Pharmaceutical organic salt: Disordered crystal structure of levofloxacin with γ-resorcylic acid

This study reports an organic salt prepared from an antibacterial drug, levofloxacin and antioxidant γ-resorcylic acid. A simple preparation method leads to a crystal with disordered structure. The idea is to prepare an organic salt comprising of pharmaceutically acceptable acidic and basic components. The salt is characterised by IR, solid state NMR, and single crystal XRD. Crystal data for C25H26N3O8F: triclinic, space group P-1 (no. 2), a = 7.0037(8) Å, b = 12.764(3) Å, c = 13.909(3) Å, α = 104.821(4)°, β = 92.039(4)°, γ = 95.334(4)°, V = 1194.6(4) Å3, Z = 2, T = 296(2) K, μ(MoKα) = 0.113 mm-1, Dcalc = 1.433 g/cm3, 16879 reflections measured (5.048° ≤ 2Θ ≤ 54.186°), 5139 unique (Rint = 0.0663, Rsigma = 0.0975) which were used in all calculations. The final R1 was 0.1121 (I>2σ(I)) and wR2 was 0.2505 (all data). SC-XRD analysis shows that the crystal packing is stabilized by strong H-bonding of type N-H···O and comparatively weak interactions of type C-H···O, C-H···π and off-set π···π stacking.

On modelling disordered crystal structures through restraints from molecule-in-cluster computations, and distinguishing static and dynamic disorder

Distinguishing disorder into static and dynamic based on multi-temperature X-ray or neutron diffraction experiments is the current state of the art, but is only descriptive, not predictive. Here, several disordered structures are revisited from the Cambridge Crystallographic Data Center `drug subset', the Cambridge Structural Database and own earlier work, where experimental intensities of Bragg diffraction data were available. Using the molecule-in-cluster approach, structures with distinguishable conformations were optimized separately, as extracted from available or generated disorder models of the respective disordered crystal structures. Re-combining these `archetype structures' by restraining positional and constraining displacement parameters for conventional least-squares refinement, based on the optimized geometries, then often achieves a superior fit to the experimental diffraction data compared with relying on experimental information alone. It also simplifies and standardizes disorder refinement. Ten example structures were analysed. It is observed that energy differences between separate disorder conformations are usually within a small energy window of RT (T = crystallization temperature). Further computations classify disorder into static or dynamic, using single experiments performed at one single temperature, and this was achieved for propionamide.

Crystal structure, microstructure, and magnetic properties of the Fe2CrSi nanostructured Heusler alloy elaborated by the mechanical alloying method

The Fe2CrSi nanostructured Heusler alloy was prepared by mechanical alloying followed by heat treatment. The structure, microstructure, and magnetic properties of the samples were studied by the following analysis methods: X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectrometry, transmission electron microscopy, and a vibrating sample magnetometer. The a-Fe (Si, Cr) solid solution with a disordered body centered cubic (bcc) crystal structure was obtained after 24 h of milling. An example of the sample milled for 32 h with a disordered crystal structure a-Fe(Si, Cr) was chosen to investigate the transformation with temperature using differential scanning calorimetry. The effect of annealing temperatures on the structural, microstructural, and magnetic properties of the ordered Fe2CrSi Heusler phase for the sample milled for 32 h was investigated.