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Peptide-mimic poly(n-hexyl isocyanate) (PHIC) with stiff chain characteristics demonstrated to selectively form a well-ordered hexagonal close packing structure with 83 helical conformation in the nansocale thin films annealed with carbon disulfide. Moreover, this polymer showed to selectively form a well-ordered multi-bilayer structure with β-sheet conformation in the thin films annealed with toluene. These two self-assembled structures were reversibly transformed by consecutive annealing with carbon disulfide and toluene. These chain conformations and self-assembled structures were confirmed by synchrotron grazing incidence X-ray scattering analysis.