The intercalation of polyfuran, by in-situ intercalative oxidative polymerization of terfuran in FeOCl is reported. The intercalation reaction proceeds to completion in methanol in a sealed tube at 100 °C. The resulting compound, polyfuran/FeOCl (I), is crystalline. An interlayer expansion of ≈7.7 A ̊ is observed upon intercalation. The formation of polyfuran in the interlayer space of the host material was confirmed by FTIR spectroscopy and by isolation of the polymers from the host. Tetrafuran could not be intercalated completely under the conditions employed. Electrical conductivity and thermoelectric power data from pressed pellets of (I) are reported and the results are compared with other FeOCl intercalated polymers. X-ray diffraction, magnetic, infrared spectroscopic and scanning and transmission electron microscopic characterization of (I) are reported.