A novel metal organo-diphosphonate compound constructed 2D layers with alkaline gas adsorption property was synthesized through hydrothermal method.The compound is isomorphous and crystallizes in the monoclinic C2/c space group.The metal ions Ni1 are connected by 4,4′-bpy ligands to form 1D chains and further connected by the organo-diphosphonate ligands to form 2D layer structure.The metal ions are six-coordinated with four oxygen atoms coming from phosphonate and coordinated aqua molecules and two nitrogen atoms coming from 4,4′-bpy.Two oxygen atoms of phosphonate are uncoordinated and the compound could absorb alkaline gas.