Hydrothermal reaction of naphthalene-1,8-dicarboxylate with Pb Cl_2 leads to a new coordination polymer compound,Pb(C_(12)H_6O_4).Single-crystal X-ray diffraction analysis reveals that it crystallizes in monoclinic,space group P2_1/c with a = 13.1648(18),b = 5.3881(8),c = 14.599(2) ?,β = 95.759(2)o,V = 1030.3(3) ?~3,Z = 4,Mr = 384.32,Dc = 2.7167 g/cm~3,F(000) = 768,μ(Mo Kα) = 16.37 mm~(-1),R = 0.043 and w R = 0.097.The structure of Pb(C_(12)H_6O_4) was refined by two components non-merohedral twinning model with the twin law of(-1000-100.224 0 1) and twinning ratio of 0.736:0.264.In this structure,the Pb atoms are surrounded by five O atoms from ligands into PbO_5 polyhedra,which are further interconnected to form a 2D layer structure parallel to the bc-plane. Hydrothermal reaction of naphthalene-1,8-dicarboxylate with Pb Cl_2 leads to a new coordination polymer compound, Pb (C_ (12) H_6O_4). Single-crystal X-ray diffraction analysis shows that it crystallizes in monoclinic space group P2_1 / c with a = 13.1648 (18), b = 5.3881 (8), c = 14.599 (2) ?, β = 95.759 (2) o, V = 1030.3 (3)? 3, Z = 4, Mr = 384.32, = 2.7167 g / cm ~ 3, F (000) = 768, μ (Mo Kα) = 16.37 mm -1, R = 0.043 and w R = 0.097.The structure of Pb (C_ (12) H_6O_4) was refined by two components non-merohedral twinning model with the twin law of (-1000-100.224 0 1) and twinning ratio of 0.736: 0.264.In this structure, the Pb atoms are surrounded by five O atoms from ligands into PbO_5 polyhedra, which are further interconnected to form a 2D layer structure parallel to the bc-plane.