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An unusual self-assembled hetero-bimetallic [Ni(II)-Sm(III)] coordination polymer, [Ni(L)Sm(NO₃)₃(4,4′-bipy)]_n, is prepared through a hexadentate chelating ligand 2,2′-[1,2-ethylenedioxybis(nitrilomethylidyne)]diphenol (H₂L). The Ni(II)-Sm(III) coordination polymer is validated through elemental analyses, Fourier-transform infrared and UV-Visible spectroscopies, and X-ray single-crystal diffraction. The Ni(II) atom forms a twisted six-coordinated octahedron, and the Sm(III) atom is ten-coordinated, adopting a twisted bicapped square antiprism. An infinite three-dimensional-layer supramolecular structure is obtained through extensive π···π stacking and intermolecular hydrogen bonding interactions. The polymer has a good antibacterial effect against Staphylococcus aureus.