A novel coordination polymer [(C10H16N)(2)(Pb2I6)(.)2DMF(.)H(2)O](n) (C10H16N=N-butyl-2-Methy-Pyridinium) was synthesized by the reaction of Pb(NO3)(2) with C6H10NI at room temperature in DMF solvent and structurally characterized by means of X-ray single diffraction. The title compound crystallizes in triclinic system, space group P (1) over bar with a=1.1237(2) nm, b=1.253 30(16) nm, c=0.808 00(12) nm, alpha=102.523(4)degrees beta=92.475(5)degrees, gamma=95.712(10)degrees, V=1.102 9(3) nm(3), Z=1, D-c=2.470 Mg(.)m(-3), F(000)=738, chemical formula C26H48N4O3Pb2I6 and M-r=1 640.46, mu(MoKalpha) = 11.849 mm(-1), the final R=0.0578 and wR=0.1665 for 3 716 observed reflections with I > 2sigma(I). The title compound consists of cations ([(C10H16N)(+)] and anion chain (PbI3-),they are combined by static attracting forces in the crystal. DMF and H2O locate between the organic and inorganic moiety.