The title compound, 3-hydroxypropionitrile, was crystallized repeatedly in situ inside a quartz capillary using a liquid nitrogen cryostream. The X-ray powder diffraction patterns obtained indicated the presence of two distinct crystalline phases. The cleanest datasets for each of the phases were used to solve the crystal structures via simulated annealing, followed by refinement and optimization via dispersion-corrected density functional theory (DFT) calculations, with a final Rietveld refinement against the experimental data. The two structures appear to correspond to those proposed in a 1960s literature vibrational spectroscopy paper, one being the more stable with a gauche molecular conformation and the second metastable phase more complex with mixed conformations. Dispersion-corrected DFT computation using lattice parameters for both phases obtained from a single 84 K dataset with co-existing phases shows the stable and metastable phases to differ in energy by less than 0.5 kJ mol−1. A comparison of experimental far infrared spectra published in the 1960s with those calculated from the proposed crystal structures provides some independent supporting evidence for the proposed structures.

Materials in a high radioactive environment undergo structural changes. X-ray diffraction (XRD) is commonly used to study the micro-structural changes of such materials. Therefore, a safe procedure is required for the preparation of specimens. In this paper, a simple methodology for the preparation of radioactive powder specimens to be analyzed in a non-nuclearized laboratory diffractometer is presented. The process is carried out inside a shielded glove box, where the milling of the radioactive sample and specimen preparation occurs. Minimum amount of sample is required (<20 mg), which is drop-casted on a polyether ether ketone (PEEK) foil and glue-sealed inside a disposable plastic holder for a safe handling of the specimen. One example using neutron-irradiated granite is shown, where unit-cell parameters and crystal density of the main phases were calculated. The developed methodology represents an easy and affordable way to study neutron irradiated materials with low activity at laboratory scale.

X-ray diffraction (XRD) characterization of Si powder was carried out using synchrotron and laboratory sources. Microstructural (size-strain) analyses of XRD patterns were carried out using the Rietveld refinement method. Experimentally observed super-Lorentzian shapes of the XRD peaks of Si powder were examined using multimodal profile fitting and bimodal model was found to be adequate. The two components obtained using a bimodal approach are referred as narrow and broad profiles based on their estimated relative peak widths. Peak shapes of crystallite size-dependent parts of narrow and broad profiles were found to be almost Gaussian and Lorentzian in nature, respectively. The simultaneous presence of such peak shapes corresponding to a bimodal microstructure is uncommon in literature. Therefore, in order to explore the role of different natures of XRD peak shapes (size dependent) of the bimodal profiles of Si, detailed microstructural analysis was carried out using the complementary method of whole powder pattern modeling (WPPM) and found to be related to the variance of crystallites' size distribution. Additionally, the effect of instrument resolution (laboratory and synchrotron sources) on the microstructural parameters was also studied. Scanning and transmission electron microscopy were used to characterize the morphology of Si powder and correlate with the microstructural findings of XRD methods.

Crystal structures, microtopography, morphologies, elemental compositions, and ionic conductivity have been investigated for Li5-xLa3(Nb,Ta)O12-y using X-ray diffraction (XRD), field-emission analytical scanning and transmission electron microscopies (S/TEM), and electrochemical impedance spectroscopy. Using Rietveld refinements with powder XRD patterns, we determined that the number of Li atoms in the formula is less than 5 and that Li5-xLa3(NbTa)O12-y crystallizes in the cubic garnet structure with a space group Ia-3d. Sintering at varying temperatures (750–1000 °C) for 5 h in an ambient atmosphere produced distinct outcomes. Rietveld refinements disclosed that the sample sintered at 1000 °C (Li3.43(2)La3Nb1.07(2)Ta0.93(2)O12-y, a = 12.8361(7) Å, V = 2114.96(3) Å3) exhibited the highest ionic conductivity, while the 850 °C sample had the lowest conductivity, characterized by lower Li concentration and impurity phases (Li(Nb,Ta)3O88, Li2CO3). Analyses, including XRD and electron microscopy, confirmed the 1000 °C sample as a relatively phase pure with enhanced Li content (Li/La = 1.2), larger grains (15 μm), and uniform crystallinity. The 1000 °C sample introduced additional partially filled Li3 (96h) sites, promoting Li migration, and enhancing ionic conductivity. The resulting XRD pattern at 1000 °C has been submitted to the Powder Diffraction File as a reference.

Surface roughness is a critical factor affecting the performance of dental implants. One approach to influence this is through sandblasted, large grit, acid-etched (SLA) modification on pure titanium implant surfaces. In this study, SLA was performed on grade IV pure titanium. Sandblasting was conducted at distances of 2, 4, and 6 cm. Subsequently, the samples were etched with a mixed acid solution of HCl, H2SO4, and H2O for 0, 30, and 60 min. Surface roughness and X-ray diffraction (XRD) characterizations were conducted on the samples. The results revealed that surface roughness increased but was not too significant as the sandblasting distance decreased. Longer etching durations for sandblasted with acid-etched samples led to reduced surface roughness (Sa and Sz). It was found that a 60 min-etched sample resulted in optimal Sa, Sz, and Ssk values, i.e., 1.19 μm, 13.76 μm, and −0.60, respectively. The XRD texture was significantly influenced by sandblasting, with compressive residual stress increasing as the sandblasting distance decreased. Normal stress causes hill formations at shorter sandblasting distances. For etched samples, the residual stress decreased with longer etching durations. Normal stress-decreasing trend aligns with the initial reduction in hill and valley within the samples and subsequent hill enhancement at extended etching duration.

The crystal structure of anhydrous Al-MFI (NH4) containing adsorbed Ar has been determined and refined using synchrotron X-ray powder diffraction data taken at 90 K, and optimized using density functional theory techniques. Six highly occupied Ar sites almost completely fill the pore volume of the zeolite. Changing the gas flow from Ar to He at 90 K decreases the Ar occupancies of all six sites, but two decrease more than the others. Warming the sample from 90 to 295 K in Ar flow results in further decreases in site occupancies, but five of the original six sites persist.

For more than 80 years, the scientific community has extensively used International Centre for Diffraction Data's (ICDD®) Powder Diffraction File (PDF®) for material characterization, including powder X-ray diffraction analysis. Historically, PDF was made available for two major material types: one for inorganic analysis and the other for organic analysis. In the early years of the PDF, this two-material approach was implemented due to limited computer capabilities. With Release 2024, ICDD provides a comprehensive database consisting of the entire PDF in one database called PDF-5+, comprised of more than one million entries (1,061,898). The PDF-5+ with a relational database (RDB) construct houses extensive chemical, physical, bibliographic, and crystallographic data, including atomic coordinates and raw data, enabling qualitative and quantitative phase analysis. This wealth of information in one database is advantageous for phase identification, materials characterization, and several data mining applications in materials science. A database of this size needs rigorous data curation and structural and chemical classifications to optimize pattern search/match and characterization methods. Each entry in the PDF has an editorially assigned quality mark. An editorial comment will describe the reason if an entry does not meet the top-quality mark. The editorial processes of ICDD's quality management system are unique in that they are ISO 9001:2015 certified. Among several classifications implemented in PDF-5+, subfiles (such as Bioactive, Pharmaceuticals, Minerals, etc.) directly impact the search/match in minimizing false positives. Scientists with specific field expertise continuously review these subfiles to maintain their quality. This paper describes the features of PDF with an emphasis on the newly released PDF-5+.

The values of the signal-to-noise ratio are determined, at which the method of processing X-ray diffraction data reveals reflections with intensity less than the noise component of the background. The possibilities of the method are demonstrated on weak reflections of α-quartz. The method of processing X-ray diffraction data makes it possible to increase the possibilities of X-ray phase analysis in determining the qualitative phase composition of multiphase materials with a small (down to 0.1 wt.%) content of several (up to eight) phases.

Physical vapor deposited (PVD) molybdenum disulfide (nominal composition MoS2) is employed as a thin film solid lubricant for extreme environments where liquid lubricants are not viable. The tribological properties of MoS2 are highly dependent on morphological attributes such as film thickness, orientation, crystallinity, film density, and stoichiometry. These structural characteristics are controlled by tuning the PVD process parameters, yet undesirable alterations in the structure often occur due to process variations between deposition runs. Nondestructive film diagnostics can enable improved yield and serve as a means of tuning a deposition process, thus enabling quality control and materials exploration. Grazing incidence X-ray diffraction (GIXRD) for MoS2 film characterization provides valuable information about film density and grain orientation (texture). However, the determination of film stoichiometry can only be indirectly inferred via GIXRD. The combination of density and microstructure via GIXRD with chemical composition via grazing incidence X-ray fluorescence (GIXRF) enables the isolation and decoupling of film density, composition, and microstructure and their ultimate impact on film layer thickness, thereby improving coating thickness predictions via X-ray fluorescence. We have augmented an existing GIXRD instrument with an additional X-ray detector for the simultaneous measurement of energy-dispersive X-ray fluorescence spectra during the GIXRD analysis. This combined GIXRD/GIXRF analysis has proven synergetic for correlating chemical composition to the structural aspects of MoS2 films provided by GIXRD. We present the usefulness of the combined diagnostic technique via exemplar MoS2 film samples and provide a discussion regarding data extraction techniques of grazing angle series measurements.

Six different types of Majiang bronze drums from Hechi City, Guangxi, China were collected from the Guangxi Museum to characterize the original scheme of polychromy and materials used for the drums. The composition of all the samples were determined by using scanning electron microscopy with energy-dispersive X-ray spectroscopy. All the bronze drums contain mainly Cu, Sn, Pb, and As. Qualitative analysis of the structure by X-ray powder diffraction indicates that each of the six bronze drums contains four or five phases, namely (Cu, As), Pb, Cu3Sn, and Cu10Sn3 or Cu, Pb, As0.2Cu1.8, Cu3Sn, and Cu10Sn3. The Rietveld structural refinement is performed first time for the quantitative analysis of ancient bronze drums and inorganic cultural relics. This paper reports the result.

The structure of Ni(3-amino-4,4′-bipyridine)[Ni(CN)4] (or known as Ni-BpyNH2) in powder form was determined using synchrotron X-ray diffraction and refined using the Rietveld refinement technique (R = 8.8%). The orthorhombic (Cmca) cell parameters were determined to be a = 14.7218(3) Å, b = 22.6615(3) Å, c = 12.3833(3) Å, V = 4131.29(9) Å3, and Z = 8. Ni-BpyNH2 forms a 3-D network, with a 2-D Ni(CN)4 net connecting to each other via the BpyNH2 ligands. There are two independent Ni sites on the net. The 2-D nets are connected to each other via the bonding of the pyridine “N” atom to Ni2. The Ni2 site is of six-fold coordination to N with relatively long Ni2–N distances (average of 2.118 Å) as compared to the four-fold coordinated Ni1–C distances (average of 1.850 Å). The Ni(CN)4 net is arranged in a wave-like fashion. The functional group, –NH2, is disordered and was found to be in the m-position relative to the N atom of the pyridine ring. Instead of having a unique position, N has ¼ site occupancy in each of the four m-positions. The powder reference diffraction pattern for Ni-BpyNH2 was prepared and submitted to the Powder Diffraction File (PDF) at the International Centre of Diffraction Data (ICDD).

The crystal structure of brimonidine hydrogen tartrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Brimonidine hydrogen tartrate crystallizes in space group P21 (#4) with a = 7.56032(2), b = 7.35278(2), c = 30.10149(9) Å, β = 90.1992(2)°, V = 1673.312(10) Å3, and Z = 4 at 295 K. The crystal structure consists of alternating layers of cations and anions parallel to the ab-plane. Each of the hydrogen tartrate anions is linked to itself by very strong charge-assisted O–H⋯O hydrogen bonds into chains along the a-axis. Each hydroxyl group of each tartrate acts as a donor in an O–H⋯O or O–H⋯N hydrogen bond. One of these is intramolecular, but the other three are intermolecular. These hydrogen bonds link the hydrogen tartrate anions into layers parallel to the ab-plane and also link the anion–cation layers. The protonated N atoms act as donors in N–H⋯O or N–H⋯N hydrogen bonds to the carboxyl groups of the tartrates and to a ring nitrogen atom. These link the cations and anions, as well as providing cation–cation links. The amino N atoms of the cations form N–H⋯O hydrogen bonds to hydroxyl groups of the anions. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)

Shark vertebrae and their centra (vertebral bodies) are high-performance structures able to survive millions of cycles of high amplitude strain despite lacking a repair mechanism for accumulating damage. Shark centra consist of mineralized cartilage, a biocomposite of bioapatite (bAp), and collagen, and the nanocrystalline bAp's contribution to functionality remains largely uninvestigated. Using the multiple detector energy-dispersive diffraction (EDD) system at 6-BM-B, the Advanced Photon Source, and 3D tomographic sampling, the 3D functionality of entire centra were probed. Immersion in ethanol vs phosphate-buffered saline produces only small changes in bAp d-spacing within a great hammerhead centrum. EDD mapping under in situ loading was performed an entire blue shark centrum, and 3D maps of bAp strain showed the two structural zones of the centrum, the corpus calcareum and intermedialia, contained opposite-signed strains approaching 0.5%, and application of ~8% nominal strain did not alter these strain magnitudes and their spatial distribution.

The crystal structure of anthraquinone-2-carboxylic acid has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Anthraquinone-2-carboxylic acid crystallizes in space group P-1 (#2) with a = 3.7942(2), b = 13.266(5), c = 22.835(15) Å, α = 73.355(30), β = 89.486(6), γ = 86.061(1)°, V = 1098.50(7) Å3, and Z = 4. The crystal structure contains two independent molecules of anthraquinone-2-carboxylic acid. Although the expected hydrogen-bonded dimers are present, the dimers are not centrosymmetric. The dimer contains one molecule of each planar low-energy conformation. The crystal structure consists of a herringbone array of centrosymmetric pairs of molecules parallel to the bc-plane. The molecules stack along the short a-axis. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

A monoclinic C form of rilpivirine hydrochloride, (N6H19C22)Cl, has been obtained and characterized using solid-state 15N, 13C, and 35Cl NMR spectroscopy and multitemperature synchrotron X-ray powder diffraction. The title compound crystallizes in the monoclinic system (space group C2/c, #15) at both room (295.0(2) K) and low (100.0(2) K) temperatures. At room temperature, the following parameters are a = 19.43051(3), b = 13.09431(14), c = 17.10254(18) Å, β = 109.3937(7), V = 4104.48(9) Å3, and Z = 8. The folded molecular conformation of the cation is similar with that of free base rilpivirine with the exception of cyanovinyl group disposition. The anion links cations to infinite chains parallel to the crystallographic c axis using N–H⋯Cl bonds where both amino groups and the protonated pyrimidine ring take part in the H-bonding. The powder patterns have been submitted to the ICDD for inclusion in the Powder Diffraction File™ (PDF®).

Equations are given which allow an analyst to obtain a correct absolute quantitative phase analysis via the internal standard method when a reference material with a known crystallinity of less than 100% is used. Comparisons are made with previous equations, and a numerical example is given.

The crystal structure of nintedanib esylate hemihydrate was refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Nintedanib esylate hemihydrate crystallizes in space group P-1 (#2) with a = 11.5137(1), b = 16.3208(4), c = 19.1780(5) Å, α = 69.0259(12), β = 84.4955(8), γ = 89.8319(6)°, V = 3347.57(3) Å3, and Z = 4 at 295 K. Hydrogen bonds are prominent in the crystal structure. The water molecule forms two medium-strength O–H⋯O hydrogen bonds to one of the esylate anions. The protonated nitrogen atom in each cation forms a N–H⋯O hydrogen bond to an esylate anion. The ring N–H groups form strong intramolecular N–H⋯O hydrogen bonds to carbonyl groups. The ring N–H groups form intramolecular N–H⋯O hydrogen bonds to esylate anions. Many C–H⋅⋅⋅O hydrogen bonds (and one C–H⋯N hydrogen bond), with aromatic C–H, methylene groups and methyl groups as donors, are present. The hydrogen bonding patterns of the two cations differ considerably. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)

The crystal structure of ribociclib hydrogen succinate (commonly referred to as ribociclib succinate) has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Ribociclib hydrogen succinate crystallizes in space group P-1 (#2) with a = 6.52215(4), b = 12.67120(16), c = 18.16978(33) Å, α = 74.0855(8), β = 82.0814(4), γ = 88.6943(1)°, V = 1430.112(6) Å3, and Z = 2 at 295 K. The crystal structure consists of alternating layers of cations and anions parallel to the ab-plane. The protonated N in each ribociclib cation acts as a donor in two strong N–H⋯O hydrogen bonds to two different succinate anions. Strong O–H⋯O hydrogen bonds link the hydrogen succinate anions into chains parallel to the a-axis. N–H⋯N hydrogen bonds link the cations into dimers, with a graph set R2,2(8). The result is a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)

The crystal structure of indacaterol hydrogen maleate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Indacaterol hydrogen maleate crystallizes in space group P-1 (#24) with a = 8.86616(9), b = 9.75866(21), c = 16.67848(36) Å, α = 102.6301(10), β = 94.1736(6), γ = 113.2644(2)°, V = 1273.095(7) Å3, and Z = 2 at 295 K. The crystal structure consists of layers of cations and anions parallel to the ab-plane. Traditional N–H⋯O and O–H⋯O hydrogen bonds link the cations and anions into chains along the a-axis. There is a strong intramolecular charge-assisted O–H⋯O hydrogen bond in the non-planar hydrogen maleate anion. There are also two C–H⋯O hydrogen bonds between the anion and cation. The cation makes a strong N–H⋯O hydrogen bond to the anion, but also acts as a hydrogen bond donor to an aromatic C in another cation. The amino group makes bifurcated N–H⋯O hydrogen bonds, one intramolecular and the other intermolecular. The hydroxyl group acts as a donor to another cation. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).