A series of isostructural 2-fold interpenetrating 2D Cd(II)-MOFs, namely G subset of CdL2(OTs)(2) (G = THF (1), PhF (2), PhCl (3), PhBr (4), PhI (5), L = 1,2-bis[(3-(pyridin-4-yl)phenoxy]ethane, and OTs- = p-toluenesulfonate anion), have been successfully synthesized from the flexible ethylene glycol ether-bridging ligand L and Cd(OTs)(2) in solution. The CdL2(OTs)(2) framework contains squarelike nonpolar channels, and the encapsulated guest molecules can be removed by heating (150 degrees C) to generate a guest-free host framework which is able to reversibly adsorb monohalobenzenes PhX (X = F, Cl, Br, I) in the liquid phase under ambient conditions without loss of framework integrity. Furthermore, it can effectively separate these monohalobenzenes and exhibits a clear affinity for monohalobenzenes according to the following order: PhI > PhBr > PhCl > PhF. In addition, PhX subset of CdL2(OTs)(2) exhibits guest-dependent luminescence properties.