ABSTRACT
The crystal structure of the title enanti-opure tetralol derivative {systematic name: (1S,2S)-2-[(S)-2,2,2-tri-fluoro-1-hy-droxy-eth-yl]-1,2,3,4-tetra-hydro-naph-thalen-1-ol}, C12H13F3O2, synthesized by asymmetric transfer hydrogenation, was elucidated by low-temperature single-crystal X-ray diffraction. The enanti-opure compound crystallizes in the Sohncke space group P212121 with one mol-ecule in the asymmetric unit and features intra-molecular as well as inter-molecular O-Hâ¯O hydrogen bonding. The absolute configuration was established from anomalous dispersion effects.
ABSTRACT
Hydraulic calcium silicate-based cements (HCSCs) have become a superior bioceramic alternative to epoxy-based root canal sealers in endodontics. A new generation of purified HCSCs formulations has emerged to address the several drawbacks of original Portland-based mineral trioxide aggregate (MTA). This study was designed to assess the physio-chemical properties of a ProRoot MTA and compare it with newly formulated RS+, a synthetic HCSC, by advanced characterisation techniques that allow for in situ analyses. Visco-elastic behaviour was monitored with rheometry, while phase transformation kinetics were followed by X-ray diffraction (XRD), attenuated total reflectance Fourier transform infrared (ATR-FTIR), and Raman spectroscopies. Scanning electron microscopy with energy-dispersive spectroscopy, SEM-EDS, and laser-diffraction analyses was performed to evaluate the compositional and morphological characteristics of both cements. While the kinetics of surface hydration of both powders, when mixed with water, were comparable, an order of magnitude finer particle size distribution of RS+ coupled with the modified biocompatible formulation proved pivotal in its ability to exert predictable viscous flow during working time, and it was more than two times faster in viscoelastic-to-elastic transition, reflecting improved handling and setting behaviour. Finally, RS+ could be completely transformed into hydration products, i.e., calcium silicate hydrate and calcium hydroxide, within 48 h, while hydration products were not yet detected by XRD in ProRoot MTA and were obviously bound to particulate surface in a thin film. Because of the favourable rheological and faster setting kinetics, synthetic, finer-grained HCSCs, such as RS+, represent a viable option as an alternative to conventional MTA-based HCSCs for endodontic treatments.
ABSTRACT
The crystal structure of the co-crystal of aqua-tri-fluorido-boron with two ethyl-ene carbonate (systematic name: 1,3-dioxolan-2-one) mol-ecules, BF3H2O·2OC(OCH2)2, was determined by low-temperature single-crystal X-ray diffraction. The co-crystal crystallizes in the ortho-rhom-bic space group P212121 with four formula units per unit cell. The asymmetric unit consists of an aqua-tri-fluorido-boron mol-ecule and two ethyl-ene carbonate mol-ecules, connected by O-Hâ¯O=C hydrogen bonds. This crystal structure is an inter-esting example of a superacidic BF3H2O species co-crystallized with an organic carbonate.
ABSTRACT
We report on a heterogeneity study, down to the atomic scale, on a representative multiple-element-modified ceramic based on potassium sodium niobate (KNN): 0.95(Na0.49K0.49Li0.02)(Nb0.8Ta0.2)O3-0.05CaZrO3 with 2 wt % MnO2. We show that different routes for incorporating the MnO2 (either before or after the calcination step) affect the phase composition and finally the functionality of the material. According to X-ray diffraction and scanning electron microscopy analyses, the ceramics consist of orthorhombic and tetragonal perovskite phases together with a small amount of Mn-rich secondary phase. The addition of MnO2 after the calcination results in better piezoelectric properties, corresponding to a ratio between the orthorhombic and tetragonal perovskite phases that is closer to unity. We also show, using microscopy techniques combined with analytical tools, that Zr-rich, Ta-rich and Mn-rich segregations are present on the nano and atomic levels. With this multi-scale analysis approach, we demonstrate that the functional properties are sensitive to minor modifications in the synthesis route, and consequently to different material properties on all scales. We believe that detecting and learning how to control these modifications will be a step forward in overcoming the irreproducibility problems with KNN-based materials.
ABSTRACT
Thermal reaction between XeF2 and excess TiF4 resulted in the unexpected formation of a highly ionized Xe(II) â species. The products [Xe2F3][Ti8F33] and [XeF]2[Ti9F38] represent the first examples of [Xe2F3](+) and [XeF](+) compounds, which differ from known Xe(II) salts containing discrete fluoride anions with pentavalent metalloid/metal centers. A new structural type of 2D polyanion [Ti8F33](-) and the formation and structure of the novel 1D [Ti9F38](2-) are discussed. Both products were characterized by single-crystal X-ray analysis and Raman spectroscopy.
