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Solvothermalreactions of Zn(NO3)2with tetrakis(4-pyridyl)cyclobutane(tpcb) and 1,4-naphthalenedicarboxylic acid (1,4-H2ndc)and 2,3-naphthalenedicarboxylic acid (2,3-H2ndc) in differentsolvents led to the formation of three polydimensional coordinationpolymers {[Zn2(H2O)(1,4-ndc)2(tpcb)]}n(1), {[Zn(1,4-ndc)(tpcb)0.5]}n(2), and {[Zn2(H2O)(2,3-ndc)2(tpcb)]}n(3). Compounds 1–3were characterized by elemental analysis, IR, powder X-raydiffraction (PXRD), and single crystal X-ray diffraction. Compound 1is a three-dimensional (3D) (3,3)-connected net with a (10·122)·(102·12) Schläfli symbol. Compound 2holds a 2-fold interpenetrating 3D framework with a (42·62·72)·(4·62·73) Schläfli symbol, which shows hexagonal-prism-likeone-dimensional channels. Compound 3shows a two-dimensional(3,8)-connected network. The solid state luminescent, optical, andthermal stability properties of 1–3at ambient temperature were also investigated. A comparative studyon their photocatalytic activity toward the degradation of methylorange and methyl blue in polluted water was explored. The resultsprovided some interesting insights into solvent effects on the structuresof zinc(II) coordination polymers and their photocatalytic applications. [ABSTRACT FROM AUTHOR]