Recent advances in 3D electron diffraction (3D ED) have succeeded in matching the capabilities of single-crystal X-ray diffraction (SCXRD), while requiring only submicron crystals for successful structural investigations. One of the many diverse areas to benefit from the 3D ED structural analysis is main-group chemistry, where compounds are often poorly crystalline or single-crystal growth is challenging. A facile method for loading and transferring highly air-sensitive and strongly oxidizing samples at low temperatures to a transmission electron microscope (TEM) for 3D ED analysis was successfully developed and tested on xenon(II) compounds from the XeF-MnF system.
View Article and Find Full Text PDFThe crystal structure of the title enanti-opure tetralol derivative {systematic name: (1,2)-2-[()-2,2,2-tri-fluoro-1-hy-droxy-eth-yl]-1,2,3,4-tetra-hydro-naph-thalen-1-ol}, CHFO, 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 222 with one mol-ecule in the asymmetric unit and features intra-molecular as well as inter-molecular O-H⋯O hydrogen bonding. The absolute configuration was established from anomalous dispersion effects.
View Article and Find Full Text PDFHydraulic 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.
View Article and Find Full Text PDFThe 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, BFHO·2OC(OCH), was determined by low-temperature single-crystal X-ray diffraction. The co-crystal crystallizes in the ortho-rhom-bic space group 222 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-H⋯O=C hydrogen bonds.
View Article and Find Full Text PDFWe 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(NaKLi)(NbTa)O-0.05CaZrO with 2 wt % MnO.
View Article and Find Full Text PDFAngew Chem Int Ed Engl
December 2014
Thermal reaction between XeF2 and excess TiF4 resulted in the unexpected formation of a highly ionized Xe(II) 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.
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