The crystal structure of butenafine hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Butenafine hydrochloride crystallizes in space group P21 (#4) with a = 13.94807(5), b = 9.10722(2), c = 16.46676(6) Å, β = 93.9663(5)°, V = 2086.733(8) Å3, and Z = 4. Butenafine hydrochloride occurs as a racemic co-crystal of R and S enantiomers of the cation. The crystal structure is characterized by parallel stacks of aromatic rings along the b-axis. Each cation forms a strong discrete N–H⋯Cl hydrogen bond. The chloride anions also act as acceptors in several C–H⋯Cl hydrogen bonds from methylene, methyl, and aromatic groups. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The electrochemical behaviour of a number of Pb-based anode alloys, under simulated electrowinning conditions, in a 1.6 M H2SO4 electrolyte at 45 °C was studied. Namely, the evolution of PbO2 and PbSO4 surface layers was investigated by quantitative in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis (QPA). In the context of seeking new anode alloys, this research shows that the industry standard Pb-0.08Ca-1.52Sn (wt%) anode, when exposed to a galvanostatic current and intermittent power interruptions, exhibited poor electrochemical performance relative to select custom Pb-based binary alloys; Pb–0.73Mg, Pb–5.05Ag, Pb–0.07Rh, and Pb–1.4Zn (wt%). The in situ S-XRD measurements and subsequent QPA indicated that this was linked to a lower proportion of β-PbO2, relative to PbSO4, on the Pb-0.08Ca-1.52Sn alloy at all stages of the electrochemical cycling. The best performing alloy, in terms of minimisation of overpotential during normal electrowinning operation and minimising the deleterious effects of repeated power interruptions – both of which are significant factors in energy consumption – was determined to be Pb–0.07Rh.

The crystal structure of indacaterol hydrogen maleate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Indacaterol hydrogen maleate crystallizes in space group P-1 (#24) with a = 8.86616(9), b = 9.75866(21), c = 16.67848(36) Å, α = 102.6301(10), β = 94.1736(6), γ = 113.2644(2)°, V = 1273.095(7) Å3, and Z = 2 at 295 K. The crystal structure consists of layers of cations and anions parallel to the ab-plane. Traditional N–H⋯O and O–H⋯O hydrogen bonds link the cations and anions into chains along the a-axis. There is a strong intramolecular charge-assisted O–H⋯O hydrogen bond in the non-planar hydrogen maleate anion. There are also two C–H⋯O hydrogen bonds between the anion and cation. The cation makes a strong N–H⋯O hydrogen bond to the anion, but also acts as a hydrogen bond donor to an aromatic C in another cation. The amino group makes bifurcated N–H⋯O hydrogen bonds, one intramolecular and the other intermolecular. The hydroxyl group acts as a donor to another cation. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

Eu3+-doped SmBa3B9O18 luminescent materials were synthesized by high temperature solid state reactions. The structure and photoluminescence properties of Sm(1−x)EuxBa3B9O18 (x = 0.2, 0.4, and 0.6) were investigated by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and photoluminescence spectra. The results show that doping of Eu3+ ions does not change the structure of SmBa3B9O18. The luminescence is mainly the characteristic Eu3+ ion luminescence. No concentration quenching processes occur with the increment of Eu3+ concentration. The work implies that SmBa3B9O18 is a potential host material and europium-doped SmBa3B9O18 may find application in display and optical devices.

In this paper, some results of neutron diffraction properties of the dispersive double-crystal Si(111) + Si(311) and Si(111) + Si(400) monochromator settings containing two bent perfect crystals but with the second one – analyzer in the strongly asymmetric diffraction geometry, are presented. For the sake of possible applications, both double crystal settings were tested in the orientation of the second crystal for the output beam compression geometry. Powder diffraction test was carried out on a α-Fe(211) pin of the diameter of 2 mm. Contrary to the Si(111) + Si(400) setting, an excellent resolution represented by full width at half maximum in the (Δd/d)-scale was obtained for the Si(111) + Si(311) double crystal monochromator in the parallel as well as in the antiparallel diffraction geometry.

We have grown intermetallic ErPd2Si2 single crystals employing laser diodes with the floating-zone method. The temperature dependence of the unit-cell parameters was determined using synchrotron and in-house X-ray powder diffraction measurements from 20 to 500 K. The diffraction patterns fit well with the tetragonal I4/mmm space group (No. 139) with two chemical formulae within the unit cell. The synchrotron powder diffraction study shows that the refined unit-cell parameters are a = 4.10320(2) Å, c = 9.88393(5) Å at 298 K and a = 4.11737(2) Å, c = 9.88143(5) Å at 500 K, resulting in the unit-cell volume V = 166.408(1) Å3 (298 K) and 167.517(2) Å3 (500 K). In the whole studied temperature range, no structural phase transition was observed. Upon cooling, the unit-cell parameters a and c are shortened and elongated, respectively.

An experimental X-ray powder diffraction pattern was produced and analyzed for imipenem monohydrate, an antimicrobial pharmaceutical agent. Although there are no experimental powder patterns in the ICDD PDF-4/Organics Database, there is one powder pattern calculated with single-crystal X-ray diffraction data from the Cambridge Structural Database. Here, we report the refined experimental powder diffraction data for imipenem monohydrate. These data for imipenem monohydrate are consistent with an orthorhombic crystal system having reduced unit-cell parameters of a = 8.2534(3) Å, b = 11.1293(4) Å, and c = 15.4609(6) Å. The resulting unit-cell volume, 1420.15(15) Å3, indicates four formula units per unit cell. Observed peaks are consistent with the P212121 space group.

The crystal structure of oxybutynin hydrochloride hemihydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Oxybutynin hydrochloride hemihydrate crystallizes in space group I2/a (#15) with a = 14.57266(8), b = 8.18550(6), c = 37.16842(26) Å, β = 91.8708(4)°, V = 4421.25(7) Å3, and Z = 8. The compound exhibits X-ray-induced photoreduction of the triple bond. Prominent in the layered crystal structure is the N–H⋅⋅⋅Cl hydrogen bond between the cation and anion, as well as O–H⋅⋅⋅Cl hydrogen bonds from the water molecule and hydroxyl group of the oxybutynin cation. C–H⋅⋅⋅Cl hydrogen bonds also contribute to the crystal energy, and help determine the conformation of the cation. The powder pattern is included in the Powder Diffraction File™ as entry 00-068-1305.

Samples of the superconducting compound (Hg,Re)–1223 of nominal composition Hg0.82Re0.18Ba2Ca2Cu3O8+δ and different oxygen contents were studied using X-ray absorption and diffraction techniques. In the synthesis process, treatments under different ratio oxygen/argon gas mixtures of 5%, 10%, and 15% O2 resulted in samples named as Sample A, Sample B, and Sample C, respectively. It was determined by using the XANES technique that in these compounds the Re cation has valence +7. The study by EXAFS determined that the octahedral coordination is distorted and the distances of Re–O bonds are of the order of 1.85 A˚ for equatorial oxygen and 2.10 A˚ for the apical ones. The Rietveld refinement of X-ray powder diffraction data revealed that the studied samples presented segregation of two superconducting phases with space group P4/mmm and distinct lattice parameters, also confirmed by anomalous X-ray scattering. The main phase was associated to the phase (Hg,Re)–1223 with higher oxygen content and the secondary superconducting phase was associated with the undoped Hg–1223 phase. Measurements of ac magnetic susceptibility showed that the sample treated under 10% O2 atmosphere presented the best superconducting properties.

Calcium monoaluminate is the main phase in calcium aluminate cements and participates in the hydration, forming calcium aluminate hydrates. The amount of incorporation of foreign ions influences the hydration behaviour. Strontium aluminate is an important phase in producing phosphorescent materials when doped with rare-earth elements (REE) such as Eu, Dy, and La. These monoaluminates occur in different forms. Monocalcium aluminate forms a monoclinic and an orthorhombic modification, whereas monostrontium aluminate forms a monoclinic low-temperature and a hexagonal high-temperature form. Monoclinic calcium monoaluminate and monoclinic strontium aluminate form a partial solid-solution series. The hydration behaviour of different solid solutions was also investigated using calorimetry. The newly formed strontium aluminate hydrates could be identified while similar strontium aluminate hydrates are formed. Solid solutions of strontium- and calcium-aluminate hydrates will be investigated.

Florencite-(Nd) [(Nd,Ce)Al3(PO4)2(OH)6], was first described by Milton and Bastron (1971) from fracture surfaces in weathered cherts of the Franciscan Complex, south of Sausalito in Marin County, California. Florencite-(Nd) occurred there as a moderate-brown pulverulent earthy material; individual crystals were not discernible under microscopic examination. A semi-quantitative spectrographic analysis showed the presence of Nd (3 wt. %) and Ce (0.5 wt. %). No powder data for florencite-(Nd) exists in the current powder diffraction file.

Ferrous nitroprusside can be obtained in three structural modifications: two different unstable phases, monoclinic trihydrate and cubic pentahydrate, and the stable one, an orthorhombic dihydrate. This contribution reports the crystal structure of the last one. Cell parameters are: a=13.9734 (2), b=7.4274 (1), and c=10.4697 (1) Å; with four formula units per cell (Z=4). The crystal structure was refined from the corresponding XRD powder pattern using the Rietveld method. Final agreement factors of the refinement process were Rwp=8.46, Rp=6.54, and S=1.38. The crystal structure is formed by a tridimensional assembling of the [Fe(CN)5NO] molecular block through iron atoms bounded at the N end of the CN ligands. The NO group remains unlinked at its O atom. The octahedral coordination of the assembling metal is completed with a coordinated water molecule which stabilizes a second water through a strong hydrogen bond interaction. The tridimensional structure appears as piled up rippled sheets leading to a system of interconnected small cavities which increase their available volume on the material dehydration. This complex loses its crystal water below 100 °C and then remains stable up to above 160 °C when the decomposition process begins with the loss of the NO ligand.

This study attempted to quantify the interstratificational broadening of the randomly interstratified illite/smectite (random I∕S) basal reflection and to evaluate the percentage of the interstratified illite layers (%I) from the result. The interstratificational broadening was quantified using the distributional discrepancy (D) defined as D=[∑t∣ft(obs)−ft(ref)∣]∕2, where ft(obs) is the frequency of a crystallite containing thickness, t (the number of layers), measured from a basal reflection broadened by interstratifications, and ft(ref) is the frequency for a basal reflection with no interstratificational broadening. The basal reflections at 5.2° 2θ under glycolation and 8.84° 2θ under thermal dehydration provided the ft(obs) and ft(ref) of random I∕S. The linear relation, D=2.17%I+2.49(0⩽%I⩽30), was obtained from simulations for SWy-2 (Wyoming, USA).

A new Tutton’s salt Tl2[Mn(OH2)6](SO4)2 was grown from aqueous solutions and characterized by chemical analysis and X-ray powder diffraction. It was found to be monoclinic, space group P21/a, a=0.93276(6), b=1.25735(8), c=0.62407(4) nm, and β=106.310(3)°. It is unstable in warm air and dissolves incongruently. A comparison of unit cell volumes for all 37 Tutton sulfate phases found in ICDD’s PDF-2 database (86 entries) reveals a reasonable correlation with Shannon and Prewitt’s ionic radii [Acta Crystallogr. 25, 925–926 (1969)] and several deviations, most of them seeming to be erroneous entries.

At the Institute of Microstructure Technology (IMT) of the Karlsruhe Institute of Technology (KIT), a new type of refractive X-ray optics has been developed. Owing to its comparably easy fabrication method and the large aperture, the so-called Rolled X-ray Prism Lenses (RXPL) have the potential to be used with X-ray tubes in an industrial environment as a low-cost alternative to existing optics. The lens itself is built out of a micro-structured foil which is cut into shape and rolled around a winding core to form a refracting element for X-rays. The resulting refractive structure can be used as illumination optics. Diffractometry experiments with an NIST 1976a sample were performed and showed up to an 18-fold enhanced integrated intensity compared to that acquired with a steel tube collimator.

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.