Anoxygen-stoichiometric, B-site-ordered perovskite Ca 2 Fe 1.1 Mn 0.9 O 6 (CFMO) with alternate stacking of Fe and Mn layers was obtained through topochemical oxidation of the corresponding brownmillerite phase under high pressure in the presence of KClO 4 . The structure crystallizes in the P2 1 /m space group with a doubling of the cell along all three crystallographic axes. Mössbauer spectroscopy, susceptibility, and resistivity measurements suggest ferromagnetic [a]