| Summary: | Four one-dimensional complexes, denoted as [NiL<sub>1</sub>][Ni(CN)<sub>4</sub>] (<b>1</b>), [CuL<sub>1</sub>][Ni(CN)<sub>4</sub>] (<b>2</b>), [NiL<sub>2</sub>][Ni(CN)<sub>4</sub>]·2H<sub>2</sub>O (<b>3</b>), and [CuL<sub>2</sub>][Ni(CN)<sub>4</sub>]·2H<sub>2</sub>O (<b>4</b>) (L<sub>1</sub> = 1,8-dimethyl-1,3,6,8,10,13-hexaaza-cyclotetradecane; L<sub>2</sub> = 1,8-dipropyl-1,3,6,8,10,13-hexaazacyclotetradecane) were synthesized by reacting nickel/copper macrocyclic complexes with K<sub>2</sub>[Ni(CN)<sub>4</sub>]. Subsequently, the synthesized complexes were characterized using elemental analysis, infrared spectroscopy analysis, thermogravimetric analysis, and X-ray powder diffraction. Single-crystal structure analysis revealed that the Ni(II)/Cu(II) atoms were coordinated by two nitrogen atoms from [Ni(CN)<sub>4</sub>]<sup>2−</sup> with four nitrogen atoms from a macrocyclic ligand, forming a six-coordinated octahedral coordination geometry. Nickel/copper macrocyclic complexes were bridged by [Ni(CN)<sub>4</sub>]<sup>2−</sup> to construct one-dimensional chain structures in <b>1</b>–<b>4</b>. The characterization results showed that the four complexes obeyed the Curie–Weiss law with a weak antiferromagnetic exchange coupling.
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