Abstract: A new three-dimensional supramolecule, [H₃N(CH₂)₃NH₃]•[Pb₂(SIP)₂]•6H₂O was synthesized under the hydrothermal condition. Its structure was determined with single crystal X-ray diffraction analysis and further characterized via XRD, IR, fluorescent spectrum and elemental analysis. The compound crystallizes in triclinic space group P1, with a=0.79946(16) nm, b=0.9881(2) nm, c=1.0343(2) nm, α=81.25(3)°, β=84.95(3)°, γ=68.13(3)°, V=0.7489(3) nm³, Z=1, R₁=0.0226, wR₂=0.0486, GOF=1.099. Along the [001] direction, binuclear cluster units [Pb₂(SIP)₂]^2- link to each other via O1 and O4 forming two-dimensional anionic layers, then these layers are stacked down the c axis and was further linked by N—H…O and O—H…O hydrogen bonds to build the three-dimensional supramolecular structure. Fluorescent spectrum of compound 1 shows that there are two strong fluorescent emission peaks at λ=349 nm and 393 nm and a weak fluorescent emission peak at 384 nm(λ_{max, excitation}=236 nm).

Key words: Sulfonate-carboxylate lead, Hydrothermal synthesis, Supramolecule, Crystal structure, Fluorescence