The crystal structure of trametinib dimethyl sulfoxide has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Trametinib dimethyl sulfoxide crystallizes in space group P-1 (#2) with a = 10.7533(4), b = 12.6056(5), c = 12.8147(6) Å, α = 61.2830(8), β = 69.9023(11), γ = 77.8038(10)°, V = 1,428.40(3) Å3, and Z = 2 at 298 K. The crystal structure contains hydrogen-bonded trametinib and dimethyl sulfoxide (DMSO) molecules. These are arranged into layers parallel to the (101) plane. There are two strong classical hydrogen bonds in the structure. One links the trametinib and DMSO molecules. Another is an intramolecular hydrogen bond. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File™.

The crystal structure of niraparib tosylate monohydrate Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Niraparib tosylate monohydrate Form I crystallizes in space group P-1 (#2) with a = 7.22060(7), b = 12.76475(20), c = 13.37488(16) Å, α = 88.7536(18), β = 88.0774(10), γ = 82.2609(6)°, V = 1,220.650(16) Å3, and Z = 2 at 298 K. The crystal structure consists of alternating double layers of cations and anions (including the water molecules) parallel to the ab-plane. Hydrogen bonds are prominent in the crystal structure. The water molecule acts as a donor to two different O atoms of the tosylate anion and as an acceptor from one of the H of the protonated piperidine ring. The other piperidyl N–H acts as a donor to the carbonyl group of another cation. Surprisingly, there are no cation–anion N–H···O hydrogen bonds. The amide group forms as a N–H···O hydrogen bond to the anion and an intramolecular N–H···N hydrogen bond to the indazole ring. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File™.

The crystal structure of aprocitentan Form A has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Aprocitentan Form A crystallizes in space group P-1 (#2) with a = 11.7381(11), b = 10.6771(12), c = 9.6624(5) Å, α = 110.4365(13), β = 92.3143(13), γ = 113.513 (2)°, V = 1,017.53(5) Å3, and Z = 2 at 298 K. The crystal structure consists of layers of aprocitentan molecules, approximately along the 1,-7,7 plane. N–H···N hydrogen bonds link the molecules within these layers. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File™.

Using a variety of analytical tools, the mineralogy of the sands and dunes at several public beaches along the coastline near Marshfield, Massachusetts was examined. X-ray powder diffraction analyses combining Rietveld methods, orientation analyses, and clustering techniques were primarily used for mineral identification. The results of the analyses point to the underlying geology, a history of glaciation, and erosion of the underlying bedrock and rocks. The sands could be termed “continental” sands since they reflect the composition of the underlying bedrock. The averaged bulk (>1%) mineral composition of the Marshfield beaches and coastal dunes is very similar and similar to other reported mineralogical analyses of Massachusetts and many New England beaches. Quartz and the alkali feldspars, microcline, and albite, comprise ~90% of dune and beach samples. These are usually followed by muscovite and clinochlore, and varieties of amphibole. Higher albite concentrations and a few characteristic minor phases (i.e., epidote) differentiate this sand from others in the region. When analyzing rocks and rock berms present on all beaches, the mineralogy is much more complex and reflects historic glacial till coverage and glacial retreat, combined with modern erosion and storm impact

The Materials Science & Technology 2024 Conference & Exhibition took place in the David L. Lawrence Convention Center in Pittsburgh, Pennsylvania from October 6 to 9, 2024. Pittsburgh is known as “The City of Bridges” and “The Steel City” for its many bridges and former steel manufacturing base. The characteristic shape of downtown is a triangular region formed by the confluence of the Monongahela River and the Allegheny River, which merge to produce the Ohio River. In 2007, Pittsburgh was named “America’s Most Livable City” by Places Rated Almanac. This year, many conference attendees were fortunate to have hotel rooms with a spectacular view of the rivers and bridges.

In the present study, the High Score Plus software (Malvern Panalytical, 2014), combined with the PDF-4+ database release 2023 (ICDD, 2018), was used to perform phase identification from all the powder XRD data sets of 0.5 g by weight of the crystalline deposits from various units of refineries and gas plants. Subsequently, the Rietveld method with the generalized spherical harmonic description for preferred orientation correction [Von Dreele (1997). Journal of Applied Crystallography 30: 517–25; Sitepu (2002). Journal of Applied Crystallography 35: 274–77; Sitepu et al., (2005). Journal of Applied Crystallography 38: 158–67; Sitepu (2009). Powder Diffraction 24: 315–26] were used to determine texture and crystal structure refinement of scale deposits (calcite – CaCO3) from the boiler equipment at a gas plant and quantitative phase analysis of (i) iron oxide corrosion products from the boiler tube, (ii) synthetic mixtures of 87.0 wt% by weight of barite (BaSO4), 10.0 wt% by weight of hematite (Fe2O3), and 3.0 wt% by weight of quartz (SiO2), (iii) iron oxide corrosion products from the affected equipment parts in a refinery, (iv) vanadium oxide (V2O5), sodium vanadium oxide (NaV2O5), sodium vanadium sulfate hydrate (Na2V(SO4)2⋅H2O), and mackinawite (FeS) compounds found in the ash deposits from an external surface of the boiler tubes in a refinery, and (v) iron sulfide corrosion products found at the affected equipment in the sulfur recovery unit. The results revealed that the phase identification of powder XRD data is an excellent tool to determine the nature, source, and formation mechanism of crystalline deposits – part of the scale and corrosion products formed by the processes in the various units of refineries and gas plants. The quantitative Rietveld analysis results serve to guide the engineers at the refinery and gas plants to overcome the problems by applying the right procedures. For example, for iron oxide corrosion products, at a high temperature, magnetite will coat the iron/steel to prevent oxygen reaching the underlying metal. At low temperature, lepidocrocite formed and with time it transformed into the most stable goethite. Akaganeite is formed in marine environments. Additionally, for iron sulfide corrosion products, pyrophoric iron sulfide (pyrrhotite – FeS) results from the corrosive action of sulfur compounds (H2S) and moisture on the iron (steel). Additionally, for the crystalline ash samples from an external surface of the boiler tubes in a refinery, if sodium and vanadium compounds appear, the fuel oil is poor. For the boiler crystalline deposits, if a hematite phase appears, it means that the boiler feed water contains dissolved oxygen; and if the metallic copper appears among the crystalline deposits, it indicates erosion in the boiler tubes, and therefore, special precaution is required to prevent the plating out of copper during cleaning operations. Finally, for crystalline deposits from the steam drum equipment at the sulfur recovery unit, if magnetite has a high quantity, it indicates the presence of dissolved oxygen in the boiler feed water.

The crystal structure of sparsentan has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Sparsentan crystallizes in space group P-1 (#2) with a = 11.4214(8), b = 12.0045(9), c = 14.1245(12) Å, α = 97.6230(22), β = 112.4353(16), γ = 110.2502(11)°, V = 1599.20(6) Å3, and Z = 2 at 298 K. The crystal structure consists of an isotropic packing of dimers of sparsentan molecules, linked by N–H···O=S hydrogen bonds. Several intra- and intermolecular C–H···O and C–H···N hydrogen bonds also link the molecules. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of flumethasone has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Flumethasone crystallizes in space group P21 (#4) with a = 6.46741(5), b = 24.91607(20), c = 12.23875(11) Å, β = 90.9512(6)°, V = 1971.91(4) Å3, and Z = 4 at 298 K. The crystal structure consists of O–H⋯O hydrogen-bonded double layers of flumethasone molecules parallel to the ac-plane. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

Sample transparency aberration in Bragg–Brentano geometry affected by interference with opaque and translucent sample holders has been formulated. The formulation for an opaque sample holder should be classified to 5 cases, depending on the apparent diffraction angle, beam width, specimen width, and specimen thickness. The cumulants of the aberration function for a translucent sample holder with an arbitrary linear attenuation coefficient can numerically be evaluated by a Gauss–Legendre quadrature. The use of a function defined by the convolution of truncated exponential and rectangular functions has been tested as the model for the aberration function. A double deconvolutional treatment (DCT) designed to cancel the effects of the first and third order cumulants of the aberration function has been applied to the XRD data of Si standard powder, NIST SRM640d. The diffraction peak profile in the data treated by the DCT method certainly shows improved symmetry. The main features of the symmetrized peak profile in the DCT data have been simulated by instrumental and specimen parameters. It is suggested that the current analytical method could be utilized for texture analysis, if the manufacturer of an XRD instrument should supply a more accurate information about the instrument.

The room-temperature X-ray powder diffraction data for bosentan monohydrate, an API used in the treatment of pulmonary arterial hypertension, is presented. Bosentan monohydrate is monoclinic, P21/c (No. 14), with unit cell parameters a = 12.4520(7) Å, b = 15.110(1) Å, c = 15.0849(9) Å, β = 95.119(5)°, V = 2827.0(3) Å3, Z = 4. All the diffraction maxima recorded were indexed and are consistent with the P21/c space group. The crystal structure of this material corresponds to the phase associated with Cambridge Structural Database entry NEQHEY, which was determined at 123 K. The successful Rietveld refinement, carried out with TOPAS-Academic, showed the single-phase nature of the material and the good quality of the data. A comprehensive analysis of intra- and intermolecular interactions corroborates that the structure is dominated by extensive hydrogen bonding, accompanied by C▬H⋯π and π⋯π interactions. Hirshfeld surface analysis and fingerprint plots indicate that the most important interactions are H⋯H and O⋯H/H⋯O in bosentan and the water molecule and C⋯H/H⋯C interactions in bosentan.

The crystal structure of diroximel fumarate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Diroximel fumarate crystallizes in space group P-1 (#2) with a = 6.12496(15), b = 8.16516(18), c = 12.7375(6) Å, α = 85.8174(21), β = 81.1434(12), γ = 71.1303(3)°, V = 595.414(23) Å3, and Z = 2 at 298 K. The crystal structure consists of interleaved double layers of hook-shaped molecules parallel to the ab-plane. The side chains form the inner portion of the layers, and the rings comprise the outer surfaces. There are no classical hydrogen bonds in the structure, but 9 C▬H⋯O hydrogen bonds contribute to the crystal energy. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).