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The size of single crystals of the metal‐organic framework CPO‐27‐Ni was incrementally increased through a series of modulated syntheses. A novel linker modulated synthesis using 2,5‐dihydroxyterephthalic acid and the isomeric ligand 4,6‐dihydroxyisophthalic acid yielded large single crystals of CPO‐27‐Ni (∼70 μm). All materials were shown to have high crystallinity and phase purity through powder...