Hydrothermal reactions of CdSO 4 with tetrakis(4-pyridyl)cyclobutane (tpcb) and 1,3-benzenedicarboxylic acid (1,3-H 2 BDC) or 5-nitro-1,3-benzenedicarboxylic acid (5-NO 2 -1,3-H 2 BDC) resulted in the formation of two coordination polymers [Cd(tpcb) 0.5 (1,3-BDC)] n (1) and {[Cd 2 (tpcb)(5-NO 2 -1,3-BDC) 2 (OH 2 ) 2 ]·4H 2 O} n (2), respectively. Compounds 1 and 2 were characterized by elemental analysis, IR, powder X-ray diffraction, and single-crystal X-ray diffraction. 1 and 2 exhibit two different types of two-fold interpenetrating 3D architectures with (6 6 ) 2 (6 4 ·8 2 ) and (5 2 ·8)(5 4 ·6∙8)(4·5 3 ·6 2 ·7·8 2 ·10) Schläfli symbols, respectively. Their thermal and photoluminescent properties were also investigated.