Sonochemical Synthesis and Characterization of A Nano-Rod Lead(II) Supramolecular, Three Dimensional Coordination Compound: New Precursor to Produce Pure Phase Nano-Sized Lead(II) Oxide

Nanorods of a lead(II) supramolecular three-dimensional (3D) coordination compound, [Pb(tfpb)₂]_n (1) (Htfpb?=?4,4,4-trifluoro-1-phenyl-1,3-butanedione), was prepared by the sonochemical method. The new nano-structure was characterized by scanning electron microscopy, X-ray powder diffraction, elemental analyses and IR spectroscopy. A single-crystal structure of the compound showed that the coordination number of Pb(II) is eight with six O-donor atoms from the tfpb ligand and two F-donors from anionic ligands. The 3D supramolecular structure of 1 is realized by weak directional C–F···F–C and π–π stacking interactions. After calcination of nano-sized 1 at 500?°C, pure phase nano-sized lead(II) oxide is produced.     

Synthesis and Characterization of a New Nano Lead(II) Two-dimensional Coordination Polymer by Sonochemical Method: A Precursor to Produce Pure Phase Nano-sized Lead(II) Oxide

A new nano-sized lead(II) coordination polymer, {[Pb₂(μ-3-bpdh)(μ-NO₃)₃(NO₃)]_n (1); (3-bpdh = 2,5-bis(3-pyridyl)-3,4-diaza-2,4-hexadiene)}, was synthesized by a sonochemical method. The structure of 1, which may be considered coordination polymer of lead(II), consists of metallocyclic chains formed by bridging NO₃ ⁻ and 3-bpdh ligands, thereby making a 2D array of Pb(NO₃)₂ and 3-bpdh. The thermal stability of compound was studied by thermogravimetric and differential thermal analyses. The new nano-structure coordination polymer was characterized by powder X-ray diffraction, elemental analysis and IR spectroscopy. The scanning electron microscopy shows the particle size of the 1 prepared by the sonochemical method is about 95 nm. The PbO nanoparticles were obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. The scanning electron microscopy shows that the size of the PbO particles are ~60 nm.     

Synthesis and Structural Characterization of New Lead(II) Discrete and Infinite Cage-Like Framework: A Precursor to Produce Pure Phase Nano-Sized Lead(II) Oxide

A novel Pb(II) complex, {[Pb₂(tpmba)₂(NO₃)₄]·MeOH} _n (1), was obtained by the reaction of a tripodal ligand, N,N′,N″-tris(pyrid-3-ylmethyl)-1,3,5-benzenetricarboxamide (tpmba), with Pb(NO₃)₂. The structure of complex was determined by X-ray crystallography. The results of structural analysis of the complex reveal that 1 is a M₂L₂ cage-like with a methanol molecule beside the cage. An entirely different structure and topology between 1 and similar complexes indicate that the nature of organic ligands affects the structure of assemblies. The results indicate that the framework of this complex is predominated by the nature of the organic ligand, anions, solvent and geometric need of the metal ions. It was found that the coordination number of Pb^II ions is eight, (PbN₃O₅) has a stereo-chemically active electron lone pair and the coordination sphere is hemi-directed. PbO nanoparticles are obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. Scanning electron microscopy shows that the size of the PbO particles is ~30 nm.     

Thermolysis Synthesis of Pure Phase Nano-Sized Cobalt(II) Oxide from Novel Cobalt(II)-Pyrazole Discrete Nano Coordination Compound

Nano-structures of a new discrete coordination compound of divalent cobalt with the pyrazol (pzH) containing the terminal isothiocyanate anions, [Co(pzH)₂(NCS)₂] (1), with discrete molecular architecture in solid state was synthesized by a sonochemical method. The new nanostructure was characterized by scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray powder diffraction, IR, and elemental analysis. The supramolecular features in these complexes are guided and controlled by weak directional intermolecular interactions. The discrete molecules interact with each other through labile interactions creating a 3D supramolecular framework. The CoO nanoparticles were obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant.     

Sonochemical Synthesis and Characterization of the New Micro-Hexagonal-Rod Lead (II)-Azido Coordination Compound

The preparation of micro hexagonal-rods of a new 1D polymeric lead(II) complex containing the Pb₂-(μ-N₃)₂ motif, [Pb(dmp)(N₃)₂] _n (dmp is the abbreviation of 2,9-dimethyl-1,10-phenanthroline) by the sonochemical method is described. The new microcrystal is characterized by scanning electron microscopy, X-ray diffraction (XRD), elemental analyses and infrared spectroscopy. A single crystalline material is obtained by applying a heat gradient applied to a solution of the reagents. The single-crystal XRD analyses show that the coordination number for the Pb(II) ions is six, PbN6, with “stereo-chemically active” electron lone pairs and the coordination sphere being hemidirected. The single-crystal X-ray data show the chains of [Pb(dmp)(N₃)₂] _n interact with each other through the π–π stacking interactions, which create a 3D framework.     

Sonochemical Synthesis of a New Lead(II) Coordination Polymer with 2-Quinoline Carboxylate Ligand: A Precursor for the Preparation of Nano-structured Lead(II) Oxide

Crystalline and nano-structure of a new Pb(II) coordination polymer, [Pb(NO₂)(2-quc)]_n (1), {Hquc?=?2-quinoline carboxylic acid} is synthesized via heat gradient and sonochemical methods, respectively. The newly synthesized structures are characterized by scanning electron microscopy (SEM), X- ray powder diffraction (XRD), IR and ¹HNMR spectroscopies, elemental analyses and single crystal X-ray diffraction is used to understand the exact structure of the crystalline 1. Thermal stability of nano and bulk samples of compound 1 are studied and compared through thermal gravimetric and differential thermal analyses. PbO nanoparticles are then produced by calcination of the nano-structure of compound 1 at 600?°C. The obtained PbO is characterized by XRD and SEM analyses.     

Sonochemical Synthesis of One-Dimensional Nano-structure of Three-Dimensional Cadmium(II) Coordination Polymer

Nano-wires and nano-rods of a new three-dimensional cadmium(II) coordination polymer, {[Cd₃(3-pyc)₄(NCS)₂(H₂O)₄]·2H₂O} _n (1); 3-Hpyc = 3-pyridinecarboxilic acid, were synthesized by a sonochemical method in two different concetrations. The morphology of the nano-structures depend strongly on reactants’ concentration. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, elemental analyses and IR spectroscopy. Compound 1 was structurally characterized by single-crystal X-ray diffraction and is a three-dimensional polymer with two types of Cd(II) coordination environments.     

Synthesis and Characterization of Pure Phase Zn(II) and Cd(II) Oxide Nanoparticles via Thermal Decomposition of Four New Zn(II) and Cd(II) Coordination Polymers

Four new Zn(II) and Cd(II) coordination polymers, [Zn(2-AMP)₂(N₃)₂]_n (1), [Zn(2-AMP)₂(SCN)₂]_n (2), [Cd(2-AMP)(N₃)₂]_n (3) and [Cd(2-AMP)₂(SCN)₂]_n (4) {2-AMP: 2-Aminomethylpyridine}, have been synthesized and characterized by single crystal X-ray diffraction, IR spectroscopy and elemental analyses. The Zinc(II) oxide and Cadmium(II) oxide nano-particles have been synthesized from thermolysis of 1–4 at 600 °C under air atmosphere for 4 h. The ZnO and CdO nanoparticles were characterized by X-ray diffraction and scanning electron microscopy (SEM). SEM images show the average size of produced ZnO and CdO nanoparticles are 60–70 nm in all compounds.     

Preparation of Cadmium(II) Oxide Nanoparticles from a New One-Dimensional Cadmium(II) Coordination Polymer Precursor; Spectroscopic and Thermal Analysis Studies

A one-dimensional Cd(II) coordination polymer containing 2-pyridinecarboxylate (2-pyc⁻) and iodide anions [Cd(μ-2-pyc)(μ-I)] _n (1), is synthesized and characterized by elemental analysis, IR spectroscopy, thermal analysis and X-ray crystallography. The single-crystal X-ray data show that the coordination number for the Cd²⁺ ion is five. The thermal stability of 1 was studied by thermogravimetry and differential thermal analyzes. Cd(II)O nanoparticles were prepared by direct calcination of 1 at different temperatures. The Cd(II)O nanoparticles were characterized by X-ray powder diffraction and scanning electron microscopy. The results show that the morphology of the Cd(II)O nanoparticles is dependent upon the thermolysis temperature.     

Sonochemical Synthesis of Two New Nano-structured Cadmium(II) Supramolecular Complexes

Nano-particles of two new Cd(II) supramolecular complexes, [Cd(4,4-di-tert-bubipy)Cl₂(DMSO)] (1) and [CdI₂(4,4′-dmbpy)(DMSO)] (2) have been synthesized by sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The structure of compound 1 has been characterized by single crystal X-ray diffraction. The prepared nano-structure was characterized by scanning electron microscopy and X-ray powder diffraction. The nano-structures of supramolecular complexes have been synthesized with calcination of complexes at oleic acid as a surfactant at 190 ºC too. The size of the samples prepared by sonochemical method and calcination are about 30–40 and 40–50 nm respectively.     

Synthesis and Characterization of One-Dimensional Cu(II) Coordination Polymer in Bulk and Nano Scales: New Precursor for Preparation of Cu(II) Oxide Nanoparticles

The hydrothermal reaction of copper(II) acetate and 1,3,5-benzenetricarboxylic acid (btcH₃) leads to the formation of a coordination polymer, [Cu(btcH)(H₂0)₃] _n (1). The product was characterized by elemental analysis and IR spectroscopy. Nanoparticles of coordination polymer (1) have been synthesized by a sonochemical process and characterized. Powder XRD and IR spectra of the compound 1 both its bulk and nano-size indicate acceptable matches for the structure. Thermal decomposition of the nano-size [Cu(btcH)(H₂0)₃] _n as a precursor leads to the formation of CuO nanoparticles. Characterization of the CuO nanoparticles was carried out using IR spectroscopy, powder XRD and scanning electron microscopy. This study demonstrates that the coordination polymers may be suitable precursors for the preparation of nanoscale materials.     

Synthesis of Lead(II) Minoxidil Coordination Polymer: A New Precursor for Lead(II) Oxide and Lead(II) Hydroxyl Bromide

A new lead(II) coordination polymer, [PbBr₂(C₉H₁₅N₅O)]_n (1), where C₉H₁₅N₅O is (2,4-diamino-6-piperidine-1-yl) pyrimidine N-oxide (minoxidil) is synthesized and characterized. Polymer 1 is synthesized in methanol by sonochemical and hydrothermal methods from lead(II) acetate, KBr and the minoxidil ligand. The crystal structure of [PbBr₂(C₉H₁₅N₅O)]_n indicates a syndiotactic coordination polymer. The Pb(II) atom lies on a mirror plane; the mirror plane is perpendicular to the pyrimidine ring bisecting the piperidine ring. N–H···O intramolecular and C–H···Br, N–H···N strong intermolecular interactions were observed. Micro-rods of PbO and nano-plates of PbOHBr were prepared by thermal decomposition of the nano-structured [PbBr₂(C₉H₁₅N₅O)]_n as a precursor. Characterization of the products was carried out using X-ray crystallography, elemental analysis, FTIR spectroscopy, scanning electron microscopy, energy dispersive X-ray analysis and thermal analysis. The sonochemical method resulted in a significant reduction of reaction time, reaction temperature and particle sizes of the products.     

Sonochemical Synthesis of New Nano-Belt One-Dimensional Double-Chain Lead(II) Coordination Polymer; As Precursor for Preparation of PbBr(OH) Nano-Structure

Nano-structure of a new 1D double-chain Pb(II) coordination polymer, [Pb(μ-HPDC)(μ-Br)(H₂O)]_n (1), {H₂PDC = 2,3-pyrazinedicarboxylic acid} was synthesized by a sonochemical method. The new nano-structure was characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The structure of compound 1 was determined by single crystal X-ray diffraction and consists of 1D double-chain polymeric units. The coordination number in compound 1 is six and each lead atom is coordinated by two oxygen atoms of HPDC⁻, two nitrogen atoms of HPDC⁻ ligands, one bromide atom and one oxygen of H₂O molecule. The thermal stability of compound 1 was studied by thermal gravimetric and differential thermal analyses. Calcination of the nano-belts of compound 1 at 500 °C under air atmospheres yielded nano-sized particles of PbBr(OH) that characterized by scanning electron microscopy and X-ray powder diffraction.     

Synthesis and Characterization of New Zinc(II) Coordination Polymer with a Flexible Hetro-coordination Ligand via In Situ Reaction as a New Precursor for Zinc(II) Oxide Nano-sphere Particles

A new coordination polymer, [Zn₃(tza)₃(H₂O)₃] _n (1) which H₂tza?=?1H-tetrazolate-5-acetic acid has been synthesized and characterized by IR spectroscopy, elemental analysis X-ray crystallography. The single-crystal X-ray data of compound 1 show existence of three different ZnII ion with different coordination spheres, hexagonal, pyramidal and pentagonal. This coordination polymer used as a precursor for preparation of zinc(II) oxide nano-particles. Nano-particles were characterized by powder X-ray powder diffraction and the its morphology characterized by scanning electron microscope.     

Synthesis and Characterization of the New Nano Flowers Lead(II) Coordination Polymer with Hemidirected Coordination Sphere

Nano flowers of a new polymeric lead(II) complex containing the azide anions, [Pb(baea)(N₃)·(N₃)] _n (“baea” is the abbreviation of bis(2-aminoethyl)amine), has been synthesized by a sonochemical method. The new nano-structure was characterized by transmission electron microscopy, scanning electron microscopy, X-ray powder diffraction, elemental analyses, and IR spectroscopy. Single crystalline material was obtained using a heat gradient applied to a solution of the reagents. Single-crystal X-ray diffraction analyses show that the coordination number for Pb^II ions is five, PbN5 and hold hemidirected coordination geometry. To the best of our knowledge, the 1D coordination polymer interact with each other via supramolecular and weak Pb···N interactions to create 2D supramolecular frameworks.     

Sonochemical Synthesis and Structural Characterization and DFT Calculations of a Novel Nano Flower Pb(II) Coordination Compound [Pb(phen)2(4-abs)2]n

Nano-structures of a new coordination polymer of divalent Pb with the ligands 1,10-phenanthroline (phen) and 4-aminobenzene sulfonic acid (4-abs), [Pb(phen)₂(4-abs)₂]_n (1), were synthesized by a sonochemical method that produced a coordination polymer of nanometer size. The new nano-structure was characterized by scanning electron microscopy, X-ray powder diffraction and IR spectroscopy and elemental analysis. Compound 1 was structurally characterized by single crystal X-ray diffraction and showed that the coordination number of the Pb(II) ions is six; i.e. (PbN₄O₂). Compound 1 also has a stereochemically active lone pair of electrons and a hemi-directed coordination sphere. The chains interact with each other through π–π stacking to create a 3D framework. The structure of 1 was optimized by density functional theory calculations. The calculated structural parameters and IR spectra of 1 are consistent with the crystal structure.     

Direct Synthesis of Cd3OSO4 Nano-particles From a New Three-dimensional Cadmium(II) Coordination Polymer Precursor

A new three-dimensional Cd(II) coordination polymer, {[Cd₃(3-pyc)₄(NCS)₂(H₂O)₄]·2H₂O} _n (1); 3-Hpyc = 3-pyridinecarboxylic acid, was prepared and characterized by elemental analyses and IR spectroscopy. Compound 1 was structurally characterized by single-crystal X-ray diffraction. The structural determination shows that the compound is a new 3D coordination polymer has different environments containing CdO₅NS and CdO₂N₄ units. This polymeric precursor has been used in the preparation of Cd₃OSO₄ nanoparticles by thermolysis in oleic acid. The new nano-structure of Cd₃OSO₄ was characterized by scanning electron microscopy and X-ray powder diffraction. This study demonstrates that coordination polymers may be suitable precursors to the preparation of desirable nanoscale materials.     

Synthesis and Characterization of Zinc(II) Oxide Nanoparticles by Thermal Decomposition of Two Zinc(II) Nitrite Coordination Polymer Precursors

Two zinc(II) coordination polymers, {[Zn(3-bpdb)(NO₂)]·0.5H₂O} _n (1) and [Zn(4-bpdb)(NO₂)₂] _n (2), 3-bpdb = 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene and 4-bpdb = 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene}, have been synthesized and characterized by elemental analyses and IR spectroscopy. Nanoparticles of zinc(II) oxide have been prepared by thermolyses of two different zinc(II) coordination polymers, 1–2. The nano-materials were characterized by scanning electron microscopy, X-ray powder diffraction and IR spectroscopy. The thermal stability of ZnO nano-particles was studied by thermal gravimetric and differential thermal analysis and showed that there is no loss of weight, which indicates that the products were zinc(II) oxide. This study demonstrates the coordination polymers may be suitable precursors for the preparation of nanoscale materials.