Dual Structure of a Vanadyl-Based Molecular Qubit Containing a Bis(β-diketonato) Ligand.

We designed [VO(bdhb)] (') as a new electronic qubit containing an oxovanadium(IV) ion ( = 1/2) embraced by a single bis(β-diketonato) ligand [Hbdhb = 1,3-bis(3,5-dioxo-1-hexyl)benzene]. The synthesis afforded three different crystal phases, all of which unexpectedly contain dimers with formula [(VO)(bdhb)] (). A trigonal form () with a honeycomb structure and 46% of solvent-accessible voids quantitatively transforms over time into a monoclinic solvatomorph and minor amounts of a triclinic solventless phase ().

Comprehensive study of nanostructured BiTe thermoelectric materials - insights from synchrotron radiation XRD, XAFS, and XRF techniques.

In this contribution, a comprehensive study of nanostructured BiTe (BT) thermoelectric material was performed using a combination of synchrotron radiation-based techniques such as XAFS, and XRF, along with some other laboratory techniques such as XRD, XPS, FESEM, and HRTEM. This study aims to track the change in morphological, compositional, average and local/electronic structures of BiTe of two different phases; nanostructure (thin film) and nanopowders (NPs). BiTe nanomaterial was fabricated as pellets using zone melting process in a one step process, while BiTe thin film was deposited on sodalime glass substrate using a vacuum thermal evaporation technique.

Praziquantel meets Niclosamide: A dual-drug Antiparasitic Cocrystal.

In this paper we report a successful example of combining drugs through cocrystallization. Specifically, the novel solid is formed by two anthelminthic drugs, namely praziquantel (PZQ) and niclosamide (NCM) in a 1:3 molar ratio, and it can be obtained through a sustainable one-step mechanochemical process in the presence of micromolar amounts of methanol. The novel solid phase crystallizes in the monoclinic space group of P2/c, showing one PZQ and three NCM molecules linked through homo- and heteromolecular hydrogen bonds in the asymmetric unit, as also attested by SSNMR and FT-IR results.

High temperature behaviour of Ag-exchanged Y zeolites used for PFAS sequestration from water.

Per- and polyfluorinated alkyl substances (PFAS) are anthropogenic compounds which have recently drawn great attention due to their high biological, chemical and physical stability and lipid/water repelling properties. The present work aims to provide for the first time insights on the thermal behaviour of Ag-exchanged Y zeolite loaded with perfluorooctanoic acid (PFOA, CHFO) and perfluorooctane sulfonate (PFOS, CHFOS) emphasizing the close link between crystal structure and desorption/dehydration processes. Elemental and isotopic abundance of carbon analysis, thermal analysis, and high-temperature synchrotron X-ray powder diffraction were used to evaluate critically if the thermal regeneration affects the initial zeolites structural features.

Correlations between structure, microstructure and ionic conductivity in (Gd,Sm)-doped ceria.

The structural, microstructural, Raman and ionic conductivity properties of (Gd,Sm)-doped ceria were studied and compared to the ones of similar ceria systems with the aim of deepening the comprehension of the correlations between defect chemistry and movement of oxygen vacancies in such materials, which are ideal candidates as electrolytes in solid oxide cells. The system was chosen as it combines the advantages of using the most effective doping ions for ceria, namely Sm and Gd, and the expected positive effects of multiple doping. The main effect of double doping on the structure is the enlargement of the compositional region where ionic conductivity takes place, due to the entrance of the smaller doping ions into defect clusters, mainly trimers and dimers (RE ≡ rare earth).

Mechanochemical Synthesis and Physicochemical Characterization of Previously Unreported Praziquantel Solvates with 2-Pyrrolidone and Acetic Acid.

Two new solvates of the widely used anthelminthic Praziquantel (PZQ) were obtained through mechanochemical screening with different liquid additives. Specifically, 2-pyrrolidone and acetic acid gave solvates with 1:1 stoichiometry (PZQ-AA and PZQ-2P, respectively). A wide-ranging characterization of the new solid forms was carried out by means of powder X-ray diffraction, differential scanning calorimetry, FT-IR, solid-state NMR and biopharmaceutical analyses (solubility and intrinsic dissolution studies).

3-Alkenyl-2-oxindoles: Synthesis, antiproliferative and antiviral properties against SARS-CoV-2.

Sets of 3-alkenyl-2-oxindoles (6,10,13) were synthesized in a facile synthetic pathway through acid dehydration (EtOH/HCl) of the corresponding 3-hydroxy-2-oxoindolines (5,9,12). Single crystal (10a,c) and powder (12a,26f) X-ray studies supported the structures. Compounds 6c and 10b are the most effective agents synthesized (about 3.

Understanding Oxygen Release from Nanoporous Perovskite Oxides and Its Effect on the Catalytic Oxidation of CH and CO.

The design of nanoporous perovskite oxides is considered an efficient strategy to develop performing, sustainable catalysts for the conversion of methane. The dependency of nanoporosity on the oxygen defect chemistry and the catalytic activity of perovskite oxides toward CH and CO oxidation was studied here. A novel colloidal synthesis route for nanoporous, high-temperature stable SrTiFeO with specific surface areas (SSA) ranging from 45 to 80 m/g and pore sizes from 10 to 100 nm was developed.

Cold Crystallization of the Organic n-Type Small Molecule Semiconductor 2-Decyl-7-phenyl-[1]benzothieno[3,2-][1]benzothiophene ,,','-Tetraoxide.

The asymmetric n-type Ph-BTBT-C derivative 2-decyl-7-phenyl-[1]benzothieno[3,2-][1]benzothiophene ,,','-tetraoxide is structurally investigated in the thin film regime. After film preparation by spin coating and physical vapor deposition, a rather disordered structure is observed, with a strong change of its internal degree of order upon heating. At 95 °C, a transition into a layered structure of upright standing molecules without any in-plane order appears, and at 135 °C, crystallization takes place.

In-Operando Diffraction and Spectroscopic Evaluation of Pure, Zr-, and Ce-Doped Vanadium Dioxide Thermochromic Films Derived via Glycolate Synthesis.

Pure and doped vanadia (VO, VZrO, VCeO) samples were prepared by wet chemistry synthesis from vanadyl glycolate intermediate phase and tape casted into films. Combining in-operando grazing incidence synchrotron X-ray diffraction and Raman spectroscopy, we studied the structural evolution of the films under isothermal conditions. The setup allowed assessment of the thermochromic functionality with continuous monitoring of the monoclinic to tetragonal transition in pure and doped vanadia phases, responsible for the transmission and reflection of light in the infrared part of the solar spectrum.

()-10-Hydroxystearic Acid: Crystals vs. Organogel.

The chiral ()-10-hydroxystearic acid (()-10-HSA) is a positional homologue of both ()-12-HSA and ()-9-HSA with the OH group in an intermediate position. While ()-12-HSA is one of the best-known low-molecular-weight organogelators, ()-9-HSA is not, but it forms crystals in several solvents. With the aim to gain information on the structural role of hydrogen-bonding interactions of the carbinol OH groups, we investigated the behavior of ()-10-HSA in various solvents.

From solid state to anticancer activity of copper(II) compounds with electronically-modulated NNO Schiff base ligands.

The copper(ii) complexes of general formula [Cu(GL)(Cl)] (1-3, G = OMe, H and NO2, respectively), bearing tridentate Schiff base ligands (GL-) and a chloride as a fourth labile one, are here reported. The Schiff bases derive from the monocondensation of ethylenediamine and substituted salicylaldehyde, where the electronic properties are modulated by the releasing or withdrawing power of the G group. The compounds were structurally characterized through single crystal Synchrotron X-ray diffraction experiments in the solid state, revealing that 1 (OMe) and 2 (H) adopt a dimeric assembly [Cu(μ-Cl)(GL)]2 through apical interaction of the chloride ions of two monomeric units, while 3 embraces a 1D polymeric chain structure [Cu(μ-Cl)(NO2L)]n with a similar bridging fashion, all supported by extended intramolecular or intrachain hydrogen bonds.

L-Lysine Amino Acid Adsorption on Zeolite L: a Combined Synchrotron, X-Ray and Neutron Diffraction Study.

Combined neutron and X-ray powder diffraction techniques highlighted the sorption capacity of the acidic L zeolite towards the L-lysine amino acid. The role of zeolite channels in the stabilization of the lysine absorbed and the effect of water on protein structure are elucidated at atomistic level. The stabilization of the L α-helical conformation is related to strong H-bonds between the tail aminogroups of lysine molecules and the Brønsted acid site as well as to complex intermolecular H-bond system between water molecules, zeolite and amino acid.

L-Lysine Amino Acid Adsorption on Zeolite L: a Combined Synchrotron, X-Ray and Neutron Diffraction Study.

Invited for this month's cover are the groups of Annalisa Martucci and Luisa Pasti at the University of Ferrara (Italy). The cover picture shows L-lysine amino acid adsorption on zeolite L. The role of zeolite channels in the stabilization of the lysine absorbed and the effect of water on protein structure are elucidated at atomistic level.

Electronic structure of MAPbI and MAPbCl: importance of band alignment.

Since their first appearance, organic-inorganic perovskite absorbers have been capturing the attention of the scientific community. While high efficiency devices highlight the importance of band level alignment, very little is known on the origin of the strong n-doping character observed in the perovskite. Here, by means of a highly accurate photoemission study, we shed light on the energy alignment in perovskite-based devices.

Exploring mechanochemical parameters using a DoE approach: Crystal structure solution from synchrotron XRPD and characterization of a new praziquantel polymorph.

A rotated Doehlert matrix was utilized to explore the experimental design space around the milling parameters of Praziquantel (PZQ) polymorph B formation in terms of frequency and milling time. Three experimental responses were evaluated on the resulting ground samples: two quantitative responses, i.e.

X-Ray Crystal Structures and Organogelator Properties of -9-Hydroxystearic Acid.

-9-hydroxystearic acid, -9-HSA, is a chiral nonracemic hydroxyacid of natural origin possessing interesting properties as an antiproliferative agent against different cancer types. Considering its potential application for medical and pharmaceutical purposes, the structures and rheological properties of -9-HSA were investigated. Oscillatory rheology measurements reveal that -9-HSA gels only paraffin oil, with less efficiency and thermal stability than its positional isomer -12-HSA.

What's underneath? A non-destructive depth profile of painted stratigraphies by synchrotron grazing incidence X-ray diffraction.

Many works of art are complex systems consisting of a core completed by the overlapping of several painted layers. In this work, we apply an innovative method based on grazing incidence X-ray diffraction (GIXRD) with synchrotron radiation (SR) to investigate polychrome stratigraphies with a completely non-destructive approach. The SR-GIXRD measurements provided direct and unambiguous compositional and stratigraphic information of the crystalline species lying in different layers.

A new soluble and bioactive polymorph of praziquantel.

Praziquantel is the only available drug to treat Schistosomiasis. However, its utilization is limited by many drawbacks, including the high therapeutic dose needed, resulting in large tablets and capsules difficult to be swallowed, especially from pediatric patients. In this study, an alternative option to overcome these disadvantages is proposed: to switch to a novel crystalline polymorph of racemic compound praziquantel.

Irreversible Conversion of a Water-Ethanol Solution into an Organized Two-Dimensional Network of Alternating Supramolecular Units in a Hydrophobic Zeolite under Pressure.

Turning disorder into organization is a key issue in science. By making use of X-ray powder diffraction and modeling studies, we show herein that high pressures in combination with the shape and space constraints of the hydrophobic all-silica zeolite ferrierite separate an ethanol-water liquid mixture into ethanol dimer wires and water tetramer squares. The confined supramolecular blocks alternate in a binary two-dimensional (2D) architecture that remains stable upon complete pressure release.

Removal of sulfonamide antibiotics from water: Evidence of adsorption into an organophilic zeolite Y by its structural modifications.

Sulfonamide antibiotics are persistent pollutants of aquatic bodies, known to induce high levels of bacterial resistance. We investigated the adsorption of sulfadiazine, sulfamethazine, and sulfachloropyridazine sulfonamides into a highly dealuminated faujasite zeolite (Y) with cage window sizes comparable to sulfonamide dimensions. At maximal solubility the antibiotics were almost completely (>90%) and quickly (t<1min) removed from the water by zeolite.