X-ray Powder Diffraction Patterns Research Articles

Controlling the Orientation-Dependent Second Harmonic Generation in Hybrid Germanium Perovskite Crystals.

Manipulating the crystal orientation plays a crucial role in the conversion efficiency during second harmonic generation (SHG). Here, we provide a new strategy in controlling the surface-dependent anisotropic SHG with the precise design of (101) and (20) MAGeI3 facets. Based on the SHG measurement, the (101) MAGeI3 single crystal exhibits larger SHG (1.3 × (20) MAGeI3). Kelvin probe force microscopy imaging shows a smaller work function for the (101) MAGeI3 compared with the (20), which indirectly demonstrates the stronger intrinsic polarization on the (101) surface. X-ray photoelectron spectroscopy confirms the band bending within the (101) facet. Temperature-dependent steady-state and time-resolved photoluminescence spectroscopy show shorter lifetime and wider emission band in the (101) MAGeI3 single crystal, revealing the higher defect states. Additionally, powder X-ray diffraction patterns show the (101) MAGeI3 possesses larger in-plane polar units [GeI3]- density, which could directly enhance the spontaneous polarization in the (101) facet. Density functional theory (DFT) calculation further demonstrates the higher intrinsic polarization in the (101) facet compared with the (20) facet, and the larger built-in electric field in the (101) facet facilitates surface vacancy defect accumulation. Our work provides a new angle in tuning and optimizing hybrid perovskite-based nonlinear optical materials.

Preparation and Properties of a High-Entropy Wolframite-Type Antiferromagnet, (Mn0.2Co0.2Ni0.2Cu0.2Cd0.2)WO4.

The homogeneous high-entropy wolframite-type solid solution (Mn1/5Co1/5Ni1/5Cu1/5Cd1/5)WO4 was prepared by solid-state reaction at 1000 °C. Elongated "crystals" were grown from the Na2WO4 flux, but their strongly broadened powder X-ray diffraction patterns indicated partial dissolution. Nevertheless, successive annealing of the homogeneous solid solution for 3-4 h at 800, 700, and 600 °C did not bring any sign of dissolution. Thus, the material is kinetically stable at low temperatures although thermodynamically unstable. The long-range antiferromagnetic order was established at TN ∼ 24.8 K. Based on magnetization and specific heat measurements, a magnetic phase diagram was built, demonstrating the presence of an additional field-induced phase. In contrast to the parent MnWO4, no dielectric anomaly has been found down to 2 K.

Crystal structures of two new high-pressure oxynitrides with composition SnGe4N4O4, from single-crystal electron diffraction.

SnGe4N4O4 was synthesized at high pressure (16 and 20 GPa) and high temperature (1200 and 1500°C) in a large-volume press. Powder X-ray diffraction experiments using synchrotron radiation indicate that the derived samples are mixtures of known and unknown phases. However, the powder X-ray diffraction patterns are not sufficient for structural characterization. Transmission electron microscopy studies reveal crystals of several hundreds of nanometres in size with different chemical composition. Among them, crystals of a previously unknown phase with stoichiometry SnGe4N4O4 were detected and investigated using automated diffraction tomography (ADT), a three-dimensional electron diffraction method. Via ADT, the crystal structure could be determined from single nanocrystals in space group P63mc, exhibiting a nolanite-type structure. This was confirmed by density functional theory calculations and atomic resolution scanning transmission electron microscopy images. In one of the syntheses runs a rhombohedral 6R polytype of SnGe4N4O4 could be found together with the nolanite-type SnGe4N4O4. The structure of this polymorph was solved as well using ADT.

Preparation, characterization and photocatalytic studies of defect pyrochlore, KMn0·33Te1·67O6 and its composite with g-C3N4

Skeletal materials belonging to the defect pyrochlore family have been the subject of considerable interest due to their remarkable properties. In this work, a highly efficient, stable and visible light active composite photocatalytic system consisting of defect pyrochlore of composition KMn0·33Te1·67O6 (KMnTeO) and g-C3N4 (g-CN) has been successfully prepared by simple physical mixing of pre-prepared KMnTeO and g-CN components synthesized in solid state and thermal treatment of low-cost melamine, respectively. Structural, morphological and optical properties of as-prepared catalysts were deduced from powder X-ray Diffraction (XRD), Fourier Transform Infrared (FT-IR), Raman, Field Emission Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy (FESEM-EDX), Transmission Electron Microscopy-High Resolution Transmission Electron Microscopy (TEM-HRTEM), Ultraviolet–Visible Diffuse Reflectance Spectroscopy (UV–Vis DRS), X-ray Photoelectron Spectroscopy (XPS) and Photoluminescence (PL) measurements. The lattice parameter “a” of parent KMnTeO was obtained from Rietveld refinement of its powder XRD pattern. The FT-IR and Raman spectra of KMnTeO gave characteristic bands belonging to the defect pyrochlore structure. The photocatalytic activities of KMnTeO and composite KMnTeO-g-CN were evaluated by the degradation of methylene blue (MB). Scavenger experiments were carried out to identify the reactive species responsible for the degradation of MB. Furthermore, the reusability and stability of the photocatalysts were explored. The probable photocatalytic mechanism for MB degradation over the composite KMnTeO-g-CN was surmised according to the scavenger experiments. The work provides a new approach for the development of novel defect pyrochlore based composite photocatalysts to treat industrial wastewater containing organic pollutants.

Morphological studies, photocatalytic degradation of organic dyes and anticancer potential of copper sulfide nanoparticles prepared from bis(diallyl dithiocarbamato)copper(II) complex

Bis(diallyl dithiocarbamato)copper(II) complex was synthesized and characterized by single crystal X-ray crystallography. The molecular structure revealed dimeric copper(II) complex consisting of two copper(II) ions that coordinate two molecules of diallydithiocarbamato anions in bidentate chelating modes and the centrosymmetrically related diallydithiocarbamato anions bridges the S-atom of the adjacent chelating ligand to formed square pyramidal geometry around the copper(II) ions. Copper sulfide nanoparticles were prepared at 160 °C by thermolysis of the copper(II) complex in dodecylamine (DDA), hexadecylamine (HDA), and octadecylamine (ODA) to study the effect of capping agents on the structural morphologies, photocatalytic properties, and anticancer potential of the as-prepared copper sulfides nanoparticles. Powder X-ray diffraction patterns confirmed Cu9S5 digenite crystalline phases for CuS-DDA and CuS-HDA while CuS-ODA is covellite crystalline phase. HRTEM images showed spherical particles with particle sizes in the range 2–25 nm. The copper sulfide nanophotocatalysts are efficient for the degradation of bromophenol blue with the highest photocatalytic efficiency of 95.14 % for CuS-DDA followed by CuS-HDA with 94.52 % and 93.95 % for CuS-ODA. The anticancer potentials of the compounds showed that CuS-HDA is the most potent with IC50 values of 1.22 µg/mL against HEK293 and 28.78 µg/mL against HeLa.

Formation of skyrmion phase in the Fe-Co-Si system by mechanochemical activation

Fe, Co and Si powders were exposed to mechanochemical activation by high-energy ball milling for 0, 2, 4, 8 and 12 h. The samples were subsequently characterized by Mössbauer spectroscopy, X-ray powder diffraction (XRPD), magnetic measurements and optical diffuse reflectance spectroscopy. The room temperature Mössbauer measurements were consistent with the occurrence of FeCo2Si and Fe0.5Co0.5Si crystalline phases. The low temperature Mössbauer spectra confirmed the absence of superparamagnetism up to 44 K in the milled system. XRPD patterns supported the phase sequence derived from Mössbauer spectroscopy. The coercive field was found to increase with the ball milling time (BMT). Zero-field-cooling-field-cooling (ZFC-FC) measurements performed at 200 Oe in the temperature range 5-300 K evidenced the transition to the skyrmion phase of the Fe0.5Co0.5Si material below the critical temperature of 44 K. The optical absorption in the UV-Vis-NIR region of the spectrum was found to increase with BMT.

Hen egg lysozyme polymorphs mediated by two ionic liquids during batch cooling crystallization

-Lysozyme batch cooling crystallization in the presence of two ionic liquids (ILs), 1-butyl-3-methylimidazolium chloride ([C4mim]Cl), and 1,3-dimethylimidazolium iodide ([C1mim]I). Microscopic observation demonstrated that the crystal morphology with [C1mim]I is needle-like, while that with [C4mim]Cl and no ILs is plate-like. FTIR spectroscopy revealed that new peaks in the range of 1300–400 cm−1 occur with the case of adding [C1mim]I, meaning that the microstructure of lysozyme crystals changed. Raman spectroscopy and X-ray powder diffraction (XRD) pattern further confirmed that crystal forms of lysozyme with adding [C4mim]Cl and no ILs is completely different from that of adding [C1mim]I. Thermogravimetry (TG) and Differential Scanning Calorimeter (DSC) results indicated that addition of [C1mim]I delay the thermal deformation and degradation temperature of lysozyme crystals, suggesting that lysozyme crystals with [C1mim]I possesses higher thermal stability. The change in lysozyme crystal forms can be attributed to changes in interaction among lysozyme molecules and conformation in solution, leading to different assembly mode of molecules and formation of polymorphs. These findings could offer instructions for regulating lysozyme crystal forms and gaining initial insight into screening of potential ILs for developing polymorphs of the protein and other macromolecule crystals.

Posaconazole-glutaric acid cocrystal tablet with improved Dissolution rate

Posaconazole is used to prevent fungal infections in patients having severely weakened immune system and has poor aqueous solubility which impairs its dissolution in upper gastric fluid producing problems in different formulations. These characteristics hinder its therapeutic application by delaying absorption rate and thereby onset of action. In the present study, an attempt was made to prepare posaconazole cocrystals with improved physicochemical properties for better therapeutic activity. Cocrystals were prepared with glutaric acid in 1:1 molar using ethanol by solvent drop grinding technique. The co-crystals formed were characterized by melting point determination, fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), and dissolution studies. Posaconazole-glutaric acid co-crystals were further formulated as fast disintegrating tablets. The IR study revealed the shifting of characteristic bands of posaconazole. The PXRD pattern indicated cocrystal crystallinity and a considerable difference in 2θ value of intense peaks. The variation in fusion endotherm, which is in agreement with melting point, was designated by DSC spectra of posaconazole cocrystal. A significant improvement in the dissolution rate was observed in the case of cocrystals based tablets than pure posaconazole tablets.

Impact of the Position of the Hydroxyl Group in Monohydroxy Chalcones with 2-Hydroxypropyl-β-Cyclodextrin on Their Spectral, Biological, and Theoretical Properties

3-Hydroxychalcone (3HOCH) and 4-hydroxychalcone (4HOCH) compounds were synthesized from the reaction between acetophenone and either 3-hydroxybenzaldehyde or 4-hydroxy benzaldehyde, using KOH as a catalyst. Then the synthesized compounds were further reacted with two cyclodextrins (CDs) (2-hydroxypropyl-β-cyclodextrin and β-cyclodextrin), by a co-precipitation method to investigate their spectral (absorption, fluorescence, and Fourier transform infrared), biological, and theoretical properties. Two absorption maximums appeared at 307 and 253 nm for 3HOCH and 346 and 254 nm for 4HOCH in aqueous solution by absorption spectrophotometry. In the excited state, dual emission was observed at 362 nm and 426 nm for 3HOCH and 360 nm and 486 nm for 4HOCH in the same medium of H2O by fluorescence spectrophotometry. The apparent changes in the absorption and emission spectra were the result of the inclusion complex with a 1:1 molar stoichiometric ratio. The interaction of 3HOCH, 4HOCH, and the CDs in the solid state was characterized by Fourier-transform infrared spectroscopy (FTIR), powder X-ray diffraction patterns (PXRD), scanning electron microscopy (SEM), antioxidant and antibacterial studies concerning the position of the hydroxyl (-OH) group at the m- or p-positions in chalcone. The optimized highest occupied molecular orbital (HOMO) diagram, lowest unoccupied molecular orbital (LUMO) diagram and molecular electrostatic potential (MEP) map for the isolated molecules and their inclusion complexes were done by Becke’s three-parameter (B3) hybrid functional method using the Lee-Yang-Parr (LYP) correlation levels of density functional theory (DFT) method with 3-21 G basis set.

Exploring the formation and diversity of secnidazole cocrystals

This study investigates the cocrystallization of secnidazole (SNZ), a potent antimicrobial drug, with several coformers, overcoming the inherent stability challenges posed by its hemihydrate form to produce novel solid states. We successfully synthesized and characterized three novel cocrystals with carvacrol (CAR), fumaric acid (FMA), and 3,5-dinitrobenzoic acid (DNZ), employing synchrotron single crystal analysis to elucidate their structures. The application of Hirshfeld surface and 2D fingerprint plots further enriched our understanding of the unique packing arrangements within these cocrystals. Moreover, preliminary powder X-ray diffraction (PXRD) patterns hinted at the emergence of additional novel solid forms with salicylic acid (SLC), oxalic acid (OXA), succinic acid (SUC), citric acid (CTR), and thymol (THY). Supported by literature and a thorough analysis of molecular interactions, we propose the existence of pharmaceutical cocrystals among these newly identified solid forms. Our findings not only augment the repertoire of SNZ based pharmaceuticals but also accentuates the strategic utilization of supramolecular synthons, offering significant advancements in the understanding of novel solid form formation, and the critical role of hydrogen bonding in these processes.

New nanometric metal complexes based on thiazole derivative as potential antitumor and antimicrobial agents: Full structural elucidation, docking simulation and biological activity studies

Novel Mn(II), Ni(II), Zr(IV) and Cd(II) nanosized complexes of thiazole Schiff base derivative (HL) were synthesized for further medicinal applications. The inspected complexes were fully characterized using elemental and thermal analyses in addition to infrared spectroscopy (IR) and nuclear magnetic resonance (1HNMR). Electronic absorption spectra, X-ray powder diffraction (XRD), transmittance electron microscopy (TEM), molar conductance and magnetic moment were also measured and explained. The brought about data revealed that the ligand–metal chelation happened through the N atom of N = N group, and the ortho-dehydrogenated phenolic O atom to form the chelates where the metal binds with one molecule of the parent ligand. All applied spectroscopic and analytical techniques confirmed tetrahedral geometry in Mn(II) and Ni(II) complexes and octahedral geometry for Cd(II) and Zr(IV) complexes. The ligand, Mn(II), Ni(II), and Zr(IV) chelates' XRD patterns indicated an amorphous character where the Cd(II) complex's nature is crystalline. Transmission electron microscopy (TEM) images of the prepared compounds showed that the surface morphology is uniform and homogeneous. Also, the metal ions distribute through the complexes' surface in a nanosized nature. The metal complexes have been simulated by docking in the co-crystal structures of the liver cancer and breast cancer proteins with PDB IDs, 2JW2 and 3S7S, successively. Antibacterial, antifungal and anticancer activities for the ligand that has been produced and its complexes were achieved. The most encouraging antitumor results were acquired by Ni(II) chelate which exhibited an IC50 of 23.52 µg/ml contra MCF-7 cells (human breast cancer) which is lower than the reference 5-Fluorouracil (5-FU, IC50 = 28.00 µg/ml).

Evidence of local structural distortions and subtle thermal disorder in transparent photochromic yttrium oxyhydride

The structural properties of photochromic yttrium oxyhydride powder in its transparent state were examined using x-ray diffraction and temperature-dependent extended x-ray absorption fine structure spectroscopy (EXAFS) combined with reverse Monte Carlo (RMC) simulations. The refinement of the x-ray powder diffraction pattern, employing the Rietveld method, indicates that yttrium oxyhydride crystallizes in the nanocrystalline phase with the cubic space group Fm-3m (225), at room temperature. The lattice parameter was determined as a = 5.404(3) Å, and the nanocrystallite size was estimated at d = 16(2) nm. The partial radial distribution functions (RDFs) g(r) for Y–O, O–O, and Y–Y atom pairs were obtained from the results of the RMC simulations of the Y K-edge EXAFS spectra measured at three temperatures (10, 150, and 300 K). The analysis of the RDFs reveals a subtle impact of the thermal disorder and splitting of the second coordination shell of yttrium atoms (the Y–Y RDF), remaining at all temperatures. This observation, also supported by our density functional theory calculations, suggests the presence of local structural distortions associated with yttrium sites, which do not affect the long-range crystal order.

Gajardoite-(NH4), (NH4)As3+4O6Cl2[(Ca0.5□0.5)(H2O)5], a new mineral from the Khovu-Aksy deposit, Eastern Siberia, Russia

The new mineral gajardoite-(NH4), ideally (NH4)As3+4O6Cl2[(Ca0.5□0.5)(H2O)5], is found at the Khovu-Aksy Ni-Co deposit, Republic of Tyva, Russia. Gajardoite-(NH4) occurs as tiny lamellar coarsely hexagonal or irregular curved and divergent crystals up to 0.01 mm in size. The crystals are combined in groups, rosette-like clusters or spherulitic aggregates up to 0.2 mm, which are intimately intergrown with annabergite, arsenolite, and pharmacolite on a matrix of skutterudite, safforite, and other minerals. The new mineral is colorless, white in aggregates, transparent with a white streak and a vitreous lustre. It is brittle, with a perfect cleavage on {001}. The Mohs hardness is ~1½. The calculated density (Dcalc ) is 2.583 g/cm3.Gajardoite-(NH4) is optically non-pleochroic, uniaxial (–), ω = 1.745(10), ε = 1.558(5) (589 nm). The chemical composition determined by electron microprobe (wt. %, H2O content calculated by stoichiometry) is as follows: (NH4)2O 3.17, Na2O 0.40, K2O 1.07, CaO 5.28, As2O3 67.25, Cl 12.21, H2O 15.30, O=Cl –2.76, total 101.92. The empirical formula based on four As and 11 O atoms per formula unit is [(NH4)0.72K0.13Na0.08]Σ0.93Ca0.55As3+4O6Cl2.03(H2O)5. Gajardoite-(NH4) is hexagonal, space group P6/mmm; the unit-cell parameters are as follows: a = 5.263(3), c = 16.078(5) Å, V = 385.8(5) Å3, Z = 1. The strongest lines of the powder X-ray diffraction pattern [d, Å (I, %) (hkl)] include 16.08 (34) (001), 5.36 (34) (003), 4.565 (41) (100), 3.466 (23) (103), 2.637 (100) (110), 2.360 (25) (113). Gajardoite-(NH4) is an ammonium analog of gajardoite KCa0.5As3+4O6Cl2 • 5H2O. Their structural identity is confrmed by powder X-ray diffraction and infrared and Raman spectroscopy.

Trivalent dysprosium activated LaSr2AlO5 nanophosphors for NUV-excited wLEDs: Insights into structural, optical, Judd-Ofelt parameters and temperature dependent photoluminescence

Gel-combustion (GC) methodology was implemented in the present research to produce a series of single phase Dy3+ doped LaSr2AlO5 nanophosphors for the usage in wLEDs. X-ray powder diffraction patterns verified the phase purity and crystal structure of the produced materials. The XRD inspection supported the successful fabrication of tetragonal structured (I4/mcm space group) phosphors and revealed good accordance with card number 70–2197 on the JCPDS database. We collected diffuse reflectance spectra (DRS) to examine how doping affects the band gap. Furthermore, energy-dispersive X-ray (EDX) spectroscopy and transmission electron microscopy (TEM) have been employed for assessing elemental composition and surface morphology. On 349 nm excitation, LaSr2AlO5:Dy3+ phosphors produce the distinctive yellow PL emissions causedby 4F9/2→6H13/2 transition. Using excitation spectra, the Judd-Ofelt (J-O) characteristic (Ω = 2, 4, 6) have been determined. The Dy3+ transition's features show that the J-O parameters followed the trend which suggested an asymmetric environment around the ligand. The electric dipole transition predominated in the luminescence spectrum, causing the LaSr2AlO5:Dy3+ phosphor to emit a yellowish whitecolor. The fundamental mechanism for the energy transfer and concentration quenching instances among activator ions was discovered to be dipole-quadrupole interactions. Temperature dependent luminescence showed that the synthesized phosphors had thermal stability up to 523 K with activation energy of 0.1312 eV. The future prospects of the synthesized phosphor as an effective choice for near-ultraviolet-activated wLEDs are substantially supported by current comprehensive research.

Strong signature of uncompensated magnetization in frustrated cobalt manganites using x-ray magnetic circular dichroism study

The present study is focused on the investigation of the distorted tetragonal phase of mixed spinel oxides, due to their technological relevance in the field of electronics, spintronics, magnetism, catalysis, and electrochemical energy storage. Herein, we report on solgel synthesized multivalent cobalt manganites, CoMn2O4 (CMO), and subjected them to a comprehensive analysis to elucidate their physicochemical characteristics at room temperature. Analysis employing powder x-ray diffraction patterns and electron microscopy (including field-emission scanning electron microscopy and high-resolution transmission electron microscopy) results confirmed the formation of a pure and exceptionally crystalline, distorted tetragonal phase of mixed CMO. Synchrotron-based x-ray absorption spectroscopic (XAS) measurements in the total electron yield mode examined local electronic structures affirming the formation of CMO with uncompensated electronic states involving Co2+, Co3+, Mn2+, Mn3+, and Mn4+ cations. Concurrently, XAS and x-ray magnetic circular dichroism analyses revealed antiferromagnetic coupling within Co and Mn sublattices in CMO, indicating the presence of uncompensated electronic states. Vibrating sample magnetometry results demonstrated clear hysteresis behavior, explicitly indicating the coexistence of super-paramagnetic and canted antiferromagnetic characteristics in CMO, as validated through the Langevin function fitting and x-ray magnetic circular dichroism results. The noticeable absence of saturated magnetization confirmed the high degree of spin canting, primarily stemming from the presence of the Yafet–Kittel spin arrangement.

Effect of Tb3+ and Ce3+ Co-doping on the Structure and Photoluminescence Properties of Hexagonal Boron Nitride Phosphors.

In the paper, we have successfully prepared hexagonal boron nitride (h-BN:Tb3+, Ce3+) phosphors with melamine as the nitrogen source. The X-ray powder diffraction patterns confirm that the sample possesses a hexagonal crystal structure within the P m2 space group. It is interesting that the co-doping combination of Tb3+ and Ce3+ can markedly enhance the threshold concentration of doped activators within the limited solid solution of h-BN phosphors. Under 302nm excitation, the h-BN:Ce3+ phosphors exhibit broadband blue light emission at 406nm. In h-BN:Tb3+, Ce3+ phosphors, the co-doping of Ce3+ not only ensures high phase purity but also results in strong green light emission. The energy transfer efficiency from Ce3+ to Tb3+ is about 55%. The fluorescence lifetime increases with the increase of Ce3+ and Tb3+ concentration, and the fluorescence lifetime of h-BN:0.025Tb3+, 0.05Ce3+ phosphor reached 2.087ms. Additionally, the h-BN:0.025Tb3+, 0.05Ce3+ phosphor exhibits excellent thermal performance with an activation energy value of 0.2825eV. Moreover, the photoluminescence quantum yield of the sample exceeds 52%. Therefore, the h-BN:Tb3+, Ce3+ samples can be used as green phosphors for solid state lighting and fluorescent labeling.

Mckelveyite group minerals – Part 4: Alicewilsonite-(YLa), Na2Sr2YLa(CO3)6 ⋅ 3H2O, a new lanthanum-dominant species from the Paratoo mine, Australia

Abstract. The new mckelveyite group mineral, alicewilsonite-(YLa), Na2Sr2YLa(CO3)6 ⋅ 3H2O, was found together with kamphaugite-(Y), paratooite-(Y), bastnäsite-(La), and decrespignyite-(Y) coating along fractures in dolomite at the Paratoo copper mine, South Australia, Australia. It occurs as pale pink to colourless pseudohexagonal tabular crystals up to 150 µm in size. The streak is white; the lustre is vitreous. The mineral has no cleavage. Dcalc is 3.37 g cm−3. Alicewilsonite-(YLa) is optically biaxial (−), α = 1.556(2), β= 1.582(2), γ= 1.592(2), 2V (meas.) = 60(2)°, 2V (calc.) = 63° (589 nm). The IR spectrum is reported. The composition (wt %, average of seven analyses) is Na2O 7.43, CaO 2.00, SrO 18.43, BaO 1.64, Y2O3 9.59, La2O3 11.74, Pr2O3 1.29, Nd2O3 5.74, Sm2O3 0.44, Eu2O3 0.09, Gd2O3 0.95, Dy2O3 1.15, Ho2O3 0.25, Er2O3 0.89, Yb2O3 0.29, CO2 29.78, H2O 6.18, total 97.88. The empirical formula calculated on the basis of six cations with 3 H2O molecules is as follows: Na2.10Ca0.31Sr1.56Ba0.10Y0.74La0.63Pr0.07 Nd0.30Sm0.03Eu0.01Gd0.04Dy0.05Ho0.01Er0.04 Yb0.01(CO3)5.92(H2O)3. The mineral is triclinic, P1, a= 8.9839(2), b= 8.9728(3), c= 6.7441(2) Å, α= 102.812(2)°, β= 116.424(2)°, γ= 60.128(2)°, and V= 422.17(2) Å3 and Z= 1. The strongest reflections of the powder X-ray diffraction pattern [d,Å(I)(hkl)] are 6.03(43)(001), 4.355(100)(11‾0, 2‾1‾1, 120), 4.020(30)(1‾11, 210, 1‾2‾1), 3.188(29)(2‾1‾2, 11‾1, 121), 2.819(96)(002, 1‾12, 211, 1‾2‾2), 2.592(40)(3‾01, 030, 3‾3‾1), 2.228(33)(2‾21, 4‾2‾1, 2‾4‾1). 2.011(36)(2‾22, 003, 420, 2‾4‾2), 1.9671(32)(3‾03, 301, 03‾2, 032, 3‾3‾3, 331). The crystal structure was solved and refined from single-crystal X-ray diffraction data (R1= 0.058).

Škáchaite, CaCo(CO3)2, a new member of the dolomite group, from the Brod deposit near Příbram, Czech Republic

Abstract Škáchaite (IMA2022–143) is a new mineral species discovered in samples from the hydrothermal vein B117, shaft No. 6 at the Brod deposit of the uranium and base-metal Příbram ore district, central Bohemia, Czech Republic. Škáchaite is a Co-dominant member of the dolomite group and forms anhedral grains up to 50 μm in size and as 20–100 μm thick growth zones in škáchaite–dolomite crystals as a part of carbonate (dolomite, calcite, siderite, spherocobaltite, ankerite, kutnohorite and minrecordite) gangue, associated with native silver, sulfides and arsenides. Škáchaite is pale to bright pink with vitreous lustre. The Mohs hardness is ca. 3½–4, similar to other members of the dolomite group. The calculated density is 3.140 g.cm–3. Škáchaite is optically uniaxial (–); the indices of refraction are ω = 1.741(3) and ɛ = 1.535(3). On the basis of electron-microprobe analyses, its empirical formula is Ca1.00(Co0.45Mg0.38Ca0.08Fe0.05Mn0.03Zn0.01)Σ1.00(CO3)2. The ideal formula is CaCo(CO3)2, which requires (in wt.%) CaO 25.60, CoO 34.21, CO2 40.19, a total of 100.00. Škáchaite is trigonal, R $\bar{3}$ , with unit-cell parameters a = 4.8177(18), c = 16.093(7) Å, V = 323.5(2) Å3 and Z = 3. The strongest reflections of the calculated powder X-ray diffraction pattern [d, Å, (Irel, %) hkl] are: 3.704 (13) 10 $\bar{2}$ ; 2.896 (100) 104; 2.409 (15) 110; 2.019 (17) 202; 1.812 (19) 10 $\bar{8}$ ; and 1.792 (16) 11 $\bar{6}$ . According to the single-crystal X-ray diffraction data (R1 = 0.0304 for 94 reflections with [I > 3σ(I)]), the crystal structure of škáchaite is isotypic with its Mg-analogue, dolomite. The Raman spectrum of škáchaite, as well as the tentative assignment of observed bands, are given in this paper. The mineral is named in honour of Pavel Škácha, a Czech mineralogist and curator of the mineralogical collection of the Mining Museum Příbram, Czech Republic.

Comparing Microcrystal Electron Diffraction (MicroED) and X-ray crystallography as methods for structure determination of Oseltamivir phosphate

Oseltamivir phosphate is a pharmaceutical used in the treatment of influenza viruses. Panče Naumov et al. took two years of dedicated single crystal cultivation and successfully obtained low-quality single crystals through a diffusion method. Cultivation of Oseltamivir phosphate single crystals was proved to be difficult and can extend over several months or more. We employed microcrystalline electron diffraction (MicroED) for direct powder measurements, eliminating the need for lengthy single-crystal cultivation, and the time to obtain the molecular structure of Oseltamivir phosphate was shortened from several months to five hours. Comparative analyses of single crystal (Crystal 1) and MicroED (Crystal 2) results revealed equivalent crystal structures, with minimal differences in hydrogen bond distances, identical powder X-ray diffraction patterns, and negligible variations in Hirshfeld surface analysis. The differential scanning calorimetry (DSC) analysis showcased a higher melting point of Oseltamivir phosphate (206.0 °C) than Oseltamivir (110.7 °C), indicating that Oseltamivir phosphate had high temperature stability, and may result in the selection of Oseltamivir phosphate as a formulation form. The study establishes and verifies a congruence between MicroED detection and traditional single-crystal detection methods and may be applied in the elucidation of compound structures and the surveillance of drug polymorphism.

Enhancing thermoelectric behavior of Bismuth Selenide crystal via substitution of Sulfur and Tellurium

Sulfur and Tellurium substituted Bismuth Selenide (Bi2Se3-x-ySxTey, x = y = 0, 0.1, 0.15, 0.2) quaternary alloy crystals were synthesized by using vertical Bridgman technique. Energy dispersive analysis of X-rays confirmed elemental composition and purity of the grown crystals. Field emission scanning electron microscopy showed that the growth of crystals has occurred by layer growth mechanism. Rhombohedral crystal structure is validated through analysis of powder X-ray diffraction pattern. Thermoelectric parameters such as electrical conductivity, Seebeck coefficient and thermal conductivity were calculated from 303 K to 773 K and from that power factor as well as figure of merit have been determined for all grown crystals. Electrical conductivity significantly increased due to Sulfur and Tellurium incorporation and maximum value obtained is 147.72 S/cm at 503 K for Bi2Se2.6S0.2Te0.2. Seebeck coefficient and thermal conductivity showed decrement with incorporation of Sulfur and Tellurium. Reduction in thermal conductivity and enhancement in electrical conductivity resulted in the improvement of figure of merit. Sulfur and Tellurium substitution showed considerable improvement in ZT from 0.31 (533 K) for pristine Bi2Se3 to 1.28 (523 K) for Bi2Se2.6S0.2Te0.2.