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®)

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 crystal structure of nicarbazin has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Nicarbazin is a co-crystal of 4,4′-dinitrocarbanilide (DNC) and 2-hydroxy-4,6-dimethylpyrimidine (HDP) molecules. Nicarbazin crystallizes in space group P-1 (#2) with a = 6.90659(8), b = 12.0794(4), c = 13.5040(7) Å, α = 115.5709(11), β = 102.3658(6), γ = 91.9270(4)°, V = 982.466(5) Å3, and Z = 2. The DNC and HDP molecules are linked by two strong N–H⋯O and N–H⋯N hydrogen bonds, and the HDP molecules are linked into centrosymmetric dimers by another N–H⋯O hydrogen bond. These strong hydrogen bonds link the molecules into layers parallel to the ab-plane and parallel stacking of both DNC and HDP molecules is prominent in the structure. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

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.

A model for the crystal structure of carbadox has been generated and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Carbadox crystallizes in space group P21 (#4) with a = 13.8155(3), b = 21.4662(1), c = 16.3297(3) Å, β = 110.0931(7)°, V = 4548.10(3) Å3, and Z = 16. The crystal structure is characterized by approximately parallel stacking of the eight independent carbadox molecules parallel to the bc-plane. There are two different molecular configurations of the eight carbadox molecules; five are in the lower-energy configuration and three are in a ~10% higher-energy configuration. This arrangement likely achieves the lowest-energy crystalline packing via hydrogen bonding. Hydrogen bonds link the molecules both within and between the planes. Each of the amino groups forms a N–H⋯O hydrogen bond to an oxygen atom of the 1,4-dioxidoquinoxaline ring system of another molecule. The result is four pairs of hydrogen-bonded molecules, which form rings with graph set R2,2(14). Variation in specimen preparation can affect the preferred orientation of particles considerably. 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®).

The crystal structure of ractopamine hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Ractopamine hydrochloride crystallizes in space group Pbca (#61) with a = 38.5871(49), b = 10.7691(3), c = 8.4003(2) Å, V = 3490.75(41) Å3, and Z = 8. The ractopamine cation contains two chiral centers, and the sample consists of a mixture of the S,S/R,R/S,R and R,S forms. Models for the two diastereomers S,S and S,R were refined, and yielded equivalent residuals, but the S,R form is significantly lower in energy. The crystal structure consists of layers of molecules parallel to the bc-plane. In each structure one of the H atoms on the protonated N atom acts as a donor in a strong discrete N–H⋯Cl hydrogen bond. Hydroxyl groups act as donors in O–H⋯Cl and O–H⋯O hydrogen bonds. Both the classical and C–H⋯Cl and C–H⋯O hydrogen bonds differ between the forms, helping to explain the large microstrain observed for the sample. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

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®).

The crystal structure of L-5-methyltetrahydrofolate calcium trihydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Calcium levomefolate trihydrate crystallizes in space group P212121 (#19) with a = 7.1706(6), b = 6.5371(5), c = 53.8357(41) Å, V = 2523.58(26) Å3, and Z = 4. The structure is characterized by alternating hydrophobic and hydrophilic layers along the c-axis. The Ca cations are 7-coordinate, and share edges to form chains along the b-axis. Each of the water molecules acts as a donor in two hydrogen bonds. The coordinated water molecule makes two strong intermolecular O–H⋯O hydrogen bonds to carboxyl and carbonyl groups. The two zeolitic water molecules form weaker hydrogen bonds, to carbonyl O atoms, ring N atoms, and aromatic C atoms. Several N–H⋯O/N hydrogen bonds, as well as C–H⋯O hydrogen bonds, also contribute to the lattice energy.

The crystal structure of danofloxacin mesylate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Danofloxacin mesylate crystallizes in space group P1 (#1) with a = 6.77474(8), b = 12.4973(4), c = 12.82826(28) Å, α = 84.8709(29), β = 87.7501(10), γ = 74.9916(4)°, V = 1044.723(11) Å3, and Z = 2. The protonation of the danofloxacin cations was established by the analysis of potential intermolecular interactions and differs from that expected from isolated-cation calculations. The crystal structure consists of alternating layers of cations and anions parallel to the ac-plane. There is parallel stacking of the oxoquinoline rings along the a-axis. The expected N–H⋯O hydrogen bonds between the cations and anions are not present. Each cation makes an N–H⋯O hydrogen bond with the other cation, resulting in zig-zag chains along the a-axis. Both cations have strong intramolecular O–H⋯O hydrogen bonds. There are several C–H⋯O hydrogen bonds between the danofloxacin cations and mesylate anions. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of meglumine diatrizoate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Meglumine diatrizoate crystallizes in space group P21 (#4) with a = 10.74697(4), b = 6.49364(2), c = 18.52774(7) Å, β = 90.2263(3), V = 1292.985(5) Å3, and Z = 2. Two different crystal structures, which yielded essentially identical refinement residuals and positions of the non-H atoms, were obtained. The differences were in the H atom positions and the hydrogen bonding. One structure was 123.0 kJ/mol/cell lower in energy than the other and was adopted for the final description. The crystal structure consists of alternating double layers of cations and anions along the c-axis. The hydrogen bonds link the cations and anions into a three-dimensional framework. Each of the hydrogen atoms on the ammonium nitrogen of the cation acts as a donor in a strong N–H⋯O hydrogen bond. One of these is to a hydroxyl group of another cation, and the other is to the carboxylate group of the anion. Each of the amide nitrogen atoms of the anion forms a strong N–H⋯O intermolecular hydrogen bond, one to a carbonyl and the other to a carboxylate group. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

Pb–Zr–Ti–O (PZT) perovskites span a large solid-solution range and have found widespread use due to their piezoelectric and ferroelectric properties that also span a large range. Crystal structure analysis via Rietveld refinement facilitates materials analysis via the extraction of the structural parameters. These parameters, often obtained as a function of an additional dimension (e.g., pressure), can help to diagnose materials response within a use environment. Often referred to as “in-situ” studies, these experiments provide an abundance of data. Viewing structural changes due to applied pressure conditions can give much-needed insight into materials performance. However, challenges exist for viewing/presenting results when the details are inherently three-dimensional (3D) in nature. For PZT perovskites, the use of polyhedra (e.g., Zr/Ti–O6 octahedra) to view bonding/connectivity is beneficial; however, the visualization of the octahedra behavior with pressure dependence is less easily demonstrated due to the complexity of the added pressure dimension. We present a more intuitive visualization by projecting structural data into virtual reality (VR). We employ previously published structural data for Pb0.99(Zr0.95Ti0.05)0.98Nb0.02O3 as an exemplar for VR visualization of the PZT R3c crystal structure between ambient and 0.62 GPa pressure. This is accomplished via our in-house CAD2VR™ software platform and the new CrystalVR plugin. The use of the VR environment enables a more intuitive viewing experience, while enabling on-the-fly evaluation of crystal data, to form a detailed and comprehensive understanding of in-situ datasets. Discussion of methodology and tools for viewing are given, along with how recording results in video form can enable the viewing experience.

X-ray powder diffraction data, including unit cell parameters and space group assignment, for the ESP15228 species of C19H34O5 formula, are here reported [a = 6.0434(6), b = 12.2543(6), c = 14.0285(8) Å, α = 86.584(3), β = 85.707(10), γ = 78.801(5)°, V = 1015.2(1) Å3, Z = 2, ρcalc = 1.152 g cm−3, and space group P-1]. All measured lines were indexed and no detectable impurities were observed.

The crystal structure of butenafine hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Butenafine hydrochloride crystallizes in space group P21 (#4) with a = 13.94807(5), b = 9.10722(2), c = 16.46676(6) Å, β = 93.9663(5)°, V = 2086.733(8) Å3, and Z = 4. Butenafine hydrochloride occurs as a racemic co-crystal of R and S enantiomers of the cation. The crystal structure is characterized by parallel stacks of aromatic rings along the b-axis. Each cation forms a strong discrete N–H⋯Cl hydrogen bond. The chloride anions also act as acceptors in several C–H⋯Cl hydrogen bonds from methylene, methyl, and aromatic groups. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of encorafenib, C22H27ClFN7O4S, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Encorafenib crystallizes in space group P21 (#4) with a = 16.17355(25), b = 9.52334(11), c = 17.12368(19) Å, β = 89.9928(22)°, V = 2637.50(4) Å3, and Z = 4. The crystal structure consists of alternating layers of stacked halogenated phenyl rings and the other parts of the molecules perpendicular to the a-axis. One molecule participates in two strong N–H⋯N hydrogen bonds (one intra- and the other intermolecular), which are not present for the other molecule. The intermolecular hydrogen bonds link molecule 2 into a spiral chain along the b-axis. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

X-ray diffraction in the Bragg-Brentano configuration (“XRD”) is a very established method. However, experimental evidence concerning its significant information depth, i.e. microstructure components from which maximum depth can affect the information evaluated from the acquired diffraction pattern, are scarce in the scientific literature. This depth is relevant to all XRD measurements performed on compact samples, especially layered composites and samples showing a crystallographic texture evolution. This article provides experimentally determined upper and lower limits to the significant information depth: XRD patterns acquired from a compact crystal layer through a layer of compact, amorphous glass indicate that the significant information depth of XRD using Cu Kα1 and Kα2 radiation is very likely larger than 48 μm, but smaller than 118 μm, in a material of the composition Mg2Al4Si5O18 with a density of ca. ~2.6 g/cm3. The depth of 48 μm correlates to the depth larger than the layer of material from which 90% of the reflected X-rays originate at 2Θ = 25.8°.

The crystal structure of oxfendazole has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Oxfendazole crystallizes in space group P21/c (#14) with a = 18.87326(26), b = 10.40333(5), c = 7.25089(5) Å, β = 91.4688(10)° V = 1423.206(10) Å3, and Z = 4. The crystal structure consists of stacks of the planar portions of the L-shaped molecules, resulting in layers parallel to the bc-plane. Only weak hydrogen bonds are present. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of besifloxacin hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Besifloxacin hydrochloride crystallizes in space group P1 (#1) with a = 5.36596(8), b = 10.3234(4), c = 17.9673(14) Å, α = 98.122(5), β = 92.9395(9), γ = 96.1135(3)°, V = 977.483(13) Å3, and Z = 2. The crystal structure is approximately centrosymmetric. Strong N–H⋯Cl hydrogen bonds form a corrugated ladder-like chain along the a-axis. The carboxylic acid group in each independent cation acts as the donor in a strong intramolecular O–H⋯O hydrogen bond to an adjacent carbonyl group. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of elvitegravir Form II has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Elvitegravir Form II crystallizes in space group P21 (#4) with a = 11.54842(7), b = 14.04367(5), c = 13.33333(8) Å, β = 90.0330(6)°, V = 2162.427(14) Å3, and Z = 4. The crystal structure consists of alternating layers of parallel molecules perpendicular to the b-axis. The mean planes of the oxoquinoline ring systems in molecules 1 and 2 are 1(22)-1 and -1(22)1. Between the stacks are layers of the halogenated phenyl rings. These exhibit herringbone stacking. In each molecule, the carboxylic acid group forms a strong intramolecular O–H⋯O hydrogen bond to the nearby carbonyl group. The hydroxyl group of each molecule forms a strong hydrogen bond to the carbonyl group of the carboxylic acid of the other molecule. These O–H⋯O hydrogen bonds link the molecules into dimers, with a graph set R2,2(18) > a > c. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of toceranib has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Toceranib crystallizes in space group P21/c (#14) with a = 10.6899(6), b = 24.5134(4), c = 7.8747(4) Å, β = 107.7737(13)°, V = 1965.04(3) Å3, and Z = 4. The crystal structure consists of stacks of approximately planar molecules, with N–H⋯O hydrogen bonds between the layers. The commercial reagent sample was a mixture of two or more phases with toceranib being the dominant phase. The difference between the Rietveld-refined and DFT-optimized structures is larger than usual. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).