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Electron diffraction enables structure determination of organic small molecules using crystals that are too small for conventional X-ray crystallography. However, because of uncertainties in the experimental parameters, notably the detector distance, the unit-cell parameters and the geometry of the structural models are typically less accurate and precise compared with results obtained by X-ray diffraction. Here, an iterative procedure to optimize the unit-cell parameters obtained from electron diffraction using idealized restraints is proposed. The cell optimization routine has been implemented as part of the structure refinement, and a gradual improvement in lattice parameters and data quality is demonstrated. It is shown that cell optimization, optionally combined with geometrical corrections for any apparent detector distortions, benefits refinement of electron diffraction data in small-molecule crystallography and leads to more accurate structural models.

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A novel electrochemical method of preparation of standard gas mixtures for calibration of gas-analytical equipment with O2, H2 and CO was elaborated. Utilization of solid state electrolyte membrane allows to perform a nearly 100%-efficient electrochemical generation or conversion of the analyte and avoid some problems typical for liquid electrolytes, such as solvent evaporation and condensation at the inner walls of the gas tubes or deviations from the Faraday's law. Analysis of uncertainties associated with the calibration procedure showed that the lowest systematic errors are achieved when the calibrant is generated during the electrolysis (i.e. anodic evolution of oxygen or cathodic generation of CO), and the major uncertainties are associated with operation of the flow controllers. For calibration with H2, where the calibrant is partially converted during the electrochemical process, the total uncertainty is essentially determined by molar fractions of the components in H2-Ar mixture, instrumental errors of the equipment, primarily by precision of mass-flow controllers or stability of the gas flow, and the initial flow rate of the calibrant-containing gas mixture. The relative total errors of calibration with oxygen are assessed to be 5-6%; similar uncertainties were calculated for analysis of oxygen content in standard gas mixtures by chromatography using the electrochemical method of calibration.

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BACKGROUND: The validity of predicting foot pronation occurring mainly at the midfoot by surrogate measures from the rearfoot, like eversion excursion, is limited. The dynamic navicular mobility in terms of vertical navicular drop (dNDrop) and medial navicular drift (dNDrift) may be regarded as meaningful clinical indicators to represent overall foot function. This study aimed to develop a minimal approach to measure the two parameters and to examine their intra- and interday reliability during walking. METHODS: The minimal markerset uses markers at the lateral and medial caput of the 1st and 5th metatarsals, respectively, at the dorsal calcaneus and at the tuberosity of the navicular bone. Dynamic navicular drop and drift were assessed with three-dimensional motion capture in 21 healthy individuals using a single-examiner test-retest study design. RESULTS: Intra- and interday repeatability were 1.1 mm (ICC21 0.97) and 2.3 mm (ICC21 0.87) for dynamic navicular drop and 1.5 mm (ICC21 0.96) and 5.3 mm (ICC21 0.46) for dynamic navicular drift. The contribution of instrumental errors was estimated to 0.25 mm for dynamic navicular drop and 0.86 mm for dynamic navicular drift. CONCLUSIONS: Interday reliability was generally worse than intraday reliability primary due to day-to-day variations in movement patterns and the contribution of instrumental errors was below 23% for dynamic navicular drop but reached 57% for dynamic navicular drift. The minimal markerset allows to simply transfer the known concepts of navicular drop and drift from quasi-static clinical test conditions to functional tasks, which is recommended to more closely relate assessments to the functional behavior of the foot.

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In motion capture systems, markers are often seen by multiple cameras. All cameras do not measure the position of the markers with the same reliability because of environmental factors such as the position of the marker in the field of view or the light intensity received by the cameras. Kalman filters offer a general framework to take the reliability of the various cameras into account and consequently improve the estimation of the marker position. The proposed process can be applied to both passive and active systems. Several reliability models of the cameras are compared for the Codamotion active system, which is considered as a specific illustration. The proposed method significantly reduces the noise in the signal, especially at long-range distances. Therefore, it improves the confidence of the positions at the limits of the field of view.