Four new compounds with general formula CdI2-2(NH2-PhX) (Ph represents phenyl radical; X represents Cl or H atoms) were obtained and characterized. Two of them, bisaniline diiodidecadmium(II) — CdI2⋅2[NH2–C6H5] {1} and bis(2-chloroaniline) diiodidecadmium(II) — CdI2⋅2[NH2–C6H4Cl] {2}, crystallize in monoclinic system, whereas another two, bis(3-chloroaniline) diiodidecadmium(II) — CdI2⋅2[NH2–C6H4Cl]{3} and bis(4-chloroaniline) diiodidecadmium(II) hemi(4-chloroanilate) — CdI2⋅2[NH2–C6H4Cl]½[NH2–C6H4Cl] {4}, crystallize in triclinic system. The investigated compounds, from chemical point of view, are similar to the so-called cisplatin—a compound used as a chemotherapy drug to treat many types of cancers. Their syntheses and results of X-ray powder diffraction studies at room and elevated temperatures are described in this paper.

A new barium copper niobate, Ba4CuNb3O12, was successfully prepared by high-temperature solid-state reaction in an inert atmosphere. Rietveld-refinement analysis of the XRD data of the compound showed that it has the 8H-type hexagonal perovskite structure with space group P63/mmc (#194), a = 5.830(1) Å, c = 19.123(1) Å, and chemical composition of Ba4Cu1.84Nb2.16O12-δ.

Two applications of parametric Rietveld refinement employing a newly developed robust computer program are presented. The first application focuses on the parametric kinetic analysis of the reactions involving phase transitions of various polymorphic forms of copper phthalocyanine pigments. The second application concerns the parameterization of crystallite size with respect to experimental temperature. XRPD data for nanocrystalline titanium dioxide measured in dependence on temperature are used in this case study. Both the applications were realized with the help of the developed program in combination with the launch mode of topas® software.

The structure of [Al2(pydc)2(μ2-OH)2(H2O)2]n(pydc = 2,5-pyridinedicarboxylate) was successfully determined from powder X-ray diffraction data. The compound crystallizes in the triclinic system (space group P -1) with a = 6.7813(1) Å, b = 7.4944(1) Å, c = 8.5013(1) Å, α = 95.256(1)°, β = 102.478(1)°, γ = 108.979(1)°. The structure consists of aluminum ions coordinating N and O in distorted octahedra, sharing an edge through two hydroxide ions. These dinuclear complexes are connected by pydc ions, which at one end coordinate by nitrogen and oxygen and only by oxygen at the other end. The pydc orientation is reversed in the neighboring pydc, forming double stranded chains interconnected by the aluminum dinuclear complexes in a ladder-like arrangement along [001].

Ag3O was synthesized by jet-milling magnetron-sputtered Ag–Ag2O thin films. Heating the jet-milled powders in air and N2 from 40 to 148 °C at ambient pressure produced Ag3O-rich powders. The phase composition and unit-cell parameters of the jet-milled powders were measured as a function of temperature with in situ X-ray powder diffraction experiments from −186 to 293 °C. Ag3O was also produced by ball milling and sonicating jet-milled films at ambient conditions. The phase composition, unit-cell parameters, and thermal-reaction rates indicate nonstoichiometric Ag3O was produced from the reaction of metastable, nonstoichiometric Ag2O (cuprite structure) and ccp Ag. The thermal expansion of Ag3O is anisotropic; below 25 °C, the a-axis expansion is about twice the c-axis expansion resulting in a negative slope of c/a(T). The reversal of the sign of c/a(T) near 25 °C is dramatic. The thermal reaction is arrested when the temperature is rapidly increased from ambient to 130 °C. Ag3O is metastable and decreases its unit-cell volume during kinetic decomposition to Ag when heated above ambient temperature in air and nitrogen. The relative volume expansion of Ag3O is about 80% less than Ag at room temperature and below. The suite of nonstoichiometric Ag3O produced by heating displays a linear relation between c/a and unit-cell volume at room temperature. The c/a and unit-cell volume of a hydrothermally grown Ag3O single crystal reported in a published structure determination was the Ag-rich, low-volume end member of the linear series. The c/a and unit-cell volume are sensitive indicators of the oxygen content and state of disorder.

Experimental X-ray powder diffraction data, unit-cell parameters, and space group for norethindrone, C20H26O2, are reported [a = 20.7484(12) Å, b = 12.1678(9) Å, c = 6.5561(2) Å, α = β = γ = 90°, unit-cell volume V = 1655.17(16) Å3, Z = 4 and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurity was observed.

The structure of bethanechol chloride C7H17ClN2O2 is solved from conventional X-ray powder diffraction data in direct space [monoclinic unit cell with a=8.8749(3) Å, b=16.4118(7) Å, c=7.1373(3) Å, β=93.803(1)°, V=1037.29(7) Å3, Z=4, and space group P21/n]. The existence of a second orthorhombic closely related form is discussed.

Eight phosphates and arsenates of manganese have been synthesized and examined using powder X-ray diffraction in order to update or extend the current powder diffraction data files. The studied compounds are MnPO4·H2O, MnAsO4·H2O, LiMnPO4(OH) LiMnAsO4(OH), LiMnAsO4, Mn2As2O7) MnAsO4, and Mn(PO3)3. The powder patterns have been indexed and the cell data are reported.

A new phase in the system BaO–MnO–SiO2 obtained by a pyrosynthetic method has been inves- tigated using electron microprobe analysis (EPMA), X-ray powder diffraction (PDA), and trans- mission electron diffraction. The lattice parameters and possible space group of the phase with a general composition BaMnSi2O6 were determined as follows: a=13.896, b=12.261, c=10.781 Å, β=103.47°, space group P21/m, Z=12.

This study examined basal peak irrationalities according to boundary conditions of the hectorite basal diffraction unit (BDU), which were recognized as the total assembly of 2:1 phyllosilicate layer plus interlayer material. The hectorite basal profiles were computer-simulated using the three kinds of BDU settings identified from the middle of octahedral sheets in the nearest neighbor (centrosymmetric model), the middle of interlayers in the nearest neighbor (centrosymmetric model), and a basal oxygen plane to the margin of interlayer in contact with the next phyllosilicate layer (non-centrosymmetric model). In the results of simulations, irrationality and asymmetry of the hectorite basal peaks relied straightforwardly on the BDU scattering modulations for the non-Bragg angles containing information on the synergic scattering events of phyllosilicate layer and interlayer material. Among the concerned BDU boundaries, the non-centrosymmetric model more effectively represented the real hectorite profile than the two previously reported centrosymmetric models.

A cover for Scintag's six and twelve-position sample changers was designed and constructed to provide an inert atmosphere for samples during diffraction batch runs. The cover is equipped with inlet and outlet gas ports and fits over the top of the sample changer. Using dry nitrogen gas fed into the inlet of the cover, a sample of lithium bromide was protected from atmospheric moisture for greater than 18 h. The cover uses a thin Mylar window that gives greater than 95% transparency for copper K-alpha X-rays. The cover is a simple device that allows our lab to run multiple moisture-sensitive samples in a batch mode. The simple approach and materials used in the construction of the cover could be applied to other brands of powder diffractometers.

The capability of whole-powder-pattern decomposition in the quantitative phase analysis (QPA) of natural products was investigated using three- to six-component mixtures and pottery bodies. Here, the term pottery body means plastic clay suitable for making pottery and it is compounded of ceramic raw materials. Average errors of the weight fractions for each phase were within 1 weight percent in each mixture of natural products. The amounts of reduced oxides in pottery bodies derived from the X-ray diffraction technique were in good agreement with results obtained by X-ray fluorescence analysis. The present procedure does not require knowledge of crystal structures; it appears adequate for the QPA of natural products.

X-ray powder diffraction data and refined unit cell parameters for the (Bi, Pb)2Sr2Ca2Cu3Ox (2223) superconducting phase, indexed using incommensurate modulation principles, are reported. Comparison of the results obtained with one- and two-component modulation wave vectors showed that the two-component modulation wave vector is superior for indexing the satellite reflections. A two-component wave vector indexing result seems likely when only the powder diffraction data are considered.

X-ray powder diffraction data and refined unit cell parameters for SrTi3Nb4O17, SrTi5Nb4O21, SrTi7Nb4O25, SrTi9Nb4O29, SrTi11Nb4O33, SrTi13Nb4O37, and SrTi15Nb4O41 are reported here. The powder patterns for these oxides suggest that they form a homologous series SrM2n+1O4n+5 (M=Ti, Nb; n=3→9), which is isostructural with the orthorhombic “chemically twinned rutile” series found previously in the K2O-TiO2-Ta2O5 and BaO-TiO2-Nb2O5 systems. The structures are built of corner-sharing slabs of the rutile structure; successive members are generated by adding 2TiO2 to the slab thickness of the previous member. The series crystallizes in space group Cmcm (No. 63), with members exhibiting similar a-, b-dimensions (∼6.6, ∼8.9 Å; respectively), and c-dimensions that linearly increase (by ∼4.4 Å per member) from 20.8 Å for n=3 to 47.1 Å for n=9.

Limitations in powder diffractometry imposed by scatter slits and/or a diffracted-beam monochromator, which have been ignored in the past, are discussed and mapped quantitatively. These limitations become manifest especially with ωoffsets, i.e.in stress measurements and with ωoscillation to improve the reproducibility of intensities in the presence of too coarse grains. The limitations can only be established with knowledge of slit sizes and with precise alignment of all slits, their holders and the diffracted-beam monochromator. To that end, concise, accurate procedures for obtaining these measurements in-situare proposed.

The Semi-manual Structure-sensitive SEARCH-MATCH procedure [Frevel, (1982), Anal. Chem. 54, 691–697] has been automated for the Hewlett-Packard HP 3354 Computer. The software is coded in the interpretive HP LAB BASIC II language. A core file of 1026 selected powder diffraction standards has been compiled covering the common crystalline phases encountered in industry, the ubiquitous crystalline minerals, and prototypes of the more frequently found crystal structures. Solid solutions can be readily identified.