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The fibrillar poly(3-hexyl thiophene) single crystals were prepared from dilute solutions of toluene, xylene, and anisole (0.01 wt%), and were investigated from the perspective of structural properties. Next, the rectangular and hexagonal poly(ethylene glycol) single crystals were developed from the dilute solutions and molten thin polymer films. The developing methodology used for all growth systems was self-seeding. The dimensions of fibrillar and rectangular/hexagonal single crystals ranged from several nanometers to some microns. Random single-co-crystals were also grown from dilute solution (0.018 wt% in amyl acetate) of crystalline–amorphous diblock copolymers and homopolymers. The small-angle X-ray scattering, grazing incidence wide-angle X-ray scattering, and atomic force microscopy analyses were employed to characterize prepared grained samples. The incident X-ray experiments …