A comparative study of the medium-entropy perovskite PbSc1/4In1/4Nb1/4Ta1/4O3 (PSINT), synthesized by solidstate reaction, melt-solution (flux) crystallization, and the gel (sol-gel) route, was carried out. High-resolution synchrotron X-ray diffraction was employed to ensure methodological consistency across all samples. In the solid-state route, prolonged annealing at 800 degrees C for 100 h completely eliminates the residual pyrochlore impurity, yielding a single-phase cubic perovskite (Pm-3m, a = 4.09538(5) & Aring;). Flux growth produces two crystal types-perovskite and pyrochlore-with compositions deviating from the nominal due to cation segregation in the melt and partial B-site ordering. Superstructure reflections, corresponding to double and triple perovskite cell with a = 4.08661(14) & Aring;, are observed at the diffraction patterns. These reflections presumably originate from mixed 1:1 and 1:2 B-site cation ordering. The gel route proceeds through a transient pyrochlore intermediate that transforms into perovskite near 800 degrees C. Stabilization of the perovskite structure has been achieved due to an optimum fluorine concentration of about 0.04 at.% per mole of PSINT, whereas reduction of this value, caused by fluorine depletion at higher temperatures (900-1100 degrees C), leads to regeneration of the pyrochlore phase. The gel-derived PSINT shows the lowest atomic displacement parameters and the highest structural homogeneity. These results provide new information on the influence of synthesis environment on the characteristics of medium-entropy oxide perovskites.

The influence of the lanthanide cation type on the structure and catalytic properties of Ln zirconates (Ln = La – Lu) obtained by coprecipitation was studied. It was found that Ln (La, Pr – Lu) zirconates are single-phase and have a face-centered cubic structure of a defect fluorite (sp. gr. Fm3̅m (225)) with nonequivalent positions of the Ln^3+ and Zr^4+ cations. Ce zirconate was a mixture of cubic CeO_2 (sp. gr. Fm3̅m ) and tetragonal (Zr_0.9Ce_0.1)O_2 (sp. gr. P4_2/nmc (137)). A study of the local structure showed possible formation of nanodomains with pyrochlore ordering in the fluorite matrix for light Ln zirconates. For heavy Ln zirconates, the emergence of δ -phase nanodomains in the fluorite matrix is revealed. The use of Ln zirconates significantly reduces the onset temperature of propane conversion and increases its conversion degree. It was established that the ionic radius and electron structure of the Ln^3+ cation determine the acidity of the active sites and the energy characteristics (i.e., adsorption energy and differential heat of adsorption), which are the main factors determining the adsorption capacity and pathways of the propane conversion process. The use of light Ln zirconates with the maximum concentration of Lewis acid sites facilitates the propane dehydrogenation reaction to form propylene. A decrease in the number of Lewis acid sites and an increase in the number of Brønsted acid sites as the 4f shell of the Ln^3+ cations gets progressively filled facilitates the propane cracking reaction to form a mixture of methane, ethylene, and ethane. Hourly screening showed that an increase in the operation time beyond 7 h leads to a significant change in the catalytic properties due to coking of the active catalytic sites.

In the BiFe1-& khcy;(Ni,M)xO3 (M = Ti, Nb, W) systems, the solubility limits of the dopant cations were determined. It was shown that solid solutions are formed in the ranges of x = 0-0.15, 0-0.09, and 0-0.05 for Ti-, Nb-, and Wcontaining systems, respectively. The samples contain minor amounts of secondary mullite and sillenite phases, and, in some cases, traces of spinel. The actual composition of W-containing solid solutions deviates from the nominal one by a factor of 1.5-2.5 with respect to tungsten due to the volatility of its oxide. Within the homogeneity regions, all solid solutions exhibit rhombohedral distortion of the unit cell (space group R3c). In the Ti-containing system, an increase in x leads to a decrease in the unit cell parameter a, while in the Nb-and Wcontaining systems a increases, which is consistent with the ionic radii of the substituting and substituted cations. In all three systems, a slight increase in the rhombohedral angle alpha is observed with increasing x. All solid solutions distinctly exhibit nonzero piezoelectric (d33 up to 6-7 pC/N) and ferromagnetic properties at room temperature. The saturation magnetization (Ms) and remanent magnetization (Mr) increase with the sequence Ti-* Nb-* W for the same x, which may be attributed to the increasing Ni content per mole of solid solution-namely, 1/2x, 2/3x, and 3/4x for Ti-, Nb-, and W-containing systems, respectively. Based on the combination of their physical characteristics, the obtained materials can be classified as high-temperature multiferroics.

The influence of the lanthanide cation type and calcination temperature on the crystal, local, and electronic structures of both individual and high-entropy (HE) Ln chromates/chromites (Ln = La - Yb, and Y) prepared by a coprecipitation is studied by using synchrotron X-ray diffraction, X-ray absorption fine structure spectroscopy, Raman and Fourier transform infrared spectroscopies, scanning electron microscopy with energy-dispersive Xray spectroscopy, simultaneous thermal analysis, and inductively coupled plasma atomic emission spectroscopy. Calcination of X-ray amorphous precursors at 550 degrees C resulted in the formation of individual LnCrO4 chromates with monoclinic (sp. gr. P21/n for Ln = La) or tetragonal (sp. gr. I41/amd for Ln = Sm - Yb, Y) structure. The PrCrO4 and NdCrO4 samples were a mixture of monoclinic and tetragonal phases. The HE LnCrO4 chromates were characterized by tetragonal structure regardless of the Ln3+ cation type involved. A further increase in temperature >= 650 degrees C led to the formation of Ln chromites having the orthorhombic symmetry (sp. gr. Pnma for LaCrO3, sp. gr. Pbnm for individual Ln = Pr - Yb, Y, and HE chromites). For all synthesized LnCrO3 samples, the lattice parameters, unit cell volumes, Cr-O-Cr bond angles, average Ln-O distances diminish with decreasing the Ln3+ cation radius. On the contrary, the octahedral distortions within CrO6 units increase with decreasing the Ln3+ cation radius. An analysis of the electronic structure showed the presence of an oxidation state (3+) for both Ln and Cr cations in all synthesized precursors and Ln chromites, and Cr5+ for Ln chromates. The local environment of the Ln3+ and Cr3+ cations in HE Ln chromites is close to that of similar ions in individual compounds. The local environment of the La3+ cation in La-containing compounds differs significantly from that of Ln3+ cations in other Ln chromites (Ln = Nd, Sm, Eu, Gd, Dy, Ho, Yb, Y).

Single crystals in the PbSc1/2Ta1/2O3-PbIn1/2Nb1/2O3-PbIn1/2Ta1/2O3-PbSc1/2Nb1/2O3 compositional space were grown by the flux method with the aim of obtaining a medium-entropy perovskite of the nominal composition PbSc1/4In1/4Nb1/4Ta1/4O3. The synthesis yielded two distinct crystal phases: a perovskite-type phase with the composition PbSc0.34In0.16Nb0.12Ta0.38O3 and a pyrochlore-type phase with composition Pb2Sc0.25In0.2Nb0.5TaO6+delta. The crystal structure and elemental distribution were analyzed using scanning electron microscopy, energy-dispersive X-ray spectroscopy, and synchrotron-based powder X-ray diffraction. Dielectric measurements of the perovskite crystal were performed over a broad range of temperatures and frequencies. The results highlight the challenges associated with phase selectivity and cation incorporation during single-crystal growth in multicomponent oxide systems.

In this study, neptunium(V) double carbonate with magnesium was synthesized by the cation exchange synthesis method. Synchrotron powder X-ray diffraction, X-ray absorption spectroscopy, scanning electron microscopy, and energy-dispersive X-ray spectroscopy were employed for comprehensive solid-phase analysis. Solubility experiments were carried out in 0.01 M and 0.05 M NaClO4 solutions in the pH range 6-10 for the evaluation of the thermodynamic stability of solid magnesium-neptunium(V) double carbonate. Based on these data, the solubility product constant was estimated from the experimental data and established to be log Ksp = -15.9. During the solubility experiments, the initial Np(V)-Mg double carbonate underwent a phase transformation. This transformation led to the formation of a Np(V)-K double carbonate, caused by increasing potassium concentrations in solution primarily from the KCl-filled pH electrode. The solubility constant for the Np(V) double carbonate with potassium was determined to be log Ksp = -16.53 ± 0.10, which is significantly lower than that reported in the literature, confirming the high thermodynamic stability of the KNpO2CO3 solid phase.

Herein, we present a comprehensive study on the dissolution behaviour of two sodium–cerium(IV) phosphate phases synthesised hydrothermally from CeO2 nanoparticles: crystalline Na2Ce(PO4)2 and nanocrystalline NaCe2(PO4)3. For the first time, experimental dissolution data were obtained for both compounds over a wide pH range (1.5–10) under long-term equilibration. The crystalline phase undergoes pH-dependent transformation, including recrystallisation at a near-neutral pH and the formation of secondary CeO2 nanoparticles above pH 7. In contrast, the nanophase NaCe2(PO4)3 exhibits exceptional structural and chemical stability, showing no signs of recrystallisation, phase transformation, or CeO2 formation, even after extended ageing. The experimental results help refine the thermodynamic stability conditions for cerium phosphate and oxide phases, providing insights into the reversible transformation pathways between CeO2 and Ce(IV) phosphates as governed by pH.

This paper presents the studies of paste-inlay samples from decorative grooves on fragments of two vessels from the Early Iron Age burial mound Peschaniy IV (Remontnensky raion, Rostov oblast). Vessel 1 is similar in type to North Caucasian ceramics and vessel 2 is similar to the ceramics of the Crimean steppe. A comprehensive study included the following methods: scanning electron microscopy, energy-dispersive X‑ray microanalysis, X-ray diffraction analysis, infrared (IR) spectroscopy. The paste of North Caucasian vessel 1 was made of natrojarosite powder mixed with kaolinite and was fired at a temperature in the range of 450–600°C. The paste of vessel 2 was made of calcite. The morphological features of the calcareous platelets of coccolithophores found in the calcite confirm that the origin of the raw material of the paste is the territory of Crimea.

Comprehensive studies of three Attic plastic vessels dated to the 4th century BC from the State Historical Museum collection have been performed. The use of X-ray tomography (XRT), large-scale X-ray fluorescence (XRF) mapping, energy-dispersive X-ray microanalysis (EDX) under scanning electron microscopy (SEM), and synchrotron X-ray diffraction (XRD-SR) analysis made it possible to study in detail their state of preservation (including restoration traces) and the manufacturing technology, as well as to identify the pigments used in painting the surface. Based on the pigment residues, identified visually and on XRF maps, a reconstruction of the polychrome painting of the vessels was proposed. Because of the poor state of preservation of the coating on the surface of two vessels, the reconstruction of their possible polychrome painting was performed based on a comparison with known analogues.

A new medium-entropy perovskite ceramics, PbSc1/4Fe1/4Nb1/4Ta1/4O3 (PSFNT), was synthesized via solid-state reaction for the first time and its structural, microstructural, and dielectric properties were systematically investigated. X-ray diffraction and Rietveld refinement revealed a cubic Pm (3) over barm phase at room temperature, with a coexisting tripled superstructure, indicative of a rare cationic ordering in the B-site sublattice. Temperature-dependent synchrotron diffraction identified a phase transition from cubic to rhombohedral symmetry below 280 K, which is confirmed by the sharp drop of the dielectric constant at this temperature and appearance of thermal hysteresis. The observed coexistence of entropy-driven disorder with partial long-range 1:2 cation ordering highlights the complex structural physics of PSFNT. This unexpected result suggests new, previously unknown aspects of structural organization in multicationic perovskites and raises questions about their entropy-driven stabilization, requiring further analysis of oxygen and lead sublattice vacancies and defects that may accompany such ordering and contribute to entropy stabilization.

Fluorescence labeling of cells is a versatile tool used to study cell behavior, which is of significant importance in biomedical sciences. Fluorescent photoconvertible markers based on polymer microcapsules have been recently considered as efficient and perspective ones for long-term tracking of individual cells. However, the dependence of photoconversion conditions on the polymeric capsule structure is still not sufficiently clear. Here, we have studied the structural and spectral properties of fluorescent photoconvertible polymeric microcapsules doped with Rhodamine B and irradiated using a pulsed laser in various regimes, and shown the dependence between the photoconversion degree and laser irradiation intensity. The effect of microcapsule composition on the photoconversion process was studied by monitoring structural changes in the initial and photoconverted microcapsules using X-ray diffraction analysis with synchrotron radiation source, and Fourier transform infrared, Raman and fluorescence spectroscopy. We demonstrated good biocompatibility of free-administered initial and photoconverted microcapsules through long-term monitoring of the RAW 264.7 monocyte/macrophage cells with unchanged viability. These data open new perspectives for using the developed markers as safe and precise cell labels with switchable fluorescent properties.

The crystal structure of palbociclib (C24H29N7O2) used as a medication for the treatment of breast cancer has been solved and refined using synchrotron radiation after density functional theory optimization. Palbociclib crystallizes in the monoclinic system (space group P21/c, #14) at room temperature with crystal parameters: a = 11.3133(2), b = 5.62626(9), c = 35.9299(9) & Aring;, beta = 101.5071(12), V = 2241.03(8) & Aring;3, and Z = 4. The crystal structure contains infinite N-H & ctdot;N bonded layers. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File (TM) (PDF (R)).

A monoclinic C form of rilpivirine hydrochloride, (N6H19C22)Cl, has been obtained and characterized using solid-state 15N, 13C, and 35Cl NMR spectroscopy and multitemperature synchrotron X-ray powder diffraction. The title compound crystallizes in the monoclinic system (space group C2/c, #15) at both room (295.0(2) K) and low (100.0(2) K) temperatures. At room temperature, the following parameters are a = 19.43051(3), b = 13.09431(14), c = 17.10254(18) Å, β = 109.3937(7), V = 4104.48(9) Å3, and Z = 8. The folded molecular conformation of the cation is similar with that of free base rilpivirine with the exception of cyanovinyl group disposition. The anion links cations to infinite chains parallel to the crystallographic c axis using N–H⋯Cl bonds where both amino groups and the protonated pyrimidine ring take part in the H-bonding. The powder patterns have been submitted to the ICDD for inclusion in the Powder Diffraction File™ (PDF®).

This article presents the results of comprehensive studies of three Attic figured vessels from the 4th century BC, drawn from the State Historical Museum collection. The application of X-ray tomography, large-scale XRF mapping, energy-dispersive X-ray microanalysis under SEM and synchrotron XRD analysis enabled a comprehensive examination of the vessels' state of preservation, including the identification of restoration traces and the delineation of the manufacturing technology employed. Additionally, the analysis facilitated the identification of the pigments utilized in the surface painting. A reconstruction of the polychrome painting of the vessels was proposed based on the pigment residues identified both visually and on XRF maps. Given the poor state of preservation of the coating on the surface of two vessels, a reconstruction of their possible polychrome painting was performed based on a comparison with known analogues.

The synthesis and detailed study of six series of high-entropy complex oxides containing lanthanides (Ln) and transition metals with the general formula Ln(2)M(2)O(7) (Ln = La-Yb, and Y; M = Ti, Zr, and Ce) with the number of different Ln cations not less than six in each case are reported. The influence of synthesis conditions (types of the Ln(3+) and M4+ cations, calcination temperature) used in the synthesis via either coprecipitation or sol-gel method on the crystal and local structures of target materials is comprehensively surveyed. The studies were carried out using a combination of long- (s-XRD), medium- (Raman, FT-IR, SEM-EDS) and short-range (XAFS) sensitive techniques, as well as AES-ICP and STA. It was established that the ratio of the cation radii gamma = (r) over bar (3+)(Ln)/(r) over bar (4+)(M) is the main factor that determines the type of initially formed crystal structure. In the boundary region (gamma similar to 1.42-1.47), the average radius of lanthanide cation ((r) over bar (3+)(Ln)), along with the (r) over bar (3+)(Ln)/(r) over bar (4+)(M) ratio, also plays a significant role in the type of the resulting crystal structure of the high-entropy lanthanide complex oxides. The presence of inhomogeneity in the distribution of elements in precursors significantly affects the phase composition of the resulting high-entropy oxides. An increase in the calcination temperature promotes not only the occurrence of subsequent phase transitions, but also an increase in the single-phase nature of the resulting high-entropy complex rare-earth oxides. At the same time, the cations included in the composition retain some independence, despite the fact that they occupy one crystallographic position in the resulting crystal structure.

The existence regions of the Y2–xMgxFeTaO7–δ (x = 0–0.15), Y2–xMgxFe1–x/2Ta1+x/2O7–δ (x = 0–0.15), Y2Fe1–xMgxTaO7–δ (x = 0–0.3), and Y2Fe1–3/2xMgxTa1+x/2O7–δ (x = 0–0.3) solid solutions were estimated. It was found that, regardless of the composition, the entry of Mg2+ into the crystal lattice of Y2FeTaO7 causes a similar distortion of the structure (space group R 3̅ → space group P3121). Based on XANES and Mössbauer spectroscopy data, it was suggested that Mg2+ ions occupied the eight-coordinated sites in the crystal lattice of solid solutions, displacing iron ions, while vacant yttrium sites in Y2–xMgxFeTaO7–δ and Y2–xMgxFe1–x/2Ta1+x/2O7–δ are occupied by tantalum ions. The XANES method confirmed the existence of Fe4+ ions in the Y2FeTaO7 solid solutions along with Fe3+. The simultaneous presence of the Ta4+ and Ta5+ ions ensures the electroneutrality of there crystal lattices. Herewith, the entry of Mg2+ does not lead to an increase in the Fe4+ concentration.

This article is about palladium-based membrane alloys with promising characteristics. Lead concentration in samples is 5 and 20 wt%. The samples are prepared from high purity metals (99.95 wt%). The samples are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. Effect of the concentration of alloying components on the Debye temperature and on the mean-square displacements of atoms is determined. Influence of defects of the first class (point defect - vacancy pairs, pores, dislocation loops of small radius) found to be dominant in alloys.

The sublimation thermodynamics of the neuroprotective and potential anticancer drug riluzole was studied by the transpiration method, and the obtained data were used in a virtual screening based on cocrystallization Gibbs free energy estimation. The method was successfully validated against 19 reported riluzole crystal forms and correctly predicted the salt formation with dihydroxybenzoic acid isomers. Variation of experimental conditions led to the isolation of the novel polymorphic modification of riluzolium 2,6-dihydroxybenzoate and the new salt cocrystal of riluzole with 2,3-dihydroxybenzoic acid with an unexpected (3:4) stoichiometry. The hydrogen bond topology was found to be identical in polymorphic forms of riluzolium 2,6-dihydroxybenzoate, and the packing difference is caused by the variable mutual orientation of hydrogen-bonded ribbons. The metastable Form 1 was found to undergo an irreversible exothermic phase transition upon heating, indicating a monotropic relationship between the polymorphs. In serial batch crystallization experiments, Form 1 was found to nucleate at a lower supersaturation level with subsequent transformation to Form 2. Thermodynamic functions of salt formation for riluzolium 2,6-dihydroxybenzoate Form 2 from parent compounds have confirmed that the process is enthalpy-driven. At pH > 4.4, the solubility of Form 2 is found to be higher than that of pure riluzole.

The crystal structure of nilotinib hydrochloride monohydrate, being an active pharmaceutical substance of the drug Tasigna for chronic myeloid leukemia, is determined by powder X-ray diffraction (XRD) using a synchrotron radiation source of the National Research Center “Kurchatov Institute”. The molecular conformation of the cation in the crystal differs from that in the initial nilotinib molecule and its solvates due to the rotation of substituents about single C–N, C–O, and C–C bonds. In the crystal, the nilotinib molecule is protonated at the nitrogen atom of the imidazolium heterocycle and involved in the N–H…N, N–H…O, and N–H…Cl hydrogen bonds with another cation, water molecule, and anion respectively. The resulting structure is determined with high accuracy. Errors in bond lengths are only slightly worse than those for the structures determined from single crystal XRD data. In addition, one of the best values of the half uncertainty window (HUW) is achieved in the refinement. The importance of this parameter is considered in the article. The structure agrees with the solid-state NMR data. The comparison of the results with the solution NMR spectroscopy data reveals noticeable changes in the nilotinib molecular structure during crystallization.