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Single-crystal X-ray and neutron diffraction data are usually collected using separate samples. This is a disadvantage when the sample is studied at high pressure because it is very difficult to achieve exactly the same pressure in two separate experiments, especially if the neutron data are collected using Laue methods where precise absolute values of the unit-cell dimensions cannot be measured to check how close the pressures are. In this study, diffraction data have been collected under the same conditions on the same sample of copper(II) sulfate pentahydrate, using a conventional laboratory diffractometer and source for the X-ray measurements and the Koala single-crystal Laue diffractometer at the ANSTO facility for the neutron measurements. The sample, of dimensions 0.40 × 0.22 × 0.20 mm3 and held at a pressure of 0.71 GPa, was contained in a miniature Merrill–Bassett diamond-anvil cell. The highly penetrating diffracted neutron beams passing through the metal body of the miniature cell as well as through the diamonds yielded data suitable for structure refinement, and compensated for the low completeness of the X-ray measurements, which was only 24% on account of the triclinic symmetry of the sample and the shading of reciprocal space by the cell. The two data-sets were combined in a single `XN' structure refinement in which all atoms, including H atoms, were refined with anisotropic displacement parameters. The precision of the structural parameters was improved by a factor of up to 50% in the XN refinement compared with refinements using the X-ray or neutron data separately.

The crystal structure of the monoclinic polymorph of the primary amino acid l‐histidine has been determined for the first time by single‐crystal neutron diffraction, while that of the orthorhombic polymorph has been reinvestigated with an untwinned crystal, improving the experimental precision and accuracy. For each polymorph, neutron diffraction data were collected at 5, 105 and 295 K. Single‐crystal X‐ray diffraction experiments were also performed at the same temperatures. The two polymorphs, whose crystal packing is interpreted by intermolecular interaction energies calculated using the Pixel method, show differences in the energy and geometry of the hydrogen bond formed along the c direction. Taking advantage of the X‐ray diffraction data collected at 5 K, the precision and accuracy of the new Hirshfeld atom refinement method implemented in NoSpherA2 were probed choosing various settings of the functionals and basis sets, together with the use of explicit clusters of molecules and enhanced rigid‐body restraints for H atoms. Equivalent atomic coordinates and anisotropic displacement parameters were compared and found to agree well with those obtained from the corresponding neutron structural models. [ABSTRACT FROM AUTHOR]

The factors affecting the accuracy of structural refinements from image‐plate neutron Laue diffractometers are analysed. From this analysis, an improved data‐processing method is developed which optimizes the intensity corrections for exposure scaling, wavelength distribution, absorption and extinction corrections, and the wavelength/spatial/time dependence of the image‐plate detector efficiencies. Of equal importance is an analysis of the sources of uncertainty in the final corrected intensities, without which bias of the merged intensities occurs, due to the dominance of measurements with small statistical errors though potentially large systematic errors. A new aspect of the impact of detector crosstalk on the counting statistics of area detectors is reported and shown to be significant for the case of neutron Laue diffraction. These methods have been implemented in software which processes data from the KOALA instrument at ANSTO and the now decommissioned VIVALDI instrument at ILL (Grenoble, France). A comparison with earlier data‐analysis methods shows a significant improvement in accuracy of the refined structures. [ABSTRACT FROM AUTHOR]

MgSeO4·7H2O is isostructural with the analogous sulfate, MgSO4·7H2O, consisting of isolated [Mg(H2O)6]2+ octahedra and [SeO4]2− tetrahedra, linked by O—H...O hydrogen bonds, with a single interstitial lattice water molecule. As in the sulfate, the [Mg(H2O)6]2+ coordination octahedron is elongated along one axis due to the tetrahedral coordination of the two apical water molecules; these have Mg—O distances of ∼2.10 Å, whereas the remaining four trigonally coordinated water molecules have Mg—O distances of ∼2.05 Å. The mean Se—O bond length is 1.641 Å and is in excellent agreement with other selenates. The unit-cell volume of MgSeO4·7H2O at 10 K is 4.1% larger than that of the sulfate at 2 K, although this is not uniform; the greater part of the expansion is along the a axis of the crystal.

Aperiodic composite crystals present long-range order without translational symmetry. These materials may be described as the intersection in three dimensions of a crystal which is periodic in a higher-dimensional space. In such materials, symmetry breaking must be described as structural changes within these crystallographic superspaces. The increase in the number of superspace groups with the increase in the dimension of the superspace allows many more structural solutions. This is illustrated in n-nonadecane-urea, revealing a fifth higher-dimensional phase at low temperature. [ABSTRACT FROM AUTHOR]

The atomic and magnetic structure of brownmillerite Ca2Fe2O5 has been refined against single-crystal neutron Laue diffraction data collected at 300, 100 and 10 K under zero-field and low-magnetic field (35 Oe = 35 × 103/4π A m−1) conditions. Ca2Fe2O5 is a canted G-type antiferromagnet with Pcm′ n′ symmetry, the magnetic moments on Fe being directed approximately along the crystallographic c axis at room temperature. The refinement results show clearly that this magnetic structure persists down to T = 10 K, despite a previous suggestion that an anomalous magnetic susceptibility enhancement observed in Ca2Fe2O5 single crystals between 40 and 140 K might signify a reorientation of the antiferromagnetic easy axis from c to a below 40 K. Alternative explanations for this susceptibility anomaly are considered in terms of the evidence for partial or short-range loss of order in the anomalous regime, possibly due to the presence of multiple competing sublattice interactions. [ABSTRACT FROM AUTHOR]

The atomic and magnetic structure of brownmillerite Ca2Fe2O5 has been refined against single-crystal neutron Laue diffraction data collected at 300, 100 and 10 K under zero-field and low-magnetic field (35 Oe = 35 × 103/4π A m−1) conditions. Ca2Fe2O5 is a canted G-type antiferromagnet with Pcm′ n′ symmetry, the magnetic moments on Fe being directed approximately along the crystallographic c axis at room temperature. The refinement results show clearly that this magnetic structure persists down to T = 10 K, despite a previous suggestion that an anomalous magnetic susceptibility enhancement observed in Ca2Fe2O5 single crystals between 40 and 140 K might signify a reorientation of the antiferromagnetic easy axis from c to a below 40 K. Alternative explanations for this susceptibility anomaly are considered in terms of the evidence for partial or short-range loss of order in the anomalous regime, possibly due to the presence of multiple competing sublattice interactions. [ABSTRACT FROM AUTHOR]

A single-crystal neutron diffraction study of a synthetic ulvöspinel sample of composition Fe0.403+Fe1.802+ Ti0.80O4 was performed to investigate the static positional disorder at the octahedrally coordinated M site. Anisotropic structural refinement was performed in the space group ... against neutron Laue diffraction data collected at 298 K from two millimetric-sized crystals. Initial structure refinements were conducted with Fe and Ti sharing the M site (at 1/2, 1/2, 1/2), and their partial site occupancy was refined. The tetrahedrally coordinated T site (at 1/8, 1/8, 1/8) was modeled as fully occupied by Fe. For both crystals, the final R1 index was about 3% for 9 refined parameters and 129 unique reflections, with no significant residuals. As the atomic displacement factors obtained were anomalously high, according to the previous experimental findings, Fobs- and (Fobs-Fcal)-difference Fourier maps of the nuclear density were generated. Fourier maps showed a significant minimum located out-of-center of the M site, and indicating a displacement of the Ti4+ from the center of the octahedron. A further test refinement was successfully conducted with two mutually exclusive sites: MTi out-of-center (at 0.49, 0.49, 0.49) and MFe on the center (at 1/2, 1/2, 1/2). The resulting displacement of Ti from the octahedral center appears to be shorter than 0.15 Å. Using bond-valence theory, the out-of-center distortion of MTi4+ is interpreted as a result of intrinsic distortions in the ulvöspinel structure. The potential implication of the octahedral distortion on the behavior of ulvöspinel at non-ambient conditions is discussed. [ABSTRACT FROM AUTHOR]

The crystal chemistry and crystal structure of hambergite from the Anjanabonoina mine, Madagascar [Be2BO3(OH)0.96F0.04, Z = 8, a = 9.762(2), b = 12.201(2), c = 4.430(1) Å, V = 527.6(2) ų, space group Pbca], were reinvestigated by means of electron microprobe analysis in wavelength-dispersive mode, secondary-ion mass spectrometry, single-crystal X-ray and neutron Laue diffraction. Chemical analyses show only a small amount of F (0.7-0.8 wt%, approximately 0.04 atoms per formula unit) substituting OH and no other substituent at a significant level. An anisotropic neutron structural refinement has been performed with final agreement index R1 = 0.0504 for 76 refined parameters and 1430 unique reflections with Fo > 4σ(Fo). The geometry of the hydroxyl group and hydrogen bonding in hambergite is now well defined: (1) only one independent H site was located and the O4-H distance, corrected for "riding motion,: is ~0.9929 Å; (2) only one hydrogen bond appears to be energetically favorable, with a symmetry-related O4 as acceptor and with O4…O4 = 2.904(1) Å, H…4 = 1.983(1) Å, and O4-H…4 = 157.5(1)°. In other words, O4 sites act both as donor and as acceptor of the hydrogen bond, with a zigzag chain of H-bonds along [001]. The hydrogen-bonding scheme in hambergite found in this study is consistent with the pleochroic scheme of the infrared spectra previously reported, with two intensive modes ascribable to stretching vibrations of the hydroxyl group, at 3415 and 3520 cm--1, respectively. The two modes suggest at least two distinct hydrogen-bonding environments, ascribable to the presence of oxygen and fluorine at the acceptor site. [ABSTRACT FROM AUTHOR]

Single crystals of composition Bi35.66W4.34O66.51 (or Bi8.2WO15.3, bismuth tungsten oxide), within the type (Ib) solid-solution region of the Bi2O3-WO3 system, were synthesized using the floating-zone furnace method. Synchrotron X-ray and neutron single-crystal diffraction data were used to confirm the previously tentative assignment of the room-temperature space group as I41. Fourier analysis of the combined X-ray and neutron datasets was used to elucidate and refine fully the cation and anion arrays for the first time. The mixed cation site M1 is shown to be coordinated by eight O atoms in an irregular cube when M = Bi, and by six O atoms in an octahedron when M = W. The resulting disorder in the average structure around M1 is discussed in the context of experimentally observed oxide-ion conductivity. [ABSTRACT FROM AUTHOR]

Single-crystal X-ray and neutron diffraction data are usually collected using separate samples. This is a disadvantage when the sample is studied at high pressure because it is very difficult to achieve exactly the same pressure in two separate experiments, especially if the neutron data are collected using Laue methods where precise absolute values of the unit-cell dimensions cannot be measured to check how close the pressures are. In this study, diffraction data have been collected under the same conditions on the same sample of copper(II) sulfate pentahydrate, using a conventional laboratory diffractometer and source for the X-ray measurements and the Koala single-crystal Laue diffractometer at the ANSTO facility for the neutron measurements. The sample, of dimensions 0.40 × 0.22 × 0.20 mm 3 and held at a pressure of 0.71 GPa, was contained in a miniature Merrill-Bassett diamond-anvil cell. The highly penetrating diffracted neutron beams passing through the metal body of the miniature cell as well as through the diamonds yielded data suitable for structure refinement, and compensated for the low completeness of the X-ray measurements, which was only 24% on account of the triclinic symmetry of the sample and the shading of reciprocal space by the cell. The two data-sets were combined in a single 'XN' structure refinement in which all atoms, including H atoms, were refined with anisotropic displacement parameters. The precision of the structural parameters was improved by a factor of up to 50% in the XN refinement compared with refinements using the X-ray or neutron data separately., (© Giulia Novelli et al. 2022.)

An overview is presented of an integrated software package for the processing of Laue data from reactor and other continuous neutron sources. LaueG appears to the user as a graphical user interface with interactive graphic modes that depend on the task being performed: simple image display, cell indexing and refinement, peak integration, wavelength normalization and intensity corrections, or identification of statistical outliers. Other capabilities under development, though still usable, include satellite spots and modulated structures, twinned crystal analysis, and ab initio indexing of unit cells. The emphasis is on accurate intensities for structure refinement using an integrated graphical approach. [ABSTRACT FROM AUTHOR]

MgSeO4·7H2O is isostructural with the analogous sulfate, MgSO4·7H2O, consisting of isolated [Mg(H2O)6](2+) octa-hedra and [SeO4](2-) tetra-hedra, linked by O-H⋯O hydrogen bonds, with a single inter-stitial lattice water mol-ecule. As in the sulfate, the [Mg(H2O)6](2+) coordination octa-hedron is elongated along one axis due to the tetra-hedral coordination of the two apical water mol-ecules; these have Mg-O distances of ∼2.10 Å, whereas the remaining four trigonally coordinated water mol-ecules have Mg-O distances of ∼2.05 Å. The mean Se-O bond length is 1.641 Å and is in excellent agreement with other selenates. The unit-cell volume of MgSeO4·7H2O at 10 K is 4.1% larger than that of the sulfate at 2 K, although this is not uniform; the greater part of the expansion is along the a axis of the crystal.