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The search for efficient, earth‐abundant electrocatalysts for water splitting has spurred significant interest in coordination polymers, particularly those incorporating redox‐active units. Herein, we discuss two isostructural, ferrocene‐bridged nickel and cobalt coordination polymers (CPs) synthesized via a solvothermal route using 1,1′‐ferrocenylenebis(H‐phosphinic) acid and 1,2‐di(pyridin‐4‐yl)ethene linkers. Single‐crystal X‐ray diffraction of the cobalt‐based framework confirms a robust three‐dimensional structure with rod‐like morphology, as corroborated by scanning electron microscopy (SEM). Powder X‐ray diffraction (PXRD) reveals that both Ni‐ and Co‐CPs exhibit virtually identical diffraction patterns before catalysis, verifying their isostructural nature. With an identical ferrocene ligand, the nature of the framework metal node strongly dictates how the polymers respond to anodic stress, leading to different OER kinetics and long-term stability. These findings emphasize the need for deeper structure–property correlations when designing ferrocene‐bridged coordination polymers for water splitting and raise provocative questions about the practical trade‐offs between crystallinity and electrocatalytic activity in future CP‐based catalyst design.
Khrizanforov et al. (Wed,) studied this question.