Standardized X-ray powder diffraction data for orthorhombic LaCo0.4Fe0.6O3 prepared by calcination of a glycine-nitrate combustion-synthesized precursor are reported. Orthorhombic unit cell parameters: a = 5.4688 (2), b = 5.5100 (2), c = 7.7462 (3) Å. The reference intensity ratio, I/Icor,= 6.12.

Indexed powder diffraction data for Lu(OH)3 are reported. The compound is cubic, Im3(No. 204), with a = 8.2221(3)Å, V = 555.84Å3, Z = 8, Dm = 5.36(4)Mg m−3 (Dx = 5.40Mg m−3). The refined cell parameter was determined by employing a Siemens Debye-Scherrer camera (Cu radiation, Ni filter). The indexed data were evaluated according to the quantitative figures of merit FN and M20 (F29 = 20(0.028,51) and M20 = 43.5). A thermal gravimetric analysis is presented. The JCPD S Diffraction File No. for Lu(OH)3 is 38–1500.

The crystal structure of salmeterol xinafoate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Salmeterol xinafoate crystallizes in space group P−1 (#2) with a = 9.173 89(13), b = 9.483 79(14), c = 21.3666(4) Å, α = 82.2646(13), β = 85.2531(12), γ = 62.1565(11)°, V = 1628.37(5) Å3, and Z = 2. Key to the structure solution was linking the two fragments by a Li atom along the expected N–H···O hydrogen bond. The salmeterol cation and xinafoate anion are linked by N–H···O and O–H···O hydrogen bonds, interactions which cause the salmeterol to adjust its conformation. The hydrogen bonds result in complex chains along the b-axis. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1430.

The X-ray powder diffraction pattern for a sample of the high-temperature superconducting phase Tl0.5Pb0.5Sr2CaCu2O6.5+δ has been determined. The sample was prepared by a molten salt technique and had a Tc of 96 K.

Powder X-ray diffraction was used to investigate the solid solution range of the Bi14SrxCa12−xO33 series in the Bi–Sr–Ca–O system. Solid solution forms over the range 1≤x≤7 in Bi14SrxCa12−xO33. Experimental X-ray reference patterns of selected members with x=1, 3, 5, and 7 have been prepared for the powder diffraction file (PDF). These phases are monoclinic, C2/m, with cell parameter a ranging from 21.473(4) to 21.868(4) Å, b from 4.3564(9) to 4.3898(9) Å, c from 12.753(2) to 12.962(2) Å, β from 102.91(2)° to 102.79(1)°, and V from 1162.9(3) to 1213.5(3) Å3, respectively. These parameters increase monotonically as Ca is continuously replaced by the larger Sr.

A powder diffraction pattern and unit cell data for nitroguanidine, C(NH2)2NNO2 are presented. The orthorhombic space group Fdd2 (43) has been confirmed by single crystal methods.

Calculated patterns for the BaR2PdO5 series, in which X is Pd and R=Nd, Sm, Eu, or Gd, have been prepared for materials characterization until experimental patterns can be determined. These compounds are isostructural to the superconductor related “brown phases” BaLa2CuO5 and BaNd2CuO5, which are tetragonal with space group P4/mbm, Z=4. The cell parameters of the Eu and Gd compounds were derived from the La and Nd analogs. The calculated patterns of these four compounds compared well to an experimental pattern of BaNd2CuO5.

Recently, Dahan and co-workers (Dahan, 1991) suggested processing the XRD data by spreadsheet computer programs. Treated in this manner the XRD data became very flexible and made comparison with other data sets, as well as graphical presentation, much easier. In this note a simple FORTRAN 77 program for conversion of PC-APD data files into ASCII files suitable for import into spreadsheets is reported.

In our laboratory XRD data are collected on a Philips 1710 diffractometer operated by the PC-APD version 2.0 (PC-APD Software, 1989). Each experiment usually generates its files containing collected raw intensity data (.RD file), background data (.BK file) and file with peak positions and their intensities (.DI file). The XRD data can be further processed: after smoothing, data are stored in files with extension .SM (.SM file) and, after Kα2 stripping, into files with extension .A2 (.A2 file). All files are stored in the binary format.

Over the past 20 years, many designer drugs derived from controlled substances have been widely distributed as easily available psychoactive substances and have become a serious problem in Japan. In order to determine the absolute structures of four new designer drugs derived from medicines (methylphenidate and phenmetrazine) X-ray single-crystal structure analyses were performed using the BL26B1 beamline of synchrotron radiation facility SPring-8. The results show that the molecular configuration of these designer drugs (having two asymmetric carbons), which were distributed in the illegal drug market had threo-forms as found for methylphenidate and phenmetrazine.

The crystal structure of daclatasvir dihydrochloride Form N-2 (Daklinza®) has been refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Daclatasvir dihydrochloride, Form N-2, crystallizes in space group P1 (#1) with a = 7.54808 (15), b = 9.5566 (5), c = 16.2641 (11) Å, α = 74.0642 (24), β = 84.0026 (13), γ = 70.6322 (5)°, V = 1064.150(11) Å3, and Z = 1. The hydrogen bonds were identified and quantified. Strong N–H⋯Cl hydrogen bonds link the cations and anions in chains along the a-axis. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

The Ba2.64Ta11.25O30.81was prepared by conventional solid-state reaction technique as a single phase. It was found that the compound crystallizes in the tetragonal system, space group P4/mbm (No. 127) and unit-cell parameters are a = 12.508 59(8) Å, c = 3.912 81(2) Å, V = 612.218(7) Å3, and Z = 1. The crystal structure of the Ba2.64Ta11.25O30.81 phase is found to be closely related to the tetragonal tungsten bronze structure type, comprising interstitial (TaO)+ inclusions. Reference data were derived from the Rietveld analysis and reported here.

Knowledge of the surface composition of planetary bodies comes from a number of sources; such as landers, remote sensing and meteorites. However, the bulk mapping of the composition of planetary surfaces has been undertaken by analysis of reflected sunlight and these data—principally collected in the near-infra-red (IR) region—are notoriously broad and ambiguous. Hence, if laboratory spectra could be tied to physical properties measurements, such as diffraction, this would substantially aid our understanding of processes occurring in these extra-terrestrial environments. This contribution presents the capability of collecting near-IR data at the same time as neutron and synchrotron X-ray diffraction in a range of conditions (low temperature, vacuum, and humidity variations) and highlights two examples where this capability could enhance our understanding of planetary surfaces.

X-ray powder diffraction data, unit-cell parameters, and space group for ruxolitinib are reported [a = 8.7211(5) Å, b = 19.6157(15) Å, c = 18.9645(10) Å, β = 90.903(6)°, unit-cell volume V = 3243.85 Å3, Z = 8, and space group P21]. All measured lines were indexed and are consistent with the corresponding space group. No detectable impurities were observed. The single-crystal data of ruxolitinib are also reported [space group P21, a = 8.7110(2) Å, b = 19.5857(4) Å, c = 18.9372(4) Å, β = 90.8570(10)°, unit-cell volume V = 3230.53(10) Å3, Z = 8]. The experimental powder diffraction pattern has been well matched with the simulated pattern derived from the single-crystal data.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to address specific aspects of the performance of X-ray powder diffraction instruments. This report describes SRM 1879b, the third generation of this powder diffraction SRM. SRM 1879b is intended for use in the preparation of calibration standards for the quantitative analyses of cristobalite by X-ray powder diffraction in accordance with National Institute for Occupational Safety and Health (NIOSH) Analytical Method 7500, or equivalent. A unit of SRM 1879b consists of approximately 5 g of cristobalite powder bottled in an argon atmosphere. It is certified with respect to crystalline phase purity, or amorphous phase content, and lattice parameter. Neutron powder diffraction, both time-of-flight and constant wavelength, was used to certify the phase purity using SRM 676a as an internal standard. A NIST-built diffractometer, incorporating many advanced design features was used for certification measurements for lattice parameters.

The crystal structures of KCaVO4 and RbBaVO4, synthesized at high-pressure/high-temperature and by a conventional solid-state reaction, respectively, were determined using X-ray powder diffraction data. These compounds were found to have the β-K2SO4 structure type (space group Pnma, Z = 4) with parameters a = 7.2628(5) Å, b = 5.7258(4) Å, c = 9.6854(7) Å (KCaVO4), and a = 7.8887(1) Å, b = 5.9589(1) Å, c = 10.3958(2) Å (RbBaVO4). The unit cell volume of KCaVO4, 402.77(5) Å3, is significantly lower than for the low-temperature modification reported previously, 436.2 Å3. The difference can be explained by a pressure-induced phase transition to a more dense state resulting from the rotation of tetrahedra and the exchange of oxygen atoms from the first and second coordination spheres for potassium and calcium atoms.

Five transition metal derivatives of maleic acid with general formula, M2+(C4H3O4−)2⋅4H2O (M2+=Mn, Fe, Co, Ni, and Zn) were prepared by slow evaporation of the aqueous solution at room temperature. Their X-ray powder diffraction patterns were recorded and evaluated. These materials are isostructural and crystallize in a triclinic unit cell. The volume of the cells vary linearly between that of the Ni complex [V=314.65(7) Å3: a=5.1769(8) Å, b=7.317(1) Å, c=9.140(2) Å, α=108.42(2)°, β=104.61(1)°, γ=92.87(1)°] and the volume of the Mn-derivative [V=330.30(8) Å3: a=5.322(1) Å, b=7.375(1) Å, c=9.752(2) Å, α=115.48(2)°, β=106.64(2)°, γ=86.63(2)°].

A poster session was held during the Annual Spring Meeting of the International Centre for Diffraction Data on 20 March 2002. Abstracts of the posters are reproduced in the following. The underlined authors can be contacted for more information.

We present a review of the application of diffraction stress∕strain analysis to small volumes. For cases in which the material properties and∕or the stress state are not homogeneous, traditional approaches may yield erroneous stress results. On the other hand, with proper care, relevant mechanical information about the system can be obtained. Through the use of conventional and synchrotron-based X-ray methods, we can determine the amount of strain transfer between thin film features that possess heterogeneous stress distributions and the underlying substrate. Two examples of such studies are presented. The resulting data are used to assess the validity of several models often used to predict the mechanical behavior in thin film∕substrate composites.