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Metal organophosphonates have been explored in energy-related fields due to their high chemical and thermal stability as a type of uniformly precursor, but only few of pristine metal organophosphonate are directly used for oxygen evolution reaction (OER) catalysts. Here, a mixed-valence iron phosphonate (Fe3-ppat) has been constructed and applied to OER catalysis considered the potential active sites in pillars FeII(H2O)4(COO)2 and inorganic layers FeIII(μ2–OH)PO3. Specifically, isostructural trimetallic framework Fe1.7Co0.3Ni1.0-ppat possesses a minimum overpotential (291 mV), small Tafel slope (91.65 mV dec−1), and high stability up to 83 h. The enhanced catalytic performance could be mainly ascribed to the synergistic effect of NiII equivalent occupancy in pillars and Co/FeIII in layers.