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.