A novel pillar-layer porous lanthanide metal-organic framework [Tb-3(ODA)(3)(BPDC)(3)Na-2](n)center dot G(x) (UTSA-222, G = guest molecules) was constructed from an organic ligand [1,1'-biphenyl]-4,4'-dicarboxylate (BPDC2-) and a lanthanide metalloligand [Tb(ODA)](+) (H(2)ODA = oxydiacetic acid). The UTSA-222 contains two-dimensional intersecting channels with the Brunauer-Emmett-Teller surface area and pore volume of 703 m(2) g(-1) and 0.344 cm(3) g(-1),respectively, for the activated sample. It shows moderately high adsorption selectivity for C2H2/CO2 and C2H2/CH4 separations at 1 atm and room temperature.