Two inorganic-organic hybrid frameworks, namely [Cu-2(pdca)(2)(bibp)(H2O)(2)]center dot H2O (1) and [Fe(pdca)(pyco)(H2O)]center dot H2O (2) (H(2)pdca = pyridine-2,6-dicarboxylic acid, bibp = 4,4'-bisimidazolylbiphenyl, pyco = picolinate N-oxide) were synthesized via hydrothermal reactions. Both compounds have been characterized by elemental analysis, spectroscopic analysis, thermogravimetric analysis (TGA) and the single crystal diffraction. Complex 1 is dinuclear and five-coordinated copper(II) complex, while complex 2 displays mono-nuclear and six-coordinated iron(III) complex. In the crystal structures of both complexes, the coordinated and crystalline water molecules and H(2)pdca ligands contribute to the formation of O-H center dot center dot center dot O and C-H center dot center dot center dot O hydrogen bonds, which link the molecules into layers parallel. Cyclic voltammetry (CV) analysis shows one reversible reduction potential at 0.14 V (E-pc) in complex 1, whereas in complex 2 shows a reduction potential at 0.15 V (E-pc) in the cathodic region.