  We show that the combination of X-ray scattering with a nanofocused beam and
X-ray cross correlation analysis is an efficient means for the full structural
characterization of mesocrystalline nanoparticle assemblies with a single
experiment. We analyze several hundred diffraction patterns of individual
sample locations, i.e. individual grains, to obtain a meaningful statistical
distribution of the superlattice and atomic lattice ordering. Simultaneous
small- and wide-angle X-ray scattering of the same sample location allows us to
determine the structure and orientation of the superlattice as well as the
angular correlation of the first two Bragg peaks of the atomic lattices, their
orientation with respect to the superlattice, and the average orientational
misfit due to local structural disorder. This experiment is particularly
advantageous for synthetic mesocrystals made by the simultaneous self-assembly
of colloidal nanocrystals and surface-functionalization with conductive
ligands. While the structural characterization of such materials has been
challenging so far, the present method now allows correlating mesocrystalline
structure with optoelectronic properties.
