New Flower-Shaped Lead(II) Coordination Polymer at the Nano Scale: Synthesis, Structural Characterization and DFT Calculations of [Pb(o-phen)(N3)2] n Containing the Pb-(μ1,1-N3)(μ1,3-N3) Motif

Bieńko

Hanifehpour

et al. 2016

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A novel nano, cauliflower-shaped lead(II) metal-organic coordination polymer, [Pb(μ-2-pinh)(N3)OH2]n (1), was synthesized using an ultrasonic method. The nanostructure was characterized by scanning electron microscopy (SEM), X-ray powder diffraction, IR spectroscopy, elemental analysis and thermal analysis. The compound was structurally characterized by single-crystal X-ray diffraction and takes the form of a zigzag onedimensional polymer in the solid-state. The coordination number of the lead(II) ions is six (PbN4O2), with one oxygen and three nitrogen donor atoms derived from two linker organic ligands, one nitrogen atom from a terminal azide anion and one oxygen from coordinated water. It has a stereochemically active lone electron pair, and the coordination sphere is hemidirected. The zigzag 1D chains interact with neighbouring chains through weak interactions, creating a 3D supramolecular metal-organic framework. Lead oxide nanoparticles were obtained by thermolysis of the new nano coordination compound at 180 °C with oleic acid as a surfactant. The morphology and size were further studied using SEM. Natural bond orbital (NBO) analyses demonstrate the electronic properties of the lead centre and other atoms.

Section: Methodsmentioning

confidence: 99%

Preparation of a Novel Nano-scale Lead (II) Zig-Zag Metal–Organic Coordination Polymer with Ultrasonic Assistance: Synthesis, Crystal Structure, Thermal Properties, and NBO Analysis of [Pb(μ-2-pinh)N3 H2O]n

Bieńko

Hanifehpour

et al. 2016

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“…Following our previous works on development of novel methods for synthesis of coordination polymers of lead(II) [13,[30][31][32][33][34][35][36][37][38], in this paper we report the new asymmetrical hemidirected lead(II) coordination compound in the presence of (1-(pyridin-2-yl)ethylidene)isonicotinohydrazide schiff-base ligand. The work presented here, describes a simple synthetic sonochemical method for preparation of nano-structures of this coordination polymer and its use in the preparation of PbO nanoparticles.…”

Section: Introductionmentioning

confidence: 92%

Hemidirected Coordination Sphere on Novel Lead(II) Nano Coordination Polymer: Synthesis, Structural Characterization and DFT Calculation of [Pb(p-2-einh)ClO4(MeOH)2]n

Alireza

Ghaedi

et al. 2015

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The novel nano lead(II) 1D zigzag coordination polymer [Pb(p-2-einh)ClO 4 (MeOH) 2 ] n (1) (p-p-2-einh = (1-(pyridin-2-yl)ethylidene)isonicotinohydrazide) was synthesized by a sonochemical method. The new nanostructure was characterized by using scanning electron microscopy (SEM) and high-resolution transmission electron microscopy, X-ray powder diffraction and elemental analysis. The single-crystal X-ray analysis reveals a one dimensional zigzag coordination polymer structure for 1, that is further extended into a three-dimensional (3-D) supramolecular structure by p-p and other labile intermolecular interactions. The coordination number of the lead(II) ions is six, PbN 3 O 3 . The PbO nanoparticles were obtained by the thermolysis of 1 at 180°C in presence of oleic acid as a surfactant. The Scherrer equation estimated the average diameter of the nanoparticles to be 15 nm. The morphology and size of the prepared PbO samples were further observed using SEM. The structure of the title complex has been optimized by density functional theory calculations. Calculated structural parameters and IR spectra for the title complex are consistent with the crystal structure.

“…The crystals of title complex was obtained by the branch tube method [29][30][31][32][33]: Schiff base ligand (0.226 g, 1 mmol) and Bi(NO 3 ) 3Á 5H 2 O (0.485 g, 1 mmol) was placed in the arm to be heated and methanol was carefully added to fill both arms. The tube was sealed and the ligand-containing arm was immersed in a bath at 60 8C while keeping the other arm at ambient temperature.…”

Section: Synthesis Of [Bimentioning

confidence: 99%

Sonochemical Synthesis of Bismuth(III) Nano Coordination Compound and Direct Synthesis of Bi2O3 Nanoparticles from a Bismuth(III) Nano Coordination Compound Precursor

Roodsari

Shaabani

et al. 2015

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A new coordination Compound [Bi(L)(NO 3 ) 2 (ONO 2 )(CH 3 OH)] (1) [L: C 5 H 4 NCH=NNHCONC 5 H 4 ] has been synthesized by the reaction of Bismuth(III) bromide with the ligand pyridine-2-carbaldehyde isoniazid and characterized by elemental analysis, FT-IR spectroscopy and single-crystal X-ray diffraction. Single crystal X-ray diffraction reveals that the compound 1 is mononuclear complex, contains Bismuth(III) in a distorted tricapped trigonal prismatic geometry environment of NNO donors of Schiff base ligand, five oxygen atoms of Nitrate molecules and one oxygen atom of methanol molecule. We also synthesized a nano form of the compound 1 by the sonochemical method and characterized it by elemental analysis, scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and IR spectroscopy. The d-Bi 2 O 3 nanoparticle was obtained by calcinations of the nano compound 1 at 500 8C under air atmosphere and was characterized by SEM and XRD.