The localization of hydrogen atoms is an essential part crystal structure analysis, but it difficult because their small scattering power. We report the direct in nanocrystalline materials, achieved using recently developed approach dynamical refinement precession electron diffraction tomography data. used this method to locate both organic (paracetamol) and inorganic (framework cobalt aluminophosphate) material. results demonstrate that technique can reliably reveal fine structural details,...

Electron diffraction tomography (EDT) data are in many ways similar to X-ray data. However, they also present certain specifics. One of the most noteworthy is specific rocking curve observed for EDT collected using precession electron method. This double-peaked (dubbed `the camel') may be described with an approximation based on a circular integral pseudo-Voigt function and used intensity extraction by profile fitting. Another aspect high likelihood errors estimation crystal orientation,...

Determination of the absolute configuration organic molecules is essential in drug development and subsequent approval process. We show that this determination possible through electron diffraction using nanocrystalline material. Ab initio structure by has so far been limited to compounds maintain their crystallinity after a dose one per square angstrom or more. present complete analysis pharmaceutical cocrystal sofosbuvir l-proline, which about order magnitude less stable. Data collection...

Abstract Small‐pore zeolites such as chabazite (CHA) are excellent candidates for the selective separation of CO 2 ; however, current synthesis involves several steps and use organic structure‐directing agent (OSDA), increasing their cost energy requirements. We report small‐pore zeolite crystals (aluminosilicate) with CHA‐type framework structure by direct in a colloidal suspension containing mixture inorganic cations only (Na + , K Cs ). The location molecules host was revealed 3D electron...

Abstract Metal–organic frameworks (MOFs) are a chemically and topologically diverse family of materials composed inorganic nodes organic linkers bound together by coordination bonds. Presented here two significant innovations in this field. The first is the use new group, phenylene‐1,4‐bis(methylphosphinic acid) (PBPA), phosphinic acid analogue commonly used terephtalic acid. Use linker group leads to formation hydrothermally stable permanently porous MOF structure. second innovation...

Determination of lattice parameters from 3D electron diffraction (3D ED) data measured in a transmission microscope is hampered by number effects that seriously limit the achievable accuracy. The distortion patterns optical elements often most severe problem. A thorough analysis experimental datasets shows that, addition to well known distortions, namely barrel-pincushion, spiral and elliptical, an additional distortion, dubbed parabolic, may be observed data. In precession data, parabolic...

Dynamical refinement is a well established method for refining crystal structures against 3D electron diffraction (ED) data and its benefits have been discussed in the literature [Palatinus, Petříček & Corrêa, (2015). Acta Cryst. A 71 , 235–244; Palatinus, Corrêa et al. B 740–751]. However, until now, dynamical refinements only conducted using independent atom model (IAM). Recent research has shown that more accurate description can be achieved by applying transferable aspherical (TAAM),...

The influence of added sucrose on the phase composition iron oxide nanoparticles was studied in Fe2O3/SiO2 nanocomposites. nanocomposites were prepared by impregnation mesoporous silica SBA-15 with nitrate containing various amounts and their subsequent annealing at 1100 1200 °C. analyzed X-ray diffraction 57Fe Mössbauer spectroscopy polycrystalline samples. Profile analysis maxima used to determine apparent crystallite size different polymorphs. content β-Fe2O3 samples increased an...

The nanoparticles of ε-Fe2O3 enriched with 57Fe isotope in amorphous silica matrix were prepared by sol-gel technique starting from a single molecular precursor for both Fe2O3 and silica. From the X-ray powder diffraction pattern was identified as major phase α-Fe2O3 β-Fe2O3 observed minor iron oxide phases. Using log-normal distribution fitting experimental data TEM micrographs, characteristic size particles d0 ∼ 25 nm derived. rather high coercivity ∼2.1 T at room temperature confirmed our...

Layered materials, like transition metal dichalcogenides, exhibit broad spectra with outstanding properties huge application potential, whereas another group of related layered trichalcogenides, remains unexplored. Here, we show the potential this interesting structural type tantalum trisulfide prepared in a form nanofibers. This material shows tailorable attractive electronic dependent on tensile strain applied to it. Structure so-called orthorhombic phase TaS3 grown long nanofibers has...

The hydration/dehydration behavior of four distinct channel hydrates sitagliptin L-tartrate (SLT) was investigated by thermoanalytical methods, dynamic vapour sorption analysis and variable humidity X-ray powder diffraction. crystal structures were determined from single diffraction data. A survey the forms revealed that SLT exhibit both stoichiometric non-stoichiometric features demonstrating characterization can be challenging as their is not inevitably unambiguous. Upon dehydration,...

Abstract Metal–organic frameworks (MOFs) are a chemically and topologically diverse family of materials composed inorganic nodes organic linkers bound together by coordination bonds. Presented here two significant innovations in this field. The first is the use new group, phenylene‐1,4‐bis(methylphosphinic acid) (PBPA), phosphinic acid analogue commonly used terephtalic acid. Use linker group leads to formation hydrothermally stable permanently porous MOF structure. second innovation...

Cerium dioxide is a scientifically and technologically important material with wide range of potential applications, particularly in solid oxide fuel cells catalysis. Herein, we report study focusing on the synthesis nanocrystalline cerium via thermal decomposition oxalate salt. Simply by changing reaction conditions (temperature, concentration, acidity, strike) during precipitation solution oxalic acid, were able to obtain different morphologies. The main parameters mapped linked morphology...

High-entropy ceramics is a new class of materials having great potential and wide application. The carbide Ti, Zr, Hf, Ta, Nb typical member this group. It has been synthesized mostly through blending, milling, high-temperature solid-state reaction metal precursors for each metal. This route needs extremely high temperature (2300 °C), which makes it energy technology demanding. We have developed chemical high-entropy powder that synthetic several hundred degrees Celsius lower. A solution...

An interdisciplinary approach to derive the structure of a disordered supramolecular system.

Four crystalline polymorphs of the proinsecticide chlorfenapyr [4-bromo-2-(4-chlorophenyl)-1-ethoxymethyl-5-trifluoromethyl-1

Many long-lasting insecticidal bed nets for protection against disease vectors consist of poly(ethylene) fibers in which insecticide is incorporated during manufacture. Insecticide molecules diffuse from within the supersaturated polymers to surfaces where they become bioavailable insects and often crystallize, a process known as blooming. Recent studies revealed that contact insecticides can be highly polymorphic. Moreover, activity polymorph-dependent, with forms having higher crystal free...