Search results for "Powder diffraction"
showing 10 items of 243 documents
ChemInform Abstract: Crystal Structures of New Ternary Compounds in RE-Pt-Pb and RE-Au-Pb Systems (RE = Rare Earth Metal).
2012
Abstract The crystal structures of the compounds RE 2 Pt 2 Pb (RE = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu; Mo 2 FeB 2 structure type, space group P 4/ mbm , Pearson code tP10 ), REPtPb (RE = La, Ce, Pr, Nd, Sm; ZrNiAl structure type, space group P 6 ¯ 2 m , Pearson code hP9 ), RE 2 Au 2 Pb (RE = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu; Er 2 Au 2 Sn structure type, space group P 4 2 / mnm , Pearson code tP20 ) and REAuPb (RE = Tm, Yb and Lu) were determined using X-ray powder diffraction.
Two polymorphs of afobazole from powder diffraction data
2012
Afobazole {systematic name: 2-[2-(morpholin-4-yl)ethylsulfanyl]-1H-benzimidazole} is a new anxiolytic drug and Actins, Auzins & Petkune [(2012). Eur. Patent EP10163962] described four polymorphic modifications. In the present study, the crystal structures of two monoclinic polymorphs, 5-ethoxy-2-[2-(morpholin-4-ium-4-yl)ethylsulfanyl]-1H-benzimidazol-3-ium dichloride, C15H23N3O2S2+·2Cl−, (II) and (IV), have been established from laboratory powder diffraction data. The crystal packing and conformation of the dications in (II) and (IV) are different. In (II), there are channels in the [001] direction, which offer atmospheric water molecules an easy way of penetrating into the crystal stru…
Crystallization, spectral, crystallographical, and thermoanalytical studies of succinobucol polymorphism.
2011
Four different polymorphs, A, C, D, and E, of succinobucol were isolated and characterized by means of solid-state nuclear magnetic resonance spectroscopy, single crystal and powder X-ray diffraction, differential scanning calorimetry, thermogravimetry, and attenuated total reflection–infrared spectroscopy. From a number of experiments, the same polymorphs (C, D, and E) and an equilibrium phase mixture B consisting of polymorphs C and D were repeatedly gained using different solvents or their mixtures. Although polymorph A was obtained directly from recrystallization only on few occasions, polymorphs C, D, and E proved to be metastable kinetic polymorphs, which slowly transform to a thermod…
Evaluation of drug-polymer solubility curves through formal statistical analysis: comparison of preparation techniques.
2014
ABSTRACT: In this study, the influence of the preparation technique (ball milling, spray drying, and film casting) of a supersaturated amorphous dispersion on the quality of solubility determinations of indomethacin in polyvinylpyrrolidone was investigated by means of statistical analysis. After annealing of the amorphous dispersions above the crystallization temperature for 2 h, the solubility curve was derived from the glass transition temperature of the demixed material using the Gordon–Taylor relationship and fitting with the Flory–Huggins model. The study showed that the predicted solubility from the ball-milled mixtures was not consistent with those from spray drying and film casting,…
Solvates of Dasatinib: Diversity and Isostructurality
2015
A series of dasatinib crystalline forms were obtained, and a hierarchical cluster analysis of their powder X-ray diffraction patterns was performed. The resulting dendrogram implies 3 structural groups. The crystal structures of several solvates representing 2 of these groups were determined. The crystal structure analysis confirms the isostructurality of solvates within structural group I and suggests a correlation between solvent molecule size and trends in crystal structures within this group. In addition, the formation relationships in 2-solvent media between different dasatinib solvate groups were determined. The formation preference of solvates was found to follow the ranking group I …
Investigation of the phase transitions occurring during and after the dehydration of xylazine hydrochloride monohydrate.
2014
This paper reports an investigation of a complex solid state phase transition where two inter-converting polymorphs (X and A) of the pharmaceutical molecule xylazine hydrochloride formed and transformed during and after the dehydration of its monohydrate (H). The crystal structures of all three forms were compared. During the investigation of this solid state phase transition it was determined that the dehydration of H produced either a pure X form, or a mixture of the X and A forms. The phase composition depended on the sample preparation procedure and the experimental conditions. It was found that grinding of the hydrate enhanced the formation of polymorph X as a product of dehydration, w…
Controlling the molecular diffusion in MOFs with the acidity of monocarboxylate modulators.
2021
The catalytic performance of metal-organic frameworks (MOFs) is related to their physicochemical properties, such as particle size, defect-chemistry and porosity, which synthetic control can be potentially achieved by coordination modulation. By combining PXRD, 1HNMR, FT-IR, N2 uptake measurements we have found insights that the different types of defects (missing linker or missing clusters consequence of the spatial distribution of missing linkers, and the combination of both) could be controlled by the type of modulator employed. We show that the molar percent of defects, either as missing linkers or as part of missing cluster defects, is related to the modulator’s acidity and subse…
The influence of the raw material and production method on the morphology, microstructure, chemical and phase composition of tetrabasic lead sulfate …
1992
Abstract Tetrabasic lead sulfate (4BS) produced by two different methods (solution and paste) and from two different raw materials (tetragonal PbO and leady oxide) were charaterized by different analytical techniques. The techniques applied were wet-chemical methods, scanning electron microscopy, transmission electron microscopy and X-ray powder diffraction. The preparation method was observed to be the most decisive factor influencing the structure and the morphology of the 4BS pastes in this study.
Unraveling the packing pattern leading to gelation using SS NMR and X-ray diffraction: direct observation of the evolution of self-assembled fibers
2010
A detailed understanding of the mode of packing patterns that leads to the gelation of low molecular mass gelators derived from bile acid esters was carried out using solid state NMR along with complementary techniques such as powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and polarizing optical microscopy (POM). Solid state 13C{1H} cross polarization (CP) magic angle spinning (MAS) NMR of the low molecular mass gel in its native state was recorded for the first time. A close resemblance in the packing patterns of the gel, xerogel and bulk solid states was revealed upon comparing their 13C{1H}CPMAS NMR spectral pattern. A doublet r…
Preparation and recrystallization behavior of spray-dried co-amorphous naproxen–indomethacin
2016
To improve the dissolution properties and the physical stability of amorphous active pharmaceutical ingredients, small molecule stabilizing agents may be added to prepare co-amorphous systems. The objective of the study was to investigate if spray-drying allows the preparation of co-amorphous drug-drug systems such as naproxen-indomethacin and to examine the influence of the process conditions on the resulting initial sample crystallinity and the recrystallization behavior of the drug(s). For this purpose, the process parameters inlet temperature and pump feed rate were varied according to a 2(2) factorial design and the obtained samples were analyzed with X-ray powder diffractometry and Fo…