The crystal structure of SiAl5O2N5 was characterized by laboratory X-ray powder diffraction (CuKα1). The title compound is hexagonal with space group P63/mmc (Z = 2). The unit-cell dimensions are a = 0.303153(3) nm, c = 3.28153(3) nm, and V = 0.261178(5)  nm3. The initial structural model was successfully derived by the direct methods and further refined by the Rietveld method. The final structural model showed the positional disordering of two of the four (Si,Al) sites. The maximum-entropy method-based pattern fitting (MPF) method was used to confirm the validity of the split-atom model, in which conventional structure bias caused by assuming intensity partitioning was minimized. The reliability indices calculated from the MPF were R wp = 5.00%, S (=R wp/R e) = 1.25, R p = 3.76%, R B = 1.26%, and R F  = 0.90%. The disordered crystal structure was successfully described by overlapping four types of domains with ordered atom arrangements. The distribution of atomic positions in each of the domains can be achieved in the space group P63 mc. Two of the four types of domains are related by a pseudo-symmetry inversion, and the two remaining domains also have each other the inversion pseudo-symmetry.

The crystal structure of a morimotoite garnet, ideally Ca3(Ti4+Fe2+)Si3O12, from the Ice River alkaline complex, British Columbia, Canada was refined by the Rietveld method, space group $Ia\overline 3 d$ , and monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. Electron-microprobe analysis indicates a homogeneous sample with a formula {Ca2.91Mg0.05Mn2+ 0.03}Σ3[Ti1.09Fe3+ 0.46Fe2+ 0.37Mg0.08]Σ2(Si2.36Fe3+ 0.51Al0.14)Σ3O12. The HRPXRD data show a two-phase intergrowth. The reduced χ 2 and overall R(F 2) Rietveld refinement values are 1.572 and 0.0544, respectively. The weight percentage, unit-cell parameter (Å), distances (Å), and site occupancy factors (sofs) for phase-1 are as follows: 76.5(1)%, a = 12.156 98(1) Å, average <Ca–O> = 2.4383, Ti–O = 2.011(1), Si–O = 1.693(1) Å, Ca(sof) = 0.943(2), Ti(sof) = 0.966(2), and Si(sof) = 1.095(3). The corresponding values for phase-2 are 23.5(1)%, a = 12.160 67(2) Å, average <Ca–O> = 2.452, Ti–O = 1.988(3), Si–O = 1.704(3) Å, Ca(sof) = 1.063(7), Ti(sof) = 1.187(7), and Si(sof) = 1.220(8). The two phases cause strain that arises from structural mismatch and gives rise to low optical anisotropy. Because the two phases are structurally quite similar, a refinement using a single-phase model with anisotropic displacement parameters shows no unusual displacement ellipsoid for the O atom that requires a “split O-atom position”, as was done in previous studies.

The heteroaryl-substituted triazolopyridines 3-phenyl-7-(pyrazin-2-yl)-[1,2,3]triazolo[1,5-a]pyridine (2) and 3-[6-(pyridazin-3-yl)-pyridin-2-yl]-[1,2,3]triazolo[1,5-a]pyridine (4) have been synthesized and characterized (by HRMS, IR, 1H and 13C NMR, XRPD, melting point). The crystal structures have been solved from laboratory powder X-ray diffraction data with the direct-space strategy TALP for molecular compounds based on fast local least-squares minimizations. The crystal structure confirmed the formation of the tridentate compound 4 from a ring chain isomerization process. The almost planar arrangement of atoms in both the structures favors the presence of intermolecular π–π interactions, although weak C–H···N electrostatic interactions seem to be also important for the stabilization of the structure. Powder diffraction data have also proved to be sensible enough to determine the relative rotations of the six-membered rings despite the weak difference in scattering power between C and N atoms.

X-ray diffraction (XRD) has been routinely employed in the Earth sciences to characterize the crystallography of rocks and minerals. Routine characterization of samples too small for analysis by classic automated powder diffraction methods becomes challenging without access to single crystal or micro-diffraction equipment. Here, we show that a traditional Gandolfi camera lined with an image-plate (IP) as the detection medium can return a fully quantitative diffraction pattern from a sub-milligram single grain specimen in a simple and straightforward manner. Data pertaining to peak positions (d-spacings) were assessed using SRM640c Si powder, while intensity data were compared to the certified values for intensity standard SRM676a alumina powder. The refined unit-cell dimension of Si powder differed from the certified value of 5.4312 Å by no more than 0.0003 Å with a standard deviation (σ) of 0.0002 Å among the three experiments. For intensity, the σ and disparity from the certified values of three diffraction experiments on SRM676a were both <2%. The results of a comparative study of the crystallographic parameters determined for a naturally occurring garnet and clinopyroxene given through the refinement of their crystal structure by single-crystal XRD method are presented. These show through Rietveld refinement of X-ray data obtained by the Gandolfi–IP method outlined here that both accurate and precise XRD data can be produced in a timely and cost-effective manner using only an IP, Gandolfi camera, and software freely available on the internet.

The crystal structure of an isotropic, single phase, Ti-rich schorlomite garnet, ideally Ca3Ti4+ 2(Fe3+ 2Si)O12, from Magnet Cove, Arkansas was refined with the Rietveld method, space group $Ia\overline 3 d$ , and monochromatic synchrotron high-resolution powder X-ray diffraction data. Electron-microprobe analysis gave an average composition {Ca2.92Na0.04Mn2+ 0.03Mg0.01}Σ3[Ti1.04Fe3+ 0.46Mg0.18Fe2+ 0.16Zr4+ 0.13V3+ 0.04]Σ2(Si2.21Fe3+ 0.71Al0.07)Σ3O12, and corresponds to the general garnet formula of [8] X 3 [6] Y 2 [4] Z 3 [4]O12. Schorlomite is the dominant component, but the composition contains significant amounts (>15 mol.%) of andradite, Ca3(Fe3+ 2)Si3O12, morimotoite, Ca3(Ti4+Fe2+)Si3O12, and morimotoite-(Mg), Ca3(Ti4+Mg)Si3O12. The crystal structure model was refined well using isotropic and anisotropic displacement parameters. Using isotropic displacement parameters, the χ 2 and R (F 2) Rietveld refinement values are 1.148 and 0.0742, respectively. The unit-cell parameter, a = 12.18599(1) (Å), is large for a natural schorlomite for which complete structural data are available. The bond distances are average <Ca–O> = 2.4461, Ti–O = 2.0085(5), Si–O = 1.7022(5) Å, and site occupancy factors (sofs) for Ca(sof) = 0.963(1), Ti(sof) = 1.045(1), and Si(sof) = 1.150(2). Comparison of schorlomite data from the type locality in Magnet Cove with morimotoite from Ice River, Canada and the type locality in Japan show that they are quite similar and cast doubts as to morimotoite being different from schorlomite.

The Debye temperature of wurtzite aluminum nitride (AlN) was determined by the Rietveld refinement method based on the room-temperature X-ray powder diffraction data. The refined lattice parameters are a = 3.11139(1) Å, c = 4.978 43(3) Å; the refined positional parameter for N is z = 0.384 59(33) Å; and the refined temperature factors of Al and N were 0.442(12) Å2 and 0.559(33) Å2, respectively. Using this refined temperature factor, the Debye temperature was evaluated as 971 K through the Debye approximation.

Ag–reduced graphene oxide (Ag/rGO) nanoparticle composites were synthesized through a facile one-step hydrothermal reaction using GO and silver carbonate (Ag2CO3) as raw materials. The homogeneous silver nanospheres with an average size of 50 nm well dispersed on the surface of rGO were obtained without other additives. During the formation process, GO both promotes the dispersion of Ag2CO3 in aqueous solution and acts as the substrate of silver cations, and the hydrolysis of Ag2CO3 provides silver cations and alkaline condition. Moreover, GO further serves as reducing agent to generate elemental silver in the alkaline condition. The as-prepared materials exhibit excellent surface-enhanced Raman scattering activities when used to detect the Raman signals of R6G absorbed on the Ag/rGO substrate.

4-hydroxy-3-methoxyphenyl-4-hydroxycoumarin chalcone (C19H14O6) was synthesized by the Claisen–Schmidt reaction with the condensation of 3-acetyl-4-hydroxycoumarin with 4-hydroxy-3-methoxybenzaldehyde (vanillin). The new compound was characterized by Fourier transform infrared microscopy, UV–vis 1H, and 13C NMR spectroscopy and its crystal structure was ab initio determined from laboratory X-ray powder diffraction data. The crystal structure is monoclinic with unit-cell parameters a = 14.3181(4), b = 8.040 71(9), c = 13.5524(3), β = 100.3559(13)°, V = 1534.84(6) Å3, and space group P21/c.

The crystal structure of the novel metal organic framework (MOF) Zn(C3H5NO2S)2 is described. This MOF can serve as a model for active sites in metalloproteins, on diverse activities such as structural or catalytic functions. Each half of the amino acid act as a bidentate ligand to one Zn and as a monodentate ligand to another Zn, while the disulphide bond presents an important structural function, stabilizing the crystal packing. The structure has been obtained ab initio from synchrotron X-ray powder diffraction data. The compound crystallizes in the orthorhombic system (space group P212121), with a = 20.0906(7), b = 9.5842(3), c = 5.018 89(13), and V = 966.40(5) Å3, with Z = 4. The structure was determined using a direct space approach, by means of the Monte Carlo technique, followed by Rietveld refinement.

The X-ray diffraction powder patterns were prepared and the crystal structures were refined for the double-perovskite series of compounds, Sr2RSbO6 (R = Pr, Nd, Sm, Eu, Gd, Dy, Ho, Y, Er, Tm, Yb, and Lu). We found the structures of the entire Sr2RSbO6 series to be monoclinic with space group P21/n (no. 14), and Z = 2. From R = Lu to Pr, the lattice parameters “a” range from 5.7779(2) to 5.879 05(8) Å, “b” range from 5.7888(2) to 5.969 52(9) Å, “c” range from 8.1767(3) to 8.369 20(12) Å, “β” range from 90.112(2)° to 90.313(1)°, and “V” range from 273.483(4) to 293.714(7) Å3. These lattice parameters follow the well-established trend of “lanthanide contraction”. The R 3+ and Sb5+ ions are found to be fully ordered in the double-perovskite arrangement of alternating corner-sharing octahedra in a zigzag fashion. The SrO12, RO6, and SbO6 cages are all found to have distorted coordination environments. Powder diffraction patterns of these compounds have been prepared, submitted, and published in the Powder Diffraction File.

A new trimetallic compound with formula (NH4)Ni2.4Co0.6O(OH)(MoO4)2•1.5H2O was obtained by hydrothermal synthesis. The solid was characterized by X-ray diffraction, thermal analysis (thermogravimetric analysis and differential thermal analysis), Fourier-transformed infrared spectroscopy, Laser Raman spectroscopy, and chemical analysis by atomic absorption, confirming the formation of the layered phase ϕ y . Crystallographic studies showed that the compound obtained is trigonal with hexagonal unit-cell parameters, a = 6.0468 ± 0.0016 Å and c = 21.8433 ± 0.0001 Å, and space group R-3m.

X-ray powder diffraction data, unit-cell parameters, and space group for a sodium azobarbituric acid dihydrate are presented [a = 3.546 (1) Å, b = 9.210 (2) Å, c = 9.738 (4) Å, α = 104.07 (4)°, β = 98.09 (6)°, γ = 98.80 (2)°, unit-cell volume V = 299.6 Å3, Z = 1, and space group P − 1]. All the measured lines were indexed. No detectable impurities were observed.

The Ba2.64Ta11.25O30.81was prepared by conventional solid-state reaction technique as a single phase. It was found that the compound crystallizes in the tetragonal system, space group P4/mbm (No. 127) and unit-cell parameters are a = 12.508 59(8) Å, c = 3.912 81(2) Å, V = 612.218(7) Å3, and Z = 1. The crystal structure of the Ba2.64Ta11.25O30.81 phase is found to be closely related to the tetragonal tungsten bronze structure type, comprising interstitial (TaO)+ inclusions. Reference data were derived from the Rietveld analysis and reported here.

X-ray powder diffraction data, unit-cell parameters and space group for a new bis(β-diiminato) Cu(II) complex, C48H62CuN4O4 are reported [a = 13.330 (3) Å, b = 11.137(2) Å, c = 8.832(2) Å, α = 78.88(2), β = 94.73(2), γ = 114.55(2), unit-cell volume V = 1170.26 Å3, Z = 1, and space group P − 1]. All measured lines were indexed and are consistent with the P−1 space group. No detectable impurity was observed.

A new quaternary compound PrAlFeNi3 was synthesized and studied by means of X-ray powder diffraction technique. The powder pattern of PrAlFeNi3 was indexed and refined, giving a hexagonal structure, space group P6/mmm (No. 191) with the CaCu5 structure type, a = 5.1132(2) Å, c = 4.0737(1) Å, V = 92.19 Å3, Z = 1, ρx = 7.20 g cm−3, F30 = 173.61 (0.0054, 32) and RIR = 0.77.

Diffraction data of calcite were collected using a conventional Bragg–Brentano diffractometer, which is a convenient, low-cost, and highly popular in-house instrument, and its crystal structure was refined by the Rietveld method. This paper shows how one treats preferred orientation and how different refinement strategies affect the accuracy of the result.

The 18th International Symposium on the Reactivity of Solids (June 9–13, 2014 in Saint-Petersburg, Russia) brought together 137 researches from 18 countries, from crystallographers to electrochemists, to discuss the new materials design, advanced methods of preparation and characterization, mechanisms of reactions involving solids, structure–property relations, and new horizons of the materials application. What emerged from the meeting was an understanding that even if up-to-date solid state chemistry cannot be limited to organic, inorganic, or physical one, different groups of researches can understand each other and find a way for collaboration. More than half of the talks were devoted to energy production and storage problems, where the researcher should take into account not only just the chemistry of solid material, but also its crystalline structure, surface morphology, and even the bath liquid phase and interface properties. It means that only the interdisciplinary partnership can lead to outstanding results.