The titled compound, Hg2[Fe(CN)5NO], was synthesized and studied by X-ray powder diffraction, infrared spectroscopy, Mössbauer spectroscopy, and atomic force microscopy. The results arising from this study indicate that this compound is anhydrous and crystallizes in the P222 orthorhombic symmetry. The unit cell parameters were quantified as a=16.5905(9) Å, b=12.3145(8) Å, and c=8.7576(5) Å. The measured and calculated density values are Dm=1.149 g/cm3 and Dc=1.145 g/cm3, respectively, with Z=2.

Diblock copolymers (BCPs) show phase separation on mesoscopic length scales and form ordered morphologies in both bulk and thin films, the latter resulting in nanostructured surfaces. Morphologies in thin films are strongly influenced by film parameters, the ratio of film thickness and bulk domain spacing. Laterally structured polymer surfaces may serve as templates for controlled assembly of nanoparticles (NPs). We investigated the BCP of poly(n-pentyl methacrylate) and poly(methyl methacrylate) which show bulk morphologies of stacked lamellae or hexagonally packed cylinders. Thin films were investigated by atomic force microscopy and grazing-incidence small-angle X-ray scattering. For film thicknesses f well below d bulk, standing cylinder morphologies were observed in appropriate molar ratios, while film thicknesses around and larger than d bulk resulted in cylinders arranged parallel to surface. To alter and/or improve the morphology also in presence of different NPs (e.g., silica, gold), solvent vapour annealing (SVA) was applied. The BCP morphology usually remains unchanged but periodicities change depending on type and amount of incorporated NPs. It was found that silica clusters enlarge lateral distances of cylinders, whereas Au NPs reduce it. The effect of SVA is weak. The quality of morphology is slightly improved by SVA and lateral distances remain constant or are slightly reduced.

The Level III Powder Diffraction File Computer Database can be used for many purposes beyond phase identification. The data file as received from the ICDD must be implemented via a data management system for efficient utilization. The results of one such implementation, and applications using the Mineral Powder Diffraction Subfile are reported. The applications include studies of space group statistics and density distributions as well as searches for cubic sulfide and uniaxial potentially pyroelectric minerals.

The present paper establishes that the ratio between the XRD pulse counts of cement clinkers at d=0.278 and 0.274 nm bears a distinct relationship with the degree of sintering of the clinker, which is one of the factors that determine the cement quality. The paper also presents a rapid and accurate method for predicting both 3- and 28-day compressive strength (CCS) of cement mortar cubes based on XRD of the cement clinkers. The method is based on an index Xn derived from the XRD pulse counts at d=0.2959 and 0.287 nm corresponding to alite (hkl=202) and belite (hkl=102) phases of the clinker, respectively. The regression equation derived for a particular plant is (1) 3 day CCS=Xn×240 kg/cm2, when Xn<1 and 240+26 (Xn−1) kg/cm2, when Xn>1, where Xnmaximum=5.5. (2) 28 day CCS=C+C×In/100, where C=3 days CCS estimated by XRD (1), In=90−10Xn, where Xnmax=5.5. Calculated CCS values, in average, vary from the conventional test values by +5.9% to −5.4% and +3.8% to −3.5% in cases of 3- and 28-day CCS, respectively.

A commercially available combined X-ray diffraction – differential scanning calorimetry (XRD-DSC) stage was adapted for studies of gas loading in microporous materials, including metal organic frameworks (MOFs). Insertion of a custom-built humid atmosphere swing chamber (HASC) between a humidity generator and the XRD-DSC stage facilitates both humid atmosphere and vacuum swing gas loading. The HASC is necessary to buffer between the humidity generator and the XRD-DSC stage, allowing the gas mixture to homogenize prior to sample exposure, so that both humid atmosphere and vacuum swings could be performed. The changes in XRD can be used to follow structural changes, including collapse, which is indicative of a lack of microporosity upon activation, and the flexibity of frameworks upon gas sorption–desorption cycles. Measurements of the area under the DSC curve allows for calculation of the isosteric heat of adsorption (Qst; kJ molGAS−1). Vacuum-atmosphere swing experiments performed at different pressure steps allow for the reconstruction of the enthalpy of gas adsorption before and after a phase transition. These modes of operation are illustrated in three case studies from a program of exploratory MOF synthesis used to discover novel materials for selective gas sorption from humid gas streams: (1) gas binding in Stony Brook metal organic framework-1, (2) zeolitic imidazolate framework-7 response to variable pressure vacuum-atmosphere swing, and (3) high throughput evaluation of the selectivity of novel MOFs synthesized from customized linkers.

This paper describes a straightforward method for the identification of the Miller indices associated with the face of a crystal of low symmetry. The method relies on orienting a crystal face parallel to the sample holder in the goniometer of a powder diffractometer. An intense diffractogram resulting from a single family of lattice planes parallel to the crystal face is obtained. The application of silicon powder to the surface of the crystal provides a means to correct 2Θ values for any misalignment of the crystal face. Calculated 2Θ and intensity values are used to assign the reflections from the corrected single-crystal diffractogram to a particular set of related lattice planes. In this paper are listed the corrected experimental 2Θ and intensity values for a particular face of a large single crystal of monoclinic hydroxylapatite and the theoretical 2Θ and intensity values for the h00 set of planes. Comparison of these parameters leads to the unambiguous assignment of that particular crystal face to the h00 Miller index.

The following fourteen reference patterns of boride, telluride, and oxide ceramics are reported. Included in the fourteen reference patterns are data for six high Tc superconducting oxide and related phases (Ba2CaCu2TI2O8, BaCuEu2O5, BaCuTm2O5, BaCuDy2O5, Ba3.2Cu1.7Y0.8O6.1·xCO2, Sr2Bi2O5). The general methods of producing these X-ray powder diffraction reference patterns are described in this journal, Vol. 1, No. 1, pg. 40 (1986).

Samples were mixed with one or two internal standards: silicon (SRM640a), silver, tungsten, or fluorophlogopite (SRM675). Expected 2θ values for these internal standards are specified in the methods described (ibid.). Data were measured with a computer controlled step-scanning diffractometer. The POWDER-PATTERN system of computer programs was used to locate peak positions, to calibrate the patterns, and to perform variable indexing and least-squares cell refinement. A check on the overall internal consistency of the data was also provided by a computer method.

Intensities were measured as peak heights above background and were read manually from strip charts. To minimize preferred orientation effects, the powders were passed through a 400 mesh sieve and were mixed with an amorphous diluent, silica gel. Sample mounts were prepared by side-drifting and/or by dusting a thin layer of sample on a glass slide coated with a thin smear of silicone grease.

We report on the X-ray diffraction data and unit-cell parameters of Mn4C, which has a cubic perovskite-type structure with a = 3.8726 Å and unit-cell volume V = 58.1 Å3. The measured lines were indexed and are consistent with the space group $ Pm { \bar {\it 3}} m$ (No. 221).

Near-surface triaxial strain/stress states in polycrystalline solids are required for a full tensorial treatment including all elements of the strain/stress tensor. A possible depth dependency of the strain/stress is at best observed by grazing incidence diffraction in Seemann–Bohlin geometry (SBG). The computer program SBGBBG calculates the full strain/stress tensor from X-ray diffraction data measured either in SBG or in Bragg–Brentano geometry (BBG). At present SBGBBG is applicable only on texture-free materials.

The effects of sample transparency in a powder diffraction experiment are discussed, and formulas including effects from horizontal divergence are derived. It is shown that the classical formula by Alexander [L. E. Alexander J. Appl. Phys. 21, 126 (1950)] is only a limiting case for zero horizontal divergence. It is also shown that in some cases extinction effects can play a role. The impact of these effects on both the line profile as well as the integrated intensity and experiments illustrating these phenomena, are discussed.

The ferroelectric liquid crystal material [4-[(4-methyloxyfenyl) carbonyloxyl] bifenyl-4′-yl]-(S)-2-methylbutoxypropionate containing a lateral methyl group on the aromatic ring of the alkoxybenzoate unit and two chiral carbons has been investigated by X-ray powder diffraction analysis at the 28 °C–105 °C temperature range. On cooling through the SmC temperature range, the layer spacing decreases from 28.3 to 27.7 Å with a small variation of average intermolecular distances. Lattice parameters of tetragonal and monoclinic crystalline phases occurring at lower temperatures have been determined.

The crystal structure of a novel high-energy density material 3-[(3,4-dinitro-1H-pyrazol-1-yl)-NNO-azoxy]-4-nitro-1,2,5-oxadiazole C5HN9O8 was determined and refined using laboratory powder diffraction data. The diffraction data and database analysis were insufficient to distinguish two candidate structures from the solution step. Density functional theory with periodic boundary conditions optimizations were used to choose the correct one. 3-[(3,4-Dinitro1H-pyrazol-1-yl)-NNO-azoxy]-4-nitro-1,2,5-oxadiazole crystallizes in space group Pbca with a = 8.3104(2) Å, b = 14.2198(5) Å, c = 19.4264(7) Å, V = 2295.66(14) Å3. The molecular conformation contains a weak intramolecular hydrogen bond C–H⋯O–N, and the structure is dominated by weak O⋯π and O⋯O contacts.

The room temperature powder pattern of lapatinib ditosylate monohydrate (active ingredient in Tykerb used to treat refractory breast cancer) was indexed and the cell from the single crystal X-ray diffraction structure was refined using the experimental capillary data. Unit-cell parameters for the orthorhombic compound with space group Pbca refined from powder diffraction data are a=9.6850±0.0009 Å, b=29.364±0.003 Å, and c=30.733±0.003 Å, α=β=γ=90°, z=8, V=8740.1 Å3. Values of 2θ, d, I, and Miller indices are reported.

Methods of chemical preparation and crystallographic data are reported for four new condensed phosphates: one hydrated cyclotriphosphate MnAg4(P3O9)2·6H2O and three long-chain polyphosphates: MnAg2(PO3)4, NiAg4(PO3)6 and NiNa4(PO3)6. Two of these new condensed phosphates, associated with manganese, belong to previously investigated structure types.

A method to characterize iron oxide microparticles by microquantity X-ray powder diffraction is presented. The method employs small sections of acrylic tubing and double sided Mylar® tape that fits over a standard 170 mm collimator for a Bruker-AXS SMART 1000 or APEXII three-circle single-crystal diffractometer (Mo X-ray tube). The tubing will hold and position a sample that is placed on the double-sided Mylar® tape and allow for rapid specimen mounting/dismounting and data collection. The method is simple, portable, and readily adapted to a variety of single-crystal X-ray diffractometers.

From 1967 to 2000 Daniel Louër of the Department of Crystal Chemistry, University of Rennes, and J. Ian Langford of the Department of Physics, University of Birmingham, collaborated in studying structural imperfections by means of high-resolution X-ray powder diffractometry. They contributed to the theory and practice of line profile analysis and investigated the microstructure of a variety of nanocrystalline materials. Although many of the projects undertaken were part of the research programme at Rennes to investigate the mechanisms of solid-state reactions, the work is relevant in other fields of materials science.

Yttrium oxalate dihydrate, Y2(C2O4)3.2H2O, has been investigated by means of X-ray powder diffraction. Unit cell dimensions were determined by an indexing program based on the variation of parameters by successive dichotomies. The diffractometer data were collected with strictly monochromatic radiation. A monoclinic cell was found: a=9.3811(8)Å, b=11.6385(15)Å, c=5.9726(7)Å, β=96.079(8)°, which is characterized by the figures of merit M20=87 and F30=112 (0.0065,41). A preliminary analysis of the anisotropic line broadening has revealed some microstructural properties. It is shown that line broadening is mainly due to a micro-strain effect.

The X-ray powder diffraction pattern for the title compound is reported in the range 5 ≤ 2θ ≤ 125°. The sample was prepared through solid-state reaction of BaCO3, CuO, and Pr6O11, and characterized with respect to oxygen content through iodometric titration. Refined parameters for the orthorhombic (space group Pmmm) unit cell are a = 3.8587(2) Å; b = 3.9302(1) Å; c= 11.7126(3) Å; a/b = 0.98181(6); a/c = 0.32945(2); b/c = 0.33555(1); Z = 1; Dx = 6.705(2) Mg m−3; V = 177.62(1) Å3; formula wt. = 717.48(16) g mol−1; SS/FOM: F30 = 48(0.005,127).

The title compound was identified as the major phase in a corrosion deposit by indexing its powder pattern, and locating an isostructural vanadium(II) compound in the NIST Crystal Data Identification File. The identity of the compound was confirmed by a Rietveld refinement. Hexaaquairon(II) trifluoromethanesulfonate crystallizes in the monoclinic space group C2/m, with a=18.6415(14), b=6.9291(5), c=6.5938(5) Å, β=104.742(6)°, V=823.68(10) Å3, and Z=2. The structure consists of alternating layers of octahedral hexaaquairon(II) cations and triflate anions. The cations and anions are linked into layers parallel to the bc plane by hydrogen bonds. Each water molecule donates two protons to sulfonate oxygens, and each sulfonate oxygen acts as an acceptor of two protons. A reference powder diffraction pattern is reported.