Sonochemical synthesis of tri-nuclear lead(II)-azido nano rods coordination polymer with 3,4,7,8-tetramethyl-1,10-phenanthroline (tmph): Crystal structure determination and preparation of nano lead(II) oxide

• Nano-rods of a new 1D Pb(II) coordination polymer was synthesized.
• Calcination of the compound at 180 °C with oleic acid yields PbO nanoparticles.
• SEM and TEM confirm formation of PbO particles around 10–20 nm.

Preparation of rod-shaped nanostructure of a new 1D lead(II) tri nuclear coordination polymer containing the Pb2-(μ-N3)2 and Pb2-(μ-N3)(NO3) motifs [Pb3(tmph)4(μ-N3)5(μ-NO3)]n (1) where “tmph” is the abbreviation of 3,4,7,8-tetramethyl-1,10-phenanthroline, using a sonochemical method is described. The new coordination polymer is characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), elemental analysis and infrared spectroscopy. The single crystalline material is obtained using a heat gradient applied to a solution of the reagents. Single-crystal XRD analysis indicates three different lead(II) centers in the structure with coordination numbers of seven and eight with a holo and hemidirected coordination geometry. They also show that the chains interact with each other through π–π stacking interactions creating a 3D framework. PbO nanoparticles are obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) confirm formation of PbO particles around 10–20 nm.

Rod-shaped nanostructure of a new 1D lead(II) tri nuclear coordination polymer containing the Pb2-(μ-N3)2 and Pb2-(μ-N3)(NO3) motifs, [Pb3(tmph)4(μ-N3)5(μ-NO3)]n (1), (tmph = 3,4,7,8-tetramethyl-1,10-phenanthroline) has been prepared using a sonochemical method. The compound 1 is characterized by single-crystal XRD analysis. PbO nanoparticles are obtained by thermolysis of 1 at 180 °C.Figure optionsDownload as PowerPoint slide