Two new Co(II) coordination polymers, [Co(Hnbta)(bth)]n (1) and {[Co3(nbta)2(bth)3(H2O)]·H2O}n (2), (H3nbta = 5‐nitro‐1,2,3‐benzenetricarboxylic acid and bth = 1,6‐bis(1,2,4‐triazole‐1‐yl)hexane), have been synthesized under different pH values through hydrothermal reactions. Both complexes were characterized by elemental analysis, IR spectra, thermogravimetric analysis (TGA), and single‐crystal X‐ray crystallography. Complex 1 exhibits a 3D polythreaded network based on 4‐connected sql 2D layer. Complex 2 has a (4,4,5)‐connected trinodal 3D pillar‐layered network with a (42·64)2(42·67·8)2(64·82) topology. Magnetic susceptibility measurements indicate that complexes 1 and 2 show weak antiferromagnetic interactions between the adjacent Co(II) ions.
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