Structural characterization of iron oxide/hydroxide nanoparticles in nine different parenteral drugs for the treatment of iron deficiency anaemia by electron diffraction (ED) and X-ray powder diffraction (XRPD)

Drug products containing iron oxide and hydroxide nanoparticles (INPs) are important for the treatment of iron deficiency anaemia. Pharmaceuticals prepared by the complexation of different kinds of INPs and carbohydrates have different physicochemical and biopharmaceutic characteristics. The increasing number of parenteral non-biological complex drugs (NBCD) containing iron requires physicochemical methods for characterization and enabling of cross comparisons. In this context the structure and the level of crystallinity of the iron phases may be connected to the in vitro and in vivo dissolution rates, which etiologically determine the therapeutic and toxic effects. X-ray powder diffraction…

Automated Diffraction Tomography: A New Era for Electron Crystallography

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Ab Initio Structure Determination of Vaterite by Automated Electron Diffraction

tion that is fundamental for understanding material properties. Still, a number of compounds have eluded such kinds of analysis because they are nanocrystalline, highly disordered, with strong pseudosymmetries or available only in small amounts in polyphasic or polymorphic systems. These materials are crystallographically intractable with conventional Xray or synchrotron radiation diffraction techniques. Single nanoparticles can be visualized by high-resolution transmission electron microscopy (HR-TEM) up to sub�ngstrom resolution, [2] but obtaining 3D information is still a difficult task, especially for highly beam-sensitive materials and crystal structures with long cell parameters. Elec…

Structural insights into M2O-Al2O3-WO3 (M = Na, K) system by electron diffraction tomography.

TheM2O–Al2O3–WO3(M= alkaline metals) system has attracted the attention of the scientific community because some of its members showed potential applications as single crystalline media for tunable solid-state lasers. These materials behave as promising laser host materials due to their high and continuous transparency in the wide range of the near-IR region. A systematic investigation of these phases is nonetheless hampered because it is impossible to produce large crystals and only in a few cases a pure synthetic product can be achieved. Despite substantial advances in X-ray powder diffraction methods, structure investigation on nanoscale is still challenging, especially when the sample i…

Synthesis of a New Copper-Azobenzene Dicarboxylate Framework in the Form of Hierarchical Bulk Solids and Thin Films without and with Patterning

Reaction of copper(II) acetate with azobenzene-4,4′-dicarboxylic acid results in the formation of a metal–organic framework with the unexpected stoichiometry of Cu(II):ligand of 2:1. The bulk synthesis results in microspheres assembled from either nanobricks or nanoflakes, depending on the ratio of the reactants in solution. While the former behaves like a bulk solid with clear reflections in the X-ray and electron diffraction experiments, the latter obviously is dominated by surface effects, with a significant fraction of slightly expanded elemental cells and a significantly increased outer surface area. The material could also be deposited on a variety of surfaces using a stepwise layer-b…

Structure analysis of titanate nanorods by automated electron diffraction tomography

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 …

Artificial granularity in two-dimensional arrays of nanodots fabricated by focused-electron-beam-induced deposition.

We have prepared 2D arrays of nanodots embedded in an insulating matrix by means of focused-electron-beam-induced deposition using the W(CO)(6) precursor. By varying the deposition parameters, i.e. the electron beam current and energy and the raster constant, we obtain an artificial granular material with tunable electrical properties. The analysis of the temperature dependence of the conductivity and of the current-voltage characteristic suggests that the transport mechanism is governed by electron tunneling between artificial grains. In order to understand the nature of the granularity and thus the microstructural origin of the electronic transport behavior, we perform TEM and micro-Raman…

Ab-initio-Strukturbestimmung von Vaterit mit automatischer Beugungstomographie

Snapshots of the Formation of NaTi3O6(OH)·2H2O Nanowires: A Time-Resolved XRD/HRTEM Study

Layered titanates are important intermediates during the formation of TiO2-related nanostructures in hot concentrated base solution. Microwave-assisted hydrothermal techniques allow a time-resolved ex-situ analysis of the reaction in one-minute intervals by rapid heating and quenching followed by separation and structure analysis of the intermediates. By a combination of powder X-ray diffraction, high resolution electron microscopy (HRTEM), and selected area electron diffraction (SAED) the individual stages of the reaction could be identified. Sodium titanate nanosheets are formed within several minutes by digesting the crystalline TiO2-P25 precursor in NaOH. These nanosheets with a low sod…

Snapshots of calcium carbonate formation – a step by step analysis

Abstract Recent advances in our understanding of CaCO3 nucleation from solution have provoked new and challenging questions. We have studied CaCO3 formation using precipitation by carbonate ester hydrolysis which ensures precipitation from a strictly homogeneous solution state and allows “titrating” carbonate to a solution with a given Ca2+ concentration on a timescale suited for kinetic studies. Nucleation and crystallization were traced by combining dynamic light scattering (DLS) and transmission electron microscopy (TEM). DLS served as in situ technique to identify the nucleation time, to monitor particle size evolution, to discriminate different precipitation mechanisms and to validate …

CCDC 1429729: Experimental Crystal Structure Determination

Related Article: Enrico Mugnaioli, Iryna Andrusenko, Timo Schüler, Niklas Loges, Robert E. Dinnebier, Martin Panthöfer, Wolfgang Tremel, Ute Kolb|2012|Angew.Chem.,Int.Ed.|51|7041|doi:10.1002/anie.201200845

CCDC 1429728: Experimental Crystal Structure Determination

Related Article: Enrico Mugnaioli, Iryna Andrusenko, Timo Schüler, Niklas Loges, Robert E. Dinnebier, Martin Panthöfer, Wolfgang Tremel, Ute Kolb|2012|Angew.Chem.,Int.Ed.|51|7041|doi:10.1002/anie.201200845