New Polymorphic Modifications of 6-Methyluracil: An Experimental and Quantum Chemical Study.

Polymorphism of 6-methyluracil, which affects the regulation of lipid peroxidation and wound healing, has been studied by experimental and quantum chemical methods. Two known polymorphic modifications and two new crystalline forms were crystallized and characterized by single crystal and powder X-ray diffraction (XRD) methods as well as by the differential scanning calorimetry (DSC) method and infrared (IR) spectroscopy. The calculations of pairwise interaction energies between molecules and lattice energies in periodic boundary conditions have shown that the polymorphic form used in the pharmaceutical industry and two new forms and , which can be formed due to temperature violations, may be considered as metastable.

Robocasting of Ceramic Fischer-Koch S Scaffolds for Bone Tissue Engineering.

Triply Periodic Minimal Surfaces (TPMS) are promising structures for bone tissue engineering scaffolds due to their relatively high mechanical energy absorption, smoothly interconnected porous structure, scalable unit cell topology, and relatively high surface area per volume. Calcium phosphate-based materials, such as hydroxyapatite and tricalcium phosphate, are very popular scaffold biomaterials due to their biocompatibility, bioactivity, compositional similarities to bone mineral, non-immunogenicity, and tunable biodegradation. Their brittle nature can be partially mitigated by 3D printing them in TPMS topologies such as gyroids, which are widely studied for bone regeneration, as evidenced by their presence in popular 3D-printing slicers, modeling systems, and topology optimization tools.

Characterisation of acylated anthocyanins from red cabbage, purple sweet potato, and Tradescantia pallida leaves as natural food colourants by HPLC-DAD-ESI(+)-QTOF-MS/MS and ESI(+)-MS analysis.

Anthocyanins in red cabbage, sweet potato, and Tradescantia pallida leaves were characterised. A total of 18 non-, mono-, and diacylated cyanidins was identified in red cabbage by high performance liquid chromatography-diode array detection coupled to high-resolution and multi-stage mass spectrometry. Sweet potato leaves contained 16 different cyanidin- and peonidin glycosides being predominantly mono- and diacylated.

Polymorphic transition due to grinding: the case of 3-[1-(tert-butoxycarbonyl)azetidin-3-yl]-1,2-oxazole-4-carboxylic acid.

A polymorphic transition as a result of grinding was found for 3-[1-(tert-butoxycarbonyl)azetidin-3-yl]-1,2-oxazole-4-carboxylic acid. The thorough study of polymorphic structures before and after crystal structure transformation has revealed some pre-conditions for a polymorphic transition and regularities of changes in molecular and crystal structure. In metastable polymorph 1a, the conformationally flexible molecule adopts a conformation with the higher energy and forms a less preferable linear supramolecular synthon.

4-[(Benzyl-amino)-carbon-yl]-1-methyl-pyridinium bromide hemihydrate: X-ray diffraction study and Hirshfeld surface analysis.

The hemihydrate of 4-[(benzyl-amino)-carbon-yl]-1-methyl-pyridinium bromide, CHNO·Br·0.5HO, was studied by single-crystal and powder X-ray diffraction methods. In the asymmetric unit, two organic cations of similar conformation, two bromide anions and one water mol-ecule are present.

4-[(Benzyl-amino)-carbon-yl]-1-methyl-pyridinium halogenide salts: X-ray diffraction study and Hirshfeld surface analysis.

Two salts of 4-[(benzyl-amino)-carbon-yl]-1-methyl-pyridinium () with chloride (CHNO·Cl) and bromide (CHNO·Br) anions were studied and compared with the iodide salt. crystallizes in the centrosymmetric space group 2/ while and form crystals in the Sohncke space group 222. Crystals of are isostructural to those of .

1-Allyl-4-hydroxy-2,2-dioxo-N-(4-methoxyphenyl)-1H-2λ,1-benzothiazine-3-carboxamide: polymorphic transition due to grinding with the loss of the biological activity.

A study of two polymorphic forms of 1-allyl-4-hydroxy-2,2-dioxo-N-(4-methoxyphenyl)-1-2λ,1-benzothiazine-3-carboxamide (a structural analogue of piroxicam) has revealed some regularities in the crystal structure formation due to different evaporation rates from the tested solvents. The monoclinic polymorph crystallized from ethyl acetate is formed due to a large number of very weak C-H..

Mixed-metal phosphates KNaTiFe(PO) and KNaTiFe(PO) with a langbeinite framework.

Single crystals of the langbeinite-type phosphates KNaTiFe(PO) and KNaTiFe(PO) were grown by crystallization from high-temperature self-fluxes in the system NaO-KO-PO-TiO-FeO using fixed molar ratios of (Na+K):P = 1.0, Ti:P = 0.20 and Na:K = 1.

Salts of 4-[(benzyl-amino)-carbon-yl]-1-methyl-pyridinium and iodide anions with different cation:iodine stoichiometric ratios.

The two iodide salts, 4-[(benzyl-amino)-carbon-yl]-1-methyl-pyridinium iodide-iodine (2/1), CHNO·I·0.5I, , and 4-[(benzyl-amino)-carbon-yl]-1-methyl-pyridinium triiodide, CHNO·I , , with different cation:iodine atoms ratios were studied. Salt contains one cation, one iodide anion and half of the neutral I mol-ecule in the asymmetric unit (cation:iodine atoms ratio is 1:2).

Structural features of the oxidonitridophosphates K (PO)N ( = Al, Ga).

Cubic crystals of tripotassium aluminium (or gallium) nitridotriphosphate, K (PO)N ( = Al, Ga), were grown by application of the self-flux method. In their isostructural crystal structures, all metal cations and the N atom occupy special positions with site symmetry 3, while the P and O atoms are situated in general positions. The three-dimensional framework of these oxidonitridophosphates is built up from [ O] octa-hedra linked together (PO)N groups.

Usage of Quantum Chemical Methods to Understand the Formation of Concomitant Polymorphs of Acetyl 2-(-(2-Fluorophenyl)imino)coumarin-3-carboxamide.

Crystallization of concomitant polymorphs is a very intriguing process that is difficult to be studied experimentally. A comprehensive study of two polymorphic modifications of acetyl 2-(-(2-fluorophenyl)imino)coumarin-3-carboxamide using quantum chemical methods has revealed molecular and crystal structure dependence on crystallization conditions. Fast crystallization associated with a kinetically controlled process results in the formation of a columnar structure with a nonequilibrium molecular conformation and more isotropic topology of interaction energies between molecules.

Scheelite-related MBiVMoO (M- Ca, Sr) solid solution-based photoanodes for enhanced photoelectrochemical water oxidation.

The photoelectrochemical properties of scheelite-related MBiVMoO (M = Ca, Sr, x = 0.1 to 0.9) solid solutions deposited on conductive glass (coated with SnO, F-doped) have been investigated as photoanodes in photoelectrochemical (PEC) water splitting.

Synthesis, Crystal Structure, and Biological Activity of Ethyl 4-Methyl-2,2-dioxo-1-2λ⁶,1-benzothiazine-3-carboxylate Polymorphic Forms.

Continuing the search for new potential analgesics among the derivatives of 4-methyl-2,2-dioxo-1-2λ⁶,1-benzothiazine-3-carboxylic acid, the possibility of obtaining its esters by the alkylation of the corresponding sodium salt with iodoethane in dimethyl sulfoxide (DMSO) at room temperature was studied. It was found that under such conditions, together with the oxygen atom of the carboxyl group, a heteroatom of nitrogen is also alkylated. Therefore, the product of the reaction studied is a mixture of ethyl 4-methyl-2,2-dioxo-1-2λ⁶,1-benzothiazine-3-carboxylate (major) and its 1-ethyl-substituted analog (minor).

New complex phosphates CsMBi(PO) (M - Ca, Sr and Pb): synthesis, characterization, crystal and electronic structure.

Herein, the peculiarities of complex phosphate formation in self-fluxes of Cs-M-Bi-P-O (M = Ca, Sr, Ba and Pb) systems with Cs/P = 0.7-1.3 at fixed ratios of Bi/P = 0.

Novel modification of anhydrous transition metal oxalates from powder diffraction.

The known metal-CO structures may be divided into two modifications, α and β. The α-modification has an order-disorder struxture, revealing one-dimensional disordering of the metal-oxalate chains, and the β-modification is ordered. The crystal structures of orthorhombic γ-MnCO {poly[μ-oxalato-manganese(II)]; space group Pmna, a = 7.

Clinical Evidence of Disease Anticipation in Families Segregating a C9orf72 Repeat Expansion.

Importance: Patients carrying a C9orf72 repeat expansion leading to frontotemporal dementia and/or amyotrophic lateral sclerosis have highly variable ages at onset of disease, suggesting the presence of modifying factors.

Objective: To provide clinical-based evidence for disease anticipation in families carrying a C9orf72 repeat expansion by analyzing age at onset, disease duration, and age at death in successive generations.

Design, Setting, And Participants: This cohort study was performed from June 16, 2000, to June 1, 2016, in 36 extended Belgian families in which a C9orf72 repeat expansion was segregating.

TBK1 Mutation Spectrum in an Extended European Patient Cohort with Frontotemporal Dementia and Amyotrophic Lateral Sclerosis.

We investigated the mutation spectrum of the TANK-Binding Kinase 1 (TBK1) gene and its associated phenotypic spectrum by exonic resequencing of TBK1 in a cohort of 2,538 patients with frontotemporal dementia (FTD), amyotrophic lateral sclerosis (ALS), or FTD plus ALS, ascertained within the European Early-Onset Dementia Consortium. We assessed pathogenicity of predicted protein-truncating mutations by measuring loss of RNA expression. Functional effect of in-frame amino acid deletions and missense mutations was further explored in vivo on protein level and in vitro by an NFκB-induced luciferase reporter assay and measuring phosphorylated TBK1.

Two pseudo-enantiomeric forms of N-benzyl-4-hydroxy-1-methyl-2,2-dioxo-1H-2λ(6),1-benzothiazine-3-carboxamide and their analgesic properties.

The fact that molecular crystals exist as different polymorphic modifications and the identification of as many polymorphs as possible are important considerations for the pharmaceutic industry. The molecule of N-benzyl-4-hydroxy-1-methyl-2,2-dioxo-1H-2λ(6),1-benzothiazine-3-carboxamide, C17H16N2O4S, does not contain a stereogenic atom, but intramolecular hydrogen-bonding interactions engender enantiomeric chiral conformations as a labile racemic mixture. The title compound crystallized in a solvent-dependent single chiral conformation within one of two conformationally polymorphic P212121 orthorhombic chiral crystals (denoted forms A and B).

Structural transformation of Bi1-x/3V1-xMoxO4 solid solutions for light-driven water oxidation.

The influence of molybdenum content in the solid solutions of Bi1-x/3V1-xMoxO4 (x = 0.05-0.20) on the morphology, band gap, structure and light-driven water oxidation properties has been studied by scanning electron microscopy, X-ray powder diffraction and vibrational spectroscopy (Raman and infrared).

Loss of TBK1 is a frequent cause of frontotemporal dementia in a Belgian cohort.

Objective: To assess the genetic contribution of TBK1, a gene implicated in amyotrophic lateral sclerosis (ALS), frontotemporal dementia (FTD), and FTD-ALS, in Belgian FTD and ALS patient cohorts containing a significant part of genetically unresolved patients.

Methods: We sequenced TBK1 in a hospital-based cohort of 482 unrelated patients with FTD and FTD-ALS and 147 patients with ALS and an extended Belgian FTD-ALS family DR158. We followed up mutation carriers by segregation studies, transcript and protein expression analysis, and immunohistochemistry.

The C9orf72 repeat size correlates with onset age of disease, DNA methylation and transcriptional downregulation of the promoter.

Pathological expansion of a G4C2 repeat, located in the 5' regulatory region of C9orf72, is the most common genetic cause of frontotemporal lobar degeneration (FTLD) and amyotrophic lateral sclerosis (ALS). C9orf72 patients have highly variable onset ages suggesting the presence of modifying factors and/or anticipation. We studied 72 Belgian index patients with FTLD, FTLD-ALS or ALS and 61 relatives with a C9orf72 repeat expansion.

The solid solution K3.84Ni0.78Fe3.19(PO4)5.

The title compound, tetra-potassium tetra-[nickel(II)/iron(III)] penta-kis-(orthophosphate), K3.84Ni0.78Fe3.

KNi(0.93)Fe(II)(0.07)Fe(III)(PO4)2: a new type of structure for a compound of composition M(I)M(II)M(III)(PO4)2.

The solid solution KNi(0.93)Fe(II)(0.07)Fe(III)(PO4)2 {potassium [nickel(II)/iron(II)] iron(III) bis(orthophosphate)} has been prepared by the flux method.