Abstract. The interdigitated coordination networks [Cu(tyty)] (1) and [Cu 1.5 (L1)(L2)(tyty)] (2) [Htyty = 5-(4-(1H-1,2,4-triazol-1-yl)phenyl)-1H-tetrazole, HL1 = 2,3,4,5-tetrachlorobenzoic acid, HL2 = 2,3,4,5,6-pentachlorobenzoic acid], were hydrothermally synthesized and further characterized by single-crystal X-ray diffraction, powder X-ray diffraction, elemental analyses, IR and UV/Vis spectroscopy, and TG analyses. Compound 1 consists of unique 2D double-bilayers, which