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®).

A qualitative phase identification system for crystalline mixtures is presented. The system provides up to five-phase qualitative identification using up to nine-peak filtration, and additive full peak matching based on the powder diffraction file of ICDD. It was implemented using Microsoft Visual C++, and runs under most common Windows systems. Screenshots and examples are included.

A new cobalt molybdate with the formula NaCo2OH(H2O)(MoO4)2 was synthesized by hydrothermal reaction at 200 °C and was found to possess the Φx type structure. The crystalline system of this material is monoclinic and its cell parameters are a=9.3792 (2), b=6.3331 (1), c=7.6281 (2) Å and β=115.832°, obeying the C2/m space group symmetry.

2,4-dichloro-5-nitrobenzoic acid (C7H3NO4Cl2) has been investigated by means of X-ray powder diffraction. The title compound is monoclinic with unit-cell parameters a=13.761 (2), b=8.435 (1), c=7.684 (1) Å, β=99.85 (1)°, V=878.5 (1) Å3, Z=4, Dx=1.772 g/cm3, space group P21/a (14).

An incident beam X-ray collimator for Mao-Bell type diamond anvil cell (DAC) has been developed. Alignment of the collimator is carried out in situ while viewing the image of the collimated X-ray spot formed on a thin layer of fluorescent material spread on the diamond anvil culets with the help of a microscope. Special precaution has been taken to meet the radiation safety requirements during alignment and routine use. This collimator is of immense help for laboratory based high pressure X-ray diffraction experiments.

The authors present and discuss a method for simultaneous quantitative analysis of total loss on ignition (LOI) (CO2 + H2O) and CO2 content separate from the LOI, in an industrial environment of quicklime production. Total LOI is determined by the Compton scattered RhKα tube radiation which is used directly in the calibration equation. The resulting calibration curve for LOI, including matrix correction shows an accuracy of 0.15 mass%. The carbon content (CO2) is distinguished from total LOI by measuring CKα radiation, which is possible with the required accuracy by employing a new multilayer analyzer with greatly improved background characteristics. The method aims at high reliability and sample throughput and at becoming a less time-consuming alternative to the conventional method of LOI determination by weighing sequences before and after “ignition” at 1050 °C.

New phosphates Ca9–xPbxEu(PO4)7 were obtained by solid state reaction techniques at 1213–1253 K in air atmosphere and were found to be isotypic with whitlockite-type β-Ca3(PO4)2. The unit cell parameters were determinate using Le Bail decomposition. Rietveld method structural refining showed that Eu3+ ions are located statistically with calcium in M1, M2, and M3 sites, whereas Pb2+-ions are preferentially located in the M3. Examination of optical second harmonic generation evidences nonlinear optical activity and confirms polar space group R3c.

The “hook effect” observed in the Warren-Averbach analysis of X-ray diffraction peaks from multiple layer thin films of copper has been investigated theoretically and experimentally. The strengths of the “hook effect” for films of different layer thicknesses were analyzed. The results showed definite correlation between the strengths of the “hook effect” and the grain size distributions in 1, 4, and 19-layer copper films.

(Na0.6H0.4)(Ta0.7Nb0.3)O3 was synthesized by heating a tantalum/niobium scale containing two sodium tantalate/niobate phases :Na14(Ta0.7Nb0.3)12O37·31H2O and NaH2Ta0.7Nb0.3O4. Powder X-ray diffraction data for (Na0.6H0.4)(Ta0.7Nb0.3)O3 indicated it to be a cubic perovskite (ABO3/ReO3 type structure) with unit cell a0=3.894 Å. The compound is analogous to the mineral lueshite (NaNbO3), and to the high temperature forms of NaTaO3 and NaNbO3. Powder diffraction data for (Na0.6H0.4)(Ta0.7Nb0.3)O3 will be useful in the analysis of synthetic tantalum/niobium concentrates.

X-ray powder diffraction data for the high temperature phase of NaBi3V2O10 obtained from in situ high temperature XRD studies are presented. NaBi3V2O10 undergoes a phase transition from triclinic to monoclinic at about 600 °C. The unit cell parameters of the high temperature monoclinic phase at 600 °C are: a=12.3899(21), b=5.5642(10), c=7.1543(18) Å and β=98.393(16)°, V=487.94(13) Å3 and Z=2, ρcal=6.20 g∕cc. On further increasing the temperature, it partially decomposes to a γ-Bi4V2O11 type phase. The details of this phase as well as the stability of NaBi3V2O10 are discussed.

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.

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.

X-ray powder diffraction data, unit-cell parameters and space group for a rare natural organic mineral refikite, C20H32O2, abiet-13(15)-en-18-oic acid, are reported [a = 22.55(2) Å, b = 10.469(6) Å, c = 7.930(9) Å, unit-cell volume V = 1871.82 Å3, Z = 4 and space group P21212]. All measured lines were indexed and are consistent with the P21212 space group. No detectable impurities were observed.

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 crystal structure of a new polymorph of germacrone has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. This polymorph (Form II) crystallizes in space group C2/c (#15) with a = 26.0073(4), b = 9.84383(10), c = 10.53713(13) Å, β = 95.7547(11)°, V = 2684.04(3) Å3, and Z = 8. The crystal structure is dominated by van der Waals interactions, but four C–H⋯O hydrogen bonds are present. The structure exhibits many similarities to the previously reported Form I polymorph FIQLOG, but is clearly different. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF).

The crystal structure of bretylium tosylate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Bretylium tosylate crystallizes in space group C2/c (#15) with a = 32.6238(4), b = 12.40353(14), c = 9.93864(12) Å, β = 101.4676(10), V = 3941.39(5) Å3, and Z = 8. The sample exhibited visible decomposition in the X-ray beam. The unusual displacement ellipsoid of the Br atom probably indicates that the decomposition in the beam involves the Br atom. The crystal structure can be viewed as layered parallel to the bc plane. The layers are double, the center consisting of the cation/anion polar interactions and the outer surface of the double layers consists of hydrocarbon interactions. In the absence of normal hydrogen bond donors, the only hydrogen bonds in the bretylium tosylate structure are C–H…O hydrogen bonds. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™.