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Quasi-two-dimensional conjugated polymers (q2DCPs) are polymers that consist of linear conjugated polymer chains assembled through non-covalent interactions to form a layered structure. In this work, w e report the synthesis of a novel crystalline q2D polypyrrole (q2DPPy) film at an air/H2 SO4 (95%) interface. The unique interfacial environment facilitated chain extension, prevented disorder, and resulted in a crystalline, layered assembly of protonated quinoidal chains with a fully extended conformation in its crystalline domains. This unique structure features highly delocalized π-electron systems within the extended chains, which is responsible for the low effective mass and narrow electronic bandgap. Thus w e investigated the temperature-dependent charge transport properties of q2DPPy using the van der Pauw (vdP) method and terahertz time-domain spectroscopy (THz-TDS). The vdP method revealed that the q2DPPy film exhibited a semiconducting behavior with a thermally activated hopping mechanism in long-range transport between the electrodes. Conversely, THz-TDS revealed a band-like transport, indicating intrinsic charge transport up to a record short-range high THz mobility of ∼107.1 cm2 V-1 s-1 . This article is protected by copyright. All rights reserved.