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

Preparation of rod-shaped nanostructure of a new 1D lead(II) tri nuclear coordination polymer containing the Pb-2-(mu-N-3)(2) and Pb-2-(mu-N-3)(NO3) motifs [Pb-3(tmph)(4)(mu-N-3)(5)(mu-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 pi-pi stacking interactions creating a 3D framework. PbO nanoparticles are obtained by thermolysis of 1 at 180 degrees 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. (C) 2014 Elsevier B.V. All rights reserved.