Synthesis and characterization of nano-peanuts of lead(II) coordination polymer [Pb(qcnh)(NO3)2]n with ultrasonic assistance: A new precursor for the preparation of pure-phase nano-sized PbO

. 2017 Jan ; 34 () : 255-261. [epub] 20160526

Status PubMed-not-MEDLINE Jazyk angličtina Země Nizozemsko Médium print-electronic

Typ dokumentu časopisecké články, práce podpořená grantem

Perzistentní odkaz   https://www.medvik.cz/link/pmid27773243
Odkazy

PubMed 27773243
DOI 10.1016/j.ultsonch.2016.05.041
PII: S1350-4177(16)30183-3
Knihovny.cz E-zdroje

A sonochemical method was used to synthesize nano-peanuts of a new lead(II) coordination 1D polymer, [Pb(qcnh)(NO3)2]n (1), where qcnh=2-quinolincarbaldehyde nicotinohydrazide. The compound was characterized by scanning electron microscopy (SEM), elemental analysis, IR spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray powder diffraction (XRD), and single crystal X-ray analysis. The X-ray structure revealed that the Pb(II) atom is coordinated by one oxygen and three nitrogen atoms from two qcnh ligands and five oxygen atoms from three nitrate ligands in an 8+1 fashion with a PbN3O6 donor set. One of the PdN distances in the vicinity of the central atom is a bit longer (Pb1N1=2.939(4) Å), which shows the effect of the 6s2 lone electron pair localized within the valence shell of the lead(II) atom. PbO nanoparticles were obtained by thermolysis of 1 at 180°C with oleic acid as a surfactant. The average diameter of the nanoparticles was estimated by XRD to be 28nm. The morphology and size of the prepared PbO nanoparticles were further studied using SEM.

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