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A novel bimetallic 4f–3d metal-isonicotinic acid inorganic–organic hybrid complex [{Eu(NC5H4COOH)3(H2O)2}(1.5ZnCl4)•(2H2O)]n (1) was synthesized via a hydrothermal reaction and structurally characterized by single-crystal X-ray diffraction. Complex 1 crystallizes in the space group C2/c of the monoclinic system with eight formula units in a cell: a = 23.878(8) Å, b = 20.573(6) Å, c = 15.358(5) Å, β = 127.276(5)°, V = 6003(3) Å3, C18H23Cl6EuN3O10Zn1.5, Mr = 904.11 g/mol, r = 2.001 g/cm3, S = 1.077, μ(MoKα) = 3.846 mm-1, F(000) = 3536, R = 0.0270 and wR = 0.0672. Complex 1 has a characteristic, one-dimensional polycationic chain-like structure. A photoluminescent investigation revealed that the title complex displays intense emissions in the orange and red regions. The luminescence spectra show that the red emission is stronger than the orange emission. Optical absorption spectra of 1 revealed the presence of an optical gap of 3.56 eV.