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The self-assembly of anisotropic nanocrystals (stabilized by organic cappingmolecules) with pre-selected composition, size, and shape allows for thecreation of nanostructured materials with unique structures and features. Forsuch a material, the shape and packing of the individual nanoparticles play animportant role. This work presents a synthesis procedure for{\omega}-thiol-terminated polystyrene (PS-SH) functionalized gold nanooctahedraof variable size (edge length 37, 46, 58, and 72 nm). The impact of polymerchain length (Mw: 11k, 22k, 43k, and 66k g/mol) on the growth of colloidalcrystals (e.g. mesocrystals) and their resulting crystal structure isinvestigated. Small-angle X-ray scattering (SAXS) and scanning transmissionelectron microscopy (STEM) methods provide a detailed structural examination ofthe self-assembled faceted mesocrystals based on octahedral gold nanoparticlesof different size and surface functionalization. Three-dimensional angularX-ray cross-correlation analysis (AXCCA) enables high-precision determinationof the superlattice structure and relative orientation of nanoparticles inmesocrystals. This approach allows us to perform non-destructivecharacterization of mesocrystalline materials and reveals their structure withresolution down to the nanometer scale.

Revealing the impact of polystyrene-functionalization of Au octahedral nanocrystals of different sizes on formation and structure of mesocrystals