The crystal structure of cariprazine dihydrochloride has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Cariprazine dihydrochloride crystallizes in space group P21/n (#14) with a = 27.26430(14), b = 7.29241(1), c = 12.80879(4) Å, β = 99.5963(2)°, V = 2511.038(8) Å3, and Z = 4 at 295 K. The crystal structure consists of layers of cations parallel to the bc-plane. The cations stack along the b-axis. Each H atom on the two protonated N atoms participates in a discrete N–H⋯Cl hydrogen bond. One Cl anion acts as an acceptor in two of these bonds, while the other Cl is an acceptor in only one bond. The result is to link the cations and anions into columns parallel to the b-axis. The powder pattern has 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 benserazide hydrochloride Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Benserazide hydrochloride Form I crystallizes in space group P21/n (#14) with a = 19.22983(15), b = 14.45066(10), c = 4.57982(2) Å, β = 93.6935(3), V = 1270.014(15) Å3, and Z = 4 at 295 K. The crystal structure contains pairs of hydrogen-bonded benserazide cations, which are hydrogen bonded to chloride anions, resulting in chains along the c-axis. In addition, O–H⋯Cl, N–H⋯O, O–H⋯N, and O–H⋯O hydrogen bonds link the cations and anions into a three-dimensional framework. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

A proposed crystal structure of lifitegrast Form A has been derived using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Lifitegrast sesquihydrate Form A crystallizes in space group P21 (#4) with a = 18.2526(4), b = 5.15219(6), c = 30.1962(6) Å, β = 90.8670(19), V = 2839.35(7) Å3, and Z = 4 at 295 K. The crystal structure consists of discrete lifitegrast molecules linked by hydrogen bonds among carboxylic acid groups, carbonyl groups, and water molecules into a three-dimensional framework. The water molecules occur in clusters. Each water molecule acts as a donor in two O–H⋯O hydrogen bonds, and as an acceptor. One water molecule acts as an acceptor in a water–water O–H⋯O hydrogen bond, and all three water molecules are acceptors in C–H⋯O hydrogen bonds. Each carboxylic acid group acts as a donor in a strong discrete O–H⋯O hydrogen bond; one to a water molecule and the other to a carbonyl group. The amino groups both form N–H⋯O hydrogen bonds to carbonyl groups. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of decoquinate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Decoquinate crystallizes in space group P21/n (#14) with a = 46.8261(5), b = 12.94937(12), c = 7.65745(10) Å, β = 91.972(1), V = 4640.48(7) Å3, and Z = 8 at 295 K. The crystal structure consists of alternating layers of hydrocarbon chains and ring systems along the a-axis. Hydrogen bonds link the ring systems along the b-axis. The rings stack along the c-axis. The two independent decoquinate molecules have very different conformations, one of which is typical and the other has an unusual orientation of the decyl chain with respect to the hydroxyquinoline ring system, facilitating chain packing. The powder pattern has been submitted to the ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of gepirone has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Gepirone crystallizes in space group P21/a (#14) with a = 16.81794(14), b = 11.71959(5), c = 10.10195(4) Å, β = 95.7012(5)°, V = 1981.239(14) Å3, and Z = 4 at 298 K. The crystal structure consists of discrete gepirone molecules. There are no classical hydrogen bonds in the crystal structure, but several intra- and intermolecular C–H⋯N and C–H⋯O hydrogen bonds contribute to the lattice energy. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

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 previously unindexed laboratory X-ray powder diffraction data of mosapride dihydrogen citrate dihydrate, an API used to stimulate gastrointestinal motility, has been recorded at room temperature. Using these data, the crystal structure of this API has been refined in space group P21/c (No. 14) with a = 18.707(4) Å, b = 9.6187(1) Å, c = 18.2176(4) Å, β = 114.164(1)°, V = 2990.74(8) Å3, and Z = 4. The structure of this material corresponds to the phase associated with CSD Refcode LUWPOL determined at 93 K. The Rietveld refinement, carried out with TOPAS-Academic, proved the single nature of the sample and the quality of the data recorded.

The crystal structure of perfluorononanoic acid (PFNA) was solved via parallel tempering using synchrotron powder diffraction data obtained from the Brockhouse X-ray Diffraction and Scattering (BXDS) Wiggler Lower Energy (WLE) beamline at the Canadian Light Source. PFNA crystallizes in monoclinic space group P21/c (#14) with lattice parameters a = 26.172(1) Å, b = 5.6345(2) Å, c = 10.9501(4) Å, and β = 98.752(2)°. The crystal structure is composed of dimers, with pairs of PFNA molecules connected by hydrogen bonds via the carboxylic acid functional groups. The Rietveld-refined structure was compared to a density functional theory-optimized structure, and the root-mean-square Cartesian difference was larger than normally observed for correct powder structures. The powder data likely exhibited evidence of disorder which was not successfully modeled.

In this work, the synthesis, characterization, and X-ray powder diffraction data for dichloridodioxido-[(4,7-dimethyl)-1,10-phenanthroline]molybdenum(VI) are reported. The crystal structure of this compound was solved from powder diffraction data using the simulated annealing method with a subsequent refinement using the Rietveld method. The dioxo-molybdenum (VI) complex C14H12Cl2MoN2O2 crystallizes in a monoclinic system with space group C2/c (N° 15) with refined unit-cell parameters a = 12.9495 (5) Å, b = 9.7752 (4) Å,c = 12.0069 (6) Å, β = 101.702 (3) °, unit-cell volume V = 1488.27 (11) Å3, and values of Z′ = 0.5 and Z = 4. The molecules are organized into chains diagonally along the a and c axis. Parallel polyhedra are observed along these axes formed by the interactions of Mo, Cl, O, and N atoms present in the coordination sphere. The crystalline packing of this dioxo-molybdenum (VI) complex is dominated by five intermolecular hydrogen bonds, two intramolecular hydrogen bonds, and the four interactions between the centroids (CgI⋯CgJ) of the aromatic rings. An analysis of the Hirshfeld surface revealed that the greatest contributions of the attractive forces are given by H⋯Cl/Cl⋯H, H⋯C/C⋯H, H⋯O/O⋯H, and H⋯H interactions.

The crystal structure of acalabrutinib dihydrate Form III has been refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Acalabrutinib dihydrate Form III crystallizes in space group P21 (#4) with a = 8.38117(5), b = 21.16085(14), c = 14.12494(16) Å, β = 94.5343(6)°, V = 2497.256(20) Å3, and Z = 4 (Z′ = 2) at 295 K. The crystal structure consists of herringbone layers parallel to the ac-plane. Hydrogen bonds between the acalabrutinib and water molecules generate a three-dimensional framework. Each water molecule acts as a donor in two hydrogen bonds and as an acceptor in at least one hydrogen bond. Amino groups and pyridine N atoms link the acalabrutinib molecules into dimers. 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 alectinib hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Alectinib hydrochloride crystallizes in space group P21/n (#14) with the following parameters: a = 12.67477(7), b = 10.44076(5), c = 20.38501(12) Å, β = 93.1438(7)°, V = 2693.574(18) Å3, and Z = 4 at 295 K. The crystal structure consists of stacks of molecules along the b-axis, and the stacks contain chains of strong N–H⋯Cl hydrogen bonds. One density functional theory calculation moved a proton from an N atom to the Cl, but another calculation yielded a more chemically reasonable result. 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®).

Leucites are tetrahedrally coordinated silicate framework structures with some of the silicon framework cations that are partially replaced by divalent or trivalent cations. These structures have general formulae A2BSi5O12 and ACSi2O6, where A is a monovalent alkali metal cation, B is a divalent cation, and C is a trivalent cation. There are also leucite analogs with analogous tetrahedrally coordinated germanate framework structures. These have general formulae A2BGe5O12 and ACGe2O6. In this paper, the Rietveld refinements of three synthetic Ge-leucite analogs with stoichiometries of AAlGe2O6 (A = K, Rb, Cs) are discussed. KAlGe2O6 is I41/a tetragonal and is isostructural with KAlSi2O6. RbAlGe2O6 and CsAlGe2O6 are $I\bar{4}3d$ cubic and are isostructural with KBSi2O6.

The crystal structure of valbenazine has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Valbenazine crystallizes in space group P212121 (#19) with a = 5.260267(17), b = 17.77028(7), c = 26.16427(9) Å, V = 2445.742(11) Å3, and Z = 4 at 295 K. The crystal structure consists of discrete molecules and the mean plane of the molecules is approximately (8,−2,15). There are no obvious strong intermolecular interactions. There is only one weak classical hydrogen bond in the structure, from the amino group to the ether oxygen atom. Two intramolecular and one intermolecular C–H⋯O hydrogen bonds also contribute to the lattice energy. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)

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®)

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®)

Riet veld X-ray powder diffraction (XRD) analysis has been evaluated as a procedure for characterizing Al-substituted goethite according to the Rietveld scale factor, unit-cell parameters, and atom positional parameters. The study was conducted with three synthetic goethite samples for which the degree of Al substitution for Fe determined by chemical analysis was 8.0 ± 0.4, 12.0 ± 0.4, and 20.1 ± 0.4 mole %. The weight fractions of crystalline material (WFCM) in the specimens, determined from the Rietveld scale factors after correcting for adsorbed water and impurities, were 0.878 (esd = 0.014), 0.919 (0.014), and 0.965 (0.015), respectively. The Al mole % substitutions, inferred from the Rietveld cell parameters according to the method of Schulze (1984), were 10.4 ± 2.5, 16.5 ± 2.6, and 17.1 ± 2.6, respectively. The cause of the significant difference between the second value and the chemical analysis result is not known. The atom positional parameters did not differ significantly within the sample suite and agreed satisfactorily with literature values. The results have demonstrated the value of using Rietveld XRD analysis to determine simultaneously the WFCM and Al mole % substitutions, as well as to confirm the non-hydrogen atom positions.

The crystal structure of a deuterated synthetic boehmite powder, γ-AIOOD, has been determined by time-of-flight neutron diffraction and Rietveld profile refinement in space group Cmcm to a weighted profile R of 3.71%. Cell dimensions are a = 2.868(1), b = 12.2336(4), and C = 3.6923(1) Å. Alternate space groups for the boehmite structure suggested in the recent literature were found to be unacceptable. Atom positions, bond distances, and angles, with the exception of those involving hydrogen, were nearly identical to those determined by R. J. Hill in 1981 who studied a single crystal of boehmite by X-ray diffraction. All atoms were refined with anisotropic thermal parameters. The b value is 0.013 Å larger, and the thermal ellipsoids of oxygen are slightly more anisotropic than those reported by Hill and may reflect the different samples studied.