We achieved a dense (IO3)-O-1 hybrid superhydrophobic porous coordination polymer (PCP), [Pb(H-BTMB)(DMF)] (1), by solvothermal methods. The single-crystal XRD structure of 1 indicated that it has a three-dimensional M-L-M framework with one-dimensional M-O-M connectivity leading to an (IO3)-O-1 network. The new PCP obtained exhibited open metal sites (OMSs) by losing a coordinated DMF molecule. The degassed phase displayed selective adsorption of CO2 gas over N-2, C2H6, and C2H4 gases. Additionally, it has a superhydrophobic surface with a contact angle of 156.4 degrees at room temperature and it is stable even at 90 degrees C, displaying a contact angle of 135.3 degrees.