Two coordination polymers [Zn 2 (H 2 L) 2 (bbi)(H 2 O) 2 ·H 2 O] n 1 and [Ni 4 (L) 2 (bbi) 2 (H 2 O) 4 ·H 2 O] n 2 {H 4 L=methylenediisophthalic acid, bbi=1,1′-(1,4-butanediyl)bis(imidazole)} have been prepared under hydrothermal conditions and structurally characterized by X-ray diffraction analyses. Mononuclear 1 is a 1D ladder chain and bbi adopts trans-configuration linking two metal centers. Plus the hydrogen binding interactions, it formed a 3D two-fold perpendicular interpenetrating (4, 5)-connected framework. Binuclear units of 2 are connected by L 4− and cis-bbi to generate a 3D (4, 6)-connected framework, in which twisted bbi with binuclear units generate the rare triflexure helix. In solid state, complex 1 exhibits yellowgreen emissions at ambient temperature. Magnetic measurements show that there exist weak ferromagnetic interactions in 2.