery of x-ray was an important breakthrough in itself, new applications appear one after the other: Medical depiction, dissemination, diffraction, DNA and protein structures, synchrotron radiation and tomography. There is reason to believe that XFEL implies a technological leap as big as the synchrotrons some decades ago. As we are now talking about studies of femtosecond and direct depiction of chemical reactions, it is obvious that we are dealing with a revolution to come, with extensive consequences, both scientifically and culturally. (EW)

  13. X-ray diagnostic apparatus

    A falling load type X-ray diagnostic apparatus comprises a low voltage power source, AC-DC converting means connected to the low voltage power source so as to apply a rectified low DC voltage, chopping means connected to the AC-DC converting means and chopping said DC voltage into a low AC voltage, high voltage applying means for transforming said low AC voltage into a high AC voltage, said high AC voltage being applied as a tube voltage to an X-ray tube from which X-rays are irradiated toward an object to be examined, means for controlling a filament heating power of the X-ray tube, programming means for supplying a control signal to said filament heating control means so as to reduce the emission current of said X-ray tube during the irradiation, and chopper control means for controlling the chopping ratio of said chopping means by evaluating said rectified DC voltage with a preset tube voltage generated in said programming means, said programming means compensating said tube voltage by receiving said control signal in such a manner that said tube voltage is maintained substantially constant during the irradiation by varying said preset tube voltage so as to control the chopping ratio based upon the reduction of the filament heating power for the X-ray tube

  14. Low energy (soft) x rays

    Dosimetry of low-energy (soft) X rays produced by the SOFTEX Model CMBW-2 was performed using Nuclear Associates Type 30 - 330 PTW, Exradin Type A2, and Shonka-Wyckoff ionization chambers with a Keithley Model 602 electrometer. Thermoluminescent (BeO chip) dosimeters were used with a Harshaw Detector 2000-A and Picoammeter-B readout system. Beam quality measurements were made using aluminum absorbers; exposure rates were assessed by the current of the X-ray tube and by exposure times. Dose distributions were established, and the average factors for non-uniformity were calculated. The means of obtaining accurate absorbed and exposed doses using these methods are discussed. Survival of V79 cells was assessed by irradiating them with soft X rays, 200 kVp X rays, and 60Co gamma rays. The relative biological effectiveness (RBE) values for soft X rays with 0, 0.2, 0.7 mm added thicknesses of aluminum were 1.6, which were compared to 60Co. The RBE of 200 kVp X rays relative to 60Co was 1.3. Results of this study are available for reference in future RERF studies of cell survival. (author)

  15. Tokamak x ray diagnostic instrumentation

    Three classes of x-ray diagnostic instruments enable measurement of a variety of tokamak physics parameters from different features of the x-ray emission spectrum. (1) The soft x-ray (1 to 50 keV) pulse-height-analysis (PHA) diagnostic measures impurity concentrations from characteristic line intensities and the continuum enhancement, and measures the electron temperature from the continuum slope. (2) The Bragg x-ray crystal spectrometer (XCS) measures the ion temperature and neutral-beam-induced toroidal rotation velocity from the Doppler broadening and wavelength shift, respectively, of spectral lines of medium-Z impurity ions. Impurity charge state distributions, precise wavelengths, and inner-shell excitation and recombination rates can also be studied. X rays are diffracted and focused by a bent crystal onto a position-sensitive detector. The spectral resolving power E/ΔE is greater than 104 and time resolution is 10 ms. (3) The x-ray imaging system (XIS) measures the spatial structure of rapid fluctuations (0.1 to 100 kHZ) providing information on MHD phenomena, impurity transport rates, toroidal rotation velocity, plasma position, and the electron temperature profile. It uses an array of silicon surface-barrier diodes which view different chords of the plasma through a common slot aperture and operate in current (as opposed to counting) mode. The effectiveness of shields to protect detectors from fusion-neutron radiation effects has been studied both theoretically and experimentally

  16. Neutron protein crystallography

    Niimura, Nobuo [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    1998-10-01

    X-ray diffraction of single crystal has enriched the knowledge of various biological molecules such as proteins, DNA, t-RNA, viruses, etc. It is difficult to make structural analysis of hydrogen atoms in a protein using X-ray crystallography, whereas neutron diffraction seems usable to directly determine the location of those hydrogen atoms. Here, neutron diffraction method was applied to structural analysis of hen egg-white lysozyme. Since the crystal size of a protein to analyze is generally small (5 mm{sup 3} at most), the neutron beam at the sample position in monochromator system was set to less than 5 x 5 mm{sup 2} and beam divergence to 0.4 degree or less. Neutron imaging plate with {sup 6}Li or Gd mixed with photostimulated luminescence material was used and about 2500 Bragg reflections were recorded in one crystal setting. A total of 38278 reflections for 2.0 A resolution were collected in less than 10 days. Thus, stereo views of Trp-111 omit map around the indol ring of Trp-111 was presented and the three-dimensional arrangement of 696H and 264D atoms in the lysozyme molecules was determined using the omit map. (M.N.)

  17. Center for X-Ray Optics, 1992

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors

  18. Multigrain crystallography

    Sørensen, Henning Osholm; Schmidt, Søren; Wright, Jonathan P.;

    2012-01-01

    We summarize exploratory work on multigrain crystallography. The experimental arrangement comprises a monochromatic beam, a fully illuminated sample with up to several hundred grains in transmission geometry on a rotary table and a 2D detector. Novel algorithms are presented for indexing, integra......We summarize exploratory work on multigrain crystallography. The experimental arrangement comprises a monochromatic beam, a fully illuminated sample with up to several hundred grains in transmission geometry on a rotary table and a 2D detector. Novel algorithms are presented for indexing...... simultaneous characterization of the 3D atomic, and 3D grain-scale structure of polycrystalline specimens with phases of unknown composition and structure....

  19. The Coherent X-ray Imaging instrument at the Linac Coherent Light Source

    Description of the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source. Recent scientific highlights illustrate the femtosecond crystallography, high power density and extreme matter capabilities of the CXI instrument. The Coherent X-ray Imaging (CXI) instrument specializes in hard X-ray, in-vacuum, high power density experiments in all areas of science. Two main sample chambers, one containing a 100 nm focus and one a 1 µm focus, are available, each with multiple diagnostics, sample injection, pump–probe and detector capabilities. The flexibility of CXI has enabled it to host a diverse range of experiments, from biological to extreme matter

  20. The Coherent X-ray Imaging instrument at the Linac Coherent Light Source

    Liang, Mengning; Williams, Garth J.; Messerschmidt, Marc; Seibert, M. Marvin; Montanez, Paul A.; Hayes, Matt; Milathianaki, Despina; Aquila, Andrew; Hunter, Mark S.; Koglin, Jason E.; Schafer, Donald W.; Guillet, Serge; Busse, Armin; Bergan, Robert; Olson, William; Fox, Kay; Stewart, Nathaniel; Curtis, Robin; Miahnahri, Alireza Alan; Boutet, Sébastien, E-mail: sboutet@slac.stanford.edu [Linac Coherent Light Source, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States)

    2015-04-15

    Description of the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source. Recent scientific highlights illustrate the femtosecond crystallography, high power density and extreme matter capabilities of the CXI instrument. The Coherent X-ray Imaging (CXI) instrument specializes in hard X-ray, in-vacuum, high power density experiments in all areas of science. Two main sample chambers, one containing a 100 nm focus and one a 1 µm focus, are available, each with multiple diagnostics, sample injection, pump–probe and detector capabilities. The flexibility of CXI has enabled it to host a diverse range of experiments, from biological to extreme matter.

  1. Structure determination of drug target proteins by neutron crystallography

    High resolution X-ray crystallography provides information for most of the atoms comprising the proteins, with the exception of hydrogen atoms. Whereas, neutron crystallography, which is a powerful technique for locating hydrogen atoms, enables us to obtain accurate atomic positions within proteins. Neutron diffraction data can provide information of the location of hydrogen atoms to the structural information determined by X-ray crystallography. Here, we show the recent results of the structural determination of drug-target proteins, porcine pancreatic elastase and human immuno-deficiency virus type-1 protease by both X-ray and neutron diffraction. The structure of porcine pancreatic elastase with its potent inhibitor was determined to 0.094 nm resolution by X-ray diffraction and 0.165 nm resolution by neutron diffraction. The structure of HIV-PR with its potent inhibitor was also determined to 0.093 nm resolution by X-ray diffraction and 0.19 nm resolution by neutron diffraction. The ionization state and the location of hydrogen atoms of the catalytic residue in these enzymes were determined by neutron diffraction. Furthermore, collaborative use of both X-ray and neutron crystallography to identify the location of ambiguous hydrogen atoms will be shown. (author)

  2. Eye formation in semi-hard cheese: X-ray computed tomography as a non-invasive tool for assessing the influence of adjunct lactic acid bacteria

    Guggisberg, Dominik; Fröhlich-Wyder, Marie-Therese; Irmler, Stefan; Greco, Mark; Wechsler, Daniel; Schuetz, Philipp

    2013-01-01

    Eye formation is an important feature for various cheese varieties. This study firstly aimed to evaluate the potential of X-ray computed tomography (CT) and image analysis software as a non-invasive method to quantify cheese eye volume. The quantification of the eye volume by CT was validated with 12 eyeless hard cheeses made with the inclusion of 0–100 hollow PP balls (Ø = 10 or 20 mm). The results obtained for the total volume of the ‘artificial eyes’ showed a good correlation with the volu...

  3. Selenium-Assisted Nucleic Acid Crystallography: Use of Phosphoroselenoates for MAD Phasing of a DNA Structure

    The combination of synchrotron radiation and a variety of atoms or ions (either covalently attached to the biomolecule prior to crystallization or soaked into crystals) that serve as anomalous scatterers constitutes a powerful tool in the X-ray crystallographer's repertoire of structure determination techniques. Phosphoroselenoates in which one of the nonbridging phosphate oxygens in the backbone is replaced by selenium offer a simplified means for introducing an anomalous scatterer into oligonucleotides by conventional solid-phase synthesis. Unlike other methods that are used to derivatize DNA or RNA by covalent attachment of a heavy atom (i.e., bromine at the C5 position of pyrimidines), tedious synthesis of specialized nucleosides is not required. Introduction of selenium is readily accomplished in solid-phase oligonucleotide synthesis by replacing the standard oxidation agent with a solution of potassium selenocyanide. This results in a diastereomeric mixture of phosphoroselenoates that can be separated by strong anion-exchange HPLC. As a test case, all 10 DNA hexamers of the sequence CGCGCG containing a single phosphoroselenoate linkage (PSe) were prepared. Crystals were grown for a subset of them, and the structure of (d(CPSeGCGCG))2 was determined by the multiwavelength anomalous dispersion technique and refined to 1.1 (angstrom) resolution.

  4. X-ray Echo Spectroscopy

    Shvyd'ko, Yuri

    2016-02-01

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >108 ) with broadband ≃5 - 13 meV dispersing systems are introduced featuring more than 103 signal enhancement. The technique is general, applicable in different photon frequency domains.

  5. X-ray echo spectroscopy

    Shvyd'ko, Yuri

    2015-01-01

    X-ray echo spectroscopy, a counterpart of neutron spin-echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a point-like x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x-rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1--0.02-meV ultra-high-resolution IXS applications (resolving power $> 10^8$) with broadband $\\simeq$~5--13~meV dispersing systems are introduced featuring more than $10^3$ signal e...

  6. Dental X-ray apparatus

    Intra-oral X-ray apparatus which reduces the number of exposures necessary to obtain panoramic dental radiographs is described in detail. It comprises an electron gun, a tubular target carrier projecting from the gun along the beam axis and carrying at its distal end a target surrounded by a shield of X-ray opaque material. This shield extends forward and laterally of the target and has surfaces which define a wedge or cone-shaped radiation pattern delimited vertically by the root tips of the patient's teeth. A film holder is located externally of the patient's mouth. A disposable member can fit on the target carrier to depress the patient's tongue out of the radiation pattern and to further shield the roof of the mouth. The electron beam can be magnetically deflected to change the X-ray beam direction. (author)

  7. Extragalactic X-ray sources

    About 40% of the X-ray sources in the third UHURU catalogue are extragalactic. One, SMC X-1 has been identified with a binary star in the lesser Magellanic Cloud, while five sources, three probably binary stars, have been found in the greater Magellanic Cloud. X-ray sources in normal galaxies (M31), radiogalaxies (NGC5128), Seyfert galaxies (NGC4151), quasars (3C273) and galaxy clusters (Virgo X-1 and Perseus X-1) are briefly discussed. The most probable explanation for the origin of X-ray emissions from galaxy clusters appears at present to be that the cluster is filled with a thin, very hot gas which emits X-radiation by thermal bremsstrahlung. The main alternative is a socalled inverse Compton effect. (JIW)

  8. Role of deoxyribonucleic acid polymerases and deoxyribonucleic acid ligase in x-ray-induced repair synthesis in toluene-treated Escherichia coli K-12

    Toluene-treated Escherichia coli mutants have been used to study the roles of deoxyribonucleic acid (DNA) polymerases I, II, and III, and of DNA ligase in repair synthesis and strand rejoining following x irradiation. In cells possessing all three DNA polymerases, both a greater amount of repair synthesis (''exaggerated'' repair synthesis) and failure of ligation are observed when DNA ligase activity is inhibited. In a mutant lacking the polymerizing activity of DNA polymerase I, exaggerated repair synthesis is not observed, and strand rejoining does not occur even if DNA ligase is fully activated. In a mutant possessing the polymerizing activity of DNA polymerase I but lacking its 5' → 3' exonuclease activity, exaggerated repair synthesis is minimal. After irradiation, DNA polymerases II and III are capable of carrying out an adenosine 5'-triphosphate-dependent repair synthesis, but rejoining of strand breaks does not occur and exaggerated synthesis is not seen whether DNA ligase is active or not. These results suggest that DNA polymerase I and DNA ligase act together to limit repair synthesis after x irradiation and that both are necessary in toluene-treated cells for strand rejoining. DNA polymerases II and III apparently cannot complete chain elongation and gap filling, and therefore repair carried out by these enzymes does not respond to ligase action

  9. Role of deoxyribonucleic acid polymerases and deoxyribonucleic acid ligase in x-ray-induced repair synthesis in toluene-treated Escherichia coli K-12

    Toluene-treated Escherichia coli mutants have been used to study the roles of deoxyribonucleic acid (DNA) polymerases I, II, and III, and of DNA ligase in repair synthesis and strand rejoining following X-irradiation. In cells possessing all three DNA polymerases, both a greater amount of repair synthesis (''exaggerated'' repair synthesis) and failure of ligation are observed when DNA ligase activity is inhibited. In a mutant lacking the polymerizing activity of DNA polymerase I, exaggerated repair synthesis is not observed, and strand rejoining does not occur even if DNA ligase is fully activated. In a mutant possessing the polymerizing activity of DNA polymerase I but lacking its 5' → 3' exonuclease activity, exaggerated repair synthesis is minimal. After irradiation, DNA polymerases II and III are capable of carrying out an adenosine 5'-triphosphate-dependent repair synthesis, but rejoining of strand breaks does not occur and exaggerated synthesis is not seen whether DNA ligase is active or not. These results suggest that DNA polymerase I and DNA ligase act together to limit repair synthesis after X irradiation and that both are necessary in toluene-treated cells for strand rejoining. DNA polymerases II and III apparently cannot complete chain elongation and gap filling, and therefore repair carried out by these enzymes does not respond to ligase action

  10. Towards phasing using high X-ray intensity

    X-ray free-electron lasers (XFELs) show great promise for macromolecular structure determination from sub-micrometre-sized crystals, using the emerging method of serial femtosecond crystallography. The extreme brightness of the XFEL radiation can multiply ionize most, if not all, atoms in a protein, causing their scattering factors to change during the pulse, with a preferential 'bleaching' of heavy atoms. This paper investigates the effects of electronic damage on experimental data collected from a Gd derivative of lysozyme microcrystals at different X-ray intensities, and the degree of ionization of Gd atoms is quantified from phased difference Fourier maps. In conclusion, a pattern sorting scheme is proposed to maximize the ionization contrast and the way in which the local electronic damage can be used for a new experimental phasing method is discussed

  11. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    Robert M. Lawrence

    2015-07-01

    Full Text Available Serial femtosecond crystallography (SFX using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ∼700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ∼40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is an important step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  12. Microbeam X-ray analysis in Poland - past and future

    The article provides an overview of the development of electron beam X-ray microanalysis (EPMA) in Poland. Since the introduction by Prof. Bojarski of EMPA over 45 years ago, tremendous advances in methodologies and in instrumentation have been made in order to improve the precision of quantitative compositional analysis, spatial resolution and analytical sensitivity. This was possible due to the activity of Applied Crystallography Committee at the Polish Academy of Sciences, as well as the groups of researches working in the Institute for Ferrous Metallurgy (Gliwice), the Technical University of Warsaw, the Silesian Technical University (Katowice), the AGH-University of Sciences and Technology (Krakow), and the Institute of Materials Science and Metallurgy Polish Academy of Sciences (Krakow). Based on the research examples realized by these teams, conferences, seminars and congresses organized, as well as books and academic textbooks issued, the evolution of electron beam X-ray microanalysis in Poland is demonstrated.

  13. Towards phasing using high X-ray intensity

    Galli, Lorenzo; Son, Sang-Kil; Barends, Thomas R. M.; White, Thomas A.; Barty, Anton; Botha, Sabine; Boutet, Sébastien; Caleman, Carl; Doak, R. Bruce; Nanao, Max H.; Nass, Karol; Shoeman, Robert L.; Timneanu, Nicusor; Santra, Robin; Schlichting, Ilme; Chapman, Henry N.

    2015-09-30

    X-ray free-electron lasers (XFELs) show great promise for macromolecular structure determination from sub-micrometre-sized crystals, using the emerging method of serial femtosecond crystallography. The extreme brightness of the XFEL radiation can multiply ionize most, if not all, atoms in a protein, causing their scattering factors to change during the pulse, with a preferential `bleaching' of heavy atoms. This paper investigates the effects of electronic damage on experimental data collected from a Gd derivative of lysozyme microcrystals at different X-ray intensities, and the degree of ionization of Gd atoms is quantified from phased difference Fourier maps. A pattern sorting scheme is proposed to maximize the ionization contrast and the way in which the local electronic damage can be used for a new experimental phasing method is discussed.

  14. X-ray imaging: Perovskites target X-ray detection

    Heiss, Wolfgang; Brabec, Christoph

    2016-05-01

    Single crystals of perovskites are currently of interest to help fathom fundamental physical parameters limiting the performance of perovskite-based polycrystalline solar cells. Now, such perovskites offer a technology platform for optoelectronic devices, such as cheap and sensitive X-ray detectors.

  15. An Exercise in X-Ray Diffraction Using the Polymorphic Transition of Nickel Chromite.

    Chipman, David W.

    1980-01-01

    Describes a laboratory experiment appropriate for a course in either x-ray crystallography or mineralogy. The experiment permits the direct observation of a polymorphic transition in nickel chromite without the use of a special heating stage or heating camera. (Author/GS)

  16. Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

    Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; Kick, Leonhard M.; Gati, Cornelius; Nelson, Garrett; Deupi, Xavier; Standfuss, Jörg; Schertler, Gebhard; Panneels, Valérie, E-mail: valerie.panneels@psi.ch [Paul Scherrer Institute, OFLC/103, 5232 Villigen-PSI (Switzerland)

    2015-06-27

    A new batch preparation method is presented for high-density micrometre-sized crystals of the G protein-coupled receptor rhodopsin for use in time-resolved serial femtosecond crystallography at an X-ray free-electron laser using a liquid jet. Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.

  17. Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

    A new batch preparation method is presented for high-density micrometre-sized crystals of the G protein-coupled receptor rhodopsin for use in time-resolved serial femtosecond crystallography at an X-ray free-electron laser using a liquid jet. Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup

  18. Simultaneous X-ray diffraction from multiple single crystals of macromolecules

    Paithankar, Karthik S.; Sørensen, Henning Osholm; Wright, Jonathan P.;

    2011-01-01

    The potential in macromolecular crystallography for using multiple crystals to collect X-ray diffraction data simultaneously from assemblies of up to seven crystals is explored. The basic features of the algorithms used to extract data and their practical implementation are described. The procedure...

  19. X-ray hot plasma diagnostics

    X-ray plasma emission study is powerful diagnostic tool of hot plasmas. In this review article the main techniques of X-ray plasma emission measurement are shortly presented: X-ray spectrometry using absorbent filters, crystal and grating spectrometers, imaging techniques using pinhole cameras, X-ray microscopes and Fresnel zone plate cameras, X-ray plasma emission calorimetry. Advances in these techniques with examples for different hot plasma devices are also presentes. (author)

  20. The effects of X-ray irradiation on the induction of α-amylase synthesis by gibberelic acid in the aleurone system of barley

    The influence of ionizing radiation on a system without DNA replication and cell division was investigated with the aid of GA3-induced α-amylase synthesis in aleurone cells of barley. The reaction of the system was determined by dose effect curves (after irradiation of one half of the endosperms in rest) for the synthesis and secretion of α-amylase, protein, and reducing sugars. The system proves to be highly radiation-resistant. The course of the synthesis of α-amylase after X-ray irradiation with varying doses during enzyme synthesis suggests that transcription occurs in the middle of the lag-phase and is the most sensitive stage in enzyme synthesis, while translation alone is less sensitive to radiation. (BSC/AK)

  1. (R,R-Tartaric Acid Dimethyl Diester from X-Ray and Ab Initio Studies: Factors Influencing Its Conformation and Packing

    J. Rychlewski

    1997-07-01

    Full Text Available The conformation of dimethyl (R,R-tartrate has been analyzed on the basis of the single crystal X-ray diffraction method as well as by ab-initio quantum chemical studies. The results showed that the extended T conformation containing two planar hydroxyester moieties predominates in both ab-initio and X-ray studies. The lowest energy conformer in ab-initio calculations has C2 symmetry and hydrogen bonds between a hydroxyl group and the nearest carbonyl oxygen. The second in energetical sequence, with an energy difference of only 1.2 kcal/mol, is the asymmetrical conformer, which differs from the lowest energy form by the rotation of one of the ester groups by 180°. Intramolecular OH...O hydrogen bonds observed in this rotamer again involve only proximal functional groups. This conformer is present in the crystal structure of the studied compound, although its conformation in the solid state is no longer stabilized by intramolecular hydrogen bonds of the type mentioned above. In the crystal, hydroxyl groups are mostly involved in intermolecular hydrogen bonds and form only a weak intramolecular hydrogen bond with each other. The planar arrangement of the α-hydroxyester moieties combined with the extended conformation of the carbon chain seems to be stabilized by the intramolecular hydrogen bonds between neighboring functional groups and by the long range dipole-dipole interactions between two pairs of CO and (βC-H bonds.

  2. Microscale X-ray Absorption Spectroscopy on the GSECARS Sector 13 at the APS

    Stephen-Sutto

    2000-01-01

    GeoSoilEnviroCARS (GSECARS) is a national user facility for frontier research in the earth sciences using synchrotrons radiation at the Advanced Photon Source, Argonne National Laboratory. GSECARS provides earth scientists with access to the high-brilliance hard x-rays from this third-generation synchrotrons light source. The research conducted at this facility will advance our knowledge of the composition, structure and properties of earth materials, the processes they control and the processes that produce them. All principal synchrotron-based analytical techniques in demand by earth scientists are being brought to bear on earth science problems: (1) high-pressure/high-temperature crystallography and spectroscopy using the diamond anvil cell; (2) high-pressure/high-temperature crystallography using the large-volume press; (3) powder, single crystal and interface diffraction; (4) x-ray absorption fine structure (XAFS) spectroscopy; (5) x-ray fluorescence microprobe analysis and microspectroscopy; and (6) mic...

  3. Bone X-Ray (Radiography)

    Full Text Available ... exam requires little to no special preparation. Tell your doctor and the technologist if there is any possibility you are pregnant. Leave jewelry at home and wear loose, comfortable clothing. You may be asked to wear a gown. What is Bone X-ray (Radiography)? What are some ...

  4. X-ray image converters

    The invention pertains to rare earth phosphor admixtures utilizing thulium-activated lanthanum or gadolinium oxyhalide phosphor material. These materials increase the relative speed and resolution of an X-ray image compared with conventional phosphors as well as reducing the still serious crossover problem now experienced with conventional phosphors. (Auth.)

  5. Bone X-Ray (Radiography)

    Full Text Available ... Images related to X-ray (Radiography) - Bone About this Site RadiologyInfo.org is produced by: Please note ... you can search the ACR-accredited facilities database . This website does not provide cost information. The costs ...

  6. Bone X-Ray (Radiography)

    Full Text Available ... Safety En Español More Info Images/Videos News Physician Resources Professions Site Index A-Z X-ray ( ... are the fastest and easiest way for your doctor to view and assess bone fractures, injuries and ...

  7. X-Ray Diffractive Optics

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

    X-ray optics were fabricated with the capability of imaging solar x-ray sources with better than 0.1 arcsecond angular resolution, over an order of magnitude finer than is currently possible. Such images would provide a new window into the little-understood energy release and particle acceleration regions in solar flares. They constitute one of the most promising ways to probe these regions in the solar atmosphere with the sensitivity and angular resolution needed to better understand the physical processes involved. A circular slit structure with widths as fine as 0.85 micron etched in a silicon wafer 8 microns thick forms a phase zone plate version of a Fresnel lens capable of focusing approx. =.6 keV x-rays. The focal length of the 3-cm diameter lenses is 100 microns, and the angular resolution capability is better than 0.1 arcsecond. Such phase zone plates were fabricated in Goddard fs Detector Development Lab. (DDL) and tested at the Goddard 600-microns x-ray test facility. The test data verified that the desired angular resolution and throughput efficiency were achieved.

  8. X-ray diagnostic equipment

    Lateral and orbital scanning movements can be carried out with the equipment. The assessment is carried out by a computer. Differences in sensitivity of the detectors can be compensated for by displacement of the electron beam of the X-ray tube compared to the anti-cathode or by bending of the electron beam by electromagnetic coils. (RW)

  9. X-ray fluorescence spectrometry

    The seventh edition of Philips' Review of Literature on x-ray fluorescence spectrometry starts with a list of conference proceedings on the subject, organised by the Philips organisation at regular intervals in various European countries. It is followed by a list of bulletins. The bibliography is subdivided according to spectra, equipment, applications and absorption analysis

  10. X-ray film processing

    X-ray films have to be highly sensitive, for radiation protection reasons. The films used in radiology are coated on both sides with a photosensitive emulsion. This applies to all dental films. Their properties and the development of the different exposed films are explained. (DG)

  11. X-ray backscatter imaging

    Dinca, Dan-Cristian; Schubert, Jeffrey R.; Callerame, J.

    2008-04-01

    In contrast to transmission X-ray imaging systems where inspected objects must pass between source and detector, Compton backscatter imaging allows both the illuminating source as well as the X-ray detector to be on the same side of the target object, enabling the inspection to occur rapidly and in a wide variety of space-constrained situations. A Compton backscatter image is similar to a photograph of the contents of a closed container, taken through the container walls, and highlights low atomic number materials such as explosives, drugs, and alcohol, which appear as especially bright objects by virtue of their scattering characteristics. Techniques for producing X-ray images based on Compton scattering will be discussed, along with examples of how these systems are used for both novel security applications and for the detection of contraband materials at ports and borders. Differences between transmission and backscatter images will also be highlighted. In addition, tradeoffs between Compton backscatter image quality and scan speed, effective penetration, and X-ray source specifications will be discussed.

  12. Bone X-Ray (Radiography)

    Full Text Available Toggle navigation Test/Treatment Patient Type Screening/Wellness Disease/Condition Safety En Español More Info Images/Videos News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone ...

  13. Bone X-Ray (Radiography)

    Full Text Available ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... cancer from excessive exposure to radiation. However, the benefit of an accurate diagnosis far outweighs the risk. The effective radiation dose for this procedure varies. ...

  14. Bone X-Ray (Radiography)

    Full Text Available ... over time. top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... cancer from excessive exposure to radiation. However, the benefit of an accurate diagnosis far outweighs the risk. ...

  15. Bone X-Ray (Radiography)

    Full Text Available ... over time. top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology ...

  16. Bone X-Ray (Radiography)

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... benefit of an accurate diagnosis far outweighs the risk. The effective ... more information about radiation dose. Women should always inform their ...

  17. Bone X-Ray (Radiography)

    Full Text Available Toggle navigation Test/Treatment Patient Type Screening/Wellness Disease/Condition Safety En Español More Info Images/Videos ... to current x-ray images for diagnosis and disease management. top of page How is the procedure ...

  18. Bone X-Ray (Radiography)

    Full Text Available ... for more information about pregnancy and x-rays. A Word About Minimizing Radiation Exposure Special care is ... encourage linking to this site. × Recommend RadiologyInfo to a friend Send to (friend's e-mail address): From ( ...

  19. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    de Groot, F. M. F.

    2001-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption process. Section II discusses 1s X-ray absorption, i.e., the K edges, and section III deals with 2p X-ray absorption, the L edges. X-ray emission is discussed in, respectively, the L edges. X-ray emis...

  20. X-ray crystallographic characterization of an adenine-cadmium (II) complex, di-. mu. -adeninium-di-. mu. -aquo-tetrakis(nitrato-0,0')dicadmium(II) dinitrate, containing a cationic nuclei acid base as a bidentate ligand

    Wei, C.H.; Jacobson, K.B.

    1981-02-01

    The reaction of the monosodium salt of adenosine-5'-monophosphoric acid with cadmium nitrate in the presence of nitric acid has resulted in the formation of a binuclear cadmium complex of adenine, ((C/sub 5/H/sub 6/N/sub 5/)Cd(NO/sub 3/)/sub 2/.H/sub 2/O)/sub 2/(NO/sub 3/)/sub 2/. The crystal structure of this complex has been characterized by single-crystal x-ray analysis based on counter data collected with an automated diffractometer. The crystals contain one centrosymmetric dimer in a reduced triclinic cell of symmetry P anti 1 and of dimensions a = 7.595 (2) A, b = 9.539 (5) A, c = 10.527 (5) A, ..cap alpha.. = 101.37 (3)/sup 0/, ..beta.. = 108.69 (3)/sup 0/, and ..gamma.. = 107.42 (3)/sup 0/.

  1. The success story of crystallography.

    Schwarzenbach, Dieter

    2012-01-01

    Diffractionists usually place the birth of crystallography in 1912 with the first X-ray diffraction experiment of Friedrich, Knipping and Laue. This discovery propelled the mathematical branch of mineralogy to global importance and enabled crystal structure determination. Knowledge of the geometrical structure of matter at atomic resolution had revolutionary consequences for all branches of the natural sciences: physics, chemistry, biology, earth sciences and material science. It is scarcely possible for a single person in a single article to trace and appropriately value all of these developments. This article presents the limited, subjective view of its author and a limited selection of references. The bulk of the article covers the history of X-ray structure determination from the NaCl structure to aperiodic structures and macromolecular structures. The theoretical foundations were available by 1920. The subsequent success of crystallography was then due to the development of diffraction equipment, the theory of the solution of the phase problem, symmetry theory and computers. The many structures becoming known called for the development of crystal chemistry and of data banks. Diffuse scattering from disordered structures without and with partial long-range order allows determination of short-range order. Neutron and electron scattering and diffraction are also mentioned. PMID:22186283

  2. Center for X-Ray Optics, 1986

    The Center for X-Ray Optics has made substantial progress during the past year on the development of very high resolution x-ray technologies, the generation of coherent radiation at x-ray wavelengths, and, based on these new developments, had embarked on several scientific investigations that would not otherwise have been possible. The investigations covered in this report are topics on x-ray sources, x-ray imaging and applications, soft x-ray spectroscopy, synchrotron radiation, advanced light source and magnet structures for undulators and wigglers

  3. One pot synthesis, molecular structure and spectroscopic studies (X-ray, IR, NMR, UV-Vis) of novel 2-(4,6-dimethoxy-1,3,5-triazin-2-yl) amino acid ester derivatives

    El-Faham, Ayman; Soliman, Saied M.; Osman, Sameh M.; Ghabbour, Hazem A.; Siddiqui, Mohammed R. H.; Fun, Hoong-Kun; Albericio, Fernando

    2016-04-01

    Novel series of 2-(4,6-dimethoxy,1,3,5-triazin-2-yl) amino acid ester derivatives were synthesized using simple one pot method in methanol. The products were obtained in high yields and purities as observed from their spectral data, elemental analyses, GC-MS and X-ray crystallographic analysis. The B3LYP/6-311G(d,p) calculated molecular structures are well correlated with the geometrical parameters obtained from the X-ray analyses. The spectroscopic properties such as IR vibrational modes, NMR chemical shifts and UV-Vis electronic transitions were discussed both experimentally and theoretically. The IR vibrational frequencies showed good correlations with the experimental data (R2 = 0.9961-0.9995). The electronic spectra were assigned based on the TD-DFT results. Intense electronic transition band is calculated at 198.1 nm (f = 0.1389), 204.2 nm (f = 0.2053), 205.0 (f = 0.1704) and 205.7 (0.2971) for compounds 6a-i, respectively. The molecular orbital energy levels contributed in the longest wavelength transition band were explained. For all compounds, the experimental wavelengths showed red shifts compared to the calculations due to the solvent effect. The NMR chemical shifts were calculated using GIAO method. The NBO analyses were performed to predict the stabilization energies due to the electron delocalization processes occur in the studied systems.

  4. One pot synthesis, molecular structure and spectroscopic studies (X-ray, IR, NMR, UV-Vis) of novel 2-(4,6-dimethoxy-1,3,5-triazin-2-yl) amino acid ester derivatives.

    El-Faham, Ayman; Soliman, Saied M; Osman, Sameh M; Ghabbour, Hazem A; Siddiqui, Mohammed R H; Fun, Hoong-Kun; Albericio, Fernando

    2016-04-15

    Novel series of 2-(4,6-dimethoxy,1,3,5-triazin-2-yl) amino acid ester derivatives were synthesized using simple one pot method in methanol. The products were obtained in high yields and purities as observed from their spectral data, elemental analyses, GC-MS and X-ray crystallographic analysis. The B3LYP/6-311G(d,p) calculated molecular structures are well correlated with the geometrical parameters obtained from the X-ray analyses. The spectroscopic properties such as IR vibrational modes, NMR chemical shifts and UV-Vis electronic transitions were discussed both experimentally and theoretically. The IR vibrational frequencies showed good correlations with the experimental data (R(2)=0.9961-0.9995). The electronic spectra were assigned based on the TD-DFT results. Intense electronic transition band is calculated at 198.1 nm (f=0.1389), 204.2 nm (f=0.2053), 205.0 (f=0.1704) and 205.7 (0.2971) for compounds 6a-i, respectively. The molecular orbital energy levels contributed in the longest wavelength transition band were explained. For all compounds, the experimental wavelengths showed red shifts compared to the calculations due to the solvent effect. The NMR chemical shifts were calculated using GIAO method. The NBO analyses were performed to predict the stabilization energies due to the electron delocalization processes occur in the studied systems. PMID:26845586

  5. Probing the surface microstructure of layer-by-layer self-assembly chitosan/poly(l-glutamic acid) multilayers: A grazing-incidence small-angle X-ray scattering study.

    Zhao, Nie; Yang, Chunming; Wang, Yuzhu; Zhao, Binyu; Bian, Fenggang; Li, Xiuhong; Wang, Jie

    2016-01-01

    This study characterized the surface structure of layer-by-layer self-assembly chitosan/poly(L-glutamic acid) multilayers through grazing-incidence small-angle X-ray scattering (GISAXS), X-ray reflectivity (XRR), and atomic force microscopy (AFM). A weakly long-period ordered structure along the in-plane direction was firstly observed in the polyelectrolyte multilayer by the GISAXS technique. This structure can be attributed to the specific domains on the film surface. In the domain, nanodroplets that were formed by polyelectrolyte molecules were orderly arranged along the free surface of the films. This ordered structure gradually disappeared with the increasing bilayer number because of the complex merging behavior of nanodroplets into large islands. Furthermore, resonant diffuse scattering became evident in the GISAXS patterns as the number of bilayers in the polyelectrolyte multilayer was increased. Notably, the lateral cutoff length of resonant diffuse scattering for these polyelectrolyte films was comparable with the long-period value of the ordered nanodroplets in the polyelectrolyte multilayer. Therefore, the nanodroplets could be considered as a basic transmission unit for structure propagation from the inner interface to the film surface. It suggests that the surface structure with length scale larger than the size of nanodroplets was partially complicated from the interface structure near the substrate, but surface structure smaller than the cutoff length was mainly depended on the conformation of nanodroplets. PMID:26478320

  6. True mechanical behavior and the associated structure morphology of poly(lactic acid) polymer in strain induced crystallization by in-situ time resolved X-ray diffraction and scattering technique

    Changes in molecular structure configuration during strain induced crystallisation of an amorphous Poly(Lactic Acid) (PLA 4032D) polymer was monitored in-situ by simultaneously recording the wide angle x-ray scattering (WAXS) and small angle x-ray scattering (SAXS) patterns together with polymer deformation images and force data. The amorphous chain orientation from the beginning of deformation until the onset of crystallisation was studied from the WAXS patterns. The true mechanical behaviour described by the true stress-true strain curve related to an amorphous chain orientation exhibited a linear behaviour. Approaching critical amorphous orientation, the true stress-true strain curve deviated from linear into non-linear behaviour. After the onset of crystallization, when the deformed polymer became a semicrystalline state, the true mechanical behaviour exhibited true strain hardening which greatly affected by the formation of the morphology. The gradual true strain hardening was associated with the formation of micro-fibrillar structure containing thin crystallite morphology whilst sharp increased in true strain hardening was associated with the formation of stacked lamellar morphology in the form of macro-lattice structure. The study was accomplished by the application of high brilliance synchrotron radiation at beamline ID2 of ESRF, Grenoble in France and the usage of the high contrast resolution of WAXS and SAXS charge-couple device (CCD) camera as well as 40 milliseconds temporal resolution of data acquisition system. (author)

  7. Lipidic phase membrane protein serial femtosecond crystallography

    Johansson, LC; Arnlund, D.; White, TA; Katona, G.; DePonte, DP; Weierstall, U.; Doak, RB; Shoeman, RL; Lomb, L; Malmerberg, E.; Davidsson, J; Nass, K.; Liang, MN; Andreasson, J.; Dell'Aquila, A.

    2012-01-01

    X-ray free electron laser (X-FEL)-based serial femtosecond crystallography is an emerging method with potential to rapidly advance the challenging field of membrane protein structural biology. Here we recorded interpretable diffraction data from micrometer-sized lipidic sponge phase crystals of the Blastochloris viridis photosynthetic reaction center delivered into an X-FEL beam using a sponge phase micro-jet.

  8. Crystallography in Four Dimensions : Methods and Applications

    Carlsson, Gunilla

    2004-01-01

    The four-electron reduction of dioxygen to water is the most exothermic non-photochemical reaction available to biology. A detailed molecular description of this reaction is needed to understand oxygen-based redox processes. Horseradish peroxidase (HRP) is a haem-containing redox enzyme capable of catalysing the reduction of dioxygen to water. We developed instrumentation and experimental methodology to capture and characterise by X-ray crystallography transient reaction intermediates in this...

  9. Radiation damage to nucleoprotein complexes in macromolecular crystallography

    Bury, Charles; Garman, Elspeth F.; Ginn, Helen Mary [University of Oxford, South Parks Road, Oxford OX1 3QU (United Kingdom); Ravelli, Raimond B. G. [Maastricht University, PO Box 616, Maastricht 6200 MD (Netherlands); Carmichael, Ian [University of Notre Dame, Notre Dame, IN 46556 (United States); Kneale, Geoff; McGeehan, John E., E-mail: john.mcgeehan@port.ac.uk [University of Portsmouth, King Henry 1st Street, Portsmouth PO1 2DY (United Kingdom)

    2015-01-30

    Quantitative X-ray induced radiation damage studies employing a model protein–DNA complex revealed a striking partition of damage sites. The DNA component was observed to be far more resistant to specific damage compared with the protein. Significant progress has been made in macromolecular crystallography over recent years in both the understanding and mitigation of X-ray induced radiation damage when collecting diffraction data from crystalline proteins. In contrast, despite the large field that is productively engaged in the study of radiation chemistry of nucleic acids, particularly of DNA, there are currently very few X-ray crystallographic studies on radiation damage mechanisms in nucleic acids. Quantitative comparison of damage to protein and DNA crystals separately is challenging, but many of the issues are circumvented by studying pre-formed biological nucleoprotein complexes where direct comparison of each component can be made under the same controlled conditions. Here a model protein–DNA complex C.Esp1396I is employed to investigate specific damage mechanisms for protein and DNA in a biologically relevant complex over a large dose range (2.07–44.63 MGy). In order to allow a quantitative analysis of radiation damage sites from a complex series of macromolecular diffraction data, a computational method has been developed that is generally applicable to the field. Typical specific damage was observed for both the protein on particular amino acids and for the DNA on, for example, the cleavage of base-sugar N{sub 1}—C and sugar-phosphate C—O bonds. Strikingly the DNA component was determined to be far more resistant to specific damage than the protein for the investigated dose range. At low doses the protein was observed to be susceptible to radiation damage while the DNA was far more resistant, damage only being observed at significantly higher doses.

  10. Digital x-ray imaging

    Digital radiography is progressively replacing conventional (film-based) radiographic techniques promising consistently high levels of image quality, more effective use of radiation and more efficient work practices. At the same time its introduction poses new challenges to those physical scientists who design radiological imaging systems and those who provide scientific/technical support to a clinical radiology service. In this review scientific aspects of those digital x-ray imaging systems which are proving most successful are described. Physical measurement techniques developed to evaluate the imaging performance and radiation dose efficiency of clinical digital radiography systems are outlined. Finally, directions in which digital x-ray imaging technology may evolve in the coming decade are discussed. (author)

  11. Soft x-ray tomoholography

    We demonstrate an x-ray imaging method that combines Fourier transform holography with tomography (‘tomoholography’) for three-dimensional (3D) microscopic imaging. A 3D image of a diatom shell with a spatial resolution of 140 nm is presented. The experiment is realized by using a small gold sphere as the reference wave source for holographic imaging. This setup allows us to rotate the sample and to collect a number of 2D projections for tomography. (paper)

  12. Soft x-ray tomoholography

    Guehrs, E.; Stadler, A.M.; Flewett, S.; Frömmel, S.; Geilhufe, J.; Pfau, B; Rander, T.; Schaffert, S.; Büldt, G; Eisebitt, S.

    2012-01-01

    We demonstrate an x-ray imaging method that combines Fourier transform holography with tomography ('tomoholography') for three-dimensional (3D) microscopic imaging. A 3D image of a diatom shell with a spatial resolution of 140 nm is presented. The experiment is realized by using a small gold sphere as the reference wave source for holographic imaging. This setup allows us to rotate the sample and to collect a number of 2D projections for tomography.

  13. X-ray tube arrangements

    A technique for ensuring the rapid correction of both amplitude and offset errors in the deflectional movement of an electron beam along an X-ray emissive target is described. The movement is monitored at at least two positions during a sweep and differences, between the two movements and a desired movement, at these positions are combined in different proportions to produce a corrective servo signal. Such arrangements find application, for example, in computerised tomographic scanners. (author)

  14. X-ray-powered macronovae

    Kisaka, Shota; Nakar, Ehud

    2015-01-01

    A macronova (or kilonova) was observed as an infrared excess several days after short gamma-ray burst, GRB 130603B. Although the $r$-process radioactivity is widely discussed as an energy source, it requires huge mass of ejecta from a neutron star (NS) binary merger. We propose that the X-ray excess simultaneously observed with the infrared excess can naturally heat the ejecta, leading to the thermal re-emission as observed in infrared. This X-ray-powered model explains both the X-ray and infrared excesses with a single energy source by the central engine like a black hole, and allows for broader parameter region, in particular smaller ejecta mass $\\sim10^{-3}-10^{-2}M_{\\odot}$ with iron mixed as suggested by general relativistic simulations for typical NS-NS mergers, than the previous models. We also discuss the other macronova candidates in GRB 060614 and GRB 080503, and implications for the search of electromagnetic counterparts to gravitational waves.

  15. X-Ray-powered Macronovae

    Kisaka, Shota; Ioka, Kunihito; Nakar, Ehud

    2016-02-01

    A macronova (or kilonova) was observed as an infrared excess several days after the short gamma-ray burst GRB 130603B. Although the r-process radioactivity is widely discussed as an energy source, it requires a huge mass of ejecta from a neutron star (NS) binary merger. We propose a new model in which the X-ray excess gives rise to the simultaneously observed infrared excess via thermal re-emission, and explore what constraints this would place on the mass and velocity of the ejecta. This X-ray-powered model explains both the X-ray and infrared excesses with a single energy source such as the central engine like a black hole, and allows for a broader parameter region than the previous models, in particular a smaller ejecta mass ˜ {10}-3{--}{10}-2{M}⊙ and higher iron abundance mixed as suggested by general relativistic simulations for typical NS-NS mergers. We also discuss the other macronova candidates in GRB 060614 and GRB 080503, and the implications for the search of electromagnetic counterparts to gravitational waves.

  16. Space station application of CCD image sensors for x-ray imaging

    Charge Coupled Device (CCD) type solid state image sensors are employed in a number of space based imaging experiments and will be the basis for a camera system to acquire x-ray diffraction images on board the Space Station. This paper will present the system engineering considerations that led to the selection of CCDs over other x-ray imaging technologies and the design of the camera system. This will include discussion of the special requirements imposed by the space environment and this x-ray crystallography mission. This systems engineering discussion will be followed by a summary of high spatial resolution CCDs that are candidates for this camera, what may become available in the future, and what improvements would make CCDs even more suited to such X-ray imaging applications on the ground as well as in space

  17. Aspergillosis - chest x-ray (image)

    ... usually occurs in immunocompromised individuals. Here, a chest x-ray shows that the fungus has invaded the lung ... are usually seen as black areas on an x-ray. The cloudiness on the left side of this ...

  18. Stabilized x-ray generator power supply

    X-ray diffraction and X-ray fluorescence analysis are very much adopted in laboratories to determine the type and structure of the constituent compounds in solid materials, chemical composition of materials, stress developed on metals etc. These experiments need X-ray beam of fixed intensity and wave length. This can only be achieved by X-ray generator having highly stabilized tube voltage and tube current. This paper describes how X-ray tube high voltage and electron beam current are stabilized. This paper also highlights generation of X-rays, diffractometry and X-ray fluorescence analysis and their wide applications. Principle of operation for stabilizing the X-ray tube voltage and current, different protection circuits adopted, special features of the mains H.V. transformer and H.T. tank are described in this report. (author)

  19. Graphene-based microfluidics for serial crystallography.

    Sui, Shuo; Wang, Yuxi; Kolewe, Kristopher W; Srajer, Vukica; Henning, Robert; Schiffman, Jessica D; Dimitrakopoulos, Christos; Perry, Sarah L

    2016-08-01

    Microfluidic strategies to enable the growth and subsequent serial crystallographic analysis of micro-crystals have the potential to facilitate both structural characterization and dynamic structural studies of protein targets that have been resistant to single-crystal strategies. However, adapting microfluidic crystallization platforms for micro-crystallography requires a dramatic decrease in the overall device thickness. We report a robust strategy for the straightforward incorporation of single-layer graphene into ultra-thin microfluidic devices. This architecture allows for a total material thickness of only ∼1 μm, facilitating on-chip X-ray diffraction analysis while creating a sample environment that is stable against significant water loss over several weeks. We demonstrate excellent signal-to-noise in our X-ray diffraction measurements using a 1.5 μs polychromatic X-ray exposure, and validate our approach via on-chip structure determination using hen egg white lysozyme (HEWL) as a model system. Although this work is focused on the use of graphene for protein crystallography, we anticipate that this technology should find utility in a wide range of both X-ray and other lab on a chip applications. PMID:27241728

  20. Phase-sensitive X-ray imager

    Baker, Kevin Louis

    2013-01-08

    X-ray phase sensitive wave-front sensor techniques are detailed that are capable of measuring the entire two-dimensional x-ray electric field, both the amplitude and phase, with a single measurement. These Hartmann sensing and 2-D Shear interferometry wave-front sensors do not require a temporally coherent source and are therefore compatible with x-ray tubes and also with laser-produced or x-pinch x-ray sources.

  1. Optical element for X-ray microscopy

    Chadzitaskos, G.

    2008-01-01

    We present a proposal for a X-ray optical element suitable for X-ray microscopy and other X-ray-based display systems. Its principle is based on the Fresnel lenses condition and the Bragg condition for X-ray scattering on a slice of monocrystal. These conditions are fulfilled simultaneously due to a properly machined shape of the monocrystal with a stress at its ends.

  2. Center for X-ray Optics, 1988

    1989-04-01

    This report briefly reviews the following topics: soft-x-ray imaging; reflective optics for hard x-rays; coherent XUV sources; spectroscopy with x-rays; detectors for coronary artery imaging; synchrotron-radiation optics; and support for the advanced light source.

  3. X-Ray Exam: Neck (For Parents)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Neck KidsHealth > For Parents > X-Ray Exam: Neck Print A A A Text Size ... español Radiografía: cuello What It Is A neck X-ray is a safe and painless test that uses ...

  4. Cryotomography x-ray microscopy state

    Le Gros, Mark; Larabell, Carolyn A.

    2010-10-26

    An x-ray microscope stage enables alignment of a sample about a rotation axis to enable three dimensional tomographic imaging of the sample using an x-ray microscope. A heat exchanger assembly provides cooled gas to a sample during x-ray microscopic imaging.

  5. Electron beam parallel X-ray generator

    Payne, P.

    1967-01-01

    Broad X ray source produces a highly collimated beam of low energy X rays - a beam with 2 to 5 arc minutes of divergence at energies between 1 and 6 keV in less than 5 feet. The X ray beam is generated by electron bombardment of a target from a large area electron gun.

  6. Center for X-ray Optics, 1988

    This report briefly reviews the following topics: soft-x-ray imaging; reflective optics for hard x-rays; coherent XUV sources; spectroscopy with x-rays; detectors for coronary artery imaging; synchrotron-radiation optics; and support for the advanced light source

  7. X-ray tracing using Geant4

    We describe an extension to the Geant4 software package that allows it to be used as a general purpose X-ray tracing package. We demonstrate the use of our extension by building a model of the X-ray optics of the X-ray observatory XMM-Newton, calculating its effective area, and comparing the results with the published calibration curves.

  8. Double conical crystal x-ray spectrometer for high resolution ultrafast x-ray absorption near-edge spectroscopy of Al K edge

    Levy, A.; Dorchies, F.; Fourment, C.; Harmand, M.; Hulin, S.; Santos, J. J.; Descamps, D.; Petit, S.; Bouillaud, R. [Centre Lasers Intenses et Applications (CELIA), Universite de Bordeaux-CNRS-CEA, Talence F-33405 (France)

    2010-06-15

    An x-ray spectrometer devoted to dynamical studies of transient systems using the x-ray absorption fine spectroscopy technique is presented in this article. Using an ultrafast laser-induced x-ray source, this optical device based on a set of two potassium acid phthalate conical crystals allows the extraction of x-ray absorption near-edge spectroscopy structures following the Al absorption K edge. The proposed experimental protocol leads to a measurement of the absorption spectra free from any crystal reflectivity defaults and shot-to-shot x-ray spectral fluctuation. According to the detailed analysis of the experimental results, a spectral resolution of 0.7 eV rms and relative fluctuation lower than 1% rms are achieved, demonstrated to be limited by the statistics of photon counting on the x-ray detector.

  9. AXSIS: Exploring the frontiers in attosecond X-ray science, imaging and spectroscopy

    Kärtner, F. X.; Ahr, F.; Calendron, A.-L.; Çankaya, H.; Carbajo, S.; Chang, G.; Cirmi, G.; Dörner, K.; Dorda, U.; Fallahi, A.; Hartin, A.; Hemmer, M.; Hobbs, R.; Hua, Y.; Huang, W. R.; Letrun, R.; Matlis, N.; Mazalova, V.; Mücke, O. D.; Nanni, E.; Putnam, W.; Ravi, K.; Reichert, F.; Sarrou, I.; Wu, X.; Yahaghi, A.; Ye, H.; Zapata, L.; Zhang, D.; Zhou, C.; Miller, R. J. D.; Berggren, K. K.; Graafsma, H.; Meents, A.; Assmann, R. W.; Chapman, H. N.; Fromme, P.

    2016-09-01

    X-ray crystallography is one of the main methods to determine atomic-resolution 3D images of the whole spectrum of molecules ranging from small inorganic clusters to large protein complexes consisting of hundred-thousands of atoms that constitute the macromolecular machinery of life. Life is not static, and unravelling the structure and dynamics of the most important reactions in chemistry and biology is essential to uncover their mechanism. Many of these reactions, including photosynthesis which drives our biosphere, are light induced and occur on ultrafast timescales. These have been studied with high time resolution primarily by optical spectroscopy, enabled by ultrafast laser technology, but they reduce the vast complexity of the process to a few reaction coordinates. In the AXSIS project at CFEL in Hamburg, funded by the European Research Council, we develop the new method of attosecond serial X-ray crystallography and spectroscopy, to give a full description of ultrafast processes atomically resolved in real space and on the electronic energy landscape, from co-measurement of X-ray and optical spectra, and X-ray diffraction. This technique will revolutionize our understanding of structure and function at the atomic and molecular level and thereby unravel fundamental processes in chemistry and biology like energy conversion processes. For that purpose, we develop a compact, fully coherent, THz-driven attosecond X-ray source based on coherent inverse Compton scattering off a free-electron crystal, to outrun radiation damage effects due to the necessary high X-ray irradiance required to acquire diffraction signals. This highly synergistic project starts from a completely clean slate rather than conforming to the specifications of a large free-electron laser (FEL) user facility, to optimize the entire instrumentation towards fundamental measurements of the mechanism of light absorption and excitation energy transfer. A multidisciplinary team formed by laser

  10. Diffracted X-ray tracking for monitoring intramolecular motion in individual protein molecules using broad band X-ray

    Ichiyanagi, Kouhei; Sekiguchi, Hiroshi; Hoshino, Masato; Kajiwara, Kentaro; Hoshisashi, Kentaro; Jae-won, Chang; Tokue, Maki; Matsushita, Yufuku; Nishijima, Masaki; Inoue, Yoshihisa; Senba, Yasunori; Ohashi, Haruhiko; Ohta, Noboru; Yagi, Naoto; Sasaki, Yuji C.

    2013-10-01

    Diffracted X-ray tracking (DXT) enables the tilting and twisting motions of single protein molecules to be monitored with micro- to milliradian resolution using a highly brilliant X-ray source with a wide energy bandwidth. We have developed a technique to monitor single molecules using gold nanocrystals attached to individual protein molecules using the BL28B2 beamline at SPring-8. In this paper we present the installation of a single toroidal X-ray mirror at BL28B2 to focus X-rays in an energy range of 10-20 keV (△E/E = 82% for an X-ray with a wide energy bandwidth). With this beamline we tracked diffraction spots from gold nanocrystals over a wide angle range than that using quasi-monochromatic X-rays. Application of the wide angle DXT technique to biological systems enabled us to observe the on-site motions of single protein molecules that have been functionalized in vivo. We further extend the capability of DXT by observing the fractional tilting and twisting motions of inner proteins under various conditions. As a proof of this methodology and to determine instrumental performance the intramolecular motions of a human serum albumin complex with 2-anthracenecarboxylic acid was investigated using the BL28B2 beamline. The random tilting and twisting intramolecular motions are shown to be directly linked to the movement of individual protein molecules in the buffer solution.

  11. Diffracted X-ray tracking for monitoring intramolecular motion in individual protein molecules using broad band X-ray

    Diffracted X-ray tracking (DXT) enables the tilting and twisting motions of single protein molecules to be monitored with micro- to milliradian resolution using a highly brilliant X-ray source with a wide energy bandwidth. We have developed a technique to monitor single molecules using gold nanocrystals attached to individual protein molecules using the BL28B2 beamline at SPring-8. In this paper we present the installation of a single toroidal X-ray mirror at BL28B2 to focus X-rays in an energy range of 10–20 keV (△E/E = 82% for an X-ray with a wide energy bandwidth). With this beamline we tracked diffraction spots from gold nanocrystals over a wide angle range than that using quasi-monochromatic X-rays. Application of the wide angle DXT technique to biological systems enabled us to observe the on-site motions of single protein molecules that have been functionalized in vivo. We further extend the capability of DXT by observing the fractional tilting and twisting motions of inner proteins under various conditions. As a proof of this methodology and to determine instrumental performance the intramolecular motions of a human serum albumin complex with 2-anthracenecarboxylic acid was investigated using the BL28B2 beamline. The random tilting and twisting intramolecular motions are shown to be directly linked to the movement of individual protein molecules in the buffer solution

  12. Structure of drug-target proteins determined by both X-ray and neutron diffraction

    Crystallography enables us to obtain accurate atomic positions within proteins. High resolution X-ray crystallography provides information for most of the atoms comprising a protein, with the exception of hydrogens. Neutron diffraction data can provide information of the location of hydrogen atoms to the structural information determined by X-ray crystallography. Here, we show the recent of the structural determination of drug-target proteins, porcine pancreatic elastase (PPE) and human immuno-deficiency virus type-1 protease (HIV-PR) by both X-ray and neutron diffraction. The structure of porcine pancreatic elastase with its potent inhibitor (FR13080) was determined to 0.94A resolution by X-ray diffraction and 1.75 A resolution by neutron diffraction. It was found that there are two characteristic hydrogen bonding interactions in which hydrogen atoms were confirmed. One is located between a catalytic aspartate and histidine, another is involved in the inhibitor recognition site. The structure of HIV-PR with its potent inhibitor (KNI-272) was also determined to 0.93 A resolution by X-ray diffraction and 2.3 A resolution by neutron diffraction. The ionization state of the catalytic residues were clarified to show that Asp125 is protonated and Asp25 is deprotonated. The ionization state and the location of hydrogen atoms of the catalytic residue in HIV-PR were firstly determined by neutron diffraction. Furthermore, collaborative use of both X-ray and neutron to identify the location of ambiguous hydrogen atoms will be shown. (author)

  13. Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging

    A comparison of X-ray diffraction and radiographic techniques for the location and characterization of protein crystals is demonstrated on membrane protein crystals mounted within lipid cubic phase material. The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required

  14. Zernike x-ray ptychography.

    Vartiainen, Ismo; Mohacsi, Istvan; Stachnik, Karolina; Guizar-Sicairos, Manuel; David, Christian; Meents, Alke

    2016-02-15

    We present an imaging technique combining Zernike phase-contrast imaging and ptychography. The contrast formation is explained by following the theory of Zernike phase-contrast imaging. The method is demonstrated with x-rays at a photon energy of 6.2 keV, showing how ptychographic reconstruction of a phase sample leads to a Zernike phase-contrast image appearing in the amplitude reconstruction. In addition, the results presented in this Letter indicate an improvement of the resolution of the reconstructed object in the case of Zernike ptychography compared with the conventional one. PMID:26872172

  15. Protonium X-ray spectroscopy

    Gotta, D

    1999-01-01

    The Lyman and Balmer transitions from antiprotonic hydrogen and deuterium were studied extensively at the low-energy-antiproton ring LEAR at CERN in order to determine the strong interaction effects. A first series of experiments $9 was performed with semiconductor and gaseous X-ray detectors. In the last years of LEAR operation using a Bragg crystal spectrometer, strong interaction parameters in the 2p states of antiprotonic hydrogen and deuterium were measured $9 directly. The results of the measurements support the meson-exchange models describing the medium and long range part of the nucleon-antinucleon interaction. (39 refs).

  16. X-ray tomographic apparatus

    An x-ray tomographic system consists of a radiation source such as gamma or x radiation which produces a fan-shaped beam. The fan is wide enough to encompass the patient circle. The system further includes means for rotating the radiation source about the patient for less than a full rotation, and detectors for detecting the radiation at positions that surround the patient by 1800 plus the angle of the fan beam plus the angle between adjacent fan detectors. Attenuation data from the detectors is sorted into detector fans of attenuation data, then processed. The convolved data is back-projected into an image memory and displayed on a video monitor

  17. X-ray Pulsations in the Supersoft X-ray Binary CAL 83

    Schmidtke, P. C.; Cowley, A. P.

    2005-01-01

    X-ray data reveal that the supersoft X-ray binary CAL 83 exhibits 38.4 minute pulsations at some epochs. These X-ray variations are similar to those found in some novae and are likely to be caused by nonradial pulsations the white dwarf. This is the first detection of pulsations in a classical supersoft X-ray binary.

  18. Insights into the mechanism of X-ray-induced disulfide-bond cleavage in lysozyme crystals based on EPR, optical absorption and X-ray diffraction studies

    Electron paramagnetic resonance (EPR) and online UV–visible absorption microspectrophotometry with X-ray crystallography have been used in a complementary manner to follow X-ray-induced disulfide-bond cleavage, to confirm a multi-track radiation-damage process and to develop a model of that process. Electron paramagnetic resonance (EPR) and online UV–visible absorption microspectrophotometry with X-ray crystallography have been used in a complementary manner to follow X-ray-induced disulfide-bond cleavage. Online UV–visible spectroscopy showed that upon X-irradiation, disulfide radicalization appeared to saturate at an absorbed dose of approximately 0.5–0.8 MGy, in contrast to the saturating dose of ∼0.2 MGy observed using EPR at much lower dose rates. The observations suggest that a multi-track model involving product formation owing to the interaction of two separate tracks is a valid model for radiation damage in protein crystals. The saturation levels are remarkably consistent given the widely different experimental parameters and the range of total absorbed doses studied. The results indicate that even at the lowest doses used for structural investigations disulfide bonds are already radicalized. Multi-track considerations offer the first step in a comprehensive model of radiation damage that could potentially lead to a combined computational and experimental approach to identifying when damage is likely to be present, to quantitate it and to provide the ability to recover the native unperturbed structure

  19. Comets: mechanisms of x-ray activity

    Ibadov, Subhon

    2016-07-01

    Basic mechanisms of X-ray activity of comets are considered, including D-D mechanism corresponding to generation of X-rays due to production of hot short-living plasma clumps at high-velocity collisions between cometary and interplanetary dust particles as well as M-M one corresponding to production of X-rays due to recombination of multicharge ions of solar wind plasma via charge exchange process at their collisions with molecules/atoms of the cometary atmospheres. Peculiarities of the variation of the comet X-ray spectrum and X-ray luminosity with variation of its heliocentric distance are revealed.

  20. Swift Observations of X-ray supernovae

    Li, K. L.; Pun, Chun. S. J.

    2011-01-01

    We present a result of X-ray supernovae (SNe) survey using the Swift satellite public archive. An automatic searching program was designed to search X-ray SNe among all of the Swift archival observations between November 2004 and February 2011. Using the C++ program, 24 X-ray detectable supernovae have been found in the archive and 3 of them were newly-discovered in X-rays which are SN 1986L, SN 2003lx, and SN 2007od. In addition, SN 2003lx is a Type Ia supernova which may be the second X-ray...

  1. X-ray Spectroscopy of Cooling Cluster

    Peterson, J.R.; /SLAC; Fabian, A.C.; /Cambridge U., Inst. of Astron.

    2006-01-17

    We review the X-ray spectra of the cores of clusters of galaxies. Recent high resolution X-ray spectroscopic observations have demonstrated a severe deficit of emission at the lowest X-ray temperatures as compared to that expected from simple radiative cooling models. The same observations have provided compelling evidence that the gas in the cores is cooling below half the maximum temperature. We review these results, discuss physical models of cooling clusters, and describe the X-ray instrumentation and analysis techniques used to make these observations. We discuss several viable mechanisms designed to cancel or distort the expected process of X-ray cluster cooling.

  2. Symbiotic stars in X-rays

    Luna, G. J. M.; Sokoloski, J. L.; Mukai, K; Nelson, T.

    2012-01-01

    Until recently, symbiotic binary systems in which a white dwarf accretes from a red giant were thought to be mainly a soft X-ray population. Here we describe the detection with the X-ray Telescope (XRT) on the Swift satellite of nine white dwarf symbiotics that were not previously known to be X-ray sources and one that had previously been detected as a supersoft X-ray source. The nine new X-ray detections were the result of a survey of 41 symbiotic stars, and they increase the number of symbi...

  3. X-ray crystal structure and activity of fluorenyl-based compounds as transthyretin fibrillogenesis inhibitors.

    Ciccone, Lidia; Nencetti, Susanna; Rossello, Armando; Tepshi, Livia; Stura, Enrico A; Orlandini, Elisabetta

    2016-10-01

    Transthyretin (TTR) is a 54 kDa homotetrameric protein that transports thyroxine (T4) and retinol (vitamin A), through its association with retinol binding protein (RBP). Under unknown conditions, it aggregates to form fibrils associated with TTR amyloidosis. Ligands able to inhibit fibril formation have been studied by X-ray crystallography. The use of polyethylene glycol (PEG) instead of ammonium sulphate or citrate has been evaluated as an alternative to obtain new TTR complexes with (R)-3-(9-fluoren-9-ylideneaminooxy)-2-methyl-N-(methylsulfonyl) propionamide (48R(1)) and 2-(9H-fluoren-9-ylideneaminooxy) acetic acid (ES8(2)). The previously described fluorenyl based inhibitors (S)-3-((9H-fluoren-9-ylideneamino)oxy)-2-methylpropanoic acid (6BD) and 3-((9H-fluoren-9-ylideneamino)oxy)propanoic acid (7BD) have been re-evaluated with the changed crystallization method. The new TTR complexes with compounds of the same family show that the 9-fluorenyl motif can occupy alternative hydrophobic binding sites. This augments the potential use of this scaffold to yield a large variety of differently substituted mono-aryl compounds able to inhibit TTR fibril formation. PMID:26235916

  4. Miniature x-ray point source for alignment and calibration of x-ray optics

    A miniature x-ray point source of high brightness similar to that of Rovinsky, et al. is described. One version of the x-ray source is used to align the x-ray optics on the Argus and Shiva laser systems. A second version is used to determine the spatial and spectral transmission functions of the x-ray optics. The spatial and spectral characteristics of the x-ray emission from the x-ray point source are described. The physical constraints including size, intensity and thermal limitations, and useful lifetime are discussed. The alignment and calibration techniques for various x-ray optics and detector combinations are described

  5. MX1: a bending-magnet crystallography beamline serving both chemical and macromolecular crystallography communities at the Australian Synchrotron

    The macromolecular crystallography beamline MX1 at the Australian Synchrotron is described. MX1 is a bending-magnet crystallography beamline at the 3 GeV Australian Synchrotron. The beamline delivers hard X-rays in the energy range from 8 to 18 keV to a focal spot at the sample position of 120 µm FWHM. The beamline endstation and ancillary equipment facilitate local and remote access for both chemical and biological macromolecular crystallography. Here, the design of the beamline and endstation are discussed. The beamline has enjoyed a full user program for the last seven years and scientific highlights from the user program are also presented

  6. Management of dental x-ray exposure

    The effects of dental x-ray exposure and how they might be minimized were reviewed. The frequency of dental x-ray exposures in Japan was presented for each year, sex, age group and site of x-ray photography separately. The doses of exposure at various parts of the body per x-ray examination were also presented, and the probabilities of genetic damage, and of development of leukemia or cancer were calculated. The allowable dose of exposure for radiation workers was discussed. It is important to take account of radiation quality, area of irradiation field, and posture of patients to minimize the radiation effect. The actual statistics on the x-ray exposure at the dentists, distribution of the dispersed radiation in the x-ray room, methods of protection against exposure, and plans and designs of the x-ray room were discussed. (Kaihara, S.)

  7. X ray imaging microscope for cancer research

    Hoover, Richard B.; Shealy, David L.; Brinkley, B. R.; Baker, Phillip C.; Barbee, Troy W., Jr.; Walker, Arthur B. C., Jr.

    1991-01-01

    The NASA technology employed during the Stanford MSFC LLNL Rocket X Ray Spectroheliograph flight established that doubly reflecting, normal incidence multilayer optics can be designed, fabricated, and used for high resolution x ray imaging of the Sun. Technology developed as part of the MSFC X Ray Microscope program, showed that high quality, high resolution multilayer x ray imaging microscopes are feasible. Using technology developed at Stanford University and at the DOE Lawrence Livermore National Laboratory (LLNL), Troy W. Barbee, Jr. has fabricated multilayer coatings with near theoretical reflectivities and perfect bandpass matching for a new rocket borne solar observatory, the Multi-Spectral Solar Telescope Array (MSSTA). Advanced Flow Polishing has provided multilayer mirror substrates with sub-angstrom (rms) smoothnesss for the astronomical x ray telescopes and x ray microscopes. The combination of these important technological advancements has paved the way for the development of a Water Window Imaging X Ray Microscope for cancer research.

  8. Accurate macromolecular structures using minimal measurements from X-ray free-electron lasers

    Hattne, Johan; Echols, Nathaniel; Tran, Rosalie; Kern, Jan; Gildea, Richard J.; Brewster, Aaron S.; Alonso-Mori, Roberto; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; White, William E.; Schafer, Donald W.; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Glatzel, Pieter; Zwart, Petrus H.; Grosse-Kunstleve, Ralf W.; Bogan, Michael J.; Messerschmidt, Marc; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Yano, Junko; Bergmann, Uwe; Yachandra, Vittal K.; Adams, Paul D.; Sauter, Nicholas K.

    2014-01-01

    X-ray free-electron laser (XFEL) sources enable the use of crystallography to solve three-dimensional macromolecular structures under native conditions and free from radiation damage. Results to date, however, have been limited by the challenge of deriving accurate Bragg intensities from a heterogeneous population of microcrystals, while at the same time modeling the X-ray spectrum and detector geometry. Here we present a computational approach designed to extract statistically significant high-resolution signals from fewer diffraction measurements. PMID:24633409

  9. Parametric X-Ray Radiation

    Shchagin, Alexander

    1997-10-01

    The main PXR properties [1,2] are considered in the paper: energy, width, smooth tuning of monochromatic PXR spectral line; fine structure and absolute differential yields of PXR in the vicinity of and at angular distances from Brag directions; angular spread of the PXR beam; the influence of incident electron energy and of the density effect on the PXR properties; linear polarization of PXR; background in PXR spectra. Experimental setups for linacs and the results of measurements are discussed. Experimental data are compared to theoretical calculations at PXR energies between 5 and 400 keV for incident electron energies ranging from 15 to 1200 MeV. Possible applications of PXR as a new source of a bright, tunable X-ray beam in science and industry are discussed. [1] A.V. Shchagin and N.A. Khizhnyak, NIM B119, 115-122 (1996). [2] A.V. Shchagin and X.K. Maruyama, "Parametric X-rays", a chapter in the book "Accelerator-based Atomic Physics Techniques and Applications", edited by S.M. Shafroth and J.C. Austin, AIP Press, 1997, pp 279-307.

  10. Using Two-Dimensional Colloidal Crystals to Understand Crystallography

    Bosse, Stephanie A.; Loening, Nikolaus M.

    2008-01-01

    X-ray crystallography is an essential technique for modern chemistry and biochemistry, but it is infrequently encountered by undergraduate students owing to lack of access to equipment, the time-scale for generating diffraction-quality molecular crystals, and the level of mathematics involved in analyzing the resulting diffraction patterns.…

  11. Full-field transmission x-ray imaging with confocal polycapillary x-ray optics

    Sun, Tianxi; MacDonald, C. A.

    2013-01-01

    A transmission x-ray imaging setup based on a confocal combination of a polycapillary focusing x-ray optic followed by a polycapillary collimating x-ray optic was designed and demonstrated to have good resolution, better than the unmagnified pixel size and unlimited by the x-ray tube spot size. This imaging setup has potential application in x-ray imaging for small samples, for example, for histology specimens.

  12. Nano structured materials studied by coherent X-ray diffraction

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  13. Nano structured materials studied by coherent X-ray diffraction

    Gulden, Johannes

    2013-03-15

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  14. X-ray microtomography: applications and developments

    Full text: X-ray microtomography has followed a classical development path being originally available only to those with the expertise to piece together the often cumbersome components to required to make a practical x-ray microtomography system. Subsequent technological and scientific advances have meant that x-ray microtomography instruments are now off-the-shelf items with a cost well within the equipment budgets of research institutions and industry. The technological advances that have contributed to the development of x-ray microtomography include commercially available x-ray micro-sources, high-resolution CCD cameras and highspeed, low-cost computers. The scientific developments have been predominantly in image reconstruction. Some of these scientific developments are, with the advantage of hindsight, very simple while others, such as resolution enhancement using the Fresnel fringes in x-ray projection images, are not so intuitive. As a consequence of the availability of 'black-box' instruments, x-ray microtomography is spreading to a wide range of applications. The materials most suited to examination by x-ray microtomography are those with a medium level of x-ray absorption such as bone, teeth, rocks, porous metals, composite materials and plant materials. For these materials, 3D information can be obtained at resolutions comparable to the resolution of a high-quality optical microscope. A few of these applications will be demonstrated in the presentation. Technological advances that aid x-ray microtomography will continue with x-ray sources becoming smaller, computers becoming faster and CCD cameras having increased numbers of pixels. It will be interesting to see if nano x-ray microtomography is achieved. Developments in x-ray microtomography are required in areas such as contrast enhancement particularly for problematic materials such as soft tissue and low-density polymers. For low-density polymers x-ray absorption is very low while for soft tissue

  15. Protein Energy Landscapes Determined by 5-Dimensional Crystallography

    Schmidt, Marius; Henning, Robert; Ihee, Hyotcherl; Purwar, Namrta; Tenboer, Jason; Tripathi, Shailesh

    2013-01-01

    Free energy landscapes decisively determine the progress of enzymatically catalyzed reactions[1]. Time-resolved macromolecular crystallography unifies transient-state kinetics with structure determination [2-4] because both can be determined from the same set of X-ray data. We demonstrate here how barriers of activation can be determined solely from five-dimensional crystallography [5]. Directly linking molecular structures with barriers of activation between them allows for gaining insight into the structural nature of the barrier. We analyze comprehensive time series of crystal-lographic data at 14 different temperature settings and determine entropy and enthalpy contributions to the barriers of activation. 100 years after the discovery of X-ray scattering, we advance X-ray structure determination to a new frontier, the determination of energy landscapes.

  16. Aqueous solubility study of salts of benzylamine derivatives and p-substituted benzoic acid derivatives using X-ray crystallographic analysis

    Parshad, Henrik; Frydenvang, Karla Andrea; Liljefors, Tommy; Sorensen, Henning Osholm; Larsen, Claus

    2004-01-01

    Twenty two p-substituted benzoic acid derivates were used to prepare salts of N-methylbenzylamine (II) and N,N-dimethylbenzylamine (III), respectively. Only five salts of (II) and two salts of (III) were obtained in a crystalline state. The solubility of these salts was orders of magnitude higher...

  17. Anomalous x-ray scattering

    The availability of tunable synchrotron radiation has made it possible systematically to perform x-ray diffraction studies in regions of anomalous scattering near absorption edges, e.g. in order to derive phase information for crystal structure determination. An overview is given of recent experimental and theoretical work and discuss the properties of the anomalous atomic scattering factor, with emphasis on threshold resonances and damping effects. The results are applied to a discussion of the very strong anomalous dispersion recently observed near the L3 edge in a cesium complex. Also given is an overview of elements and levels where similar behavior can be expected. Finally, the influence of solid state and chemical effects on the absorption edge structure is discussed. 64 references

  18. Submicron X-ray diffraction

    At the Advanced Light Source in Berkeley the authors have instrumented a beam line that is devoted exclusively to x-ray micro diffraction problems. By micro diffraction they mean those classes of problems in Physics and Materials Science that require x-ray beam sizes in the sub-micron range. The beam line has a unity magnification toroidal mirror that produces a 50 by 200 micron focus just inside an x-ray hutch at the position of an x-y slit. The beam path in the hutch consists of source defining slits, a four bounce Ge or Si monochromator, followed by elliptically bent Kirkpatrick-Baez mirror pair which focuses the beam from the slits to sub micron dimensions (0.8 x 0.8 microns). An important feature of this arrangement is the ability to switch between white and monochromatic beams that are essential for characterizing crystals or crystal grains in the sub-micron range. Since sample rotation is fixed they have facilities for precision translation of the specimen to allow them to scan different crystal regions or grains. The sample stage rests on a state of the art six-circle diffractometer equipped with encoders in the main rotation stages calibrated to a second of arc. The detector is a 4K x 4K CCD (Bruker) with a 9 x 9 cm view area mounted on a detector arm that can be positioned around the sample. The detector itself can also be positioned to better than 1 micron along the detector arm. Using this facility they have been able to measure the orientation structure of single grains of passivated or buried Al interconnect test structures. Such structures or their equivalents are important in connecting individual components on integrated circuits. Their sub-micron dimensions result in very high current densities that can result in interconnect failures. The variation in sub-grain structure in a single grain is rich in detail. They have obtained detailed maps of misorientations in single grains using white beam Laue diffraction patterns From these they have been

  19. X-ray intensifying screens

    An x-ray intensifying screen comprises a support which has a luminescent composition comprising an isotropic phosphor and a polymer having an index of refraction within 0.02 of that of the phosphor over at least 80 percent of its emission spectrum. The support has an index of refraction up to or equal to 0.05 units higher than that of the phosphor and has a reflection optical density of at least 1.7 to light emitted by the phosphor. A preferred luminescent composition comprises Kl:Tl, Rbl:Tl at BaSrFCl:Eu mixed with two monomers such as 1-naphthylmethylmethacrylate, S(1-naphthylmethyl) thioacrylate, 1-bromo-2-naphthylacrylate, and benzyl methacrylate, coated on black anodised Al and polymerised in situ. The ratio of monomers is adjusted to give the desired refractive index. Other phosphors, polymers and supports are specified together with the preparation of the monomers and polymers. (author)

  20. X-ray flat panel detectors and X-ray tubes contributing to development of X-ray diagnostic systems

    X-ray flat panel detectors (FPDs) and X-ray tubes are key devices allowing X-ray diagnostic systems to support more sophisticated medical care. FPDs provide valuable information for the diagnosis of various diseases through the conversion of X-ray images of the human body into electronic signals, while X-ray tubes are used in a wide range of applications such as computed tomography (CT), angiography, fluoroscopy, mammography, and dental systems. Toshiba Electron Tubes and Devices Co., Ltd. has developed and commercialized FPDs providing high-quality diagnostic X-ray images with low dose exposure through the development of cutting-edge technologies including a fine crystal formation technology for cesium iodide (CsI) scintillators, thin-film transistor (TFT) arrays with photodiodes, and so on. In the field of X-ray tubes that can generate a high output of X-rays, we have developed a liquid metal hydrodynamic bearing (LM bearing) technology for various diagnostic systems including medical CT systems with a long lifetime and high rotation speed, and cardiovascular imaging systems with quiet operation. Furthermore, LM bearing technology reduces the burden on the environment by replacing insulating oil with water coolant for the cooling system and making the X-ray tubes more compact. (author)

  1. Characterization of monel alloys by X-ray fluorescence technique

    Method for the determination of Ni, Cu, Fe, Mn, Si, Al, Ti, Co, Cr and Mo in Monel alloys using thin film for sample preparation and X-ray fluorescence techniques is described. Samples in filings form were completely dissolved with inorganic acids and they were made up to a known volume. Then, these samples were deposited in a filter paper, reducing in this form the effect of the matrix. For all elements the first order emission Kα lines were selected for measurements and for excitation a rhodium X-ray tub was utilized. For the heavier elements the LiF (200). (author)

  2. Development of confocal micro X-ray fluorescence instrument using two X-ray beams

    A new confocal micro X-ray fluorescence instrument was developed. This instrument has two independent micro X-ray tubes with Mo targets. A full polycapillary X-ray lens was attached to each X-ray tube. Another half polycapillary lens was attached to a silicon drift X-ray detector (SDD). The focal spots of the three lenses were adjusted to a common position. The effects of the excitation of two X-ray beams were investigated. The instrument enabled highly sensitive three-dimensional X-ray fluorescence analysis. We confirmed that the X-ray fluorescence intensity from the sample increased by applying the two independent X-ray tubes in confocal configuration. Elemental depth profiling of black wheat was demonstrated with the result that each element in the surface coat of a wheat grain showed unique distribution

  3. Acoustooptics of x-rays

    Balakhanov, M.V.; Pustovoyt, V.I.; Radzhabov, R.U.; Khabibullayev, P.K.

    Scattering of x-rays by acoustic phonons in crystals during excitation of a noise phonon flux thermodynamically at equilibrium is analyzed from the standpoint of the dynamic diffraction theory, emphasis being put on the differences with the conventional acoustooptic effect attributable to lower frequencies and smaller amplitudes. The structural peak and the diffusional peak are calculated from known relations for the intensity of scattering in each mode, assuming that the Laue condition is satisfied. Interaction of x-rays and an acoustic wave is considered, the conditions for a diffraction peak being determined by the relations between location of that peak and angular dimensions of the structural peak. Experiments were performed in crystals of photosensitive piezoelectric semiconductors with phonon generation. Rectangular or variable-shape voltage pulses with amplitudes up to 800 V were applied to 6-60 ..mu..m thick CdS crystals at repetition rates up to 800 Hz. The electron concentration was (1.3-4.5) x 10/sup 14/ cm/sup -3/ and the electron mobility, according to saturation of the current-voltage characteristics, was differentially in time. The results reveal sharp anisotropy of scattering, evident in the dependence of scattering intensity on the angle of crystal rotation and the resulting lobar scattering pattern. Structural scattering varies exponentially and diffusional scattering varies linearly with increasing amplitude of the applied voltage. According to the dependence of the spectral density of phonon generation on the concentration of charge carriers, the phase of the scattering effect changes upon transition from the structural range to the diffusional range. 8 references, 3 figures.

  4. Soft x-ray interferometry

    The purpose of the soft x-ray interferometry workshop held at Lawrence Berkeley Laboratory was to discuss with the scientific community the proposed technical design of the soft x-ray Fourier-transform spectrometer being developed at the ALS. Different design strategies for the instrument's components were discussed, as well as detection methods, signal processing issues, and how to meet the manufacturing tolerances that are necessary for the instrument to achieve the desired levels of performance. Workshop participants were encouraged to report on their experiences in the field of Fourier transform spectroscopy. The ALS is developing a Fourier transform spectrometer that is intended to operate up to 100 eV. The motivation is solely improved resolution and not the throughput (Jaquinot) or multiplex (Fellgett) advantage, neither of which apply for the sources and detectors used in this spectral range. The proposed implementation of this is via a Mach-Zehnder geometry that has been (1) distorted from a square to a rhombus to get grazing incidence of a suitable angle for 100 eV and (2) provided with a mirror-motion system to make the path difference between the interfering beams tunable. The experiment consists of measuring the emergent light intensity (I(x)) as a function of the path difference (x). The resolving power of the system is limited by the amount of path difference obtainable that is 1 cm (one million half-waves at 200 angstrom wavelength) in the design thus allowing a resolving power of one million. The free spectral range of the system is limited by the closeness with which the function I(x) is sampled. It is proposed to illuminate a helium absorption cell with roughly 1%-band-width light from a monochromator thus allowing one hundred aliases without spectral overlap even for sampling of I(x) at one hundredth of the Nyquist frequency

  5. Macromolecular crystallography research at Trombay

    Neutron diffraction studies of hydrogen positions in small molecules of biological interest at Trombay have provided valuable information that has been used in protein and enzyme structure model-building and in developing hydrogen bond potential functions. The new R-5 reactor is expected to provide higher neutron fluxes and also make possible small-angle neutron scattering studies of large biomolecules and bio-aggregates. In the last few years infrastructure facilities have also been established for macromolecular x-ray crystallography research. Meanwhile, the refinement of carbonic hydrases and lyysozyme structures have been carried out and interesting results obtained on protein dynamics and structure-function relationships. Some interesting presynaptic toxin phospholipases have also taken up for study. (author)

  6. Sample mounts for microcrystal crystallography

    Thorne, Robert E. (Inventor); Stum, Zachary (Inventor); O'Neill, Kevin (Inventor); Kmetko, Jan (Inventor)

    2009-01-01

    Sample mounts (10) for mounting microcrystals of biological macromolecules for X-ray crystallography are prepared by using patterned thin polyimide films (12) that have curvature imparted thereto, for example, by being attached to a curved outer surface of a small metal rod (16). The patterned film (12) preferably includes a tip end (24) for holding a crystal. Preferably, a small sample aperture is disposed in the film for reception of the crystal. A second, larger aperture can also be provided that is connected to the sample aperture by a drainage channel, allowing removal of excess liquid and easier manipulation in viscous solutions. The curvature imparted to the film (12) increases the film's rigidity and allows a convenient scoop-like action for retrieving crystals. The polyimide contributes minimally to background and absorption, and can be treated to obtain desired hydrophobicity or hydrophilicity.

  7. Synchrotron X-ray induced solution precipitation of nanoparticles

    Lee, H J; Hwu, Y; Tsai, W L

    2003-01-01

    By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100-300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (e sub a sub q sup -), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

  8. Discrete tomographic reconstruction of 2D polycrystal orientation maps from X-ray diffraction projections using Gibbs priors

    Rodek, L.; Knudsen, E.; Poulsen, H.F.;

    2005-01-01

    The determination of crystalline structures is a demanding and fundamental task of crystallography. This paper offers a new approach for rendering a 2D grain map of a polycrystal based on an orientation map reconstructed from X-ray diffraction patterns. The orientation map is produced by a Bayesi...... orientations is defined by means of quaternions....

  9. Soft x-ray polarimeter laboratory tests

    Murphy, Kendrah D.; Marshall, Herman L.; Schulz, Norbert S.; Jenks, Kevin; Sommer, Sophie J. B.; Marshall, Eric A.

    2010-07-01

    Multilayer-coated optics can strongly polarize X-rays and are central to a new design of a broad-band, soft X-ray polarimeter. We have begun laboratory work to verify the performance of components that could be used in future soft X-ray polarimetric instrumentation. We have reconfigured a 17 meter beamline facility, originally developed for testing transmission gratings for Chandra, to include a polarized X-ray source, an X-ray-dispersing transmission grating, and a multilayer-coated optic that illuminates a CCD detector. The X-rays produced from a Manson Model 5, multi-anode source are polarized by a multilayer-coated flat mirror. The current configuration allows for a 180 degree rotation of the source in order to rotate the direction of polarization. We will present progress in source characterization and system modulation measurements as well as null and robustness tests.

  10. X-rays for medical use

    Hessenbruch, A.

    1995-11-01

    1995 is the centenary of the discovery of X-rays by the German physicist Wilhelm C Rontgen. In the past hundred years, the new rays have developed from being unknown to finding application in many walks of life, not least in medicine. This is so much so that in common speech the word `x-ray` refers not to a form of radiation but to an X-ray photograph taken for the purposes of diagnosis (as in: `I had an X-ray done to see if my leg was broken`). X-rays are now used routinely, and they are used both for diagnosis and for therapy. This paper will give an outline of the use of X-rays in medicine throughout our present century.

  11. Handbook of X-Ray Data

    Zschornack, Günter

    2007-01-01

    This sourcebook is intended as an X-ray data reference for scientists and engineers working in the field of energy or wavelength dispersive X-ray spectrometry and related fields of basic and applied research, technology, or process and quality controlling. In a concise and informative manner, the most important data connected with the emission of characteristic X-ray lines are tabulated for all elements up to Z = 95 (Americium). This includes X-ray energies, emission rates and widths as well as level characteristics such as binding energies, fluorescence yields, level widths and absorption edges. The tabulated data are characterized and, in most cases, evaluated. Furthermore, all important processes and phenomena connected with the production, emission and detection of characteristic X-rays are discussed. This reference book addresses all researchers and practitioners working with X-ray radiation and fills a gap in the available literature.

  12. Clinical X-ray diagnostics. v. 1

    After introductory remarks on historical aspects of the development of X-ray diagnostics, the physical and technological fundamentals of the generation and recording of radiographs are elaborated. In a comprehensive chapter such topics as X-rays, X-ray tubes, X-ray generators, contrast media, interrelations between X-rays and patients as well as classical and recent methods of recording with regard to geometrical conditions, and of picture quality are outlined. Brief notes on analysis, documentation and filing of radiographs are added. Physico-technological fundamentals of radiation protection, remarks concerning radiation protection in the GDR, and special problems of radiation protection as to X-ray diagnostics are discussed

  13. Radiation safety in X-ray facilities

    The guide specifies the radiation safety requirements for structural shielding and other safety arrangements used in X-ray facilities in medical and veterinary X-ray activities and in industry, research and education. The guide is also applicable to premises in which X-ray equipment intended for radiation therapy and operating at a voltage of less than 25 kV is used. The guide applies to new X-ray facilities in which X-ray equipment that has been used elsewhere is transferred. The radiation safety requirements for radiation therapy X-ray devices operating at a voltage exceeding 25 kV, and for the premices in which such devices are used, are set out in Guide ST 2.2

  14. Radiation safety in X-ray facilities

    NONE

    2001-09-01

    The guide specifies the radiation safety requirements for structural shielding and other safety arrangements used in X-ray facilities in medical and veterinary X-ray activities and in industry, research and education. The guide is also applicable to premises in which X-ray equipment intended for radiation therapy and operating at a voltage of less than 25 kV is used. The guide applies to new X-ray facilities in which X-ray equipment that has been used elsewhere is transferred. The radiation safety requirements for radiation therapy X-ray devices operating at a voltage exceeding 25 kV, and for the premices in which such devices are used, are set out in Guide ST 2.2.

  15. X-ray microlaminography with polycapillary optics

    We demonstrate layer-by-layer x-ray microimaging using polycapillary optics. The depth resolution is achieved without sample or source rotation and in a way similar to classical tomography or laminography. The method takes advantage from large angular apertures of polycapillary optics and from their specific microstructure, which is treated as a coded aperture. The imaging geometry is compatible with polychromatic x-ray sources and with scanning and confocal x-ray fluorescence setups.

  16. X-ray microlaminography with polycapillary optics

    Dąbrowski, K. M.; Dul, D. T.; Wróbel, A.; Korecki, P.

    2013-06-01

    We demonstrate layer-by-layer x-ray microimaging using polycapillary optics. The depth resolution is achieved without sample or source rotation and in a way similar to classical tomography or laminography. The method takes advantage from large angular apertures of polycapillary optics and from their specific microstructure, which is treated as a coded aperture. The imaging geometry is compatible with polychromatic x-ray sources and with scanning and confocal x-ray fluorescence setups.

  17. X-ray spot film device

    Improvements are described in an X-ray spot film device which is used in conjunction with an X-ray table to make a selected number of radiographic exposures on a single film and to perform fluoroscopic examinations. To date, the spot film devices consist of two X-ray field defining masks, one of which is moved manually. The present device is more convenient to use and speeds up the procedure. (U.K.)

  18. X-ray microlaminography with polycapillary optics

    Dabrowski, K. M.; Dul, D. T.; Wrobel, A.; Korecki, P. [Institute of Physics, Jagiellonian University, Reymonta 4, 30-059 Krakow (Poland)

    2013-06-03

    We demonstrate layer-by-layer x-ray microimaging using polycapillary optics. The depth resolution is achieved without sample or source rotation and in a way similar to classical tomography or laminography. The method takes advantage from large angular apertures of polycapillary optics and from their specific microstructure, which is treated as a coded aperture. The imaging geometry is compatible with polychromatic x-ray sources and with scanning and confocal x-ray fluorescence setups.

  19. Applications of soft x-ray lasers

    Skinner, C.H.

    1993-08-01

    The high brightness and short pulse duration of soft x-ray lasers provide unique advantages for novel applications. Imaging of biological specimens using x-ray lasers has been demonstrated by several groups. Other applications to fields such as chemistry, material science, plasma diagnostics, and lithography are beginning to emerge. We review the current status of soft x-ray lasers from the perspective of applications, and present an overview of the applications currently being developed.

  20. X-ray data booklet. Revision

    A compilation of data is presented. Included are properties of the elements, electron binding energies, characteristic x-ray energies, fluorescence yields for K and L shells, Auger energies, energy levels for hydrogen-, helium-, and neonlike ions, scattering factors and mass absorption coefficients, and transmission bands of selected filters. Also included are selected reprints on scattering processes, x-ray sources, optics, x-ray detectors, and synchrotron radiation facilities

  1. X-ray data booklet. Revision

    Vaughan, D. (ed.)

    1986-04-01

    A compilation of data is presented. Included are properties of the elements, electron binding energies, characteristic x-ray energies, fluorescence yields for K and L shells, Auger energies, energy levels for hydrogen-, helium-, and neonlike ions, scattering factors and mass absorption coefficients, and transmission bands of selected filters. Also included are selected reprints on scattering processes, x-ray sources, optics, x-ray detectors, and synchrotron radiation facilities. (WRF)

  2. Novel optics for X-ray telescopes

    Hudec, René; Pína, L.; Semencová, V.; Inneman, A.; Skulinová, Michaela; Nekola, Martin

    Berlin : Springer, 2009 - (Brandl, B.), s. 1-8 ISBN 978-90-481-2232-5. [400 Years of Astronomical Telescopes. Leiden (NL), 29.09.2008-02.10.2008] R&D Projects: GA AV ČR IAAX01220701; GA ČR GP202/07/P510 Institutional research plan: CEZ:AV0Z10030501 Keywords : X-ray telescopes * X-ray optics * X-ray astronomy Subject RIV: BN - Astronomy, Celestial Mechanics, Astrophysics

  3. Polarizable Atomic Multipole X-Ray Refinement: Hydration Geometry and Application to Macromolecules

    Fenn, Timothy D.; Schnieders, Michael J; Brunger, Axel T.; Pande, Vijay S.

    2010-01-01

    We recently developed a polarizable atomic multipole refinement method assisted by the AMOEBA force field for macromolecular crystallography. Compared to standard refinement procedures, the method uses a more rigorous treatment of x-ray scattering and electrostatics that can significantly improve the resultant information contained in an atomic model. We applied this method to high-resolution lysozyme and trypsin data sets, and validated its utility for precisely describing biomolecular elect...

  4. Multi-wavelength anomalous diffraction at high x-ray intensity

    Son, Sang-Kil; Santra, Robin

    2011-01-01

    The multi-wavelength anomalous diffraction (MAD) method is used to determine phase information in x-ray crystallography by employing dispersion corrections from heavy atoms on coherent x-ray scattering. X-ray free-electron lasers (FELs) show promise for revealing the structure of single molecules or nanocrystals within femtoseconds, but the phase problem remains largely unsolved. Due to the ultrabrightness of x-ray FEL, samples experience severe electronic radiation damage, especially to heavy atoms, which hinders direct implementation of the MAD method with x-ray FELs. We propose a generalized version of the MAD phasing method at high x-ray intensity. We demonstrate the existence of a Karle--Hendrickson-type equation for the MAD method in the high-intensity regime and calculate relevant coefficients with detailed electronic damage dynamics of heavy atoms. Our results show that the bleaching effect on the scattering strength of the heavy atoms can be advantageous to the phasing method. The present method offe...

  5. Experimental measurement of metal multilayer x-ray reflectivity degradation due to intense x-ray flux

    The degradation of the x-ray reflection characteristics of metal multilayer Bragg diffractors due to intense x-ray flux was investigated. The Z-pinch plasma produced by PROTO II of Sandia National Laboratories, Albuquerque, New Mexico, was used as the source. The plasma generated total x-ray yields of as much as 40 kJ with up to 15 kJ in the neon-, hydrogen-, and helium-like resonance lines in nominal 20-ns pulses. Molybdenum-carbon, palladium-carbon, and tungsten-carbon metal multilayers were placed at 50 and 150 cm from the plasma center. The multilayers were at nominal angels of 50 and 100 to diffract the neon resonance lines. The time-integated x-ray reflection of the metal multilayers was monitored by x-ray film. Data for two separate shots were analyzed. For a pure neon gas shot at a power level of 420 TW, the reflectivity of the multilayer at 15 cm decayed rapidly with respect to the still-rising signal of the multilayer at 150 cm. The onset time of the decay corresponded to an integrated dose of 5.27 J/cm2. For a neon implosion onto a vanadium-doped polyacrylic acid foam target shot, detailed modeling was attempted. The spectral flux was determined with data from 5 XRD channels and deconvolved using the code SHAZAM. The observed decay in reflectivity was assumed to correspond to the melting of the first tungsten layer

  6. X-ray transient AGN and galaxies

    Grupe, D.

    2001-01-01

    X-ray transience is the most extreme form of variability observed in AGN or normal in-active galaxies. While factors of 2-3 on timescales of days to years are quite commen among AGN, X-ray transients appear only once and vanish from the X-ray sky years later. The ROSAT All-Sky Survey was the tool to discover these sources. X-ray transience in AGN or galaxies can be caused by dramatic changes in the accretion rate of the central black hole or by changes of the properties of the accretion disk.

  7. Microfabrication of hard x-ray lenses

    Stöhr, Frederik

    characterization details that cannot be obtained by other means. The respective x-ray techniques largely benefit from continuously improved x-ray sources, x-ray detectors and x-ray optics. For instance, some techniques aiming for structural investigation of poly-crystalline materials directly benefit from more...... by their potential for compact integration, which makes them cost-effective, easy to handle and stable on-axis optics. A Si-CRL comprises multiple bi-parabolic cylindrical cavities. The bi-parabolic patterns are defined lithographically and vertically transferred into the Si substrate using deep reactive ion etching...

  8. Advanced X-ray diffractive optics

    Vila-Comamala, J.; Jefimovs, K.; Pilvi, T.; Ritala, M; Sarkar, S S; Solak, H H; Guzenko, V.A.; Stampanoni, M.; Marone, F.; J. Raabe; G. Tzvetkov; Fink, R H; Grolimund, D.; Borca, C.N.; Kaulich, B

    2009-01-01

    X-ray microscopy greatly bene�ts from the advances in x-ray optics. At the Paul Scherrer Institut, developments in x-ray di�ractive optics include the manufacture and optimization of Fresnel zone plates (FZPs) and di�ractive optical elements for both soft and hard x-ray regimes. In particular, we demonstrate here a novel method for the production of ultra-high resolution FZPs. This technique is based on the deposition of a zone plate material (iridium) onto the sidewalls of a p...

  9. Microscopic x-ray luminescence computed tomography

    Zhang, Wei; Zhu, Dianwen; Zhang, Kun; Li, Changqing

    2015-03-01

    X-ray luminescence computed tomography (XLCT) was emerged as a new hybrid imaging modality, in which the x-rays are used to excite phosphors emitting optical photons to be measured for imaging. In this paper, we reported a microscopic x-ray luminescence computed tomography (microXLCT) with a spatial resolution up to hundreds of micrometers for deep targets. We use a superfine x-ray pencil beam to scan the phosphor targets. The superfine x-ray pencil beam is generated by a small collimator mounted in front of a powerful x-ray tube (93212, Oxford Instrument). A CT detector is used to image the x-ray beam. We have generated an x-ray beam with a diameter of 192 micrometers with a collimator of 100 micrometers in diameter. The emitted optical photons on the top surface of phantom are reflected by a mirror and acquired by an electron multiplier charge-coupled device (EMCCD) camera (C9100-13, Hamamatsu Photonics). The microXLCT imaging system is built inside an x-ray shielding and light tight cabinet. The EMCCD camera is placed in a lead box. All the imaging components are controlled by a VC++ program. The optical photon propagation is modeled with the diffusion equation solved by the finite element method. We have applied different regularization methods including L2 and L1 in the microXLCT reconstruction algorithms. Numerical simulations and phantom experiments are used to validate the microXLCT imaging system.

  10. Imaging with x-ray lasers

    Da Silva, L.B.; Cauble, B.; Frieders, G.; Koch, J.A.; MacGowan, B.J.; Matthews, D.L.; Mrowka, S.; Ress, D.; Trebes, J.E.; Weiland, T.L.

    1993-11-01

    Collisionally pumped soft x-ray lasers now operate over a wavelength range extending from 35--300 {Angstrom}. These sources have high peak brightness and are now being utilized for x-ray imaging and plasma interferometry. In this paper we will describe our efforts to probe long scalelength plasmas using Moire deflectrometry and soft x-ray imaging. The progress in the development of short pulse x-ray lasers using a double pulse irradiation technique which incorporates a travelling wave pump will also be presented.

  11. X-ray Emission from Elliptical Galaxies

    Sarazin, Craig L.

    1996-01-01

    Elliptical galaxies are generally luminous sources of X-ray radiation, and contain large amounts of hot, interstellar gas. In the brighter X-ray galaxies, the inferred masses of hot gas are consistent with those expected given the present rates of stellar mass loss. The required rates of heating of the gas are also roughly consistent with those expected from the motions of gas losing stars. X-ray observations, particularly X-ray spectra, require a low rate of Type Ia supernova heating and che...

  12. X-ray Observations of Planetary Nebulae

    Guerrero, M. A.; Chu, Y.-H.; Gruendl, R A

    2003-01-01

    Planetary nebulae (PNe) are an exciting addition to the zoo of X-ray sources. Recent Chandra and XMM-Newton observations have detected diffuse X-ray emission from shocked fast winds in PN interiors as well as bow-shocks of fast collimated outflows impinging on the nebular envelope. Point X-ray sources associated with PN central stars are also detected, with the soft X-ray (>0.5 keV) emission from instability shocks in the fast stellar wind itself or from a low-mass companion's coronal activit...

  13. Hard X-ray Modulation Telescope

    LU Fangjun

    2011-01-01

    The Hard X-ray Modulation Telescope (HXMT) will be China's first astronomical satellite. On board HXMT there are three kinds of slat-collimated telescopes, the High Energy X-ray Telescope (HE, 20-250 keV, 5000 cm^2), the Medium Energy X-ray Telescope (ME, 5-30 keV, 952 cm^2), and the Low Energy X-ray Telescope (LE, 1-15 keV, 384 cm^2).

  14. X-ray pulsar rush in 1998

    We present recent remarkable topics about discoveries of X-ray pulsars. 1. Pulsations from two Soft Gamma-ray Repeaters: These pulsars have enormously strong magnetic field (B ∼ 1015 G), thus these are called as 'magnetar', new type of X-ray pulsars. 2. New Crab-like pulsars: These discoveries lead to suggesting universality of Crab-like pulsars. 3. An X-ray bursting millisecond pulsar: This is strong evidence for the recycle theory of generating radio millisecond pulsars. 4. X-ray pulsar rush in the SMC: This indicates the younger star formation history in the SMC. (author)

  15. The Lunar X-ray Observatory (LXO)

    Porter, F. Scott

    2008-01-01

    X-ray emission from charge exchange recombination between the highly ionized solar wind and neutral material i n Earth's magnetosheath has complicated x-ray observations of celestial objects with x-ray observatories including ROSAT, Chandra, XMM-Newton, and Suzaku. However, the charge-exchange emission can also be used as an important diagnostic of the solar-wind interacting with the magnetosheath. Soft x-ray observations from low-earth orbit or even the highly eccentric orbits of Chandra and XMM-Newton are likely superpositions of the celestial object of interest, the true extra-solar soft x-ray background, geospheric charge exchange, and heliospheric charge exchange. We show that with a small x-ray telescope placed either on the moon, in a similar vein as the Apollo ALSOP instruments, or at a stable orbit near L1, we can begin t o disentangle the complicated emission structure in the soft x-ray band. Here we present initial results of a feasibility study recently funded by NASA t o place a small x-ray telescope on the lunar surface. The telescope operates during lunar night to observe charge exchange interactions between the solar wind and magnetospheric neutrals, between the solar wind and the lunar atmosphere, and an unobstructed view of the soft x-ray background without the geospheric component.

  16. Ultrashort X-ray pulse science

    Chin, Alan Hap [Univ. of California, Berkeley, CA (US). Dept. of Physics; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    1998-05-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90{sup o} Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated {approx} 300 fs, 30 keV (0.4 {angstrom}) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has

  17. X-ray pulsars: a review

    Caballero, I

    2012-01-01

    Accreting X-ray pulsars are among the most luminous objects in the X-ray sky. In highly magnetized neutron stars (B~10^12 G), the flow of matter is dominated by the strong magnetic field. The general properties of accreting X-ray binaries are presented, focusing on the spectral characteristics of the systems. The use of cyclotron lines as a tool to directly measure a neutron star's magnetic field and to test the theory of accretion are discussed. We conclude with the current and future prospects for accreting X-ray binary studies.

  18. Ultrashort X-ray pulse science

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90o Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ∼ 300 fs, 30 keV (0.4 (angstrom)) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been

  19. X-rays pinpoint tumour targets

    When a surgeon in Birmingham used an X-ray photograph to guide the removal of a needle buried in a woman's hand in January 1896, it became the first X-ray guided operation in medical history. Since then X-rays have been widely used for medical imaging, and 'computed tomography' now provides us with exquisite 2D cross-sectional images of the human body. The technique creates images by passing X-rays along a plane through the body and recording the transmitted signals from various angles. A 'CT scan' lets us locate and visualize tumours with a resolution of 1 mm. But there is more to X-rays than imaging - they can also treat patients by killing cancerous tumours. When X-rays interact with tissue, they release highly reactive radicals that break the double strands in DNA molecules and cause the rapidly dividing cancerous cells to die. But because X-rays kill both healthy and diseased tissue in equal measure, it is vital to minimize the radiation received by healthy organs and tissue surrounding the tumour. The goal of radiotherapy is to find the precise location of a tumour using a CT scan - or other imaging technique - and then concentrate the X-rays on it to destroy the diseased tissue. In the August issue of Physics World Matin Durrani describes how intensity-modulated radiation therapy can deliver precise doses of X-rays to tumours while leaving surrounding, healthy tissue relatively unscathed. (U.K.)

  20. Single molecule imaging with longer x-ray laser pulses

    Martin, Andrew V; Caleman, Carl; Quiney, Harry M

    2015-01-01

    In serial femtosecond crystallography, x-ray laser pulses do not need to outrun all radiation damage processes because Bragg diffraction exceeds the damage-induced background scattering for longer pulses ($\\sim$ 50--100 fs). This is due to a "self-gating pulse" effect whereby damage terminates Bragg diffraction prior to the pulse completing its passage through the sample, as if that diffraction were produced by a shorter pulse of equal fluence. We show here that a similar gating effect applies to single molecule diffraction with respect to spatially uncorrelated damage processes like ionization and ion diffusion. The effect is clearly seen in calculations of the diffraction contrast, by calculating the diffraction of average structure separately to the diffraction from statistical fluctuations of the structure due to damage ("damage noise"). Our results suggest that sub-nanometer single molecule imaging with longer pulses, like those produced at currently operating facilities, should not yet be ruled out. The...