Search results for " powder diffraction"

Electron diffraction, X-ray powder diffraction and pair-distribution-function analyses to determine the crystal structures of Pigment Yellow 213, C23…

2009

The crystal structure of the nanocrystalline alpha phase of Pigment Yellow 213 (P.Y. 213) was solved by a combination of single-crystal electron diffraction and X-ray powder diffraction, despite the poor crystallinity of the material. The molecules form an efficient dense packing, which explains the observed insolubility and weather fastness of the pigment. The pair-distribution function (PDF) of the alpha phase is consistent with the determined crystal structure. The beta phase of P.Y. 213 shows even lower crystal quality, so extracting any structural information directly from the diffraction data is not possible. PDF analysis indicates the beta phase to have a columnar structure with a si…

Structure analysis of titanate nanorods by automated electron diffraction tomography

2011

A hitherto unknown phase of sodium titanate, NaTi3O6(OH)·2H2O, was identified as the intermediate species in the synthesis of TiO2 nanorods. This new phase, prepared as nanorods, was investigated by electron diffraction, X-ray powder diffraction, thermogravimetric analysis and high-resolution transmission electron microscopy. The structure was determined ab initio using electron diffraction data collected by the recently developed automated diffraction tomography technique. NaTi3O6(OH)·2H2O crystallizes in the monoclinic space group C2/m. Corrugated layers of corner- and edge-sharing distorted TiO6 octahedra are intercalated with Na+ and water of crystallization. The nanorods are typically …

Heterovalent BiIII/PbII ionic substitution in one-dimensional trimethylsulfoxonium halide pseudo-perovskites (X = I, Br)

2021

We report on the synthesis and characterization of novel lead and bismuth hybrid (organic-inorganic) iodide and bromide pseudo-perovskites (ABX3) containing the trimethylsulfoxonium cation (CH3)3SO+ (TMSO) in the A site, Pb/Bi in the B site, and Br or I as X anions. All of these compounds are isomorphic and crystallize in the orthorhombic Pnma space group. Lead-based pseudo-perovskites consist of one-dimensional (1D) chains of face-sharing [PbX6] octahedra, while in the bismuth-based ones, the chains of [BiX6] are interrupted, with one vacancy every third site, leading to a zero-dimensional (0D) local structure based on separated [Bi2I9]3- dimers. Five solid solutions for the iodide with di…

Synthesis, characterization and thermal properties of new aromatic quaternary ammonium bromides

2004

Series of new aromatic R 2R′ 2N +Br - (R=benzyl, 4-methylbenzyl, 2-phenylethyl, 3-phenylpropyl; R′=ethyl, methyl, isopropyl) or RR′ 2NH +Br --type (R=benzyl, R′=isopropyl) quaternary ammonium bromides were prepared by using novel synthetic route in which a formamide (N,N-diethylformamide, N,N-dimethylformamide, N,N-diisopropylformamide) is treated with aralkyl halide in presence of a weak base. The compounds were characterized by 1H-NMR and 13C-NMR spectroscopy and mass spectrometry. Structures of the crystalline compounds were determined by X-ray single crystal diffraction, and in addition the powder diffraction method was used to study the structural similarities between the single crysta…

The comparison of seven different methods to quantify the amorphous content of spray dried lactose

2006

The purpose of this work was to verify the usefulness, advantages and disadvantages of seven methods that are widely used to detect, and quantify the amorphous contents in pharmaceutical solids. Here, StepScan DSC, a type of modulated temperature calorimetry method, was applied for the first time to quantify amorphicity. The comparison of the analytical methods was undertaken with real (non-artificial) test samples, i.e. spray-dried lactose samples with various degrees of crystallinity. In these samples, it was essential that the amorphous and the crystalline portions are not present as separate particles, which is the case when physical (artificial) mixtures of totally amorphous and totall…

Proton sponge lead halides containing 1D polyoctahedral chains

2021

Hybrid one-dimensional lead halides, containing the protonated 1,8-bis(dimethylamino)naphthalene moiety (C14H19N2, monoprotonated "proton sponge"), were prepared by simple one-pot methods and investigated in terms of crystal structure, morphology, thermal stability and electronic properties. The as-precipitated (C14H19N2)PbBr3 and (C14H19N2)PbI3 species are isostructural and crystallize in the orthorhombic Pbca space group, resulting in 1D crystal phases with ([PbX3](-))(infinity) chains (built by face-sharing [PbX6] octahedra; X = Br, I), among which the (C14H19N2)(+) cations are inserted. The two compounds display complete miscibility in the solid state: both (C14H19N2)PbI2Br and (C14H19N…

Neutron powder diffraction study in the mixed molecular system (NaCN)1−x(KCN)x

1989

A detailed structural analysis of (NaCN${)}_{1\mathrm{\ensuremath{-}}\mathrm{x}}$(KCN${)}_{\mathrm{x}}$ mixed crystals with x=0.02, 0.19, and 0.95 was performed by neutron powder diffraction. The structural parameters of the cubic phases were refined, applying a model of preferred orientations. Different noncubic low-temperature phases were observed for x=0.02 and 0.95. For x=0.02 the antiferroelectric ordering of ${\mathrm{CN}}^{\mathrm{\ensuremath{-}}}$ dipoles at low temperatures is accompanied by significant alkali-alkali and alkali-${\mathrm{CN}}^{\mathrm{\ensuremath{-}}}$ sublattice shifts. Structural data are presented together with previous results for mixed crystals with x=0.59 and…

Location of Water and Xylene Molecules Adsorbed on Prehydrated Zeolite BaX. A Low-Temperature Neutron Powder Diffraction Study

1999

Magnetoelectric coupling driven by inverse magnetostriction in multiferroic BiMn3Mn4O12

2013

By means of neutron powder diffraction, we investigated the effect of the polar Bi$^{3+}$ ion on the magnetic ordering of the Mn$^{3+}$ ions in BiMn$_3$Mn$_4$O$_{12}$, the counterpart with \textit{quadruple} perovskite structure of the \textit{simple} perovskite BiMnO$_3$. The data are consistent with a \textit{noncentrosymmetric} spacegroup $Im$ which contrasts the \textit{centrosymmetric} one $I2/m$ previously reported for the isovalent and isomorphic compound LaMn$_3$Mn$_4$O$_{12}$, which gives evidence of a Bi$^{3+}$-induced polarization of the lattice. At low temperature, the two Mn$^{3+}$ sublattices of the $A'$ and $B$ sites order antiferromagnetically (AFM) in an independent manner …

Impact of the use of sterically congested Ir(III) complexes on the performance of light-emitting electrochemical cells

2018

International audience; The synthesis, structural and optoelectronic characterization of a family of sterically congested cyclometalated cationic Ir(iii) complexes of the form [Ir(C^N)2(dtBubpy)]PF6 (with dtBubpy = 4,4′-di-tert-butyl-2,2′-bipyridine and C^N = a cyclometalating ligand decorated at the 4-position of the pyridine ring and/or the 3-position of the phenyl ring with a range of sterically bulky substituents) are reported. This family of complexes is compared to the unsubstituted analogue complex R1 bearing 2-phenylpyridinato as cyclometalating ligand. The impact of sterically bulky substituents on the C^N ligands on both the solid state photophysics and light-emitting electrochemi…