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Two new Cu(II) crystals, {[Cu(dtp)]·H₂O}_n (<b>1</b>) and [Cu(Hdtp)(bdc)_0.5]_n (<b>2</b>) (H₂dtp = 4′-(3,5-dicarboxyphenyl)-2,2′:6′,2‴-terpyridine, H₂bdc = 1,4-benzenedicarboxylic acid) were synthesized under hydrothermal conditions. X-ray single-crystal structural analysis revealed that the 5-connective Cu(II) is in a distorted tetragonal-pyramidal coordination sphere for both compounds. Crystal <b>1</b> shows a “wave-shaped” 2D layer in the structure, while <b>2</b> bears a 1D coordination chain structure and a supermolecular 2D layer structure with a thickness of 7.9 Å via 1D chain stacking. PXRD and TGA measurements showed that <b>1</b> and <b>2</b> are air stable, with thermal stabilities near 300 °C.