Temperature-induced mobility in octacalcium phosphate impacts crystal symmetry: water dynamics studied by NMR crystallography.

Octacalcium phosphate (OCP, Ca(PO)(HPO)·5HO) is a notable calcium phosphate due to its biocompatibility, making it a widely studied material for bone substitution. It is known to be a precursor of bone mineral, but its role in biomineralisation remains unclear. While the structure of OCP has been the subject of thorough investigations (including using Rietveld refinements of X-ray diffraction data, and NMR crystallography studies), important questions regarding the symmetry and H-bonding network in the material remain.

Probing the electronic structure and hydride occupancy in barium titanium oxyhydride through DFT-assisted solid-state NMR.

Perovskite-type oxhydrides such as BaTiOH exhibit mixed hydride ion and electron conduction and are an attractive class of materials for developing energy storage devices. However, the underlying mechanism of electric conductivity and its relation to the composition of the material remains unclear. Here we report detailed insights into the hydride local environment, the electronic structure and hydride conduction dynamics of barium titanium oxyhydride.

Half-integer-spin quadrupolar nuclei in magic-angle spinning paramagnetic NMR: The case of NaMnO.

A combination of solid-state NMR methods for the extraction of Na shift and quadrupolar parameters in the as-synthesized, structurally complex NaMnO Na-ion cathode material, under magic-angle spinning (MAS) is presented. We show that the integration of the Magic-Angle Turning experiment with Rotor-Assisted Population transfer (RAPT) can be used both to identify shifts and to extract a range of magnitudes for their quadrupolar couplings. We also demonstrate the applicability of the two-dimensional one pulse (TOP) based double-sheared Satellite Transition Magic-Angle Spinning (TOP-STMAS) showing how it can yield a spectrum with separated shift and second-order quadrupolar anisotropies, which in turn can be used to analyze a quadrupolar lineshape free of anisotropic bulk magnetic susceptibility (ABMS) induced shift dispersion and determine both isotropic shift and quadrupolar products.

Crystal and electronic facet analysis of ultrafine NiP particles by solid-state NMR nanocrystallography.

Structural and morphological control of crystalline nanoparticles is crucial in the field of heterogeneous catalysis and the development of "reaction specific" catalysts. To achieve this, colloidal chemistry methods are combined with ab initio calculations in order to define the reaction parameters, which drive chemical reactions to the desired crystal nucleation and growth path. Key in this procedure is the experimental verification of the predicted crystal facets and their corresponding electronic structure, which in case of nanostructured materials becomes extremely difficult.

Indium(III) in the "Periodic Table" of Di(2-pyridyl) Ketone: An Unprecedented Transformation of the Ligand and Solid-State In NMR Spectroscopy as a Valuable Structural Tool.

Reactions of di(2-pyridyl) ketone, (py)CO, with indium(III) halides in CHNO have been studied, and a new transformation of the ligand has been revealed. In the presence of In, the C═O bond of (py)CO is subjected to nucleophilic attack by the carbanion :CHNO, yielding the dinuclear complexes [InX{(py)C(CHNO)(O)}] (X = Cl, ; X = Br, ; X = I, ) in moderate to good yields. The alkoxo oxygens of the two η:η:η-(py)C(CHNO)(O) ligands doubly bridge the In centers and create a {In(μ-OR)} core.

Resolving Dirac electrons with broadband high-resolution NMR.

Detecting the metallic Dirac electronic states on the surface of Topological Insulators (TIs) is critical for the study of important surface quantum properties (SQPs), such as Majorana zero modes, where simultaneous probing of the bulk and edge electron states is required. However, there is a particular shortage of experimental methods, showing at atomic resolution how Dirac electrons extend and interact with the bulk interior of nanoscaled TI systems. Herein, by applying advanced broadband solid-state Te nuclear magnetic resonance (NMR) methods on BiTe nanoplatelets, we succeeded in uncovering the hitherto invisible NMR signals with magnetic shielding that is influenced by the Dirac electrons, and we subsequently showed how the Dirac electrons spread inside the nanoplatelets.

Synthesis and Physical Properties of the Oxofluoride Cu(SeO)F.

Single crystals of the new compound Cu(SeO)F were successfully synthesized via a hydrothermal method, and the crystal structure was determined from single-crystal X-ray diffraction data. The compound crystallizes in the orthorhombic space group Pnma with the unit cell parameters a = 7.066(4) Å, b = 9.