| Summary: | Two coordination polymers (CPs), with chemical formulas {[Ni<sub>2</sub>(bpp)<sub>2</sub>(BT)(H<sub>2</sub>O)<sub>6</sub>] 1.5(EtOH) 1.5H<sub>2</sub>O}<sub>n</sub> (<b>1</b>) and [Zn(bpp)(BT)<sub>0.5</sub>]·5H<sub>2</sub>O (<b>2</b>) (bpp = 1,3-bis(4-pyridyl)propane, and BT<sup>4−</sup> = tetraanion of 1,2,4,5-Benzenetetracarboxylic acid), have been synthesized and structurally characterized by single-crystal X-ray diffraction methods. In compound <b>1</b>, the coordination environments of two crystallographically independent Ni(II) ions are both distorted octahedral bonded to two nitrogen donors from two bpp ligands and four oxygen donors from one BT<sup>4-</sup> ligand and three water molecules. Both bpp and BT<sup>4−</sup> act as bridging ligands with <i>bis</i>-monodentate and 1,4-<i>bis</i>-monodentate coordination modes, respectively, connecting the Ni(II) ions to form a 2D layered metal-organic framework (MOF). Adjacent 2D layers are then arranged orderly in an ABAB manner to complete their 3D supramolecular architecture. In <b>2</b>, the coordination environment of Zn(II) ion is distorted tetrahedral bonded to two nitrogen donors from two bpp ligands and two oxygen donors from two BT<sup>4−</sup> ligands. Both bpp and BT<sup>4-</sup> act as bridging ligands with <i>bis</i>-monodentate and 1,2,4,5-<i>tetrakis</i>-monodentate coordination modes, respectively, connecting the Zn(II) ions to form a 3D MOF. The reversible water de-/adsorption behavior of <b>1</b> between dehydrated and rehydrated forms has been verified by cyclic Thermogravimetric (TG) analyses through de-/rehydration processes. Compound <b>1</b> also exhibits significant water vapor hysteresis isotherms.
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