A new 2D Ca(Ⅱ) coordination polymer, [Ca(H2btc)(H2O)2]n(1, H4 btc = biphenyl-3,3',5,5'-tetracarboxylic acid), has been synthesized using the hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, IR, thermogravimetric analysis, and photoluminescent analysis. Complex 1 crystallizes in the monoclinic system, space group C2/c with a = 17.5676(15), b = 11.4496(8), c = 7.6197(8)A, β = 102.787(2)o, V = 1494.6(2) A3, Z = 4, D3 c = 1.797 Mg·m-, μ = 0.483 mm-1, F(000) = 832, the final R = 0.0348 and wR = 0.0915 for 1521 observed reflections with I > 2σ(I). Complex 1 has a 2D network containing 1D calcium-oxygen chains. These 2D networks are further connected by O–H···O hydrogen bonding interactions to generate a 3D supramolecular structure.
