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A series of hybrid hetero bimetallic metal–organic frameworks, as solid metal–organic precursors, have been prepared via a conventional hydrothermal method. Herein, we report a facile approach for the synthesis of novel crystalline organic–inorganic hybrid compounds of diaquabis(acetylacetonato)[nickel(II)/zinc(II)] in the presence of varying mole ratios of Ni(II)/Zn(II) mixed metal ions. C10H18O6Ni0.7Zn0.3 (N0.7Z0.3AA.2H2O) as an instance of the series has been investigated through detailed characterization. The crystal is composed of N0.7Z0.3AA units and two coordinated water molecules to form a monoclinic structure with space group P21/c. All the solid‐state structures have the metals in octahedral environments forming six‐membered chelate rings. The unit cell dimensions were obtained using single‐crystal X‐ray diffraction. Thermogravimetric analysis reveals that the hybrid compounds can be considered as suitable precursors for the synthesis of oxides via metal–organic chemical vapour deposition. At room temperature, all crystals clearly exhibit paramagnetic behaviour. Besides varying molar ratios of hybrid, the transition point of magnetic behaviour occurs at Ni critical concentration of around 10% in the hybrid. In addition, the magnetic susceptibility increases with increasing Ni content in the compounds.