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Two novel Cu(II) compounds [Cu2(btb)3.5(C4AS)(H2O)]·2.5(H2O) (1) and [Cu2.5(btp)2(C4AS)(htz)(H2O)3]·4.75(H2O) (2) have been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction analyses (btb = 1,4-bis(1,2,4-triazol-1-yl)butane, btp = 1,5-bis(1,3,4-triazol-1-yl)pentane, htz = 1,3,4-triazolate, and C4AS = p-sulfonato-calix[4]arene). In 1, the btb ligands connect Cu(II) atoms to form a 3D porous framework. The 1D chains constructed by C4AS and Cu(II) atoms are further bonded to the 3D porous framework through the Cu–O bonds. Topologically, structure 1belongs to a 3D (3,6)-connected net with the Schläfli symbol of (42·6)(46·68·8). In 2, the C4AS links the Cu(II) atoms to form 1D chains, which are further connected by the btp and htz to generate a 3D (3,4,6)-connected framework with the Schläfli symbol of (62·8)(52·62·7·8)(54·62·7·87·9). The two compounds have been further characterized by infrared spectra (IR), elemental analyses, powder X-ray diffraction (PXRD), thermogravimetric (TG) analyses, and UV–vis absorption spectra. [ABSTRACT FROM AUTHOR]