Synthesis of a new Hg(II) coordination polymer: Ultrasonic-assisted synthesis and mechanical preparation of nanostructure

A new mercury(II) coordination polymer, [Hg(4-bpmo)I₂]_n (1), (4-bpmo = N,N′-bis(pyridin-4-ylmethyl)oxalamide), was synthesized, by branched tube method, and structurally characterized by single-crystal X-ray diffraction. Compound 1 is a polymer with a distorted tetrahedral HgN₂I₂ coordination environment. The thermal stability of 1 was studied by thermal gravimetric (TG) and differential thermal (DTA) analyses. Also 1 was prepared by a sonochemical process at ambient temperature. Reaction time and concentration of initial reagents effects on the size and morphology were studied. Nanoparticles of 1, was synthesized easily by a mechanical method (neat grinding). The resulting structures were characterized by scanning electron microscopy (SEM), IR spectroscopy and X-ray powder diffraction (XRD).     

Sonochemical syntheses of a new fibrous-like nano-scale manganese(II) coordination supramolecular compound; precursor for the fabrication of octahedral-like Mn3O4 nano-structure

Nanoparticles of a new three-dimensional Mn(II) coordination supramolecular compound, [Mn(L)₂(H₂O)₂] (1), (L⁻ = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses. Structural determination of compound 1 reveals the Mn(II) ion is six coordinated, bonded to two nitrogen atoms, two oxygen atoms from the L⁻ ligand and two water molecules. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied and shows that low concentrations of initial reagents decreased particles size and also leaded to fibrous-like nanostructures morphology. Mn₃O₄ nano-structure with an octahedral-like morphology were simply synthesized by solid-state transformation of compound 1 at 650 °C.     

Synthesis and characterization of a new nano lead(II) 0-D coordination supramolecular compound: A precursor to produce pure phase nano-sized lead(II) oxide

Nano-structure of a new 0D Pb(II) coordination supramolecular compound, [Pb₄(8-Quin)₆](ClO₄)₂(1), L = 8-HQuin = 8-hydroxyquinolin ligand has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) and elemental analyses. The structure of compound 1 was determined by single-crystal X-ray diffraction. The single crystal X-ray data of compound 1 implies that the Pb⁺² ions are five coordinated. Each lead atom is coordinated to nitrogen and oxygen atoms of 8-hydroxyquinolin ligand. Topological analysis shows that the compound 1 is 1,2,3,4,4M12-1net. Nanoparticles of lead(II) oxide have been prepared by calcination of lead(II) coordination polymer at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD) and IR spectroscopy.     

Sonochemical synthesis and characterization of nano-sized lead(II) 3D coordination polymer: Precursor for the synthesis of lead(II) oxybromide nanoparticles

Nanoparticles of a three-dimensional coordination polymer, [Pb(L)(μ₂-Br)(H₂O)]_n (1), (L^? = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by an ultrasonic method and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal (DTA) analyses and compared each other. Concentration of initial reagents effects and the role of power ultrasound irradiation on size and morphology of nano-structured compound 1, have been studied. Calcination of the compound 1 at 500 °C under air atmosphere yields Pb₃O₂Br₂ nanoparticles.     

Sonochemical synthesis and characterization of new one-dimensional manganese(II) coordination polymer nanostructures

A new Mn(II) coordination polymer, [Mn (L₁)₂(NCS)₂]_n (1) [L₁ = 3,4-bis(4-pyridyl)-5-(2-pyridyl)-1,2,4-triazole] was synthesized by the reaction of ligand L₁ and mixtures of manganese(II) acetate and potassium thiocyanate using the heat gradient method. Compound 1 has been characterized by IR spectroscopy, elemental analyses and X-ray crystallography. The crystal structure of compound 1 was determined by single-crystal X-ray diffraction and shows a new interesting one-dimensional coordination polymer. Nanostructures of compound 1 have been synthesized by sonochemical method. The products were characterized by X-ray powder diffraction, scanning electron microscopy (SEM), and IR spectroscopy. The thermal stability of nano particles of compound 1 was studied by thermal gravimetric and differential thermal analyses.     

Sonochemical syntheses of binuclear lead(II)-azido supramolecule with ligand 3,4,7,8-tetramethyl-1,10-phenanthroline as precursor for preparation of lead(II) oxide nanoparticles

The new neutral binuclear lead(II) azido coordination compound, [Pb₂(tmph)₂(μ-N₃)₂(CH₃COO)₂] (1) [tmph = 3,4,7,8-tetramethyl-1,10-phenanthroline], has been synthesized by a sonochemical method. Single crystal X-ray structure shows that the overall structure of 1 is binuclear unit. Complex 1 has a bridging azido pathway, end-to-end bridging azides between a pair of lead(II) centers. This is further extended into a one-dimensional (1D) and three-dimensional (3D) supramolecular structure by Pb⋯C and π–π weak directional intermolecular interactions. The coordination number of lead(II) ions is seven, PbN₄O₃, with two N-donor atoms from tmph ligands and three O-donors from acetate anions and two N-donors from two azide anions. It has a “stereo-chemically active” electron lone pair, and the coordination sphere is hemidirected. The PbO nanoparticles were obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. The morphology and size of the prepared PbO samples were further observed using scanning electron microscopy (SEM).     

Effect of two sonochemical procedures on achieving to different morphologies of lead(II) coordination polymer nano-structures

Micro and nano-structures of a lead(II) coordination polymer, [Pb₂(2-Me-8-Hq)₂(MeOH)₂]_n (1), [2-Me-8-HqH = 2-methyl-8-hydroxyquinoline]_, were synthesized by two sonochemical methods. These new micro and nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compound 1 was structurally characterized by single-crystal X-ray diffraction and consists of primary dimeric unit of [Pb₂(2-Me-8-Hq)₂(MeOH)₂]. Self assembly between the dimmeric units of [Pb₂(2-Me-8-Hq)₂(MeOH)₂] from Pb-O bonds results in formation of a one-dimensional lead(II) coordination polymer. The Pb^II-ion in compound 1 has PbO₆N₁ coordination sphere with a stereo-chemically ‘active’ electron lone pair on the metals. By a reversible solid-state structural transformation, we successfully prepared [Pb₂(2-Me-8-Hq)₂]_n (2) by thermal desolvation of 1. Thermal stability of compound 1 was studied by thermo gravimetric and differential thermal analyses. In addition nano-structure of PbO was prepared from calcination process of compound 1 at 873 K.     

Sonochemical synthesis and structural characterization of a new nanostructured Co(II) supramolecular coordination polymer with Lewis base sites as a new catalyst for Knoevenagel condensation

A new Co(II) mixed-ligand coordination supramolecular polymer with composition [Co₂(ppda)(4-bpdh)₂(NO₃)₂]_n (1) (where, ppda = p-phenylenediacrylic acid, 4-bpdh = 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene) was synthesized using solvothermal, mechanochemical and sonochemical methods. Compound 1 and the new nanostructure have been characterized by single-crystal X-ray, infrared spectroscopy (IR), powder X-ray diffraction (PXRD) analysis and scanning electron microscopy (SEM). The thermal stability of compound 1 was also studied by thermal gravimetric analysis (TGA). The surface area of these compounds was determined by BET. The single-crystal X-ray data shows a new interesting two-dimensional coordination polymer (CP). In addition, the effect of various sonication concentrations of initial reagents, power of ultrasound irradiation and also the time on the size and morphology of nano-structured coordination polymer 1 were evaluated. Moreover, it has been demonstrated that the nanostructure of the CP1 can be used as a catalyst in Knoevenagel condensation reaction.     

Ultrasonic-assisted synthesis and structural characterization of two new nano-structured Hg(II) coordination polymers

Two new Hg(II) coordination polymers containing N,N′-Bis-pyridin-3-ylmethylene-naphtalene-1,5-diamine ligand were synthesized by conventional and sonochemical methods, characterized by spectroscopic techniques (FT-IR and elemental analysis), and their X-ray crystallographic structures were determined. The crystal packing and supramolecular features of these coordination polymers were studied using geometrical analysis and Hirshfeld surface analysis. The crystal structure analysis revealed that H⋯H contacts, C–H⋯π and C–H⋯X (X = Cl for 1 and X = Br for 2) hydrogen bonding interactions are strong enough to govern the supramolecular architecture. The BFDH analysis helps us to compare the predicted morphology to that obtained under ultrasonication. This study may provide further insight into discovering the role of weak intermolecular interactions in the context of nano-supramolecular assembly.     

Sonochemical synthesis,characterization, and effects of temperature,power ultrasound and reaction time on the morphological properties of two new nanostructured mercury(II) coordination supramolecule compounds

Two new mercury(II) coordination supramolecular compounds (CSCs) (1D and 0D), [Hg(L)(I)₂]_n (1) and [Hg₂(L′)₂(SCN)₂]·2H₂O (2) (L = 2-amino-4-methylpyridine and L′ = 2,6-pyridinedicarboxlic acid), have been synthesized under different experimental conditions. Micrometric crystals (bulk) or nano-sized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by field emission scanning electron microscope (FESEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD) and FT-IR spectroscopy. Single crystal X-ray analyses on compounds 1 and 2 show that Hg²⁺ ions are 4-coordinated and 5-coordinated, respectively. Topological analysis shows that the compound 1 and 2 have 2C1, sql net. The thermal stability of compounds 1 and 2 in bulk and nano-size has been studied by thermal gravimetric (TG), differential thermal analyses (DTA) for 1 and differential scanning calorimetry (DSC) for 2, respectively. Also, by changing counter ions were obtained various structures 1 and 2 (1D and 0D, respectively). The role of different parameters like power of ultrasound irradiation, reaction time and temperature on the growth and morphology of the nano-structures are studied. Results suggest that increasing power ultrasound irradiation and temperature together with reducing reaction time and concentration of initial reagents leads to a decrease in particle size.     

Ultrasound irradiation effect on morphology and size of two new potassium coordination supramolecule compounds

Two new potassium coordination supramolecular compounds (2D and 1D), [K(H₃L)(H₂L)(H₂O)]_n·H₂O (1) and [K(H₂L′)(HL′)(H₂O)₂]·H₂O (2), (L = 1,3,5-tricarboxylic acid, L′ = 2,6-pyridinedicarboxylic acid), have been synthesized under different experimental conditions. Micrometric crystals (bulk) or nano-sized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by field emission scanning electron microscopy (FE-SEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), FT-IR spectroscopy and elemental analyses. Single crystal X-ray analyses on compounds 1 and 2 show that K⁺ ions are 3- and 7-coordinated, respectively. Additionally, H-bonds incorporate the layers and chains in 1 and 2 into 3D and 2D (along (0,0,1) direction) frameworks. Topological analysis shows that the compound 1 and 2 are 3,6-coordinated kgd and 2,4-coordinated 2,4C4 net. The thermal stability of compounds 1 and 2 in bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. The role of different parameters like temperature, reaction time and ultrasound irradiation power on the growth and morphology of the nano-structures are studied. Results suggest that an increase of temperature, sonication power and reduction of reaction time led to a particle size decrease.     

Sonochemical synthesis of nano-scale mixed-ligands lead(II) coordination polymers as precursors for preparation of PbO and PbBr(OH) nano-structures; thermal,structural and X-ray powder diffraction studies

Nano-structures of two new lead(II) two-dimensional coordination polymers, [Pb₂(2-pyc)₂(I)₂]_n (1) and [Pb₂(2-pyc)₂(Br)₂]_n (2), {2-Hpyc = 2-pyridinecarboxilic acid } were synthesized by a sonochemical method that produce the coordination polymers at nano-size. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction and consist of two-dimensional polymeric units. The thermal stability of compounds 1 and 2 were studied by thermal gravimetric and differential thermal analyses. PbO and PbBr(OH) nano-structures were obtained by calcination of the nano-structures of compounds 1 and 2 at 400 °C, respectively.     

Sonochemical synthesis of a new nano-sized cerium(III) supramolecular compound; Precursor for nanoceria

Using a sonochemical method, nanoparticles of a new Ce(III) supramolecular compound, (NAMH⁺)₂[Ce₄(pydc)₆(pydcH)₂(H₂O)₈]·8H₂O (1), (H₂pydc = 2,6-pyridinedicarboxylic acid, NAM = nicotinamide), have been synthesized. Compound 1 was characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses, and its structure was determined by X-ray crystallography. It has been revealed that its structure consists of tetra-nuclear building units that extend to a 3D supramolecular network via non-covalent interactions mainly hydrogen bonding. The thermal stability of complex 1 both for its crystals and nanostructures has been studied by the thermal gravimetric (TG) method and compared with each other. The role of ultrasound irradiation power and the concentration of initial reactants on the size and morphology of the nano-structured complex 1, has been investigated. Ceria nanoparticles were obtained upon the calcination of complex 1 at 800 °C under atmospheric air. Furthermore, the fluorescent properties of complex 1 at room temperature were studied.     

Application of ultrasound to the synthesis of a new nanostructured Mn(II) supramolecular compound: A precursor for γ-Mn2O3 nanoparticles

A new nanostructured Mn(II) supramolecular compound [Mn(hpydcH₂)₂(H₂O)₄] (1) (hpydcH₃ = 4-hydroxy-2,6-pyridinedicarboxylic acid) has been synthesized using a sonochemical process. The structure of compound 1 was determined by single crystal X-ray diffraction and it was revealed that each hpydcH₂⁻ anionic ligand has been coordinated to Mn(II) ion in a novel monodentate fashion leaving another functional carboxylic acid group intact. Compound 1 was also characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analysis. Thermal stability of compound 1 was studied by thermal gravimetric (TG) analysis and compared to that of its crystalline analogue. Subsequently, the role of concentration of the initial reactants on the size of nanostructures of compound 1, has been investigated. Compound 1 was proved to be a precursor for γ-Mn₂O₃ nanoparticles.     

Sonochemical synthesis of nanoscale mixed-ligands lead(II) coordination polymers as precursors for preparation of Pb2(SO4)O and PbO nanoparticles; thermal,structural and X-ray powder diffraction studies

Nano-structures of two new Pb(II) two-dimensional coordination polymers, [Pb(μ-4-pyc)(μ-NCS)(μ-H₂O)]_n (1) and [Pb(μ-4-pyc)(μ-N₃)(μ-H₂O)]_n (2), 4-Hpyc = 4-pyridinecarboxylic acid were synthesized by a sonochemical method. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction and consist of two-dimensional polymeric units. The thermal stability of compounds 1 and 2 were studied by thermal gravimetric and differential thermal analyses and compared. Pb₂(SO₄)O and PbO nanoparticles were obtained by calcination of the nano-structures of compounds 1 and 2 at 600 °C, respectively.     

Sonochemical synthesis of two new nano structure zinc(II) 1,10-phenanthroline coordination supramolecular compounds: New precursors to produce nano-sized zinc(II) oxide

Nanoparticles of two zinc(II) coordination supramolecule compounds (CSCs), [Zn(L)Cl2] (1) and [Zn(L)Br2] (2) L = 1,10-phen = 1,10-phenanthroline ligand, have been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared (FTIR) spectroscopy and elemental analyses. The single crystal X-ray data of compounds 1 and 2 imply that the Zn⁺² ions are four coordinated. Topological analysis shows that the compound 1 and 2 are new topology for net: 1,3M4-1. Nanoparticles of zinc(II) oxide have been prepared by calcination of two different zinc(II) CPs at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and IR spectroscopy.     

Recombination luminescence of CsI(Tl) under electron pulse irradiation

The luminescence kinetics of CsI(Tl) exposed to an electron pulse irradiation (E_e = 250 keV, t_1/2 = 10 ns, j = 2 ÷ 160 mJ/cm²) has been studied. It has been discovered that the slow emission rise is due to hole V_k–Tl⁰ recombination luminescence at temperature from 100 to 160 K and electron–V_kA recombination, where electrons released from single Tl⁰ at temperature from 180 to 300 K. The effect of Tl concentration on both processes has been investigated.     

Sonochemical synthesis of two new nano lead(II) coordination polymers: Evaluation of structural transformation via mechanochemical approach

Two new lead(II) mixed-ligand coordination polymers, [Pb(PNO)(SCN)]_n (1) and [Pb(PNO)(N₃)]_n (2), (HPNO = picolinic acid N-oxide) were synthesized by a sonochemical method and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analysis. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction. The thermal behavior of 1 and 2 were studied by thermal gravimetric analysis. Structural transformations of compounds 1 and 2 were evaluated through anion-replacement processes by mechanochemical method. Moreover, the effect of sonication conditions including time, concentrations of initial reagents and power of irradiation were evaluated on size and morphology of compounds 1 and 2.     

Syntheses and structural characterization of two new nanostructured Bi(III) supramolecular polymers via sonochemical method

Two new bismuth(III) coordination supramolecular polymers, {[Bi₂(Hbpp)(bpp)(μ-I)₂I₆](Hbpp)·MeOH}_n (1) and [Bi(Hbpp)(Br₄)] (2), (bpp = 1,3-di(pyridin-4-yl)propane) were prepared and were structurally characterized by single crystal X-ray diffraction. Single crystalline one-dimensional materials were prepared using a heat gradient applied a solution of the reagents using the branched tube method. The structural determination by single crystal X-ray crystallography shows that compounds 1 and 2 form monoclinic polymers with symmetry space group P2₁ in the solid state. These new nanostructured Bi(III) supramolecular compounds, {[Bi₂(Hbpp)(bpp)(μ-I)₂I₆](Hbpp)·MeOH} (1) and [Bi(Hbpp)(Br₄)] (2), were also synthesized by sonochemical method. The nanostructures were characterized by Field Emission-scanning electron microscopy (FE-SEM), powder X-ray diffraction (PXRD) and IR spectroscopy.     

Sonochemical synthesis of two nanostructured silver(I) coordination polymers based on semi-rigid bis(benzimidazole) ligands

Nanoparticles of two silver(I) coordination polymers (CPs), [Ag₂(L1)₂(DCTP)]_n (1) and [Ag₂(L2)(DCTP)]_n (2) (L1 = 1,3-bis(5,6-dimethylbenzimidazol-1-ylmethyl)benzene, L2 = 1,4-bis(benzimidazol-1-yl)-2-butene, H₂DCTP = 2,5-dichloroterephthalic acid), were synthesized by the sonochemical approach and hydrothermal method. Both CPs were characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction, scanning electron microscopy (SEM), and thermogravimetric analyses (TGA). CP 1 exhibits a 2D 4-connected sql net with the point symbol {4⁴.6²}. While CP 2 displays a 2D 3,4-connected 3,4L13 net with the point symbol {4.6²}₂{4².6².8²}. The structural diversity indicates that semi-rigid bis(benzimidazole) co-ligands play important roles in tuning the structures of the mixed Ag(I) CPs. The ultrasound irradiation time, temperature, and power showed significant effects on the morphology and growth process of the nanoparticles of two silver(I) CPs. The luminescence and photocatalytic properties of the nanoparticles of CPs 1–2 on the degradation of methyl blue (MB) were also investigated in detail.