http://journals.iucr.org/s/issues/2013/04/00/isscontsbdy.html Synchrotron radiation research is rapidly expanding with many new sources of radiation being created globally. Synchrotron radiation plays a leading role in pure science and in emerging technologies. The Journal of Synchrotron Radiation provides comprehensive coverage of the entire field of synchrotron radiation research including instrumentation, theory, computing and scientific applications in areas such as biology, nanoscience and materials science. Rapid publication ensures an up-to-date information resource for scientists and engineers in the field. en Copyright (c) 2013 International Union of Crystallography 2013-05-20 International Union of Crystallography International Union of Crystallography http://journals.iucr.org urn:issn:0909-0495 Synchrotron radiation research is rapidly expanding with many new sources of radiation being created globally. Synchrotron radiation plays a leading role in pure science and in emerging technologies. The Journal of Synchrotron Radiation provides comprehensive coverage of the entire field of synchrotron radiation research including instrumentation, theory, computing and scientific applications in areas such as biology, nanoscience and materials science. Rapid publication ensures an up-to-date information resource for scientists and engineers in the field. text/html Journal of Synchrotron Radiation, Volume 20, Part 4, 2013 text yearly 6 2002-01-01T00:00+00:00 4 20 2013-05-20 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation 517 urn:issn:0909-0495 med@iucr.org May 2013 2013-05-20 http://journals.iucr.org/logos/rss10s.gif http://journals.iucr.org/s/issues/2013/04/00/isscontsbdy.html Still image http://scripts.iucr.org/cgi-bin/paper?ve5020 Aiming at advancing storage-ring-based ultrafast X-ray science, over the past few years many upgrades have been undertaken to continue improving beamline performance and photon flux at the Femtoslicing facility at BESSY II. In this article the particular design upgrade of one of the key optical components, the zone-plate monochromator (ZPM) beamline, is reported. The beamline is devoted to optical pump/soft X-ray probe applications with 100 fs (FWHM) X-ray pulses in the soft X-ray range at variable polarization. A novel approach consisting of an array of nine off-axis reflection zone plates is used for a gapless coverage of the spectral range between 410 and 1333 eV at a designed resolution of E/ΔE = 500 and a pulse elongation of only 30 fs. With the upgrade of the ZPM the following was achieved: a smaller focus, an improved spectral resolution and bandwidth as well as excellent long-term stability. The beamline will enable a new class of ultrafast applications with variable optical excitation wavelength and variable polarization. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Brzhezinskaya, M. Firsov, A. Holldack, K. Kachel, T. Mitzner, R. Pontius, N. Schmidt, J.-S. Sperling, M. Stamm, C. Föhlisch, A. Erko, A. 2013-05-01 doi:10.1107/S0909049513008613 International Union of Crystallography The design and commissioning of a novel monochromator approach based on off-axis reflection zone-plate arrays for experiments with ultrashort soft X-ray pulses is described. EN femtosecond X-ray pulses storage ring elliptical undulators slicing diffractive optics reflection zone plates time-resolved X-ray spectroscopy Aiming at advancing storage-ring-based ultrafast X-ray science, over the past few years many upgrades have been undertaken to continue improving beamline performance and photon flux at the Femtoslicing facility at BESSY II. In this article the particular design upgrade of one of the key optical components, the zone-plate monochromator (ZPM) beamline, is reported. The beamline is devoted to optical pump/soft X-ray probe applications with 100 fs (FWHM) X-ray pulses in the soft X-ray range at variable polarization. A novel approach consisting of an array of nine off-axis reflection zone plates is used for a gapless coverage of the spectral range between 410 and 1333 eV at a designed resolution of E/ΔE = 500 and a pulse elongation of only 30 fs. With the upgrade of the ZPM the following was achieved: a smaller focus, an improved spectral resolution and bandwidth as well as excellent long-term stability. The beamline will enable a new class of ultrafast applications with variable optical excitation wavelength and variable polarization. text/html A novel monochromator for experiments with ultrashort X-ray pulses text 4 20 2013-05-01 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?ve5015 The interplay between the angle-dependent X-ray reflectivity, X-ray absorption and the photoelectron attenuation length in the photoelectron emission process determines the optimal X-ray incidence angle that maximizes the photoelectron signal. Calculations in the wide VUV to the hard X-ray energy range show that the optimal angle becomes more grazing with increasing energy, from a few tens of degrees at 50 eV to about one degree at 3.5 keV. This is accompanied by an intensity gain of a few tens of times, as long as the X-ray footprint on the sample stays within the analyzer field of view. This trend is fairly material-independent. The obtained results bear immediate implications for the design of (synchrotron-based) photoelectron spectrometers. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Strocov, V.N. 2013-05-01 doi:10.1107/S0909049513007747 International Union of Crystallography The interplay between X-ray reflectivity, X-ray absorption and photoelectron attenuation in the photoelectron emission process is analyzed. The optimal X-ray incidence angle to maximize the photoelectron signal is evaluated in a wide VUV to hard X-ray energy range. EN photoemission X-ray absorption photoelectron attenuation photoelectron spectrometers The interplay between the angle-dependent X-ray reflectivity, X-ray absorption and the photoelectron attenuation length in the photoelectron emission process determines the optimal X-ray incidence angle that maximizes the photoelectron signal. Calculations in the wide VUV to the hard X-ray energy range show that the optimal angle becomes more grazing with increasing energy, from a few tens of degrees at 50 eV to about one degree at 3.5 keV. This is accompanied by an intensity gain of a few tens of times, as long as the X-ray footprint on the sample stays within the analyzer field of view. This trend is fairly material-independent. The obtained results bear immediate implications for the design of (synchrotron-based) photoelectron spectrometers. text/html Optimization of the X-ray incidence angle in photoelectron spectrometers text 4 20 2013-05-01 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?wa5048 This paper reports X-ray microtomographic visualization of the microorganism Escherichia coli overexpressing a metalloprotein ferritin. The three-dimensional distribution of linear absorption coefficients determined using a synchrotron radiation microtomograph with a simple projection geometry revealed that the X-ray absorption was homogeneously distributed, suggesting that every E. coli cell was labeled with the ferritin. The ferritin-expressing E. coli exhibited linear absorption coefficients comparable with those of phosphotungstic acid stained cells. The submicrometer structure of the ferritin-expressing E. coli cells was visualized by Zernike phase contrast using an imaging microtomograph equipped with a Fresnel zone plate. The obtained images revealed curved columnar or bunching oval structures corresponding to the E. coli cells. These results indicate that the metalloprotein overexpression facilitates X-ray visualization of three-dimensional cellular structures of biological objects. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Mizutani, R. Taguchi, K. Ohtsuka, M. Kimura, M. Takeuchi, A. Uesugi, K. Suzuki, Y. 2013-05-01 doi:10.1107/S0909049513008467 International Union of Crystallography Three-dimensional structures of Escherichia coli overexpressing a metalloprotein ferritin were visualized by synchrotron radiation microtomography. EN bacteria ferritin high-Z element micro-CT three-dimensional structure This paper reports X-ray microtomographic visualization of the microorganism Escherichia coli overexpressing a metalloprotein ferritin. The three-dimensional distribution of linear absorption coefficients determined using a synchrotron radiation microtomograph with a simple projection geometry revealed that the X-ray absorption was homogeneously distributed, suggesting that every E. coli cell was labeled with the ferritin. The ferritin-expressing E. coli exhibited linear absorption coefficients comparable with those of phosphotungstic acid stained cells. The submicrometer structure of the ferritin-expressing E. coli cells was visualized by Zernike phase contrast using an imaging microtomograph equipped with a Fresnel zone plate. The obtained images revealed curved columnar or bunching oval structures corresponding to the E. coli cells. These results indicate that the metalloprotein overexpression facilitates X-ray visualization of three-dimensional cellular structures of biological objects. text/html X-ray microtomographic visualization of Escherichia coli by metalloprotein overexpression text 4 20 2013-05-01 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?wa5051 Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Madden, J.T. Toth, S.J. Dettmar, C.M. Newman, J.A. Oglesbee, R.A. Hedderich, H.G. Everly, R.M. Becker, M. Ronau, J.A. Buchanan, S.K. Cherezov, V. Morrow, M.E. Xu, S. Ferguson, D. Makarov, O. Das, C. Fischetti, R. Simpson, G.J. 2013-05-03 doi:10.1107/S0909049513007942 International Union of Crystallography Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction for combined single-platform analysis, examining the viability of NLO microscopy as an alternative to the conventional X-ray raster scan for the purposes of sample centering. Second-harmonic generation microscopy and two-photon excited ultraviolet fluorescence microscopy were evaluated for crystal detection, and assessed by X-ray raster scanning. EN XRD NLO SHG SONICC centering protein TPE-UVF microscopy LCP two-photon Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. text/html Integrated nonlinear optical imaging microscope for on-axis crystal detection and centering at a synchrotron beamline text 4 20 2013-05-03 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?ie5091 The resonant scattering and diffraction beamline P09 at PETRA III is designed for X-ray experiments requiring small beams, energy tunability, variable polarization and high photon flux. It is highly flexible in terms of beam size and offers full higher harmonic suppression. A state-of-the-art double phase-retarder set-up provides variable linear or circular polarization. A high-precision Psi-diffractometer and a heavy-load diffractometer in horizontal Psi-geometry allow the accommodation of a wide variety of sample environments. A 14 T cryo-magnet is available for scattering experiments in magnetic fields. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Strempfer, J. Francoual, S. Reuther, D. Shukla, D.K. Skaugen, A. Schulte-Schrepping, H. Kracht, T. Franz, H. 2013-05-04 doi:10.1107/S0909049513009011 International Union of Crystallography The resonant scattering and diffraction beamline P09 at the new third-generation synchrotron radiation source PETRA III has been designed for resonant and non-resonant scattering experiments in the energy range from 2.7 keV to 32 keV requiring small beams, energy tunability, variable polarization and high photon flux. EN resonant scattering beamline phase retarder mirror diffractometer The resonant scattering and diffraction beamline P09 at PETRA III is designed for X-ray experiments requiring small beams, energy tunability, variable polarization and high photon flux. It is highly flexible in terms of beam size and offers full higher harmonic suppression. A state-of-the-art double phase-retarder set-up provides variable linear or circular polarization. A high-precision Psi-diffractometer and a heavy-load diffractometer in horizontal Psi-geometry allow the accommodation of a wide variety of sample environments. A 14 T cryo-magnet is available for scattering experiments in magnetic fields. text/html Resonant scattering and diffraction beamline P09 at PETRA III text 4 20 2013-05-04 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?ve5019 X-ray crystal monochromators exposed to white-beam X-rays in third-generation synchrotron light sources are subject to thermal deformations that must be minimized using an adequate cooling system. A new approach was used to measure the crystal shape profile and slope of several cryogenically cooled (liquid nitrogen) silicon monochromators as a function of beam power in situ and under heat load. The method utilizes multiple angular scans across the Bragg peak (rocking curve) at various vertical positions of a narrow-gap slit downstream from the monochromator. When increasing the beam power, the surface of the liquid-nitrogen-cooled silicon crystal deforms from a concave shape at low heat load to a convex shape at high heat load, passing through an approximately flat shape at intermediate heat load. Finite-element analysis is used to calculate the crystal thermal deformations. The simulated crystal profiles and slopes are in excellent agreement with experiments. The parameters used in simulations, such as material properties, absorbed power distribution on the crystal and cooling boundary conditions, are described in detail as they are fundamental for obtaining accurate results. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Zhang, L. Sánchez del Río, M. Monaco, G. Detlefs, C. Roth, T. Chumakov, A.I. Glatzel, P. 2013-05-08 doi:10.1107/S0909049513009436 International Union of Crystallography The shape of cryogenically cooled monochromator crystals deformed by the heat load of the X-ray beam is derived from rocking curve measurements at various vertical positions of a narrow-gap slit downstream from the monochromator. Experimentally, it is observed that the crystal shape changes from concave to convex when beam power increases. The observations are accurately modelled by finite-element analysis, showing an excellent quantitative agreement with experiments. EN silicon crystal X-ray monochromator cryogenic cooling liquid nitrogen thermal deformation finite element heat load experiment rocking curve in situ metrology X-ray crystal monochromators exposed to white-beam X-rays in third-generation synchrotron light sources are subject to thermal deformations that must be minimized using an adequate cooling system. A new approach was used to measure the crystal shape profile and slope of several cryogenically cooled (liquid nitrogen) silicon monochromators as a function of beam power in situ and under heat load. The method utilizes multiple angular scans across the Bragg peak (rocking curve) at various vertical positions of a narrow-gap slit downstream from the monochromator. When increasing the beam power, the surface of the liquid-nitrogen-cooled silicon crystal deforms from a concave shape at low heat load to a convex shape at high heat load, passing through an approximately flat shape at intermediate heat load. Finite-element analysis is used to calculate the crystal thermal deformations. The simulated crystal profiles and slopes are in excellent agreement with experiments. The parameters used in simulations, such as material properties, absorbed power distribution on the crystal and cooling boundary conditions, are described in detail as they are fundamental for obtaining accurate results. text/html Thermal deformation of cryogenically cooled silicon crystals under intense X-ray beams: measurement and finite-element predictions of the surface shape text 4 20 2013-05-08 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?pp5034 An imaging model and an image reconstruction algorithm for a transparent X-ray beam imaging and position measuring instrument are presented. The instrument relies on a coded aperture camera to record magnified images of the footprint of the incident beam on a thin foil placed in the beam at an oblique angle. The imaging model represents the instrument as a linear system whose impulse response takes into account the image blur owing to the finite thickness of the foil, the shape and size of camera's aperture and detector's point-spread function. The image reconstruction algorithm first removes the image blur using the modelled impulse response function and then corrects for geometrical distortions caused by the foil tilt. The performance of the image reconstruction algorithm was tested in experiments at synchrotron radiation beamlines. The results show that the proposed imaging system produces images of the X-ray beam cross section with a quality comparable with images obtained using X-ray cameras that are exposed to the direct beam. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Kachatkou, A. Kyele, N. Scott, P. van Silfhout, R. 2013-05-18 doi:10.1107/S0909049513011060 International Union of Crystallography This paper presents an imaging model and a reconstruction algorithm for obtaining X-ray beam cross-sectional images from the data recorded by an X-ray beam monitor based on a coded aperture camera that collects radiation scattered from a thin foil placed in the X-ray beam at an oblique angle. EN X-ray imaging pinhole camera scattering measurements deconvolution beam diagnostics An imaging model and an image reconstruction algorithm for a transparent X-ray beam imaging and position measuring instrument are presented. The instrument relies on a coded aperture camera to record magnified images of the footprint of the incident beam on a thin foil placed in the beam at an oblique angle. The imaging model represents the instrument as a linear system whose impulse response takes into account the image blur owing to the finite thickness of the foil, the shape and size of camera's aperture and detector's point-spread function. The image reconstruction algorithm first removes the image blur using the modelled impulse response function and then corrects for geometrical distortions caused by the foil tilt. The performance of the image reconstruction algorithm was tested in experiments at synchrotron radiation beamlines. The results show that the proposed imaging system produces images of the X-ray beam cross section with a quality comparable with images obtained using X-ray cameras that are exposed to the direct beam. text/html In situ X-ray beam imaging using an off-axis magnifying coded aperture camera system text 4 20 2013-05-18 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?ie5088 One-dimensional kinoform and prism refractive lenses with large aperture and high transmittance at 22 keV have been investigated. A 12.0 µm focus size (full width at half-maximum) and an effective aperture of 0.85 mm, at a focal length of 705 mm and 21.747 keV, were achieved. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Fukui, H. Simon, M. Nazmov, V. Mohr, J. Evans-Lutterodt, K. Stein, A. Baron, A.Q.R. 2013-05-18 doi:10.1107/S0909049513011722 International Union of Crystallography Large-aperture focusing lenses have been evaluated for momentum-resolved and flux-limited spectroscopy with hard X-rays. EN refractive lens large aperture hard X-ray focusing momentum-resolved spectroscopy One-dimensional kinoform and prism refractive lenses with large aperture and high transmittance at 22 keV have been investigated. A 12.0 µm focus size (full width at half-maximum) and an effective aperture of 0.85 mm, at a focal length of 705 mm and 21.747 keV, were achieved. text/html Large-aperture refractive lenses for momentum-resolved spectroscopy with hard X-rays text 4 20 2013-05-18 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?hf5225 The evaluation of uncertainty in temperature-dependent EXAFS measurements is discussed, considering the specific case of a recent experiment performed on CdTe. EXAFS at both Cd and Te K-edges was measured at different times and at different beamlines in a temperature range from 5 to 300 K. Attention is focused on the nearest-neighbours parameters: bond thermal expansion, parallel and perpendicular mean-square relative displacements and the third cumulant. Different causes of uncertainty, a comparison of experimental results with theoretical models, the difference between EXAFS and crystallographic thermal expansions and the meaning of the third cumulant are discussed. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Abd el All, N. Thiodjio Sendja, B. Grisenti, R. Rocca, F. Diop, D. Mathon, O. Pascarelli, S. Fornasini, P. 2013-05-21 doi:10.1107/S0909049513012053 International Union of Crystallography The uncertainty in temperature-dependent EXAFS measurements on CdTe is discussed, focusing on the first-shell bond thermal expansion, parallel and perpendicular mean square relative displacements and the third cumulant. EN EXAFS thermal expansion mean-square relative displacements Einstein model Debye model The evaluation of uncertainty in temperature-dependent EXAFS measurements is discussed, considering the specific case of a recent experiment performed on CdTe. EXAFS at both Cd and Te K-edges was measured at different times and at different beamlines in a temperature range from 5 to 300 K. Attention is focused on the nearest-neighbours parameters: bond thermal expansion, parallel and perpendicular mean-square relative displacements and the third cumulant. Different causes of uncertainty, a comparison of experimental results with theoretical models, the difference between EXAFS and crystallographic thermal expansions and the meaning of the third cumulant are discussed. text/html Accuracy evaluation in temperature-dependent EXAFS measurements of CdTe text 4 20 2013-05-21 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?hf5227 The ability of molecular dynamics (MD) simulations to support the analysis of X-ray absorption fine-structure (XAFS) data for metals is evaluated. The low-order cumulants (ΔR, σ2, C3) for XAFS scattering paths are calculated for the metals Cu, Ni, Fe, Ti and Au at 300 K using 28 interatomic potentials of the embedded-atom method type. The MD cumulant predictions were evaluated within a cumulant expansion XAFS fitting model, using global (path-independent) scaling factors. Direct simulations of the corresponding XAFS spectra, χ(R), are also performed using MD configurational data in combination with the FEFF ab initio code. The cumulant scaling parameters compensate for differences between the real and effective scattering path distributions, and for any errors that might exist in the MD predictions and in the experimental data. The fitted value of ΔR is susceptible to experimental errors and inadvertent lattice thermal expansion in the simulation crystallites. The unadjusted predictions of σ2 vary in accuracy, but do not show a consistent bias for any metal except Au, for which all potentials overestimate σ2. The unadjusted C3 predictions produced by different potentials display only order-of-magnitude consistency. The accuracy of direct simulations of χ(R) for a given metal varies among the different potentials. For each of the metals Cu, Ni, Fe and Ti, one or more of the tested potentials was found to provide a reasonable simulation of χ(R). However, none of the potentials tested for Au was sufficiently accurate for this purpose. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Karolewski, M.A. Cavell, R.G. Gordon, R.A. Glover, C.J. Cheah, M. Ridgway, M.C. 2013-05-21 doi:10.1107/S0909049513010303 International Union of Crystallography Molecular dynamics simulations that employ different interatomic potentials are found to vary significantly in their predictions of XAFS scattering path cumulants and synthetic XAFS spectra for metallic solids. EN XAFS metals molecular dynamics potentials cumulants The ability of molecular dynamics (MD) simulations to support the analysis of X-ray absorption fine-structure (XAFS) data for metals is evaluated. The low-order cumulants (ΔR, σ2, C3) for XAFS scattering paths are calculated for the metals Cu, Ni, Fe, Ti and Au at 300 K using 28 interatomic potentials of the embedded-atom method type. The MD cumulant predictions were evaluated within a cumulant expansion XAFS fitting model, using global (path-independent) scaling factors. Direct simulations of the corresponding XAFS spectra, χ(R), are also performed using MD configurational data in combination with the FEFF ab initio code. The cumulant scaling parameters compensate for differences between the real and effective scattering path distributions, and for any errors that might exist in the MD predictions and in the experimental data. The fitted value of ΔR is susceptible to experimental errors and inadvertent lattice thermal expansion in the simulation crystallites. The unadjusted predictions of σ2 vary in accuracy, but do not show a consistent bias for any metal except Au, for which all potentials overestimate σ2. The unadjusted C3 predictions produced by different potentials display only order-of-magnitude consistency. The accuracy of direct simulations of χ(R) for a given metal varies among the different potentials. For each of the metals Cu, Ni, Fe and Ti, one or more of the tested potentials was found to provide a reasonable simulation of χ(R). However, none of the potentials tested for Au was sufficiently accurate for this purpose. text/html Predicting XAFS scattering path cumulants and XAFS spectra for metals (Cu, Ni, Fe, Ti, Au) using molecular dynamics simulations text 4 20 2013-05-21 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation research papers 0 0 http://scripts.iucr.org/cgi-bin/paper?vv5059 A multipurpose six-axis κ-diffractometer, together with the brilliance of the ESRF light source and a CCD area detector, has been explored for studying epitaxial relations and crystallinity in thin film systems. The geometrical flexibility of the six-axis goniometer allows measurement of a large volume in reciprocal space, providing an in-depth understanding of sample crystal relationships. By a set of examples of LaAlO3 thin films deposited by the atomic layer deposition technique, the possibilities of the set-up are presented. A fast panoramic scan provides determination of the crystal orientation matrices, prior to more thorough inspection of single Bragg nodes. Such information, in addition to a broadening analysis of families of single reflections, is shown to correlate well with the crystallinity, crystallite size, strain and epitaxial relationships in the thin films. The proposed set-up offers fast and easy sample mounting and alignment, along with crucial information on key features of the thin film structures. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Sønsteby, H.H. Chernyshov, D. Getz, M. Nilsen, O. Fjellvåg, H. 2013-05-01 doi:10.1107/S0909049513009102 International Union of Crystallography The flexible geometry of a multipurpose κ-diffractometer has been utilized in the study of a range of various thin film systems. EN synchrotron X-ray diffraction epitaxial thin films six-axis κ-diffractometer A multipurpose six-axis κ-diffractometer, together with the brilliance of the ESRF light source and a CCD area detector, has been explored for studying epitaxial relations and crystallinity in thin film systems. The geometrical flexibility of the six-axis goniometer allows measurement of a large volume in reciprocal space, providing an in-depth understanding of sample crystal relationships. By a set of examples of LaAlO3 thin films deposited by the atomic layer deposition technique, the possibilities of the set-up are presented. A fast panoramic scan provides determination of the crystal orientation matrices, prior to more thorough inspection of single Bragg nodes. Such information, in addition to a broadening analysis of families of single reflections, is shown to correlate well with the crystallinity, crystallite size, strain and epitaxial relationships in the thin films. The proposed set-up offers fast and easy sample mounting and alignment, along with crucial information on key features of the thin film structures. text/html On the application of a single-crystal κ-diffractometer and a CCD area detector for studies of thin films text 4 20 2013-05-01 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation short communications 0 0 http://scripts.iucr.org/cgi-bin/paper?wa5046 XANES (X-ray absorption near-edge structure) spectra of the Ti K-edges of ATiO3 (A = Ca and Sr), A2TiO4 (A = Mg and Fe), TiO2 rutile and TiO2 anatase were measured in the temperature range 20–900 K. Ti atoms for all samples were located in TiO6 octahedral sites. The absorption intensity invariant point (AIIP) was found to be between the pre-edge and post-edge. After the AIIP, amplitudes damped due to Debye–Waller factor effects with temperature. Amplitudes in the pre-edge region increased with temperature normally by thermal vibration. Use of the AIIP peak intensity as a standard point enables a quantitative comparison of the intensity of the pre-edge peaks in various titanium compounds over a wide temperature range. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Hiratoko, T. Yoshiasa, A. Nakatani, T. Okube, M. Nakatsuka, A. Sugiyama, K. 2013-05-01 doi:10.1107/S0909049513009175 International Union of Crystallography The absorption intensity invariant point (AIIP) was found to be between the pre-edge and post-edge in XANES spectra of various titanium compounds. Use of the AIIP peak intensity as a standard point enables a quantitative comparison of the intensity of the pre-edge peaks in various titanium compounds over a wide temperature range. EN pre-edge peak Ti K-edge temperature dependence Ti compounds absorption intensity invariant point XANES (X-ray absorption near-edge structure) spectra of the Ti K-edges of ATiO3 (A = Ca and Sr), A2TiO4 (A = Mg and Fe), TiO2 rutile and TiO2 anatase were measured in the temperature range 20–900 K. Ti atoms for all samples were located in TiO6 octahedral sites. The absorption intensity invariant point (AIIP) was found to be between the pre-edge and post-edge. After the AIIP, amplitudes damped due to Debye–Waller factor effects with temperature. Amplitudes in the pre-edge region increased with temperature normally by thermal vibration. Use of the AIIP peak intensity as a standard point enables a quantitative comparison of the intensity of the pre-edge peaks in various titanium compounds over a wide temperature range. text/html Temperature dependence of pre-edge features in Ti K-edge XANES spectra for ATiO3 (A = Ca and Sr), A2TiO4 (A = Mg and Fe), TiO2 rutile and TiO2 anatase text 4 20 2013-05-01 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation short communications 0 0 http://scripts.iucr.org/cgi-bin/paper?ie5090 Small-angle X-ray scattering (SAXS) measurements of proteins in solution are becoming increasingly popular with biochemists and structural biologists owing to the presence of dedicated high-throughput beamlines at synchrotron sources. As part of the ESRF Upgrade program a dedicated instrument for performing SAXS from biological macromolecules in solution (BioSAXS) has been installed at the renovated BM29 location. The optics hutch has been equipped with new optical components of which the two principal elements are a fixed-exit double multilayer monochromator and a 1.1 m-long toroidal mirror. These new dedicated optics give improved beam characteristics (compared with the previous set-up on ID14-3) regarding the energy tunability, flux and focusing at the detector plane leading to reduced parasitic scattering and an extended s-range. User experiments on the beamline have been successfully carried out since June 2012. A description of the new BioSAXS beamline and the set-up characteristics are presented together with examples of obtained data. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Pernot, P. Round, A. Barrett, R. De Maria Antolinos, A. Gobbo, A. Gordon, E. Huet, J. Kieffer, J. Lentini, M. Mattenet, M. Morawe, C. Mueller-Dieckmann, C. Ohlsson, S. Schmid, W. Surr, J. Theveneau, P. Zerrad, L. McSweeney, S. 2013-05-18 doi:10.1107/S0909049513010431 International Union of Crystallography A description of the new ESRF BioSAXS beamline is given. The beamline presented is dedicated to small-angle X-ray scattering of macromolecules in solution operating with a high-throughput sample-changer robot and automated data analysis for quality control and feedback. EN small-angle X-ray scattering proteins in solution automation and high throughput online HPLC structural biology Small-angle X-ray scattering (SAXS) measurements of proteins in solution are becoming increasingly popular with biochemists and structural biologists owing to the presence of dedicated high-throughput beamlines at synchrotron sources. As part of the ESRF Upgrade program a dedicated instrument for performing SAXS from biological macromolecules in solution (BioSAXS) has been installed at the renovated BM29 location. The optics hutch has been equipped with new optical components of which the two principal elements are a fixed-exit double multilayer monochromator and a 1.1 m-long toroidal mirror. These new dedicated optics give improved beam characteristics (compared with the previous set-up on ID14-3) regarding the energy tunability, flux and focusing at the detector plane leading to reduced parasitic scattering and an extended s-range. User experiments on the beamline have been successfully carried out since June 2012. A description of the new BioSAXS beamline and the set-up characteristics are presented together with examples of obtained data. text/html Upgraded ESRF BM29 beamline for SAXS on macromolecules in solution text 4 20 2013-05-18 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation beamlines 0 0 http://scripts.iucr.org/cgi-bin/paper?ie5096 The macromolecular crystallography beamline I911-3, part of the Cassiopeia/I911 suite of beamlines, is based on a superconducting wiggler at the MAX II ring of the MAX IV Laboratory in Lund, Sweden. The beamline is energy-tunable within a range between 6 and 18 keV. I911-3 opened for users in 2005. In 2010–2011 the experimental station was completely rebuilt and refurbished such that it has become a state-of-the-art experimental station with better possibilities for rapid throughput, crystal screening and work with smaller samples. This paper describes the complete I911-3 beamline and how it is embedded in the Cassiopeia suite of beamlines. Copyright (c) 2013 International Union of Crystallography urn:issn:0909-0495 Ursby, T. Unge, J. Appio, R. Logan, D.T. Fredslund, F. Svensson, C. Larsson, K. Labrador, A. Thunnissen, M.M.G.M. 2013-05-18 doi:10.1107/S0909049513011734 International Union of Crystallography The updated macromolecular crystallography beamline I911-3 at the MAX II storage ring is described. EN macromolecular crystallography beamline anomalous dispersion phasing beamline automation crystal dehydration The macromolecular crystallography beamline I911-3, part of the Cassiopeia/I911 suite of beamlines, is based on a superconducting wiggler at the MAX II ring of the MAX IV Laboratory in Lund, Sweden. The beamline is energy-tunable within a range between 6 and 18 keV. I911-3 opened for users in 2005. In 2010–2011 the experimental station was completely rebuilt and refurbished such that it has become a state-of-the-art experimental station with better possibilities for rapid throughput, crystal screening and work with smaller samples. This paper describes the complete I911-3 beamline and how it is embedded in the Cassiopeia suite of beamlines. text/html The macromolecular crystallography beamline I911-3 at the MAX IV laboratory text 4 20 2013-05-18 Copyright (c) 2013 International Union of Crystallography Journal of Synchrotron Radiation beamlines 0 0