Synchrotron X-ray diffraction images are increasingly used to characterize crystallographic preferred orientation distributions (texture) of fine-grained polyphase materials. Diffraction images can be analyzed quantitatively with the Rietveld method as implemented in the software package Materials Analysis Using Diffraction. Here we describe the analysis procedure for diffraction images collected with high energy X-rays for a complex, multiphase shale, and for those collected in situ in diamond anvil cells at high pressure and anisotropic stress.

The crystal structure of one isotropic [(1) Brazil] and three birefringent spessartine samples [(2) California, (3) Tanzania, and (4) Colorado] were refined using the Rietveld method, cubic space group $Ia\overline 3 d$ , and monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. The results of electron-microprobe analysis (EMPA) indicate homogeneous compositions, in terms of end-members, as follows: (1) Sps54Alm43, (2) Sps90Alm8, (3) Sps64Prp27Grs3, and (4) Sps73Alm19. Their crystal structures were modeled well as indicated by the Rietveld refinement statistics where the reduced χ 2 and overall R (F 2) values for each sample are: (1) 1.395 and 0.0329, (2) 1.082 and 0.0354, (3) 1.025 and 0.0347, and (4) 1.016 and 0.0413. Two cubic phases occur in samples 2–4, and a single cubic phase occurs in sample-1. The dominant cubic phase-1 with locality, weight fraction (%), unit-cell parameter (Å), distances (Å), and site occupancy factors (sofs) are as follows: (1) Brazil: 100%, a = 11.581 54 (1), average <Mn–O> = 2.3156, Al–O = 1.8949 (3), Si–O = 1.6376 (3) Å, Mn(sof) = 0.961(1), Al(sof) = 0.945(1), and Si(sof) = 0.936(1); (2) California: 96.67(7)%, a = 11.613 32(1), average <Mn–O> = 2.3249, Al–O = 1.8956 (4), Si–O = 1.6416 (4) Å, Mn(sof) = 0.951(1), Al(sof) = 0.946(1), and Si(sof) = 0.927(1); (3) Tanzania: 69.46(6)%, a = 11.598 45(1), average <Mn–O> = 2.3199, Al–O = 1.8964 (5), Si–O = 1.6398 (5) Å, Mn(sof) = 0.808(1), Al(sof) = 0.942(1), and Si(sof) = 0.922(1); and (4) Colorado: 98.58(6)%, a = 11.606 89(1), average <Mn–O> = 2.3204, Al-O = 1.8948 (6), Si–O = 1.6450 (6) Å, Mn(sof) = 0.949(1), Al(sof) = 0.967(2), and Si(sof) = 0.913(2). The two-phase intergrowth causes strain that arises from mismatch of the structural parameters and gives rise to strain-induced birefringence.

The high cohesive interaction between reduced graphene oxide (RGO) sheets usually makes them difficult to disperse, which limits their utilization in achieving effective hybridization with polymers. We report here a new two-step route for preparing non-aggregated and high-conductive RGO powders. Graphene oxide precursor was first reduced by hydrazine hydrate in presence of a thermal unstable surfactant of cetyltrimethylammonium chloride (CTAC). Then a thermal annealing process under H2/Ar atmosphere was further used to remove the non-conductive CTAC molecules. The prepared RGO powder exhibited an electrical conductivity of 2.23 × 104 S m−1 – about ten times higher than the one (N-RGO) simply reduced by hydrazine hydrate. After incorporating into polymethylmethacrylate with a 5 wt% loading, the composite showed a conductivity of 4.11 S m−1, which was 60 times as high as that of the same composite based on N-RGO powder. The addition and subsequent removal of CTAC molecules is an effective method for preparing non-aggregated and highly conductive graphene powder and obtaining good incorporation into polymer matrices.

High-resolution neutron powder diffraction (NPD) data were recorded on a series of cathode material LiFe1−xMnxPO4 (x = 0, 0.2, 0.5, 0.8, and 1.0) solid solutions using the HRPD machine at SINQ/PSI, Switzerland. Ab initio crystal structure solution via program FOX indicates demonstrably that the space group of LiFePO4 is Pnma with Li1+ occupying octahedral (4a) sites and Fe2+ octahedral (4c) sites, respectively, in the olivine structure. Rietveld refinement (program FullProf suite version July-2011), complementary with X-ray diffraction data, shows that Fe2+ may partially (about 2%) distribute over Li1+ sites. NPD data for LiFe1−xMnxPO4 (x = 0, 0.2, 0.5, 0.8, and 1.0) reveal that the Mn2+ replaces Fe2+ at the octahedral (4c) sites. The cell parameters a, b, and c increase linearly and the interatomic distances (in Å) of Li–O(2) and Li–O(1) increase, while the interatomic distances (in Å) of Li–O(3) decrease on the addition of Mn, respectively, partially explaining a higher potential plateau of ~4.1 eV in LiMnPO4 compared to ~3.5 eV in LiFePO4.

CaTi1−xSnxO3 (x = 0.0–1.0) solid solutions were prepared by solid-state reaction at 1450 °C. Rietveld refinement of their powder X-ray diffraction patterns revealed that all the solid solutions crystallized in orthorhombic cells with the perovskite-type structure, the space group Pbnm. The refined unit-cell parameters linearly increased with nominal tin contents x.

The crystal structure and powder X-ray diffraction (XRD) patterns for three skutterudite samples, Fe(Sb2+ x Te1− x ), x = 0.05, 0.10, 0.20, have been determined. These compounds crystallize in the cubic space group $Im\bar 3$ . Te was found to randomly substitute in the Sb site. Because of the fact the covalent radius of Sb is greater than that of Te, a trend of increasing lattice parameter has been observed as the x value in Fe(Sb2+ x Te1− x ) increases [cell parameters range from 9.10432(4) to 9.11120(3) Å for x = 0.0 to 0.2, respectively]. The Fe–Sb/Te bond distance also increases progressively [from 2.5358(4) to 2.5388(4) Å] as the Te content decreases. While average Sb/Te–Sb/Te distances in the four-membered rings are similar in these three compounds, the average Sb/Te–Sb/Te edge distances in the octahedral framework increase progressively from 3.5845(12) to 3.5900(13) Å. Reference XRD patterns of these three phases have been prepared to be included in the Powder Diffraction File (PDF).

In the conventional X-ray reflectivity (XRR) analysis, the reflectivity is calculated based on the Parratt formalism, incorporating the effect of the interface roughness according to Nevot and Croce. However, the results of calculations of the XRR have shown strange outcomes, where interference effects increase at a rough surface because of a lack of consideration of diffuse scattering within the Parratt formalism. Therefore, we have developed a new improved formalism in which the effects of the surface and interface roughness are included correctly. In this study, for deriving a more accurate formalism of XRR, we tried to compare the measurements of surface roughness of the same sample by atomic force microscopy (AFM) and XRR. It is found that the AFM result could not be completely reproduced even with the improved XRR formalism. By careful study of the AFM results, we determined the need for an additional effective roughness term within the XRR simulation that depends on the angle of incidence of the beam.

Commercial atomoxetine hydrochloride crystallizes in the orthorhombic space group P212121 (#19), with a = 7.362 554(12), b = 13.340 168(27), c = 16.701 887(33) Å, V = 1640.421(5) Å3, and Z = 4. The structure was solved and refined using synchrotron powder diffraction data, and Rietveld and density functional techniques. The most prominent feature of the structure is zigzag chains of N–H···Cl hydrogen bonds along the a-axis. The powder pattern has been submitted to the ICDD for inclusion in future releases of the Powder Diffraction File™.

Commercial dutasteride crystallizes in the orthorhombic space group P212121 (#19), with a = 7.587 44(3), b = 9.960 80(5), c = 33.500 42(12) Å, V = 2531.862(17) Å3, and Z = 4. The structure was solved and refined using synchrotron powder diffraction data, Rietveld, and density functional techniques. The most prominent feature of the structure is a zigzag chain of strong N–H···O = C hydrogen bonds along the a-axis. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.

Crystal structures of N-(2-chlorophenyl) acetamide (1) and phenyl (2-bromomethyl) benzoate (2) have been determined from laboratory X-ray powder diffraction data. In addition to intermolecular N–H···O and C–H···O hydrogen bonds, the crystal packing in (1) and (2) exhibits weak C–H···Cl/Br interactions, which facilitate formation of three-dimensional architectures. Hirshfeld surface analysis of compounds (1), (2), and a few related chloro- and bromo-phenyl derivatives retrieved from the CSD indicates that 83–97% of Hirshfeld surface areas in this class of compounds are due to H···H, H···π, H···O, and H···Cl/Br contacts.

Clotrimazole (C22H17ClN2, 1-[(2-chlorophenyl)(diphenyl)methyl]-1H-imidazole) and fluconazole (C13H12F2N6, 2-(2,4-difluorophenyl)-1,3-bis(1H-1,2,4-triazole-1-yl)propan-2-ol) are two active pharmaceutical ingredients commonly used in the treatment and prevention of superficial and systemic fungal infections. The X-ray powder diffraction data and the unit cell parameters of anhydrous clotrimazole [Triclinic, P ${\bar 1}$ , a  = 8.776(1) Å, b  = 10.571(2) Å, c  = 10.622(3) Å, α = 114.08(2)°, β = 96.87(2)°, γ = 97.61(2)°, V = 875.2(2) Å3, Z = 2] and monohydrated fluconazole [Triclinic, P ${\bar 1}$ , a  = 5.6353(4) Å, b  = 11.753(1) Å, c  = 12.326(1) Å, α = 71.220(8)°, β = 79.896(9)°, γ = 84.35(1)°, V = 760.13(9) Å3, Z = 2] are reported.

In this paper, X-ray powder diffraction data, unit-cell parameters, and space group for bisacodyl, C22H19NO4, are reported [a = 9.081(3) Å, b = 10.631(5) Å, c = 11.549(6) Å, α = 111.492(4)°, β = 108.082(3)°, γ = 101.501(3)°, unit-cell volume V = 922.368 Å3, Z = 2, and space group P-1]. All measured lines were indexed, and no detectable impurity was observed.

The CeCo3Ni2 compound was synthesized by arc melting under argon atmosphere. High-quality powder X-ray diffraction (XRD) data of CeCo3Ni2 have been collected using a Rigaku SmartLab X-ray powder diffractometer. The refinement of the XRD pattern for the CeCo3Ni2 compound shows that the CeCo3Ni2 is a hexagonal structure, space group P6/mmm (No.191) with a = b = 4.9081(2) Å, c = 4.0034(2) Å, V = 83.52 Å3, Z = 1, and ρ x  = 8.6347 g cm−3. The Smith–Snyder FOM F 30 = 112.7(0.0089, 30) and the intensity ratio RIR = 0.48.

Preparation, analytical characterization, and crystal structures of N,N′-bis(thiophen-2-ylmethyl)ethane-1,2-diaminium hydrochloride (1) and of its gold derivative, N,N′-bis(thiophen-2-ylmethyl)ethane-1,2-diaminium tetrachloroaurate(III) (2) are reported. Compound (1) was obtained by reduction of the Schiff base N,N′-bis(thiophen-2-ylmethyl)ethane-1,2-diamine followed by HCl solution addition, whereas compound (2) was prepared reacting (1) with K[AuCl4] in aqueous solution. Compound (1) crystallizes in the orthorhombic system with space group Iba2 and cell parameters a = 29.856(1), b = 5.1372(2), and c = 10.1635(4) Å. Crystals of (2) belong to the monoclinic system with space group P21/c and cell parameters a = 11.0829(1), b = 9.5852(1), c = 11.6054(2) Å, and β = 75.49(1)°. Both structures contain diprotonated organic moieties, counterbalanced by hydrogen-bonded Cl−, or [AuCl4]− ions, in compounds (1) and (2), respectively.

Diketopyrrolopyrrole (DPP) is a pigment widely used in modern paints for industrial and artistic applications. Identification of this pigment in paint for art authentication and forensics has previously been accomplished with gas chromatography/mass spectrometry or Laser Raman. Three commercial artist's paints containing DPP were analyzed by x-ray diffraction (XRD). Alpha phase DPP was identified in two of the samples, barite extender the only crystalline component identified in the other sample. In conclusion, XRD analysis of paint samples can identify DPP, as can other organic analyses, but has the advantage of being non-destructive and also identifying the crystal structure. However, the fact that in one sample only extender could be identified does impose some limitations on the analysis of paints.