Crystallography in the 21st century

The field of crystallography, which has had a major impact on the sciences in the last 100 years, is continuing to expand scientific horizons as technical and conceptual boundaries are overcome. Structure–function–dynamics will become an integrated theme for many studies as will obtaining structures without the `benevolent tyranny' of crystals.

A strenuous experimental journey searching for spectroscopic evidence of a bridging nickel–iron–hydride in [NiFe] hydrogenase

Direct spectroscopic evidence for a hydride bridge in the Ni–R form of [NiFe] hydrogenase has been obtained using iron-specific nuclear resonance vibrational spectroscopy. This article focuses on the long and strenuous experimental journey to search for and identify this first spectroscopic evidence for a hydride in Ni–R.

Sorting algorithms for single-particle imaging experiments at X-ray free-electron lasers

A new approach for classification of diffraction patterns measured in single-particle imaging experiments at XFELs on the basis of a set of parameters that take into account the underlying diffraction physics and specific relations between the real-space structure of a particle and its reciprocal-space intensity distribution is presented.

Applications of VUV extra-focus mechanism: high-performance dual-mode monochromator from VUV to soft X-ray

A new monochromator scheme is presented in which an extra-focus constant-included-angle varied-line-spacing cylindrical-grating monochromator is conveniently combined with a variable-included-angle varied-line-spacing plane-grating monochromator.

In situ removal of carbon contamination from a chromium-coated mirror: ideal optics to suppress higher-order harmonics in the carbon K-edge region

Carbon contamination of a chromium-coated mirror was removed by exposure to oxygen activated with non-monochromated synchrotron radiation. Higher-order harmonics of the chromium-coated mirror are much smaller than those of a gold-coated mirror in the carbon K-edge region.

Custom AFM for X-ray beamlines: in situ biological investigations under physiological conditions

The performance of a custom atomic force microscope for grazing-incidence X-ray experiments on hydrated soft and biological samples is presented.

A modular and compact portable mini-endstation for high-precision, high-speed fixed target serial crystallography at FEL and synchrotron sources

A portable sample viewing and alignment system is described which provides fast and reliable motion positioning for fixed target arrays at synchrotrons and free-electron laser sources.

Structural characterization and low-temperature properties of Ru/C multilayer monochromators with different periodic thicknesses

Ru/C multilayer monochromators with different periodic thicknesses were quantitatively characterized by X-ray reflectivity and scattering. The structural parameters were compared before and after cryogenic cooling.

In situ X-ray data collection and structure phasing of protein crystals at Structural Biology Center 19-ID

Prior to data collection at the synchrotron, protein crystals are harvested and cryo-cooled, which may damage the fragile samples. A new plate scanner implemented at the APS 19-ID eliminates this manipulation and allows high-quality data collection in situ from crystals in their crystallization device permitting structure determination using molecular replacement and selenium SAD phasing.

Pixelated transmission-mode diamond X-ray detector

Preparation and testing results of a pixelated transmission-mode diamond X-ray detector prototype are presented.

Investigation of a CPG-array CdZnTe γ-ray imaging detector with single collecting electrodes readout

A CPG-array CdZnTe detector with single collecting electrodes readout is presented to facilitate imaging applications of CPG detectors.

X-ray third-order nonlinear plane-wave Bragg-case dynamical diffraction effects in a perfect crystal

Two-wave third-order nonlinear symmetric Bragg-case dynamical diffraction of a plane X-ray wave in a perfect crystal is investigated theoretically. An analytical solution is found and results of numerical calculations are presented.

X-ray fluorescence induced by standing waves in the grazing-incidence and grazing-exit modes: study of the Mg–Co–Zr system

Characterization of Mg–Co–Zr tri-layer stacks using X-ray fluorescence induced by X-ray standing waves, in both grazing-incidence and grazing-exit modes, is presented.

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃

The performance of the XMaS beamline for soft X-ray spectroscopy in the 2–4 keV range is assessed with particular relation to in situ studies of functional materials and their chemistry.

The competitive growth of cubic domains in Ti_1–xAl_xN films studied by diffraction anomalous near-edge structure spectroscopy

Ti K-edge X-ray absorption spectroscopy and X-ray diffraction anomalous fine structure are carried out on Ti_1–xAl_xN films deposited by magnetron sputtering on Si substrates. The Ti K pre-edge fine structure allows determination of the symmetry of the sites occupied by Ti atoms in crystallized domains regardless of disordered area.

Influence of crystal structure, ligand environment and morphology on Co L-edge XAS spectral characteristics in cobalt compounds

Various cobalt-based compounds, differing in crystal structure, ligands surrounding the central metal ion and morphology, have been studied by soft X-ray absorption spectroscopy (XAS) at the Co L-edge in order to measure the effect of these parameters on the electronic structure.

Synchrotron study of metal localization in Typha latifolia L. root sections

Synchrotron micro-X-ray fluorescence measurements for micro-scale study of metal transport and distribution in Typha latifolia L. root system is described.

An EXAFS spectroscopic study of Am(III) complexation with lactate

Complexation of Am(III) with lactate is investigated as a function of the pH value using EXAFS spectroscopy. EXAFS measurements are combined with thermodynamic speciation calculations and iterative transformation factor analysis.

Structural investigation of mM Ni(II) complex isomers using transmission XAFS: the significance of model development

High-accuracy transmission XAFS of dilute solutions of bis(N-n-propyl-salicylaldiminato) nickel(II) and the i-propyl isomer with statistically valid estimates of their uncertainty has been determined using the hybrid technique. For these square planar and tetrahedral complexes the XAFS analysis, with error propogation, provides a more reliable guide to the coordination geometry than the relative intensities of the pre-edge features.

In situ microradioscopy and microtomography of fatigue-loaded dental two-piece implants

Results of a novel in situ microradiography and microtomography setup for the study of fatigue processes are presented. This setup is optimized for the requirements of dental implants and use at synchrotron imaging beamlines.

Coherent diffractive imaging: towards achieving atomic resolution

A general formalism for predicting the spatial resolution achievable in coherent diffractive imaging and the X-ray dose necessary to reach atomic resolution is described.

A feasibility study of X-ray phase-contrast mammographic tomography at the Imaging and Medical beamline of the Australian Synchrotron

Quantitative analysis of X-ray phase-contrast mammographic tomography carried out at the Imaging and Medical beamline of the Australian Synchrotron is presented.

X-ray-induced Cu deposition and patterning on insulators at room temperature

X-ray irradiation triggers the deposition of Cu from solution, at room temperature, on different insulating substrates.

Effect of X-ray spot size on liquid jet photoelectron spectroscopy

A small pinhole is used to reduce the X-ray spot size for liquid jet photoelectron spectroscopy applications.

Design, development and first experiments on the X-ray imaging beamline at Indus-2 synchrotron source RRCAT, India

The design, implementation and performance evaluation of the X-ray imaging beamline (BL-4) is reported. Some of the first experiments on propagation-based phase contrast imaging and micro-tomography are also reported.

MASSIF-1: a beamline dedicated to the fully automatic characterization and data collection from crystals of biological macromolecules

MASSIF-1 (ID30A-1) is a new beamline dedicated to the completely automatic characterization and data collection from crystals of biological macromolecules.

The time-resolved and extreme conditions XAS (TEXAS) facility at the European Synchrotron Radiation Facility: the general-purpose EXAFS bending-magnet beamline BM23

BM23 is the general-purpose EXAFS bending-magnet beamline at the ESRF, replacing the former BM29 beamline in the framework of the ESRF upgrade. Its mission is to serve the whole XAS user community by providing access to a basic service in addition to the many specialized instruments available at the ESRF. BM23 offers high-signal-to-noise ratio EXAFS in a large energy range (5–75 keV), continuous energy scanning for quick-EXAFS on the second timescale and a micro-XAS station delivering a spot size of 4 µm × 4 µm FWHM.

A miniature closed-circle flow cell for high photon flux X-ray scattering experiments

A closed-circle miniature flow cell for high X-ray photon flux experiments on radiation-sensitive liquid samples is presented.

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