Laboratory X-ray powder diffraction was used to solve and refine the crystal structures of appended guest molecules within the pores of metal–organic frameworks (MOFs). Herein, we report the crystal structure of 1-propanethiol adsorbed in the pores of Co2(dobdc) (dobdc4– = 2,5-dioxido-1,4-benzenedicarboxylate, MOF-74). Soaking the activated MOF in neat 1-propanethiol resulted in the formation of 1-propanethiol–Co2(dobdc). The thiol appendant MOF maintained the crystal symmetry, with a rhombohedral space group R-3 and unit-cell parameters a = 25.9597(9) Å, c = 6.8623(5) Å, and V = 4005.0(4) Å3. As expected, the thiol sulfur formed a bond with the open cobalt metal site. The alkane chain was directed toward the center of the pore, participating in numerous van der Waals weak interactions with neighboring molecules. For the final Rietveld refinement, soft restrains were applied using bond distances obtained by periodic density functional theory (DFT) geometry optimization.

In this paper, grandite core with Grs64±1Adr36±1Sps2 composition was crystallographically studied. This core represents zone A of the macroscopically visible five A–E zones of the optically anisotropic Grs58–64Adr36–42Sps2 grandite. The applied procedure includes the detailed analysis of the powder diffraction patterns, and the Rietveld refinements of the crystal structures in a series of 18 space groups and two mixtures, which were followed by the comparative analysis of the R-values, site occupancy factors, and the bond lengths and angles. Synthesis of all of the presented results allows us to undoubtedly conclude that studied grandite is not cubic, neither as monophase nor as multiple phases in a mixture. Namely, it was established that structural dissymmetrization occurred and that it crystallized in the disordered rhombohedral $R\bar{3}c$ or orthorhombic Fddd space groups, whereby the first one is more probable. Beside the established lower symmetry of the studied grandite, which could be treated as the primary cause, the residual strain is also not excluded as the second possible cause for its slight optical anisotropy.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to evaluate specific aspects of instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 660c, the fourth generation of this powder diffraction SRM, which is used primarily for calibrating powder diffractometers with respect to line position and line shape for the determination of the instrument profile function (IPF). It is certified with respect to lattice parameter and consists of approximately 6 g of lanthanum hexaboride (LaB6) powder. So that this SRM would be applicable for the neutron diffraction community, the powder was prepared from an isotopically enriched 11B precursor material. The microstructure of the LaB6 powder was engineered specifically to yield a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the LaB6 powder. Both Type A, statistical, and Type B, systematic, uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.415 682 6 ± 0.000 008 nm (95% confidence).

Ba3−xSrxTb3−xCexO9 (x = 1 and 1.5) ceramics (BSTC) with a relative density of 93% and a grain size distribution of 0.2–3 µm were prepared by the mixed-oxides reaction route. The crystalline structures, microstructures, valence states, and electrical properties of two ceramics were analyzed using X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), electron paramagnetic resonance (EPR), and electrical measurements. Rietveld analyses of XRPD patterns show that BSTC1 is indexed as a trigonal structure with the space group R-3c, and BSTC3/2 is indexed as an orthorhombic perovskite structure with the space group Pmcn. The EPR, XPS, and electrical conductivity results confirm that Ce and Tb ions in BSTC exist as Ce4+ and mixed-valence states of Tb4+/Tb3+, respectively. At room temperature, the two BSTC ceramics exhibit a similar semiconducting behavior. The relationships between electrical conductivity and temperature/frequency are provided. The defect chemistry is discussed.

Single crystals of Sm0.55Sr0.45Mn0.4Fe0.6O3 were grown by an optical floating zone technique in an oxygen atmosphere. The powder X-ray diffraction pattern for the grown crystal revealed single-crystalline nature. The lattice parameters and atomic structure were refined and indexed using a General Structure Analysis System (GSAS) to an orthorhombic structure with lattice parameters a = 5.4415 (32) Å, b = 7.6994 (27) Å, c = 5.43868 (28) Å, and space group Pnma.

The crystal structure of bisoprolol fumarate Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Bisoprolol fumarate Form I crystallizes in space group P-1 (#2) with a = 8.165 70(5) Å, b = 8.516 39(12) Å, c = 16.751 79(18) Å, α = 89.142(1)°, β = 78.155(1)°, γ = 81.763(1)°, V = 1128.265(10) Å3, and Z = 2. The neutral side chain of the bisoprolol cation is probably disordered. The cation and anion are linked by N–H⋯O and O–H⋯O hydrogen bonds. The cations are also linked by N–H⋯O hydrogen bonds. The result is alternating layers of hydrophilic and hydrophobic layers parallel to the ab-plane. The density of the structure is relatively low at 1.130 g cm−3, but there are no obvious voids in the structure. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1625.

The new compound (4R)-methyl-3-(1-(4-chlorophenyl)-1H-1,2,3-triazole-4-carbonyl)thiazolidin-4-carboxylate was synthesized by the 1,3-dipolar cycloaddition reaction between (4R)-methyl-3-propionyl-thiazolidin-4-carboxylate (1) and 4-chlorophenylazide using the click chemistry approach. Molecular characterization was carried out by infrared spectroscopy and mass spectrometry. The X-ray powder diffraction study determined that the title compound crystallized in an orthorhombic system with unit-cell parameters a = 20.876 (2) Å, b = 12.111 (1) Å, and c = 6.288 (9) Å. The volume of the unit cell is V = 1589.7 (2) Å3. All measured diffraction maxima were indexed and are consistent with the P2221 space group (No. 17). No detectable impurities were observed.

The crystal structures of two forms of alclometasone dipropionate have been solved and refined using a single synchrotron X-ray powder diffraction pattern and optimized using density functional techniques. Both forms crystallize in the space group P212121 (#19) with Z = 4. The lattice parameters of Form 1 are a = 10.44805(7), b = 14.68762(8), c = 17.31713(9) Å, and V = 2657.44(2) Å3, and those of Form 2 are a = 10.69019(13), b = 14.66136(23), c = 17.17602(23) Å, and V = 2692.05(5) Å3. Both density functional theory and molecular mechanics optimizations indicate that Form 2 is lower in energy, but the differences are within the expected uncertainties of such calculations. In both forms, the only traditional hydrogen bond is between the hydroxyl group and the ketone in the steroid A ring. The chlorine atom acts as an acceptor in two intramolecular C–H⋯Cl hydrogen bonds involving ring hydrogens, as well as in an intermolecular hydrogen bond involving a methyl group. There are several C–H⋯O hydrogen bonds, mainly to ketone oxygens, but also to the hydroxyl group and an ether oxygen. The powder patterns have been submitted to ICDD for inclusion in the Powder Diffraction File™.

The crystal structure of pantoprazole sodium sesquihydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Pantoprazole sodium sesquihydrate crystallizes in space group Pbca (#61) with a = 33.4862(6), b = 17.29311(10), c = 13.55953(10) Å, V = 7852.06(14) Å3, and Z = 16. The crystal structure is characterized by layers parallel to the bc-plane. One layer contains the Na coordination spheres. The two independent sodium ions are trigonal bipyramidal and octahedral. The NaO3N2 and NaO4N2 coordination spheres share an edge to form pairs. The sodium bond valence sums are 1.17 and 1.15. The difluoromethyl groups are probably disordered. Two water molecules act as hydrogen bond donors to pyridine nitrogen atoms and sulfoxide oxygen atoms. The third water molecule participates in bifurcated hydrogen bonds, but one of its hydrogen atoms does not participate in hydrogen bonds. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1424.

The crystal structure of ipratropium bromide monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Ipratropium bromide monohydrate crystallizes in the space group P21/c (#14) with a = 8.21420(7) Å, b = 10.54617(13) Å, c = 24.0761(39) Å, β = 99.9063(7) °, V = 2054.574(22) Å3, and Z = 4. Both hydrogen atoms of the water molecule act as donors to the bromide cation, forming a ring with the graph set R2,4(8). The hydroxyl group also acts as a donor to Br. Several C–H⋯Br hydrogen bonds are present. The water molecule acts as an acceptor in two C–H⋯O hydrogen bonds from methyl groups. The ketone acts as an acceptor in C–H⋯O hydrogen bonds from methyl groups, a methylene group, and a methyne group. The hydroxyl group acts as an acceptor in a C–H⋯O hydrogen bond from a phenyl carbon atom. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1611.

Flucytosine, CAS #2022-85-7, crystallizes in the tetragonal space group P41212 (#94) with a = 6.643768(27), c = 23.89009(10) Å, V = 1054.500(7) Å3, and Z = 8. In this work, the sample was obtained from the United States Pharmacopeial Convention (USP) Lot #R03100 and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using the density functional theory (DFT). When looking down the a-axis, the crystal structure consists of multiple ribbon-like structures stacked into columns. The powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®). The agreement of the Rietveld-refined and DFT-optimized structures is good, with the largest difference in the external amine group with an overall root mean displacement of 0.056 Å. There is also evidence of unit cell expansion at higher temperatures, as the volume of the unit cell at 298 K was 1.6–1.9% greater than the two unit cells obtained at 150 K. A N–H⋯O hydrogen bond exists in the inter-ribbon region between the flucytosine molecules, resulting in a 3D hydrogen bond network.

Trimethoprim crystallizes in the triclinic space group P-1 (#2) with a = 10.5085(3), b = 10.5417(2), c = 8.05869(13) Å, α = 101.23371(21), β = 112.1787(3), γ = 112.6321(4)°, V = 743.729 Å3, and Z = 2. A reduced cell search in the Cambridge Structural Database yielded three previous structure determinations, using data collected at 100 K, 173 K, and room temperature. In this work, the sample was ordered from the United States Pharmacopeial Convention (USP) and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using density functional theory techniques. We found similar hydrogen bonding patterns with the previous determinations. In addition, we identified two C–H⋯O hydrogen bonds, which also contribute to the crystal energy. When comparing the previously reported trimethoprim structure determinations, the unit cell length lattice parameters were found to contract at lower temperatures, particularly 100 K. All structures show reasonable agreement, with unit cell length differences ranging between 0.05 and 0.15 Å. The diffraction data for this study were collected on beamline 11-BM at the Advanced Photon Source, and the powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

Commercial fluorometholone, CAS #426-13-1, crystallizes in the monoclinic space group P21 (#4) with a = 6.40648(2), b = 13.43260(5), c = 11.00060(8) Å, β = 92.8203(5)°, V = 945.517(5) Å3, and Z = 2. A reduced cell search in the Cambridge Structural Database yielded one previous structure determination, using single-crystal data at 292 K. In this work, the sample was ordered from the United States Pharmacopeial Convention (Lot # R032K0) and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using density functional theory (DFT) techniques. Hydrogen positions were included as a part of the structure and were re-calculated during the refinement. The diffraction data were collected on beamline 11-BM at the Advanced Photon Source, Argonne National Laboratory, and the powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™. The agreement of the Rietveld-refined and DFT-optimized structures is excellent; the root-mean-square Cartesian displacement is 0.060 Å. In addition to the O–H⋯O hydrogen bonds observed by Park et al. (Park, Y. J., Lee, M. Y., and Cho, S. I. (1992). “Fluorometholone,” J. Korean Chem. Soc. 36, 812–817), C–H⋯O hydrogen bonds contribute to the crystal energy.