Search results for "Powder diffraction"
showing 10 items of 243 documents
Hexakis(dimethylformamide)iron(II) complex cation in hexahalorhenate(IV)-based salts: synthesis, X-ray structure and magnetic properties
2018
Two iron(II)-rhenium(IV) compounds of general formula [FeII(dmf)6][ReIVX6] [X = Cl (1) and Br (2); dmf = N,N-dimethylformamide] have been prepared and characterized. X-ray powder diffraction measurements on samples of 1 and 2 support the same structure for both systems. The crystal structure of 1 was determined by single-crystal X-ray diffraction. 1 crystallizes in the triclinic system with space group Pī. Each iron(II) is six-coordinate and bonded to six oxygens from six dmf molecules building a distorted octahedral environment. Rhenium(IV) is six-coordinate by six halide anions in an almost regular octahedral geometry. The magnetic properties were investigated from variable-temperature ma…
The essential identity of the framework structures of ZSM-8 and ZSM-5
1994
The crystal structures of TEA-ZSM-8 and its calcined template-free form have been studied by Rietveld analyses based on X-ray powder diffraction data. The results show that the aluminosilicate framework structure of ZSM-8 is essentially identical to that of ZSM-5. The tetraethylammonium molecule could be located in the difference Fourier analysis yielding positions similar to its TPA counterpart in ZSM-5. Lattice constants of ZSM-8 are in the same range as for ZSM-5. Contrary results are related to incorrectly indexed powder patterns. Optical investigations of ZSM-5 and ZSM-8 crystals showed that the zeolites studied here are both twinned exhibiting differently shaped twin individuals.
Spin-Crossover and Liquid Crystal Properties in 2D Cyanide-Bridged FeII−MI/II Metalorganic Frameworks
2010
Novel two-dimensional heterometallic Fe(II)-M(Ni(II), Pd(II), Pt(II), Ag(I), and Au(I)) cyanide-bridged metalorganic frameworks exhibiting spin-crossover and liquid crystal properties, formulated as {FeL(2)[M(I/II)(CN)(x)](y)}·sH(2)O, where L are the ligands 4-(4-alkoxyphenyl)pyridine, 4-(3,4-dialkoxyphenyl)pyridine, and 4-(3,4,5-trisalkoxyphenyl)pyridine, have been synthesized and characterized. The physical characterization has been carried out by means of EXAFS, X-ray powder diffraction, magnetic susceptibility, differential scanning measurements, and Mössbauer spectroscopy. The 2D Fe(II) metallomesogens undergo incomplete and continuous thermally induced spin transition at T(1/2) ≈ 170 …
Iron(II) metallomesogens based on symmetrical tripod ligands
2012
Abstract Novel mononuclear tripodand-based iron(II) complexes showing liquid crystal properties have been synthesized and characterized. These are based on ligands tris[3-aza-4-((5-Cn)(6-R-2-pyridyl))but-3-enyl]amine, where R = hydrogen or methyl, 1,3,5-cis,cis-tris[1-aza-2-((5-alkyloxy)(2-pyridyl))vinyl]cyclohexane and 2,2,2-tris(2-aza-3-((5-alkyloxy)(2-pyridyl))prop-2-enyl)ethane. The physical characterization has been carried out by means of single-crystal X-ray diffraction measurements, magnetic susceptibility, differential scanning calorimetry, X-ray powder diffraction and Mossbauer spectroscopy.
Validation of Powder X-Ray Diffraction Following EN ISO/IEC 17025
2012
: Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase iden…
Optimization of sample preparation conditions for detecting trace amounts of β-tegafur in α- and β-tegafur mixture.
2012
We report a semiquantitative method for determining trace amounts (<1%) of thermodynamically stable forms in polymorphic mixtures, focusing on sample preparation ef- fects on solid phase transitions. Tegafur (5-fluoro-1-(oxolan-2-yl)-1,2,3,4-tetrahydropyrimidine- 2,4-dione) was used as a model material in this study. The amounts of the thermodynamically stable $ tegafur were increased to levels detectable by powder X-ray diffractometry by grind- ing the samples in a ball mill in the presence of water. The limit of detection for this method was as low as 0.0005% of $ tegafur in " and $ tegafur mixtures. The amount of $ tegafur after sample preparation was found to be proportional to the init…
High-pressure crystal structure, lattice vibrations, and band structure of BiSbO4
2016
The high-pressure crystal structure, lattice-vibrations HP crystal structure, lattice vibrations, and band , and electronic band structure of BiSbO4 were studied by ab initio simulations. We also performed Raman spectroscopy, infrared spectroscopy, and diffuse-reflectance measurements, as well as synchrotron powder X-ray diffraction. High-pressure X-ray diffraction measurements show that the crystal structure of BiSbO4 remains stable up to at least 70 GPa, unlike other known MTO4-type ternary oxides. These experiments also give information on the pressure dependence of the unit-cell parameters. Calculations properly describe the crystal structure of BiSbO4 and the changes induced by pressur…
Anisotropic lattice distortions in biogenic calcite induced by intra-crystalline organic molecules.
2006
9 pages; International audience; We have performed precise structural measurements on five different calcitic seashells by high-resolution X-ray powder diffraction on a synchrotron beam line and by laboratory single crystal X-ray diffraction. The unit cell parameters a and c of biogenic calcite were found to be systematically larger than those measured in the non-biogenic calcite. The maximum lattice distortion (about 2.10(-3)) was detected along the c-axis. Under heat treatment above 200 degrees C, a pronounced lattice relaxation was observed, which allowed us to conclude that anisotropic lattice swelling in biogenic calcite is induced by organic macromolecules incorporated within the sing…
Structural properties of magnesium stearate pseudopolymorphs: effect of temperature.
2003
A thorough review of the relevant literature reveals that the interaction between water vapour and magnesium stearate, in contrast to many other metal soaps, is not properly understood. The structural modifications associated with the up-take or loss of water of vegetable-derived commercial magnesium stearate powders exposed to humid air or vacuum at room temperature are investigated using standard powder X-ray diffractometry. It is found that in such conditions magnesium stearate reacts reversibly with the vapour phase with structural consequences very similar to the high temperature transition between the crystalline and rotator phases of other anhydrous metal soaps. When temperature is i…
High-pressure powder x-ray diffraction study of EuVO4
2015
The high-pressure structural behavior of europium orthovanadate has been studied using in-situ, synchrotron based, high-pressure x-ray powder diffraction technique. Angle-dispersive x-ray diffraction measurements were carried out at room temperature up to 34.7 GPa using a diamond-anvil cell, extending the pressure range reported in previous experiments. We confirmed the occurrence of zircon-scheelite phase transition at 6.8 GPa and the coexistence of low- and high-pressure phases up to 10.1 GPa. In addition, clear evidence of a scheelite-fregusonite transition is found at 23.4 GPa. The fergusonite structure remains stable up to 34.7 GPa, the highest pressure reached in the present measureme…