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Abstract Herein, the synthesis of Cu₃(HAB)_x(TATHB)_2‐x(HAB: hexaaminobenzene, TATHB: triaminotrihydroxybenzene) is reported. Synthetic improvement of Cu₃(TATHB)₂leads to a more crystalline framework with higher electrical conductivity value than previously reported. The improved crystallinity and analogous structure between TATHB and HAB enable the synthesis of Cu₃(HAB)_x(TATHB)_2‐xwith ligand compositions precisely controlled by precursor ratios. The electrical conductivity is tuned from 4.2 × 10⁻⁸to 2.9 × 10⁻⁵ S cm⁻¹by simply increasing the nitrogen content in the crystal lattice. Furthermore, computational calculation supports that the solid solution facilitates the band structure tuning. It is envisioned that the findings not only shed light on the ligand‐dependent structure–property relationship but create new prospects in synthesizing multicomponent electrically conductive metal‐organic frameworks (MOFs) for tailoring optoelectronic device applications.