Three porous coordination polymers Cu 3 (btc) 2 (HKUST-1) (btc=benzene-1,3,5-tricarboxylate) (1), Zn 2 (bdc) 2 dabco (2) (bdc=benzene-1,4-dicarboxylate, dabco=1,4-diazabicyclo[2.2.2]octane), and Cr 3 F(H 2 O) 2 O(bdc) 3 (MIL-101) (3) were evaluated as methane storage materials. The compounds were synthesized using solvothermal method and identified as pure phases using powder X-ray diffraction. Nitrogen physisorption at 77K revealed a high specific micropore volume ranging from 0.75 to 1.303cm 3 g −1 . Methane adsorption isotherms were measured using gravimetric method at 303K up to 200bar. A volumetric miniature tank system was used to measure the effective volumetric storage capacity taking the packing density into account. Among the three materials, Cu 3 (btc) 2 shows the highest excess adsorption at 303K (15.7wt.%) and effective volumetric storage capacity of 228m 3 m −3 (150bar), whereas for Zn 2 (bdc) 2 dabco and MIL-101 the maximum excess adsorption is lower (14.3 and 14.2wt.%, respectively). For MIL-101, the maximum in the excess adsorption is observed at higher pressure (125bar) as compared to Cu 3 (btc) 2 and Zn 2 (bdc) 2 dabco (75bar).