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Experimental charge-density studies: data reduction and model quality: the more the better?

In this review, recent developments concerning data and model quality in experimental charge-density investigations from a personal view-point are described. Data quality is not only achieved by the high resolution, high I/σ(I) values, low merging R values and high multiplicity. The quality of the innermost reflections especially is crucial for mapping the density distribution of the outermost valence electrons and can be monitored by (I/σ)asymptotic. New detector technologies seem to be promising improvements. Empirical corrections to correct for low-energy contamination of mirror-focused X-ray data and for resolution- and temperature-dependent errors caused by factors such as thermal diffuse scattering are described. Shashlik-like residual density patterns can indicate the need for an anharmonic description of the thermal motion of individual atoms. The physical reliability of the derived model must be thoroughly analysed. The derived probability density functions for the mean-squared atomic vibrational displacements especially should have only small negative values. The treatment of H atoms has been improved by methods to estimate anisotropic thermal motion. For very high resolution data, the polarization of the core density cannot be neglected. Several tools to detect systematic errors are described. A validation tool is presented that easily detects when the refinement of additional parameters yields a real improvement in the model or simply overfits the given data. In all investigated structures, it is proved that the multipole parameters of atoms with a comparable chemical environment should be constrained to be identical. The use of restraints could be a promising alternative.