Ab-initio crystal structure analysis and refinement approaches of oligo p-benzamides based on electron diffraction data

Ab-initio crystal structure analysis of organic materials from electron diffraction data is presented. The data were collected using the automated electron diffraction tomography (ADT) technique. The structure solution and refinement route is first validated on the basis of the known crystal structure of tri-p-benzamide. The same procedure is then applied to solve the previously unknown crystal structure of tetra-p-benzamide. In the crystal structure of tetra-p-benzamide, an unusual hydrogen-bonding scheme is realised; the hydrogen-bonding scheme is, however, in perfect agreement with solid-state NMR data

CXCL16 and oxLDL are induced in the onset of diabetic nephropathy

Diabetic nephropathy (DN) is a major cause of end-stage renal failure worldwide. Oxidative stress has been reported to be a major culprit of the disease and increased oxidized low density lipoprotein (oxLDL) immune complexes were found in patients with DN. In this study we present evidence, that CXCL16 is the main receptor in human podocytes mediating the uptake of oxLDL. In contrast, in primary tubular cells CD36 was mainly involved in the uptake of oxLDL. We further demonstrate that oxLDL down-regulated α3-integrin expression and increased the production of fibronectin in human podocytes. In addition, oxLDL uptake induced the production of reactive oxygen species (ROS) in human podocytes. Inhibition of oxLDL uptake by CXCL16 blocking antibodies abrogated the fibronectin and ROS production and restored α3 integrin expression in human podocytes. Furthermore we present evidence that hyperglycaemic conditions increased CXCL16 and reduced ADAM10 expression in podocytes. Importantly, in streptozotocin-induced diabetic mice an early induction of CXCL16 was accompanied by higher levels of oxLDL. Finally immunofluorescence analysis in biopsies of patients with DN revealed increased glomerular CXCL16 expression, which was paralleled by high levels of oxLDL. In summary, regulation of CXCL16, ADAM10 and oxLDL expression may be an early event in the onset of DN and therefore all three proteins may represent potential new targets for diagnosis and therapeutic intervention in DN

A Fast and Sustainable Route to Bassanite Nanocrystals from Gypsum

Calcium sulfate is an important construction material. More than 1600 million square meters of interior surfaces are covered with plasterboards in Europe each year. Plasterboard is manufactured by transforming mined or recycled gypsum (CaSO4 × 2 H2O) to bassanite (CaSO4 × ½H2O) in a time- and energy-consuming heating process. A fast and sustainable way to produce bassanite by solvent-assisted milling, thereby eliminating the need for energy-intensive dehydration, is described. The milling reaction is complete after ≈200 min. Kinetic studies revealed that gypsum crystals transform to bassanite by shear forces during milling. 1H nuclear magnetic resonance (NMR) spectroscopic techniques and Fourier-transform infrared spectroscopy (FT-IR) show that the resulting bassanite nanocrystals are stabilized by surface functionalization with the auxiliary solvent methanol. Bassanite particles produced over extended milling times of 990 min form long-term stable dispersions without stabilizers and no signs of precipitation. Addition of water to bassanite leads to instant agglomeration, followed by a phase change to gypsum. The dispersibility in volatile methanol and the elucidation of the crystallization mechanism allow also for applications of the bassanite nanocrystals in hybrid materials. © 2022 The Authors. Advanced Functional Materials published by Wiley-VCH GmbH

Electrochemical Reduction and Oxidation of Ruddlesden–Popper-Type La2_{2}NiO3_{3}F2_{2} within Fluoride-Ion Batteries

Within this article, it is shown that an electrochemical defluorination and additional fluorination of Ruddlesden–Popper-type La$_2$NiO$_3$F$_2$ is possible within all-solid-state fluoride-ion batteries. Structural changes within the reduced and oxidized phases have been examined by X-ray diffraction studies at different states of charging and discharging. The synthesis of the oxidized phase La$_2$NiO$_3$F$_{2+x}$ proved to be successful by structural analysis using both X-ray powder diffraction and automated electron diffraction tomography techniques. The structural reversibility on re-fluorinating and re-defluorinating is also demonstrated. Moreover, the influence of different sequences of consecutive reduction and oxidation steps on the formed phases has been investigated. The observed structural changes have been compared to changes in phases obtained via other topochemical modification approaches such as hydride-based reduction and oxidative fluorination using F$_2$ gas, highlighting the potential of such electrochemical reactions as alternative synthesis routes. Furthermore, the electrochemical routes represent safe and controllable synthesis approaches for novel phases, which cannot be synthesized via other topochemical methods. Additionally, side reactions, occurring alongside the desired electrochemical reactions, have been addressed and the cycling performance has been studied