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The self-assembly of anisotropic nanocrystals (stabilized by organic capping molecules) with pre-selected composition, size, and shape allows for the creation of nanostructured materials with unique structures and features. For such a material, the shape and packing of the individual nanoparticles play an important role. This work presents a synthesis procedure for {\omega}-thiol-terminated polystyrene (PS-SH) functionalized gold nanooctahedra of variable size (edge length 37, 46, 58, and 72 nm). The impact of polymer chain length (Mw: 11k, 22k, 43k, and 66k g/mol) on the growth of colloidal crystals (e.g. mesocrystals) and their resulting crystal structure is investigated. Small-angle X-ray scattering (SAXS) and scanning transmission electron microscopy (STEM) methods provide a detailed structural examination of the self-assembled faceted mesocrystals based on octahedral gold nanoparticles of different size and surface functionalization. Three-dimensional angular X-ray cross-correlation analysis (AXCCA) enables high-precision determination of the superlattice structure and relative orientation of nanoparticles in mesocrystals. This approach allows us to perform non-destructive characterization of mesocrystalline materials and reveals their structure with resolution down to the nanometer scale., Comment: 46 pages, 5 figures, 12 Supplementary Information figures, 1 Table in the main text, 1 Table in Supplementary Information