A three-dimensional metal organic framework (1) with fourfold interpenetrating diamondoid networks was constructed using a macrocyclic nickel(II) complex and a tetracarboxylic ligand 4,4',4",4"-(cyclohexane-1,2-diyibis(azanetriyl))tetrakis(methylene)-tetrabenzoic acid as building blocks. Despite the fourfold interpenetration, 1 possesses one-dimensional channels that are occupied by water and CH3CN guest molecules. Once the guest molecules were removed, the framework and pores in desolvated 1 are dynamic with large adsorption hysteresis loops, which exhibit selective gas adsorption for CO2 at 195 K over N-2 and H-2 at 77 K and selective adsorption for methanol, ethanol, and n-propanol over isopropanol at 298 K.