http://journals.iucr.org/j/issues/2012/04/00/isscontsbdy.html Journal of Applied Crystallography covers a wide range of crystallographic topics from the viewpoints of both techniques and theory. The journal presents papers on the application of crystallographic techniques and on the related apparatus and computer software. For many years, the Journal of Applied Crystallography has been the main vehicle for the publication of small-angle scattering papers and powder diffraction techniques. The journal is the primary place where crystallographic computer program information is published. en Copyright (c) 2012 International Union of Crystallography 2012-08-01 International Union of Crystallography International Union of Crystallography http://journals.iucr.org urn:issn:0021-8898 Journal of Applied Crystallography covers a wide range of crystallographic topics from the viewpoints of both techniques and theory. The journal presents papers on the application of crystallographic techniques and on the related apparatus and computer software. For many years, the Journal of Applied Crystallography has been the main vehicle for the publication of small-angle scattering papers and powder diffraction techniques. The journal is the primary place where crystallographic computer program information is published. text/html Journal of Applied Crystallography, Volume 45, Part 4, 2012 text yearly 6 2002-02-01T00:00+00:00 4 45 2012-08-01 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography 621 urn:issn:0021-8898 med@iucr.org August 2012 2012-08-01 http://journals.iucr.org/logos/rss10j.gif http://journals.iucr.org/j/issues/2012/04/00/isscontsbdy.html Still image http://scripts.iucr.org/cgi-bin/paper?ks5312 In this work, a study of the mirror symmetries appearing in multiple diffraction patterns of face-centred cubic crystals is carried out. Several different X-ray and neutron multiple diffraction patterns have been simulated for different face-centred cubic structures. The patterns were plotted in circular plots which showed that two types of symmetry mirrors coexist in the patterns: isomorphic and anamorphic mirrors. The number and types of mirrors depend on the n-fold symmetry of the scattering vector associated with the primary reflection. For n even, only n isomorphic mirrors appear in the patterns. For n odd, n isomorphic mirrors are formed intercalated between n anamorphic mirrors. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Parente, C.B.R. Mazzocchi, V.L. Sasaki, J.M. Cardoso, L.P. 2012-07-14 doi:10.1107/S0021889812026830 International Union of Crystallography In this work, a study of the mirror symmetries appearing in multiple diffraction patterns of face-centred cubic crystals is carried out. It is shown that isomorphic and anamorphic mirrors coexist in these patterns. EN multiple diffraction mirror symmetry isomorphic mirrors anamorphic mirrors In this work, a study of the mirror symmetries appearing in multiple diffraction patterns of face-centred cubic crystals is carried out. Several different X-ray and neutron multiple diffraction patterns have been simulated for different face-centred cubic structures. The patterns were plotted in circular plots which showed that two types of symmetry mirrors coexist in the patterns: isomorphic and anamorphic mirrors. The number and types of mirrors depend on the n-fold symmetry of the scattering vector associated with the primary reflection. For n even, only n isomorphic mirrors appear in the patterns. For n odd, n isomorphic mirrors are formed intercalated between n anamorphic mirrors. text/html Mirror symmetries in multiple diffraction patterns of face-centred cubic crystals text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 621 626 http://scripts.iucr.org/cgi-bin/paper?rw5013 A genetic algorithm was implemented in order to optimize the selection of parameters within a polycrystalline plasticity model. Previously collected experimental data from tests performed on textured Zircaloy-2, consisting of macroscopic flow curves, lattice strains and Lankford coefficients, all measured in both tension and compression in three principle directions of a plate, were reproduced by the model. The results obtained were found to be comparable to prior attempts to optimize the model parameters manually. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Skippon, T. Mareau, C. Daymond, M.R. 2012-07-14 doi:10.1107/S0021889812026854 International Union of Crystallography A genetic algorithm was used to successfully optimize the work hardening coefficients of a polycrystalline plasticity model. EN zirconium alloys neutron diffraction texture plastic deformation A genetic algorithm was implemented in order to optimize the selection of parameters within a polycrystalline plasticity model. Previously collected experimental data from tests performed on textured Zircaloy-2, consisting of macroscopic flow curves, lattice strains and Lankford coefficients, all measured in both tension and compression in three principle directions of a plate, were reproduced by the model. The results obtained were found to be comparable to prior attempts to optimize the model parameters manually. text/html On the determination of single-crystal plasticity parameters by diffraction: optimization of a polycrystalline plasticity model using a genetic algorithm text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 627 643 http://scripts.iucr.org/cgi-bin/paper?aj5187 The present work reports the structural analysis of magnetic nanocrystals of Fe- and Mn-containing phases formed during annealing of the glass 13.6Na2O–62.9SiO2–8.5MnO–15.0Fe2O3−x (mol%) at 823 K for different periods of time. X-ray diffraction investigation shows the formation of a mixture of MnFe2O4 and Fe3O4 phases. Furthermore, small-angle X-ray scattering and anomalous small-angle X-ray scattering (ASAXS) experiments were used to extract quantitative information about the structure of the formed nano-sized crystals, as well as their phase compositions, volume fractions and size distributions. ASAXS analysis reveals the formation of spherical core–shell particles with the size of the particles between 10 and 50 nm. The concentrations of iron atoms in the core are higher than those in the shell and in the remaining matrix. With increasing annealing time, the ratio of Mn to Fe increases in the nanoparticles and the crystalline phase moves toward the pure jacobsite phase. Evaluated compositions reveal the presence of SiO2 in the shell. This shell acts as a diffusion barrier for the nanocrystal-forming ions, and the growth of the particles is kinetically constrained. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Raghuwanshi, V.S. Tatchev, D. Haas, S. Harizanova, R. Gugov, I. Rüssel, C. Hoell, A. 2012-06-20 doi:10.1107/S002188981202064X International Union of Crystallography The anomalous small-angle X-ray scattering technique is applied to determine quantitative information about the structure and composition of magnetic nanoparticles and their environment in silicate glasses. EN glasses nanostructure nanocrystallization small-angle X-ray scattering anomalous small-angle X-ray scattering The present work reports the structural analysis of magnetic nanocrystals of Fe- and Mn-containing phases formed during annealing of the glass 13.6Na2O–62.9SiO2–8.5MnO–15.0Fe2O3−x (mol%) at 823 K for different periods of time. X-ray diffraction investigation shows the formation of a mixture of MnFe2O4 and Fe3O4 phases. Furthermore, small-angle X-ray scattering and anomalous small-angle X-ray scattering (ASAXS) experiments were used to extract quantitative information about the structure of the formed nano-sized crystals, as well as their phase compositions, volume fractions and size distributions. ASAXS analysis reveals the formation of spherical core–shell particles with the size of the particles between 10 and 50 nm. The concentrations of iron atoms in the core are higher than those in the shell and in the remaining matrix. With increasing annealing time, the ratio of Mn to Fe increases in the nanoparticles and the crystalline phase moves toward the pure jacobsite phase. Evaluated compositions reveal the presence of SiO2 in the shell. This shell acts as a diffusion barrier for the nanocrystal-forming ions, and the growth of the particles is kinetically constrained. text/html Structural analysis of magnetic nanocrystals embedded in silicate glasses by anomalous small-angle X-ray scattering text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 644 651 http://scripts.iucr.org/cgi-bin/paper?ce5132 Circumventing radiation damage remains a major problem for X-ray macromolecular crystallography. Analysis of diffraction data collected from normal-sized cryocooled lysozyme crystals shows that the dose required to collect a data set of prescribed resolution and signal-to-noise ratio, assuming an ideally efficient detector, decreases with increasing photon energy in the investigated 6.5–33 keV range. For example, the data collection efficiency is increased by a factor of ∼8 from 8 to 33 keV. Monte Carlo simulations on lysozyme crystals in the range 5–80 keV, taking into account electron escape from samples of different size, also show a positive effect of high energy (albeit less pronounced than in experiments), especially for micrometre-sized samples, and suggest that the optimum energy range is ∼24–41 keV, depending on crystal size. The importance of counting pixel detectors with a good efficiency at high energy is underlined. Macromolecular crystallography beamlines should be modified, or purposely designed, in order to benefit from higher-energy radiation through reduction of global radiation damage, better data accuracy and extension of phasing by anomalous dispersion. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Fourme, R. Honkimäki, V. Girard, E. Medjoubi, K. Dhaussy, A.-C. Kahn, R. 2012-06-12 doi:10.1107/S0021889812019164 International Union of Crystallography X-ray photons with energy higher than usual improve both the number and the quality of diffraction data from a given macromolecular crystal. EN macromolecular crystallography radiation damage short wavelengths Circumventing radiation damage remains a major problem for X-ray macromolecular crystallography. Analysis of diffraction data collected from normal-sized cryocooled lysozyme crystals shows that the dose required to collect a data set of prescribed resolution and signal-to-noise ratio, assuming an ideally efficient detector, decreases with increasing photon energy in the investigated 6.5–33 keV range. For example, the data collection efficiency is increased by a factor of ∼8 from 8 to 33 keV. Monte Carlo simulations on lysozyme crystals in the range 5–80 keV, taking into account electron escape from samples of different size, also show a positive effect of high energy (albeit less pronounced than in experiments), especially for micrometre-sized samples, and suggest that the optimum energy range is ∼24–41 keV, depending on crystal size. The importance of counting pixel detectors with a good efficiency at high energy is underlined. Macromolecular crystallography beamlines should be modified, or purposely designed, in order to benefit from higher-energy radiation through reduction of global radiation damage, better data accuracy and extension of phasing by anomalous dispersion. text/html Reduction of radiation damage and other benefits of short wavelengths for macromolecular crystallography data collection text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 652 661 http://scripts.iucr.org/cgi-bin/paper?kk5097 A comprehensive method allowing experimentalists to perform a quantitative analysis of small-angle scattering patterns of powdered mesoporous materials of hexagonal symmetry is presented in this paper. Thanks to the rigorous processing of experimental data, and to a straightforward model for the small-angle scattering data simulation, the direct comparison of experimental and calculated patterns is made without any artificial background correction or ad hoc function. This allows the specific surface of mesopores to be estimated without resorting to other methods such as adsorption methods. This approach and its precision are discussed on the basis of the analysis of two real samples. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Cambedouzou, J. Diat, O. 2012-06-20 doi:10.1107/S0021889812020298 International Union of Crystallography Small-angle scattering profiles of mesoporous materials are measured in absolute units and quantitatively compared with calculated profiles. This treatment allows the determination of the mesoporous specific surface of these materials without resorting to gas adsorption measurements. EN mesopores SBA-15 MCM-41 specific surfaces small-angle scattering A comprehensive method allowing experimentalists to perform a quantitative analysis of small-angle scattering patterns of powdered mesoporous materials of hexagonal symmetry is presented in this paper. Thanks to the rigorous processing of experimental data, and to a straightforward model for the small-angle scattering data simulation, the direct comparison of experimental and calculated patterns is made without any artificial background correction or ad hoc function. This allows the specific surface of mesopores to be estimated without resorting to other methods such as adsorption methods. This approach and its precision are discussed on the basis of the analysis of two real samples. text/html Quantitative small-angle scattering on mesoporous silica powders: from morphological features to specific surface estimation text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 662 673 http://scripts.iucr.org/cgi-bin/paper?he5549 Serial femtosecond crystallography (SFX) using X-ray free-electron laser (FEL) sources has the potential to determine the structures of macromolecules beyond the limitation of radiation damage and without the need for crystals of sufficient size for conventional crystallography. In SFX, a liquid microjet is used to inject randomly oriented crystals suspended in their storage solution into the FEL beam. Settling of crystals in the reservoir prior to the injection has been found to complicate the data collection. This article details the development of an anti-settling sample delivery instrument based on a rotating syringe pump, capable of producing flow rates and liquid pressures necessary for the operation of the injector. The device has been used successfully with crystals of different proteins, with crystal sizes smaller than 20 µm. Even after hours of continuous operation, no significant impairment of the experiments due to sample settling was observed. This article describes the working principle of the instrument and sets it in context with regard to the experimental conditions used for SFX. Hit rates for longer measuring periods are compared with and without the instrument operating. Two versions of the instrument have been developed, which both deliver sample at a constant flow rate but which differ in their minimum liquid flow rates and maximum pressures. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Lomb, L. Steinbrener, J. Bari, S. Beisel, D. Berndt, D. Kieser, C. Lukat, M. Neef, N. Shoeman, R.L. 2012-07-04 doi:10.1107/S0021889812024557 International Union of Crystallography A simple and robust instrument, which overcomes the crystal settling that impairs serial femtosecond crystallography experiments, is described. EN serial femtosecond crystallography X-ray free-electron lasers macromolecular crystallography anti-settling sample delivery instruments Serial femtosecond crystallography (SFX) using X-ray free-electron laser (FEL) sources has the potential to determine the structures of macromolecules beyond the limitation of radiation damage and without the need for crystals of sufficient size for conventional crystallography. In SFX, a liquid microjet is used to inject randomly oriented crystals suspended in their storage solution into the FEL beam. Settling of crystals in the reservoir prior to the injection has been found to complicate the data collection. This article details the development of an anti-settling sample delivery instrument based on a rotating syringe pump, capable of producing flow rates and liquid pressures necessary for the operation of the injector. The device has been used successfully with crystals of different proteins, with crystal sizes smaller than 20 µm. Even after hours of continuous operation, no significant impairment of the experiments due to sample settling was observed. This article describes the working principle of the instrument and sets it in context with regard to the experimental conditions used for SFX. Hit rates for longer measuring periods are compared with and without the instrument operating. Two versions of the instrument have been developed, which both deliver sample at a constant flow rate but which differ in their minimum liquid flow rates and maximum pressures. text/html An anti-settling sample delivery instrument for serial femtosecond crystallography text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 674 678 http://scripts.iucr.org/cgi-bin/paper?ks5311 A large (∼20 mm diameter and 80 mm length) single crystal of l-arginine phosphate monohydrate (LAP) has been grown for the first time by the unidirectional Sankaranarayanan–Ramasamy method in an aqueous medium in a specially designed constant-temperature bath. The crystal structure has been confirmed by powder X-ray diffraction. The crystalline perfection was assessed by high-resolution X-ray diffractometry (HRXRD) which found that the quality of the grown single crystal is quite good. HRXRD studies along different directions show that the crystal contains a low density of edge-type dislocations formed along the growth direction. The thermal stability was assessed using thermogravimetric/differential thermal analysis. The mechanical behaviour was studied using an Omnitech micro-hardness tester. The dielectric studies were carried out over a wide frequency range of 10 Hz to 5 MHz at room temperature. The characterization studies reveal that the grown bulk single crystal of LAP is suitable for device applications. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Riscob, B. Shakir, M. Vijayan, N. Maurya, K.K. Wahab, M.A. Bhagavannarayana, G. 2012-06-12 doi:10.1107/S0021889812016822 International Union of Crystallography A large and unidirectional single crystal of technologically important l-arginine phosphate monohydrate has been grown for the first time by the recently invented Sankaranarayanan–Ramasamy method. The crystalline perfection and the mechanical and dielectric properties have been assessed and correlated. EN crystal growth high-resolution X-ray diffractometry rocking curves dielectric properties l-arginine phosphate monohydrate A large (∼20 mm diameter and 80 mm length) single crystal of l-arginine phosphate monohydrate (LAP) has been grown for the first time by the unidirectional Sankaranarayanan–Ramasamy method in an aqueous medium in a specially designed constant-temperature bath. The crystal structure has been confirmed by powder X-ray diffraction. The crystalline perfection was assessed by high-resolution X-ray diffractometry (HRXRD) which found that the quality of the grown single crystal is quite good. HRXRD studies along different directions show that the crystal contains a low density of edge-type dislocations formed along the growth direction. The thermal stability was assessed using thermogravimetric/differential thermal analysis. The mechanical behaviour was studied using an Omnitech micro-hardness tester. The dielectric studies were carried out over a wide frequency range of 10 Hz to 5 MHz at room temperature. The characterization studies reveal that the grown bulk single crystal of LAP is suitable for device applications. text/html Unidirectional crystal growth and crystalline perfection of l-arginine phosphate monohydrate text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 679 685 http://scripts.iucr.org/cgi-bin/paper?mn5008 Techniques and equipment have been developed that enable large protein crystals (1–6 mm3) flash-cooled in liquid nitrogen at 77 K to be transferred and mounted on a liquid helium Displex cryorefrigerator and cooled to temperatures down to 15 K for accurate neutron diffraction analysis. In preliminary experiments, it was possible to collect high-quality high-resolution neutron diffraction data to 1.55 Å resolution from several large crystals of triclinic hen egg white lysozyme cooled to 15 K. This enabled the subsequent cryogenic analysis of two further proteins, rubredoxin and concanavalin A, at 1.7 and 2.5 Å, respectively, demonstrating the generality of the approach. The ability to flash-cool such large crystals for cryogenic neutron analysis should significantly broaden the range of scientific questions examined by neutron protein crystallography, allowing the analysis of structures and transitions as a function of temperature and enabling freeze-trapped capture of kinetic intermediates in protein systems. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Myles, D.A.A. Dauvergne, F. Blakeley, M.P. Meilleur, F. 2012-06-20 doi:10.1107/S0021889812019784 International Union of Crystallography Techniques used to cryocool large protein crystals (1–6 mm3) successfully are described. High-resolution cryo-neutron crystallography data were collected at 15 K for three test systems. EN neutron protein crystallography flash cooling cryocrystallography Techniques and equipment have been developed that enable large protein crystals (1–6 mm3) flash-cooled in liquid nitrogen at 77 K to be transferred and mounted on a liquid helium Displex cryorefrigerator and cooled to temperatures down to 15 K for accurate neutron diffraction analysis. In preliminary experiments, it was possible to collect high-quality high-resolution neutron diffraction data to 1.55 Å resolution from several large crystals of triclinic hen egg white lysozyme cooled to 15 K. This enabled the subsequent cryogenic analysis of two further proteins, rubredoxin and concanavalin A, at 1.7 and 2.5 Å, respectively, demonstrating the generality of the approach. The ability to flash-cool such large crystals for cryogenic neutron analysis should significantly broaden the range of scientific questions examined by neutron protein crystallography, allowing the analysis of structures and transitions as a function of temperature and enabling freeze-trapped capture of kinetic intermediates in protein systems. text/html Neutron protein crystallography at ultra-low (<15 K) temperatures text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 686 692 http://scripts.iucr.org/cgi-bin/paper?rw5009 A data-analysis methodology is presented for the characterization of three-dimensional microstructures of polycrystalline materials from data acquired using three-dimensional X-ray diffraction (3DXRD). The method is developed for 3DXRD microscopy using a far-field detector and yields information about the centre-of-mass position, crystallographic orientation, volume and strain state for thousands of grains. This first part deals with pre-processing of the diffraction data for input into the algorithms presented in the second part [Sharma, Huizenga & Offerman (2012). J. Appl. Cryst. 45, 705–718] for determination of the grain characteristics. An algorithm is presented for accurate identification of overlapping diffraction peaks from X-ray diffraction images, which has been an issue limiting the accuracy of experiments of this type. The algorithm works in two stages, namely the identification of overlapping peaks using a seeded watershed algorithm, and then the fitting of the peaks with a pseudo-Voigt shape function to yield an accurate centre-of-mass position and integrated intensity for the peaks. Regions consisting of up to six overlapping peaks can be successfully fitted. Two simulations and an experiment are used to verify the results of the algorithms. An example of the processing of diffraction images acquired in a 3DXRD experiment with a sample consisting of more than 1600 grains is shown. Furthermore, a procedure for the determination of the parameters of the experimental setup (global parameters) without the need for a calibration sample is presented and validated using simulations. This is immensely beneficial for simplifying experiments and the subsequent data analysis. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Sharma, H. Huizenga, R.M. Offerman, S.E. 2012-07-14 doi:10.1107/S0021889812025563 International Union of Crystallography A fast and robust methodology is developed for the analysis of two-dimensional diffraction data containing peak overlap, acquired from polycrystalline materials consisting of thousands of grains using three-dimensional X-ray diffraction. This first part outlines the procedure for the accurate identification and characterization of overlapping diffraction peaks and the determination of the parameters of the experimental setup without the need for calibration samples. EN three-dimensional X-ray diffraction peak fitting peak overlap experimental parameters synchrotron radiation diffraction microscopy A data-analysis methodology is presented for the characterization of three-dimensional microstructures of polycrystalline materials from data acquired using three-dimensional X-ray diffraction (3DXRD). The method is developed for 3DXRD microscopy using a far-field detector and yields information about the centre-of-mass position, crystallographic orientation, volume and strain state for thousands of grains. This first part deals with pre-processing of the diffraction data for input into the algorithms presented in the second part [Sharma, Huizenga & Offerman (2012). J. Appl. Cryst. 45, 705–718] for determination of the grain characteristics. An algorithm is presented for accurate identification of overlapping diffraction peaks from X-ray diffraction images, which has been an issue limiting the accuracy of experiments of this type. The algorithm works in two stages, namely the identification of overlapping peaks using a seeded watershed algorithm, and then the fitting of the peaks with a pseudo-Voigt shape function to yield an accurate centre-of-mass position and integrated intensity for the peaks. Regions consisting of up to six overlapping peaks can be successfully fitted. Two simulations and an experiment are used to verify the results of the algorithms. An example of the processing of diffraction images acquired in a 3DXRD experiment with a sample consisting of more than 1600 grains is shown. Furthermore, a procedure for the determination of the parameters of the experimental setup (global parameters) without the need for a calibration sample is presented and validated using simulations. This is immensely beneficial for simplifying experiments and the subsequent data analysis. text/html A fast methodology to determine the characteristics of thousands of grains using three-dimensional X-ray diffraction. I. Overlapping diffraction peaks and parameters of the experimental setup text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 693 704 http://scripts.iucr.org/cgi-bin/paper?rw5010 This second part of the paper on an analysis strategy for data acquired using three-dimensional X-ray diffraction (3DXRD) describes the procedure for the determination of the grain characteristics for thousands of grains. The approach developed here is orders of magnitude faster than those presently available for indexing thousands of grains. Using information obtained from the steps described in Part I [Sharma, Huizenga & Offerman (2012). J. Appl. Cryst. 45, 693–704], the volume, crystallographic orientation, centre-of-mass position and strain state of grains in the sample can be determined. The algorithms dealing with the determination of the orientation, centre-of-mass position and strain state of the grains are divided into two parts. The first deals with indexing, i.e. it assigns diffraction spots to individual grains assuming an unstrained lattice, and the second deals with the refinement of the crystallographic orientation, centre-of-mass position and strain state of the grains using the diffraction spots assigned during indexing. The different approaches to indexing that exist in the literature are presented and compared with the novel approach developed here. Indexing can be run in two modes depending on the number of grains. For large numbers of grains, the approach employs a novel sample `surface' scanning technique, in combination with a reduced number of search orientations, to achieve high robustness and computation efficiency. For small numbers of grains, the approach neglects the position of the diffracting grains in the sample in order to improve the computation efficiency. For unstrained samples, both modes of indexing and the subsequent process of refinement are validated using simulated data for 60 and 3000 grains. In both cases, the centre-of-mass position of the grains was determined with a mean error of 0.7 µm and the orientation was determined with a mean error of 0.0003°. Furthermore, an experiment was `mimicked' by introducing experimental errors into the simulation for 3000 grains. The resulting mean errors in the centre-of-mass position (2.1 µm) and orientation (0.008°) of the grains are higher than those for the ideal simulations, and the errors in an experiment will depend on the `true' experimental errors. The algorithms dealing with strained samples are validated using a simulation for 3000 grains with mimicked experimental errors. The centre-of-mass position, crystallographic orientation, normal strain tensor components and shear strain tensor components of the grains were determined with mean errors of 8 µm, 0.006°, 5.2 × 10−5 and 2.8 × 10−5, respectively. The possibility of obtaining grain-level information for thousands of grains with a high speed of acquisition makes the technique very attractive for in situ studies of thermomechanical processes in polycrystalline materials. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Sharma, H. Huizenga, R.M. Offerman, S.E. 2012-07-14 doi:10.1107/S0021889812025599 International Union of Crystallography A fast and robust methodology is developed for the analysis of two-dimensional diffraction data acquired from samples containing thousands of grains using three-dimensional X-ray diffraction. This second part deals with the procedure for the determination of grain characteristics. The volume, crystallographic orientation, centre-of-mass position and strain state of individual grains can be determined simultaneously. EN three-dimensional X-ray diffraction grain volume indexing synchrotron radiation diffraction microscopy centre of mass centroid orientation strain This second part of the paper on an analysis strategy for data acquired using three-dimensional X-ray diffraction (3DXRD) describes the procedure for the determination of the grain characteristics for thousands of grains. The approach developed here is orders of magnitude faster than those presently available for indexing thousands of grains. Using information obtained from the steps described in Part I [Sharma, Huizenga & Offerman (2012). J. Appl. Cryst. 45, 693–704], the volume, crystallographic orientation, centre-of-mass position and strain state of grains in the sample can be determined. The algorithms dealing with the determination of the orientation, centre-of-mass position and strain state of the grains are divided into two parts. The first deals with indexing, i.e. it assigns diffraction spots to individual grains assuming an unstrained lattice, and the second deals with the refinement of the crystallographic orientation, centre-of-mass position and strain state of the grains using the diffraction spots assigned during indexing. The different approaches to indexing that exist in the literature are presented and compared with the novel approach developed here. Indexing can be run in two modes depending on the number of grains. For large numbers of grains, the approach employs a novel sample `surface' scanning technique, in combination with a reduced number of search orientations, to achieve high robustness and computation efficiency. For small numbers of grains, the approach neglects the position of the diffracting grains in the sample in order to improve the computation efficiency. For unstrained samples, both modes of indexing and the subsequent process of refinement are validated using simulated data for 60 and 3000 grains. In both cases, the centre-of-mass position of the grains was determined with a mean error of 0.7 µm and the orientation was determined with a mean error of 0.0003°. Furthermore, an experiment was `mimicked' by introducing experimental errors into the simulation for 3000 grains. The resulting mean errors in the centre-of-mass position (2.1 µm) and orientation (0.008°) of the grains are higher than those for the ideal simulations, and the errors in an experiment will depend on the `true' experimental errors. The algorithms dealing with strained samples are validated using a simulation for 3000 grains with mimicked experimental errors. The centre-of-mass position, crystallographic orientation, normal strain tensor components and shear strain tensor components of the grains were determined with mean errors of 8 µm, 0.006°, 5.2 × 10−5 and 2.8 × 10−5, respectively. The possibility of obtaining grain-level information for thousands of grains with a high speed of acquisition makes the technique very attractive for in situ studies of thermomechanical processes in polycrystalline materials. text/html A fast methodology to determine the characteristics of thousands of grains using three-dimensional X-ray diffraction. II. Volume, centre-of-mass position, crystallographic orientation and strain state of grains text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 705 718 http://scripts.iucr.org/cgi-bin/paper?aj5193 Face-centred cubic Cr-rich carbide is known to precipitate in a face-centred cubic matrix with a cube–cube orientation relationship, thereby minimizing the elastic strain energy. In the present study, for the first time, the precipitation was observed of an abnormal Cr-rich carbide, which did not have the cube–cube orientation relationship in its face-centred cubic matrix. The abnormally oriented carbides nucleated and grew around random grain boundaries, and were observed to have a lamellar or plate-like morphology. The crystallographic orientation anomaly was characterized by measuring the tilt angles of the three crystal poles of the matrices, carbides and adjacent grains, using a transmission electron microscope to find the closest coincidence site lattice boundary. The carbides showed a slight deviation from a cube–cube orientation with adjacent grains and did not present any particular orientational relationship with the matrix. The deviation angles from coincidence site lattice boundaries between the matrices and carbides were smaller than those between matrices and adjacent grains. The abnormally oriented carbides appeared to nucleate on adjacent grains, and underwent a rotation within the matrix during the initial stage of growth to release the phase boundary energy between the carbides and the matrix. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Jeong, H.W. Kim, I.S. Seo, S.M. Yoo, Y.S. Choi, B.G. Jo, C.Y. 2012-07-14 doi:10.1107/S002188981202599X International Union of Crystallography In the present study, the precipitation of a face-centred cubic carbide in a face-centred cubic matrix was observed for the first time in the absence of the cube–cube orientation relationship. This crystallographic orientation anomaly was characterized by a new method using transmission electron microscopy. EN crystallographic anomalies M23C6 carbides Ni-base superalloys Face-centred cubic Cr-rich carbide is known to precipitate in a face-centred cubic matrix with a cube–cube orientation relationship, thereby minimizing the elastic strain energy. In the present study, for the first time, the precipitation was observed of an abnormal Cr-rich carbide, which did not have the cube–cube orientation relationship in its face-centred cubic matrix. The abnormally oriented carbides nucleated and grew around random grain boundaries, and were observed to have a lamellar or plate-like morphology. The crystallographic orientation anomaly was characterized by measuring the tilt angles of the three crystal poles of the matrices, carbides and adjacent grains, using a transmission electron microscope to find the closest coincidence site lattice boundary. The carbides showed a slight deviation from a cube–cube orientation with adjacent grains and did not present any particular orientational relationship with the matrix. The deviation angles from coincidence site lattice boundaries between the matrices and carbides were smaller than those between matrices and adjacent grains. The abnormally oriented carbides appeared to nucleate on adjacent grains, and underwent a rotation within the matrix during the initial stage of growth to release the phase boundary energy between the carbides and the matrix. text/html Characterization of an anomaly in the crystallographic orientation of plate-like carbides precipitated in a wrought Ni-base superalloy text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 719 725 http://scripts.iucr.org/cgi-bin/paper?ks5299 The high-pressure structures of nickel monosilicide (NiSi) have been investigated to 124 GPa by synchrotron-based X-ray powder diffraction studies of quenched samples from laser-heated diamond anvil cell experiments, and the equations of state of three of these phases have been determined at room temperature. NiSi transforms from the MnP (B31) structure (space group Pnma) to the ∊-FeSi (B20) structure (space group P213) at 12.5 ± 4.5 GPa and 1550 ± 150 K. Upon further compression, the CsCl (B2) structure (space group Pm3m) becomes stable at 46 ± 3 GPa and 1900 ± 150 K. Thus, NiSi will be in the B2 structure throughout the majority of the Earth's mantle and its entire core, and will likely form a solid solution with FeSi, which is already known to undergo a B20 → B2 transition at high pressure. Data from the quenched (room-temperature) samples of all three phases have been fitted to the third-order Birch–Murnaghan equation of state. For the MnP (B31) structure this yields K0 = 165 ± 3 GPa with K0′ fixed at 4 and V0 fixed at 12.1499 Å3 atom−1 [V0 from unpublished neutron diffraction measurements on the same batch of starting material; Wood (2011), personal communication]. For the ∊-FeSi (B20) structure, K0 =161± 3 GPa and K0′ = 5.6 ± 0.2 with V0 fixed at 11.4289 Å3 atom−1. For the CsCl (B2) structure, K0 = 200 ± 9 GPa, K0′ = 4.6 ± 0.1 and V0 = 11.09 ± 0.05 Å3 atom−1. The ambient volume of NiSi, therefore, decreases by 6% at the first phase transition and then by a further 3% at the transition to the CsCl structure. Traces of additional NiSi structures predicted by Vočadlo, Wood & Dobson [J. Appl. Cryst. (2012), 45, 186–196; part I], and labelled therein as Pbma-I, Pnma-II, and possibly also Pnma-III and P4/nmm, have been detected. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Lord, O.T. Vočadlo, L. Wood, I.G. Dobson, D.P. Clark, S.M. Walter, M.J. 2012-06-12 doi:10.1107/S0021889812016809 International Union of Crystallography The high-pressure structures of NiSi and their room-temperature equations of state have been investigated using synchrotron X-ray diffraction in a diamond anvil cell, coupled with laser annealing. An ∊-FeSi-structured phase was found to form above ∼13 GPa and a CsCl-structured phase above ∼61 GPa. EN NiSi nickel silicide diamond anvil cells equations of state high pressure Earth's core The high-pressure structures of nickel monosilicide (NiSi) have been investigated to 124 GPa by synchrotron-based X-ray powder diffraction studies of quenched samples from laser-heated diamond anvil cell experiments, and the equations of state of three of these phases have been determined at room temperature. NiSi transforms from the MnP (B31) structure (space group Pnma) to the ∊-FeSi (B20) structure (space group P213) at 12.5 ± 4.5 GPa and 1550 ± 150 K. Upon further compression, the CsCl (B2) structure (space group Pm3m) becomes stable at 46 ± 3 GPa and 1900 ± 150 K. Thus, NiSi will be in the B2 structure throughout the majority of the Earth's mantle and its entire core, and will likely form a solid solution with FeSi, which is already known to undergo a B20 → B2 transition at high pressure. Data from the quenched (room-temperature) samples of all three phases have been fitted to the third-order Birch–Murnaghan equation of state. For the MnP (B31) structure this yields K0 = 165 ± 3 GPa with K0′ fixed at 4 and V0 fixed at 12.1499 Å3 atom−1 [V0 from unpublished neutron diffraction measurements on the same batch of starting material; Wood (2011), personal communication]. For the ∊-FeSi (B20) structure, K0 =161± 3 GPa and K0′ = 5.6 ± 0.2 with V0 fixed at 11.4289 Å3 atom−1. For the CsCl (B2) structure, K0 = 200 ± 9 GPa, K0′ = 4.6 ± 0.1 and V0 = 11.09 ± 0.05 Å3 atom−1. The ambient volume of NiSi, therefore, decreases by 6% at the first phase transition and then by a further 3% at the transition to the CsCl structure. Traces of additional NiSi structures predicted by Vočadlo, Wood & Dobson [J. Appl. Cryst. (2012), 45, 186–196; part I], and labelled therein as Pbma-I, Pnma-II, and possibly also Pnma-III and P4/nmm, have been detected. text/html High-pressure phase transitions and equations of state in NiSi. II. Experimental results text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 726 737 http://scripts.iucr.org/cgi-bin/paper?to5013 This paper describes a new method for extracting the individual contributions to the diffracted intensity of subsets of atoms in the crystal structure. The periodic perturbation of the scattering process, required for untangling the scattered intensity, is provided by altering the resonant contributions. The theory of modulation enhanced diffraction (MED) is briefly recalled in the context of resonant scattering. A periodic variation in the atomic form factor has been achieved by changing the X-ray energy in such a way that the MED theory holds. Simulated results and experimental data are presented, together with necessary corrections. Two data analysis schemes are presented, both illustrating the advantages and drawbacks of the novel modulation technique. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Beek, W. van Emerich, H. Urakawa, A. Palin, L. Milanesio, M. Caliandro, R. Viterbo, D. Chernyshov, D. 2012-06-12 doi:10.1107/S0021889812018109 International Union of Crystallography Atomic selectivity in X-ray diffraction has been achieved by varying the X-ray energy, and thus the resonant scattering contributions, using the recently proposed modulation enhanced diffraction approach. A general experimental recipe is given, and possible schemes for data analysis are introduced, tested and discussed. EN modulation enhanced diffraction powder diffraction interference resonant scattering This paper describes a new method for extracting the individual contributions to the diffracted intensity of subsets of atoms in the crystal structure. The periodic perturbation of the scattering process, required for untangling the scattered intensity, is provided by altering the resonant contributions. The theory of modulation enhanced diffraction (MED) is briefly recalled in the context of resonant scattering. A periodic variation in the atomic form factor has been achieved by changing the X-ray energy in such a way that the MED theory holds. Simulated results and experimental data are presented, together with necessary corrections. Two data analysis schemes are presented, both illustrating the advantages and drawbacks of the novel modulation technique. text/html Untangling diffraction intensity: modulation enhanced diffraction on ZrO2 powder text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 738 747 http://scripts.iucr.org/cgi-bin/paper?ks5313 The isothermal austenite-to-martensite transformation kinetics in a maraging steel have been studied by time-dependent microbeam diffraction measurements with high-energy X-rays. The transformation kinetics are shown to be accelerated significantly when a magnetic field of 8 T is applied. The average phase behaviour, obtained from a Rietveld refinement of the powder-averaged diffraction data, demonstrates that the martensite formation does not lead to a macroscopic strain in the austenite and martensite phases. An analysis of individual austenite reflections in the microbeam diffraction patterns, however, indicates that within the transforming austenite grains a transformation strain develops as a result of the formed martensite. The development of elastic strains during the transformation is explained by a partial strain confinement within the untransformed part of the austenite grain. The strain relaxation to the surrounding austenite grains is found to be dependent on the austenite volume. For a set of individual austenite grains the martensite nucleation is correlated with the initial austenite volume and the strain developed prior to the transformation as a result of martensite formation in the neighbouring grains. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 San Martin, D. Jiménez-Melero, E. Duffy, J.A. Honkimäki, V. Zwaag, S. van der Dijk, N.H. van 2012-07-04 doi:10.1107/S0021889812024892 International Union of Crystallography Time-dependent microbeam X-ray diffraction experiments have been performed on the isothermal austenite-to-martensite transformation in maraging steel. The transformation behaviour of a set of individual austenite grains is monitored in detail and correlated to the microstructural features. EN martensitic transformations maraging steel metastable austenite synchrotron X-ray diffraction The isothermal austenite-to-martensite transformation kinetics in a maraging steel have been studied by time-dependent microbeam diffraction measurements with high-energy X-rays. The transformation kinetics are shown to be accelerated significantly when a magnetic field of 8 T is applied. The average phase behaviour, obtained from a Rietveld refinement of the powder-averaged diffraction data, demonstrates that the martensite formation does not lead to a macroscopic strain in the austenite and martensite phases. An analysis of individual austenite reflections in the microbeam diffraction patterns, however, indicates that within the transforming austenite grains a transformation strain develops as a result of the formed martensite. The development of elastic strains during the transformation is explained by a partial strain confinement within the untransformed part of the austenite grain. The strain relaxation to the surrounding austenite grains is found to be dependent on the austenite volume. For a set of individual austenite grains the martensite nucleation is correlated with the initial austenite volume and the strain developed prior to the transformation as a result of martensite formation in the neighbouring grains. text/html Real-time synchrotron X-ray diffraction study on the isothermal martensite transformation of maraging steel in high magnetic fields text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 748 757 http://scripts.iucr.org/cgi-bin/paper?he5552 In vapor diffusion protein crystallization screening, it has been reported that replacing the reservoir solution with desiccant can increase the crystallization success rate. Therefore, the desiccation method is a potentially powerful method in practical protein crystallization screening. However, this method is difficult to apply broadly because the optimal amount of desiccant for a specific screening task is unknown. Utilizing an unsuitable amount of desiccant can result in even worse screening results than would be obtained from the traditional vapor diffusion method. Here, it is shown that by employing a modified strategy, named the gradual desiccation method, the problem can be solved without knowing the optimal amount of desiccant, and the crystallization success rate can be further increased compared with the one-time desiccation method. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Lu, Q.-Q. Xie, X.-Z. Chen, R.-Q. Wu, Z.-Q. Cheng, Q.-D. Shang, P. Yin, D.-C. 2012-07-14 doi:10.1107/S0021889812025757 International Union of Crystallography A modification to the vapor diffusion protein crystallization method, named the gradual desiccation method, is reported. It was found that this method can significantly enhance crystallization of proteins. EN protein crystallization screening strategies desiccants vapor diffusion gradual desiccation method In vapor diffusion protein crystallization screening, it has been reported that replacing the reservoir solution with desiccant can increase the crystallization success rate. Therefore, the desiccation method is a potentially powerful method in practical protein crystallization screening. However, this method is difficult to apply broadly because the optimal amount of desiccant for a specific screening task is unknown. Utilizing an unsuitable amount of desiccant can result in even worse screening results than would be obtained from the traditional vapor diffusion method. Here, it is shown that by employing a modified strategy, named the gradual desiccation method, the problem can be solved without knowing the optimal amount of desiccant, and the crystallization success rate can be further increased compared with the one-time desiccation method. text/html A gradual desiccation method for improving the efficiency of protein crystallization screening text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 758 765 http://scripts.iucr.org/cgi-bin/paper?nb5017 Tetragonal, rhombohedral and monoclinic ferroelectric domains can all occur in morphotropic PbZr1−xTixO3 (PZT) ceramics. In this article, the influence of these domains on the splitting of reflections in selected area electron diffraction (SAED) patterns along the main pseudo-cubic zone axes is reported. The orientation of the domain wall in a transmission electron microscopy image with respect to the splitting of reflections in the diffraction pattern has to be considered for the interpretation. The distinction of tetragonal and rhombohedral splitting is achieved for a pronounced splitting except for 〈111〉 with the domain wall edge on. As the monoclinic structure contains tetragonal as well as rhombohedral distortions, the distinction of monoclinic symmetry from tetragonal and rhombohedral based only on the splitting of reflections is not possible. Conceivable models of configurations of monoclinic subdomains inside the existing tetragonal or rhombohedral microdomains are derived from group–subgroup relations. Some experimental observations are given, which can only be explained by these models. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Schierholz, R. Fuess, H. 2012-06-20 doi:10.1107/S0021889812022583 International Union of Crystallography Selected area electron diffraction (SAED) patterns along the main pseudo-cubic axes, which show a splitting of reflections, are calculated for tetragonal and rhombohedral distortions present around the morphotropic phase boundary of PbZr1−xTixO3 (PZT). If a defined splitting is observed it might be used to estimate the lattice distortion, although for a detailed analysis, especially to distinguish the monoclinic phase, convergent-beam electron diffraction is required. EN ferroelectric domains PZT ceramics morphotropic phase boundaries selected area electron diffraction Tetragonal, rhombohedral and monoclinic ferroelectric domains can all occur in morphotropic PbZr1−xTixO3 (PZT) ceramics. In this article, the influence of these domains on the splitting of reflections in selected area electron diffraction (SAED) patterns along the main pseudo-cubic zone axes is reported. The orientation of the domain wall in a transmission electron microscopy image with respect to the splitting of reflections in the diffraction pattern has to be considered for the interpretation. The distinction of tetragonal and rhombohedral splitting is achieved for a pronounced splitting except for 〈111〉 with the domain wall edge on. As the monoclinic structure contains tetragonal as well as rhombohedral distortions, the distinction of monoclinic symmetry from tetragonal and rhombohedral based only on the splitting of reflections is not possible. Conceivable models of configurations of monoclinic subdomains inside the existing tetragonal or rhombohedral microdomains are derived from group–subgroup relations. Some experimental observations are given, which can only be explained by these models. text/html Ferroelectric domains in PZT ceramics at the morphotropic phase boundary. Can the splitting of reflections in SAED patterns be used for the distinction of different pseudo-cubic phases? text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 766 777 http://scripts.iucr.org/cgi-bin/paper?nb5018 A complex three-dimensional quantitative image of an extended zinc oxide (ZnO) crystal has been obtained using Bragg coherent diffraction imaging integrated with ptychography. By scanning a 2.5 µm-long arm of a ZnO tetrapod across a 1.3 µm X-ray beam with fine step sizes while measuring a three-dimensional diffraction pattern at each scan spot, the three-dimensional electron density and projected displacement field of the entire crystal were recovered. The simultaneously reconstructed complex wavefront of the illumination combined with its coherence properties determined by a partial coherence analysis implemented in the reconstruction process provide a comprehensive characterization of the incident X-ray beam. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Huang, X. Harder, R. Leake, S. Clark, J. Robinson, I. 2012-06-20 doi:10.1107/S0021889812018900 International Union of Crystallography A complex three-dimensional quantitative image of an extended zinc oxide crystal has been obtained using Bragg coherent diffraction imaging integrated with ptychography. EN three-dimensional quantitative imaging coherent diffraction imaging ptychography zinc oxide A complex three-dimensional quantitative image of an extended zinc oxide (ZnO) crystal has been obtained using Bragg coherent diffraction imaging integrated with ptychography. By scanning a 2.5 µm-long arm of a ZnO tetrapod across a 1.3 µm X-ray beam with fine step sizes while measuring a three-dimensional diffraction pattern at each scan spot, the three-dimensional electron density and projected displacement field of the entire crystal were recovered. The simultaneously reconstructed complex wavefront of the illumination combined with its coherence properties determined by a partial coherence analysis implemented in the reconstruction process provide a comprehensive characterization of the incident X-ray beam. text/html Three-dimensional Bragg coherent diffraction imaging of an extended ZnO crystalThis article also forms part of a special issue dedicated to advanced diffraction imaging methods of materials, which will be published as a virtual special issue of the journal in 2012/2013. text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 778 784 http://scripts.iucr.org/cgi-bin/paper?he5555 Protein microcrystals of less than 10 µm in size are now applicable to X-ray studies by synchrotron microbeam technology. However, because of their small size, they are difficult to handle and mount. In addition, the deterioration of data quality by scattering from the mounting apparatus and crystallization solvent is not negligible. To address these issues, a simple mounting method is proposed using a fine-needle capillary similar to that used for microinjection in cell biology. In this method, microcrystals are pulled up by capillary action or pipetting, and are held at the tip together with a small amount of cryoprotectant. The quality of the diffraction data using this method is comparable to that of data from conventional cryoloops. This solid apparatus is hopefully suitable for automation of microcrystal handling coupled with optical tweezers. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Makino, M. Wada, I. Mizuno, N. Hirata, K. Shimizu, N. Hikima, T. Yamamoto, M. Kumasaka, T. 2012-07-04 doi:10.1107/S0021889812024545 International Union of Crystallography It is demonstrated that a cryocrystallographic mounting method using a fine-needle capillary is suitable for protein microcrystals. EN microcrystals capillaries cryocrystallography Protein microcrystals of less than 10 µm in size are now applicable to X-ray studies by synchrotron microbeam technology. However, because of their small size, they are difficult to handle and mount. In addition, the deterioration of data quality by scattering from the mounting apparatus and crystallization solvent is not negligible. To address these issues, a simple mounting method is proposed using a fine-needle capillary similar to that used for microinjection in cell biology. In this method, microcrystals are pulled up by capillary action or pipetting, and are held at the tip together with a small amount of cryoprotectant. The quality of the diffraction data using this method is comparable to that of data from conventional cryoloops. This solid apparatus is hopefully suitable for automation of microcrystal handling coupled with optical tweezers. text/html Fine-needle capillary mounting for protein microcrystals text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 785 788 http://scripts.iucr.org/cgi-bin/paper?ce5136 A new procedure (COVMAP) has been developed with the aim of recovering the full structure from very poor models, such as those provided by direct methods in unfavorable conditions. The procedure is based on the concept of covariance between points of an electron density map, mathematically set out by the authors in a recent paper: i.e. the density at one point depends on the density at another point of the map if their covariance is not vanishing. This concept suggested a procedure of electron density modification that uses pairs of model peaks to restrict the region where the density modification should be applied. Such modified densities lead to additional peaks, which in turn are submitted to two other important phasing tools present in EXPO2011, the resolution bias minimization and weighted least-squares procedures, which relocate, refine or reject these peaks. The procedure is cyclic and often leads to the correct structure even if the starting model is very poor. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Altomare, A. Cuocci, C. Giacovazzo, C. Moliterni, A. Rizzi, R. 2012-07-04 doi:10.1107/S002188981201953X International Union of Crystallography A new method for recovering atom positions missing in a structure model obtained at the end of the ab initio solution process has been developed. EN crystal structure solution powder diffraction structure model optimization computer programs COVMAP EXPO A new procedure (COVMAP) has been developed with the aim of recovering the full structure from very poor models, such as those provided by direct methods in unfavorable conditions. The procedure is based on the concept of covariance between points of an electron density map, mathematically set out by the authors in a recent paper: i.e. the density at one point depends on the density at another point of the map if their covariance is not vanishing. This concept suggested a procedure of electron density modification that uses pairs of model peaks to restrict the region where the density modification should be applied. Such modified densities lead to additional peaks, which in turn are submitted to two other important phasing tools present in EXPO2011, the resolution bias minimization and weighted least-squares procedures, which relocate, refine or reject these peaks. The procedure is cyclic and often leads to the correct structure even if the starting model is very poor. text/html COVMAP: a new algorithm for structure model optimization in the EXPO package text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 789 797 http://scripts.iucr.org/cgi-bin/paper?rw5017 Ordered nanoporous silica materials containing cylindrical pores on a two-dimensional hexagonal lattice are known to deform upon adsorption and condensation of fluids. These sorption strains can be measured by in situ small-angle X-ray scattering by analysing the shift of the Bragg peaks from the ordered pore lattice. Besides the real lattice deformation due to the interaction of the solid pore walls with the fluid, a hitherto unexplained apparent lattice expansion is found experimentally in SBA-15 nanoporous silica in a narrow pressure region for three different fluids (pentane, perfluoropentane and water). It is shown that the Bragg peak shift in this region results partly from a subtle contrast effect. The pore form factor changes during capillary condensation owing to the sequential filling of pores according to their diameter. Together with the structure factor from a lattice of finite size, this leads to an effective shift of the Bragg peaks, resulting in the measured apparent lattice strain. Two simple models are presented, which aim to quantitatively describe these apparent strains. The first model employs cylindrical pores with a size distribution on a two-dimensional hexagonal lattice. Filling of pores is achieved by changing the contrast between the pores of a certain size with respect to the surrounding matrix, and the peak shift is calculated from the power spectrum of this lattice. The second model derives analytical expressions for the peak shifts as a function of pore filling fraction by using a Taylor expansion of the pore form factor and a uniform pore size distribution. Both models are able to reproduce the experimental results satisfactorily, providing the possibility to separate these apparent lattice strains from real pore wall deformation in nanoporous materials. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Prass, J. Müter, D. Erko, M. Paris, O. 2012-07-04 doi:10.1107/S0021889812025058 International Union of Crystallography A Bragg peak shift suggests a pore lattice expansion in ordered nanoporous silica at the onset of capillary condensation of fluids. In depth analysis by a numerical and an analytical approach leads to the conclusion that this shift is due not to a mechanical deformation of the pore lattice but to a subtle interplay between the form factor and the structure factor from crystallites of finite size. EN small-angle X-ray scattering adsorption SBA-15 nanopores mesopores scattering contrast expansion contraction Ordered nanoporous silica materials containing cylindrical pores on a two-dimensional hexagonal lattice are known to deform upon adsorption and condensation of fluids. These sorption strains can be measured by in situ small-angle X-ray scattering by analysing the shift of the Bragg peaks from the ordered pore lattice. Besides the real lattice deformation due to the interaction of the solid pore walls with the fluid, a hitherto unexplained apparent lattice expansion is found experimentally in SBA-15 nanoporous silica in a narrow pressure region for three different fluids (pentane, perfluoropentane and water). It is shown that the Bragg peak shift in this region results partly from a subtle contrast effect. The pore form factor changes during capillary condensation owing to the sequential filling of pores according to their diameter. Together with the structure factor from a lattice of finite size, this leads to an effective shift of the Bragg peaks, resulting in the measured apparent lattice strain. Two simple models are presented, which aim to quantitatively describe these apparent strains. The first model employs cylindrical pores with a size distribution on a two-dimensional hexagonal lattice. Filling of pores is achieved by changing the contrast between the pores of a certain size with respect to the surrounding matrix, and the peak shift is calculated from the power spectrum of this lattice. The second model derives analytical expressions for the peak shifts as a function of pore filling fraction by using a Taylor expansion of the pore form factor and a uniform pore size distribution. Both models are able to reproduce the experimental results satisfactorily, providing the possibility to separate these apparent lattice strains from real pore wall deformation in nanoporous materials. text/html Apparent lattice expansion in ordered nanoporous silica during capillary condensation of fluids text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 798 806 http://scripts.iucr.org/cgi-bin/paper?rg5010 X-ray photon correlation spectroscopy (XPCS) was employed to measure the time-dependent intermediate scattering function in an organic molecular glass former. Slow translational dynamics were probed in the glassy state and the correlation functions were calculated from two-dimensional speckle patterns recorded by a CCD detector. The image frames were analysed using a droplet algorithm together with an event correlation scheme. This method provides results analogous to standard intensity correlation algorithms but is much faster, hence addressing the recurrent problem of insufficient computing power for online analysis in XPCS. The event correlator has a wide range of potential future applications at synchrotrons and free-electron laser sources. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Chushkin, Y. Caronna, C. Madsen, A. 2012-06-20 doi:10.1107/S0021889812023321 International Union of Crystallography Structural relaxations in a molecular glass former were probed by X-ray photon correlation spectroscopy. The time-dependent intermediate scattering function was calculated using a novel event correlation algorithm that takes both single- and multiple-photon events into account. EN X-ray photon correlation spectroscopy event correlation scheme speckle patterns X-ray free-electron lasers X-ray photon correlation spectroscopy (XPCS) was employed to measure the time-dependent intermediate scattering function in an organic molecular glass former. Slow translational dynamics were probed in the glassy state and the correlation functions were calculated from two-dimensional speckle patterns recorded by a CCD detector. The image frames were analysed using a droplet algorithm together with an event correlation scheme. This method provides results analogous to standard intensity correlation algorithms but is much faster, hence addressing the recurrent problem of insufficient computing power for online analysis in XPCS. The event correlator has a wide range of potential future applications at synchrotrons and free-electron laser sources. text/html A novel event correlation scheme for X-ray photon correlation spectroscopy text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 807 813 http://scripts.iucr.org/cgi-bin/paper?fs5012 The different Zeeman beam-splitting effects in neutron reflectivity experiments in reflection and refraction are discussed. Different possible representations of the experimental Zeeman splitting data in various coordinate systems are investigated. Some of these representations are useful to unambiguously identify the off-specular splitting arising from Zeeman energy and discriminate it from the usual diffuse scattering. Some representations are more suited for the direct extraction of quantitative information about the systems by using the Zeeman splitting effect. The Zeeman splitting can thus be used as a tool rather than being treated as a parasitic effect. Parameters such as the optical and magnetic potentials of buried layers can be directly extracted. The magnetic induction in demagnetized samples can also be probed. These representative characteristics are illustrated by experimental data measured on different systems. In thick AlSiFe films (20 µm), the magnetic induction is determined at the top and bottom interfaces. In thin Co layers (250 nm), the magnetic induction of ferromagnetic domains in the demagnetized state is evaluated. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Kozhevnikov, S. Ott, F. Radu, F. 2012-07-14 doi:10.1107/S0021889812018043 International Union of Crystallography The different Zeeman energy effects in neutron reflectivity experiments and their influence on beam splitting are reviewed. The representation of Zeeman splitting data in several coordinate systems is discussed, and the use of such data to directly extract information on magnetic thin-film systems is examined. EN neutron reflectivity Zeeman energy beam splitting magnetic layers off-specular scattering The different Zeeman beam-splitting effects in neutron reflectivity experiments in reflection and refraction are discussed. Different possible representations of the experimental Zeeman splitting data in various coordinate systems are investigated. Some of these representations are useful to unambiguously identify the off-specular splitting arising from Zeeman energy and discriminate it from the usual diffuse scattering. Some representations are more suited for the direct extraction of quantitative information about the systems by using the Zeeman splitting effect. The Zeeman splitting can thus be used as a tool rather than being treated as a parasitic effect. Parameters such as the optical and magnetic potentials of buried layers can be directly extracted. The magnetic induction in demagnetized samples can also be probed. These representative characteristics are illustrated by experimental data measured on different systems. In thick AlSiFe films (20 µm), the magnetic induction is determined at the top and bottom interfaces. In thin Co layers (250 nm), the magnetic induction of ferromagnetic domains in the demagnetized state is evaluated. text/html Data representations of Zeeman spatial beam splitting in polarized neutron reflectometry text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 814 825 http://scripts.iucr.org/cgi-bin/paper?rw5012 The implantation of He ions in UO2 polycrystals induces a strain in the implanted layer which can be characterized using Laue micro X-ray diffraction (µ-XRD). The strain tensor resulting from the ion implantation may not be reduced to a single out-of-plane strain component: it also has nonzero shear components. Their strong dependence upon crystal orientation is modeled using elasticity theory. This work demonstrates the potential of Laue µ-XRD for characterizing radiation effects in materials. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Richard, A. Palancher, H. Castelier, É Micha, J.-S. Gamaleri, M. Carlot, G. Rouquette, H. Goudeau, P. Martin, G. Rieutord, F. Piron, J.P. Garcia, P. 2012-07-14 doi:10.1107/S0021889812027665 International Union of Crystallography Micro X-ray diffraction and mechanical modeling on low-energy (60 keV) light-ion (He)-implanted polycrystals have shown that the strain tensor has only three nonzero components, which depend on grain orientation. EN micro X-ray diffraction polycrystals light-ion implantation grain orientation The implantation of He ions in UO2 polycrystals induces a strain in the implanted layer which can be characterized using Laue micro X-ray diffraction (µ-XRD). The strain tensor resulting from the ion implantation may not be reduced to a single out-of-plane strain component: it also has nonzero shear components. Their strong dependence upon crystal orientation is modeled using elasticity theory. This work demonstrates the potential of Laue µ-XRD for characterizing radiation effects in materials. text/html Strains in light-ion-implanted polycrystals: influence of grain orientation text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 826 833 http://scripts.iucr.org/cgi-bin/paper?kk5107 The space group of a crystal pattern is the intersection group of the eigensymmetries of the crystallographic orbits corresponding to the occupied Wyckoff positions. Polar space groups without symmetry elements with glide or screw components smaller than 1/2 do not contain characteristic orbits and cannot be realized in patterns (structures) made by only one crystallographic type of object (atom). The space-group diagram of the general orbit for this type of group has an eigensymmetry that corresponds to a special orbit in a centrosymmetric supergroup of the generating group. This fact is often overlooked, as shown in the proposed solution for Plates (i)–(vi) of IUCr Teaching Pamphlet No. 14, and an alternative interpretation is given. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Suescun, L. Nespolo, M. 2012-06-12 doi:10.1107/S002188981201998X International Union of Crystallography The common misinterpretation of a special orbit in centrosymmetric space groups as a general orbit in a polar subgroup is pointed out through some of the examples in IUCr Teaching Pamphlet No. 14, and an alternative interpretation is given. EN space groups eigensymmetries crystallographic orbits IUCr Teaching Pamphlet No. 14 The space group of a crystal pattern is the intersection group of the eigensymmetries of the crystallographic orbits corresponding to the occupied Wyckoff positions. Polar space groups without symmetry elements with glide or screw components smaller than 1/2 do not contain characteristic orbits and cannot be realized in patterns (structures) made by only one crystallographic type of object (atom). The space-group diagram of the general orbit for this type of group has an eigensymmetry that corresponds to a special orbit in a centrosymmetric supergroup of the generating group. This fact is often overlooked, as shown in the proposed solution for Plates (i)–(vi) of IUCr Teaching Pamphlet No. 14, and an alternative interpretation is given. text/html From patterns to space groups and the eigensymmetry of crystallographic orbits: a reinterpretation of some symmetry diagrams in IUCr Teaching Pamphlet No. 14 text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography teaching and education 834 837 http://scripts.iucr.org/cgi-bin/paper?ks5319 Errors in the article by Popa & Balzar [J. Appl. Cryst. (2001), 34, 187–195], caused by an equation from literature used without checking, are corrected. It is expected that other published papers will have been affected as the source error is in a reference book. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Popa, N.C. Balzar, D. 2012-07-04 doi:10.1107/S0021889812024879 International Union of Crystallography Errors in the article by Popa & Balzar [J. Appl. Cryst. (2001), 34, 187–195], caused by an equation from literature used without checking, are corrected. It is expected that other published papers will have been affected as the source error is in a reference book. EN stress strain texture polycrystals Laue classes Rietveld refinement Errors in the article by Popa & Balzar [J. Appl. Cryst. (2001), 34, 187–195], caused by an equation from literature used without checking, are corrected. It is expected that other published papers will have been affected as the source error is in a reference book. text/html Elastic strain and stress determination by Rietveld refinement: generalized treatment for textured polycrystals for all Laue classes. Corrigenda text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography short communications 838 839 http://scripts.iucr.org/cgi-bin/paper?nb5019 Coherent X-ray diffraction imaging has received considerable attention as a nondestructive method for probing material structure at the nanoscale. However, tools for reconstructing and analysing data in both two and three dimensions have lagged somewhat behind. Bonsu, the interactive phase retrieval suite, is the first software package that allows real-time visualization of the reconstruction of phase information in both two and three dimensions. It comes complete with an inventory of algorithms and routines for data manipulation and reconstruction. Bonsu is open source, is designed around the Python language (with C++ bindings) and is largely platform independent. Bonsu is made available under version three of the GNU General Public License and can be found at http://www.code.google.com/p/bonsu. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Newton, M.C. Nishino, Y. Robinson, I.K. 2012-07-14 doi:10.1107/S0021889812026751 International Union of Crystallography Bonsu is an open-source software package primarily for the reconstruction of phase information from coherent X-ray diffraction measurements. EN phase retrieval computer programs Python SciPy NumPy FFTW Bonsu Coherent X-ray diffraction imaging has received considerable attention as a nondestructive method for probing material structure at the nanoscale. However, tools for reconstructing and analysing data in both two and three dimensions have lagged somewhat behind. Bonsu, the interactive phase retrieval suite, is the first software package that allows real-time visualization of the reconstruction of phase information in both two and three dimensions. It comes complete with an inventory of algorithms and routines for data manipulation and reconstruction. Bonsu is open source, is designed around the Python language (with C++ bindings) and is largely platform independent. Bonsu is made available under version three of the GNU General Public License and can be found at http://www.code.google.com/p/bonsu. text/html Bonsu: the interactive phase retrieval suite text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 840 843 http://scripts.iucr.org/cgi-bin/paper?he5554 DAJUST is the generic name of a software package for powder diffraction formed by the core programs AJUST and SGAID (both written in Fortran) controlled by an easy-to-use Java user interface (DAJUST_UI). While AJUST performs whole-pattern matching (cell-parameter refinement, profile fitting and intensity extraction), SGAID provides a list of the most probable space groups. For the extraction of the integrated intensities, AJUST uses the Le Bail procedure but with a different formula for refining the integrated intensities. Laboratory, synchrotron X-ray and neutron sources, and both reflection and transmission experimental geometries, are supported. Other program options include automated background estimation, asymmetry correction, and corrections for absorption, variable divergence and/or illumination. The extracted intensity data are written in text format and can be directly processed by the direct methods program XLENS [Rius (2011). Acta Cryst. A67, 63–67] and the multisolution direct-space structure determination program TALP [Vallcorba, Rius, Frontera & Miravitlles (2011). Acta Cryst. A67, C272]. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Vallcorba, O. Rius, J. Frontera, C. Peral, I. Miravitlles, C. 2012-06-20 doi:10.1107/S0021889812021152 International Union of Crystallography The interactive powder diffraction program DAJUST for whole-pattern matching, space-group determination and extraction of integrated intensities is described. The resulting intensity data files are compatible with the XLENS (Patterson function direct methods) and TALP (direct-space multisolution methods) programs of the authors' laboratory (ICMAB, CSIC). EN powder diffraction pattern matching intensity extraction DAJUST computer programs DAJUST is the generic name of a software package for powder diffraction formed by the core programs AJUST and SGAID (both written in Fortran) controlled by an easy-to-use Java user interface (DAJUST_UI). While AJUST performs whole-pattern matching (cell-parameter refinement, profile fitting and intensity extraction), SGAID provides a list of the most probable space groups. For the extraction of the integrated intensities, AJUST uses the Le Bail procedure but with a different formula for refining the integrated intensities. Laboratory, synchrotron X-ray and neutron sources, and both reflection and transmission experimental geometries, are supported. Other program options include automated background estimation, asymmetry correction, and corrections for absorption, variable divergence and/or illumination. The extracted intensity data are written in text format and can be directly processed by the direct methods program XLENS [Rius (2011). Acta Cryst. A67, 63–67] and the multisolution direct-space structure determination program TALP [Vallcorba, Rius, Frontera & Miravitlles (2011). Acta Cryst. A67, C272]. text/html DAJUST: a suite of computer programs for pattern matching, space-group determination and intensity extraction from powder diffraction data text 4 45 2012-06-20 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 844 848 http://scripts.iucr.org/cgi-bin/paper?he5558 The WinGX suite provides a complete set of programs for the treatment of small-molecule single-crystal diffraction data, from data reduction and processing, structure solution, model refinement and visualization, and metric analysis of molecular geometry and crystal packing, to final report preparation in the form of a CIF. It includes several well known pieces of software and provides a repository for programs when the original authors no longer wish to, or are unable to, maintain them. It also provides menu items to execute external software, such as the SIR and SHELX suites of programs. The program ORTEP for Windows provides a graphical user interface (GUI) for the classic ORTEP program, which is the original software for the illustration of anisotropic displacement ellipsoids. The GUI code provides input capabilities for a wide variety of file formats, and extra functionality such as geometry calculations and ray-traced outputs. The programs WinGX and ORTEP for Windows have been distributed over the internet for about 15 years, and this article describes some of the more modern features of the programs. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Farrugia, L.J. 2012-07-14 doi:10.1107/S0021889812029111 International Union of Crystallography The programs WinGX and ORTEP for Windows have been distributed over the internet for about 15 years, and this article describes some of the more modern features of the programs. EN WinGX ORTEP for Windows computer programs The WinGX suite provides a complete set of programs for the treatment of small-molecule single-crystal diffraction data, from data reduction and processing, structure solution, model refinement and visualization, and metric analysis of molecular geometry and crystal packing, to final report preparation in the form of a CIF. It includes several well known pieces of software and provides a repository for programs when the original authors no longer wish to, or are unable to, maintain them. It also provides menu items to execute external software, such as the SIR and SHELX suites of programs. The program ORTEP for Windows provides a graphical user interface (GUI) for the classic ORTEP program, which is the original software for the illustration of anisotropic displacement ellipsoids. The GUI code provides input capabilities for a wide variety of file formats, and extra functionality such as geometry calculations and ray-traced outputs. The programs WinGX and ORTEP for Windows have been distributed over the internet for about 15 years, and this article describes some of the more modern features of the programs. text/html WinGX and ORTEP for Windows: an update text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 849 854 http://scripts.iucr.org/cgi-bin/paper?to5015 The FraGen (framework generator) program has been developed for real-space structure solution. It has been designed especially for the generation of extended inorganic frameworks in a given unit cell. FraGen is based on the parallel tempering global optimization method. Various restraints can be introduced into FraGen, such as restraints on bonding geometry, relative reflection intensities and three-dimensional density maps. The basic inputs for FraGen are the space group and cell parameters. The number of unique atoms is not a necessary input, since it can be estimated from certain constraints. FraGen also has the ability to exit unpromising simulation cycles to save computation time for promising ones. Program features, methods and three examples are demonstrated. The FraGen program for the Windows platform is available from the authors upon request. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Li, Y. Yu, J. Xu, R. 2012-06-12 doi:10.1107/S002188981201878X International Union of Crystallography A computer program is reported for the structure solution of extended inorganic frameworks in real space. The space group and cell parameters are the basic inputs required by this program. Prior chemical and crystallographic knowledge can significantly enhance its computation efficiency. EN structure solution real space global optimization extended inorganic frameworks computer programs FraGen The FraGen (framework generator) program has been developed for real-space structure solution. It has been designed especially for the generation of extended inorganic frameworks in a given unit cell. FraGen is based on the parallel tempering global optimization method. Various restraints can be introduced into FraGen, such as restraints on bonding geometry, relative reflection intensities and three-dimensional density maps. The basic inputs for FraGen are the space group and cell parameters. The number of unique atoms is not a necessary input, since it can be estimated from certain constraints. FraGen also has the ability to exit unpromising simulation cycles to save computation time for promising ones. Program features, methods and three examples are demonstrated. The FraGen program for the Windows platform is available from the authors upon request. text/html FraGen: a computer program for real-space structure solution of extended inorganic frameworks text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 855 861 http://scripts.iucr.org/cgi-bin/paper?nb5023 The processing and quantification of electron diffraction patterns have become vital in advanced electron crystallographic analysis work. A computer program, QPCED2.0, has been developed for the handling of selected-area electron diffraction patterns for polycrystalline materials. QPCED2.0 can be used to enhance the visibility of electron diffraction patterns, to convert electron diffraction patterns into intensity profiles, and to retrieve precisely the lattice d spacings and the integral intensities of the diffraction rings. The design and implementation of QPCED2.0 are elucidated and application examples are given. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Li, X.-Z. 2012-07-14 doi:10.1107/S0021889812027173 International Union of Crystallography A computer program, QPCED2.0, has been developed for the handling of selected-area electron diffraction patterns for polycrystalline materials. The design and implementation of QPCED2.0 are elucidated and application examples are given. EN QPCED2.0 polycrystalline diffraction selected-area electron diffraction pattern processing pattern quantification computer programs The processing and quantification of electron diffraction patterns have become vital in advanced electron crystallographic analysis work. A computer program, QPCED2.0, has been developed for the handling of selected-area electron diffraction patterns for polycrystalline materials. QPCED2.0 can be used to enhance the visibility of electron diffraction patterns, to convert electron diffraction patterns into intensity profiles, and to retrieve precisely the lattice d spacings and the integral intensities of the diffraction rings. The design and implementation of QPCED2.0 are elucidated and application examples are given. text/html QPCED2.0: a computer program for the processing and quantification of polycrystalline electron diffraction patterns text 4 45 2012-07-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 862 868 http://scripts.iucr.org/cgi-bin/paper?rg5012 A first-generation-synchrotron-class X-ray laboratory microsource, coupled to a three-pinhole camera, is presented. It allows (i) small- and wide-angle X-ray scattering images to be acquired simultaneously, and (ii) scanning small- and wide-angle X-ray scattering microscopy to be carried out. As representative applications, the structural complexity of a biological natural material (human bone biopsy) and of a metamaterial (colloidal nanocrystal assembly) are inspected at different length scales, studying the atomic/molecular ordering by (grazing-incidence) wide-angle X-ray scattering and the morphological/structural conformation by (grazing-incidence) small-angle X-ray scattering. In particular, the grazing-incidence measurement geometries are needed for inspecting materials lying on top of surfaces or buried underneath surfaces. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Altamura, D. Lassandro, R. Vittoria, F.A. De Caro, L. Siliqi, D. Ladisa, M. Giannini, C. 2012-07-04 doi:10.1107/S0021889812025733 International Union of Crystallography A first-generation-synchrotron-class X-ray laboratory microsource, coupled to a three-pinhole camera, is presented. It allows small- and wide-angle X-ray scattering images to be acquired simultaneously, and scanning small- and wide-angle X-ray scattering microscopy to be carried out. EN microfocus X-ray imaging small-angle X-ray scattering wide-angle X-ray scattering grazing-incidence small-angle X-ray scattering grazing-incidence wide-angle X-ray scattering A first-generation-synchrotron-class X-ray laboratory microsource, coupled to a three-pinhole camera, is presented. It allows (i) small- and wide-angle X-ray scattering images to be acquired simultaneously, and (ii) scanning small- and wide-angle X-ray scattering microscopy to be carried out. As representative applications, the structural complexity of a biological natural material (human bone biopsy) and of a metamaterial (colloidal nanocrystal assembly) are inspected at different length scales, studying the atomic/molecular ordering by (grazing-incidence) wide-angle X-ray scattering and the morphological/structural conformation by (grazing-incidence) small-angle X-ray scattering. In particular, the grazing-incidence measurement geometries are needed for inspecting materials lying on top of surfaces or buried underneath surfaces. text/html X-ray microimaging laboratory (XMI-LAB) text 4 45 2012-07-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography laboratory notes 869 873 http://scripts.iucr.org/cgi-bin/paper?pf0098 Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Paufler, P. 2012-06-12 doi:10.1107/S0021889812021139 International Union of Crystallography EN book received text/html Nonlinear Mechanics of Crystals. By John D. Clayton. Pp. 700. Dordrecht, Heidelberg, London, New York: Springer, 2011. Price (hardcover) Euros 169.95. ISBN-978-94-007-0349-0. text 4 45 2012-06-12 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography books received 874 874