Sonochemical syntheses and characterization of a new nano-sized 2-D lead(II) coordination polymer as precursor for preparation of PbBr(OH) nano-structure

Nano-particles of a new 2-D Pb(II) coordination polymer, [Pb(4-pyc)(Br)(H₂O)] _n (1) (4-Hpyc = 4-pyridinecarboxylic acid), were synthesized by a sonochemical method. Crystal structure of 1 was determined by X-ray crystallography. The nano-particles were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy, and elemental analyses. PbBr(OH) nano-structure was obtained by the calcination of nano-particles of 1 at 400°C.     

Nanoparticles of a new mercury(II) coordination polymer: synthesis,characterization, thermal and structural studies

Nanoparticles of a new Hg(II) one-dimensional coordination polymer, {[Hg(4-bpdb)I₂] _n , 4-bpdb?=?1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene} were synthesized by reaction of HgI₂ and 4-bpdb by a sonochemical method. The new nanoparticles were characterized by scanning electron microscopy, X-ray powder diffraction (XRD) and FT-IR spectroscopy; [Hg(4-bpdb)I₂] _n was structurally characterized by single crystal X-ray diffraction. This compound consists of one-dimensional polymeric units of [Hg(4-bpdb)I₂]. The thermal stability of [Hg(4-bpdb)I₂] _n was studied by thermal gravimetric (TG) and differential thermal analyses (DTA).     

Nanoparticles of a new zinc(II) coordination polymer: synthesis,characterization, thermal,and structural studies

Nanoparticles of a Zn(II) coordination polymer {[Zn(DADMBTZ)(CH₃COO)₂] _n , DADMBTZ?=?2,2′-diamino-5,5′-dimethyl-4,4′-bithiazole} were synthesized by reaction of Zn(NO₃)₂?·?4H₂O, CH₃COONH₄ and DADMBTZ by a sonochemical method. The nanoparticles were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), and Fourier transform infrared (FT-IR) spectroscopy. [Zn(DADMBTZ)(CH₃COO)₂] _n was structurally characterized by single-crystal X-ray diffraction. In this four-coordinate compound with nearly C₂ symmetry, DADMBTZ is bidentate. The metal lies in a pseudo-tetrahedral environment and is ligated by the two bithiazole ring nitrogen atoms and an oxygen from each of the two monodentate acetates; 2-D networks are formed via N–H···O hydrogen bonds. Thermal stability of [Zn(DADMBTZ)(CH₃COO)₂] _n was studied by thermal gravimetric and differential thermal analyses. A ZnO nanostructure was obtained by direct thermolyses at 500°C under air. The ZnO nanostructure was characterized by SEM, XRD, and FT-IR spectroscopy.     

Sonochemical syntheses of a straw-like nano-structure two-dimensional mixed-ligand zinc(II) coordination polymer as precursor for preparation of nano-sized ZnO

Straw-like nano-structure of a new mixed-ligand Zn(II) two-dimensional coordination polymer, {[Zn(μ-4,4′-bipy)(μ-3-bpdb)(H₂O)₂](ClO₄)₂·4,4′-bipy·3-bpdb·H₂O}_n (1) {4,4′-bipy = 4,4′-bipyridine and 3-bpdb = 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene}, was synthesized by a sonochemical method. The new nano-structure was characterised by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compound 1 was structurally characterised by single crystal X-ray diffraction and consists of two-dimensional polymeric units. ZnO nanoparticles were obtained by calcination of compound 1 at 500 °C under air atmosphere and were characterised by X-ray diffraction (XRD) and scanning electron microscopy (SEM).     

Sonochemical synthesis and characterization of a nanostructured 3-D lead(II) coordination polymer with 4-methoxybenzoyltrifluoroacetone

Nanoparticles of a 3-D coordination polymer, [Pb₂(mbtfa)₄] _n (1) (Hmbtfa?=?4-methoxybenzoyltrifluoroacetone), have been synthesized by a sonochemical method. The nanomaterial was 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. The structure of 1 shows the compound is triclinic and consists of 3-D polymeric units.     

Ultrasound assisted syntheses of a nano-structured two-dimensional mixed-ligand cadmium(II) coordination polymer and direct thermolyses for the preparation of cadmium(II) oxide nanoparticles

A nano-sized mixed-ligand Cd(II) coordination polymer, {[Cd(bpa)(4,4′-bipy)₂(H₂O)₂](ClO₄)₂}_n (1); bpa = trans-1,2-bis(4-pyridyl)ethane and 4,4′-bipy = 4,4′-bipyridine, has been synthesized by a sonochemical method and characterized by IR and ¹H NMR spectroscopy. Compound 1 grows in one dimension by two different bridging ligands, 4,4′-bipy and bpa. The thermal stability of compound 1 in the bulk form and nano-sized was studied by thermogravimetric (TG) and differential thermal analysis (DTA). The crystallinity of this compound was studied by X-ray powder diffraction and compared with an XRD simulation of the single crystal data. CdO nanoparticles were obtained by direct calcination at 500 °C and decomposition in oleic acid at 200 °C of the nano-sized compound 1. The obtained cadmium(II) oxide nano-particles were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM).     

Syntheses and characterization of a new nano-structured bismuth(III) bromide coordination polymer; new precursor for preparation of bismuth(III) bromide and bismuth(III) oxide nanostructures

Nanoparticles of a Bi(III) coordination polymer, {[Bi(μ-4,4′-bipy)Br₄] · (4,4′-Hbipy)} _n (1) (4,4′-bipy = 4,4′-bipyridine), were synthesized by a sonochemical method. The new nanoparticles were characterized by scanning electron microscopy, X-ray powder diffraction (XRD), IR spectroscopy, and elemental analyses. Compound 1 was structurally characterized by single-crystal X-ray diffraction. The thermal stabilities of 1 as bulk and at nanosize were studied by thermal gravimetric (TG) and differential thermal analyses (DTA). The Bi₂O₃ and BiBr₃ nanostructures were obtained by calcinations of nanostructure of 1 in air and argon.     

Ultrasonic-assisted synthesis of two new nano-structured 3D lead(II) coordination polymers: Precursors for preparation of PbO nano-structures

Nano-structures of two new Pb(II) three-dimensional coordination polymers, [Pb₂(4-pyc)₂I₂(H₂O)]_n (1), {4-Hpyc = 4-pyridinecarboxilic acid} and [Pb(3-pyc)I]_n (2), {3-Hpyc = 3-pyridinecarboxilic acid} were synthesized by 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 are three-dimensional coordination polymers. The thermal stability of compounds 1 and 2 both their bulk and nano-size were studied by thermal gravimetric and differential thermal analyses and compared. PbO block-structures were obtained by calcination of the nano-structures of compounds 1 and 2 at 400 °C.     

A new mixed ligand coordination polymer of Mn(II): structural aspect and cryomagnetic study

A new 1-D polymeric chain complex [Mn(pydc)(1,10-phen)]_n· nH₂O (pydc = pyridine-2,3-dicarboxylate, 1,10-phen = 1,10-phenanthroline) has been synthesised and characterised by elemental analysis, FT-IR spectrum, thermal analysis and variable temperature magnetic susceptibility studies. Single crystal X-ray diffraction study reveals that the central Mn(II) ion is in a distorted octahedral coordination geometry, and is coordinated to pydc and 1,10-phen. The complex shows interesting hydrogen bond modes involving the dicarboxylates and lattice water molecules. The presence of weak antiferromagnetic coupling with J = −0.72 cm⁻¹ for the complex has been concluded from the cryomagnetic susceptibility studies.     

Dicarboxylate assisted synthesis of the monoclinic heterometallic tetrathiocyanato bridged copper(II) and mercury(II) coordination polymer {Cu[Hg(SCN)4]}n: Synthesis, structural, vibration, luminescence, EPR studies and DFT calculations

The synthesis of the monoclinic polymorph of {Cu[Hg(SCN)₄]}_n is reported. The compound, as determined by X-ray diffraction of a twinned crystal, consists of mercury and copper atoms linked by μ_1,3-SCN bridges. The crystal packing shows a highly porous infinite 3D structure. Diagnostic resonances for the SCN^- ligand and metal-ligand bonds in the IR, far-IR and Raman spectra are assigned and discussed. The electronic band structure along with density of states (DOS) calculated by the DFT method indicates that the compound is an indirect band gap semiconductor. The DFT calculations show that the observed luminescence of the compound arises mainly from an excited LLCT state with small MLCT contributions (from the copper to unoccupied π^? orbital of the thiocyanate groups). The X-band EPR spectrum of the powdered sample at room temperature reveals an axial signal with anisotropic g factors consistent with the unpaired electron of Cu(II) ion in the d_x²−y² orbital.     

Synthesis,crystal structures,and characterization of two Co(II) coordination polymers with 3-pyrid-3-ylbenzoic acid

Two pyridinecarboxylato-bridged coordination polymers {[Co(pbc)₂(H₂O)] · H₂O} _n (1) and [Co(pbc)₂] _n (2) (Hpbc = 3-pyrid-3-ylbenzoic acid) have been synthesized by the hydrothermal method and characterized by X-ray single crystal diffraction. In 1, pbc^? ligands link two Co(II) centers as μ₂-N,O and μ₂-N,O,O. Co(II) is six coordinate, octahedral. In 2, Co(II) is coordinated by four oxygens and two nitrogens. The ligands are μ₂-N,O,O and μ₃-N,O,O. Through different pbc^? ligands, 2 generates a 3-D network composed of six-connected nodes. Compound 2 exhibits good photoluminescence, whereas 1 is nonemissive at room temperature.     

Syntheses and characterization of different zinc(II) oxide nano-structures from direct thermal decomposition of 1D coordination polymers

Three zinc(II) nitrite coordination polymers, [Zn(4-bpdb)(NO₂)₂]_n (1), {[Zn(3-bpdb)(NO₂)]·0.5H₂O}_n (2) and [Zn(3-bpdh)(NO₂)₂]_n (3), 4-bpdb = 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene, 3-bpdb = 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene and 3-bpdh = 2,5-bis(3-pyridyl)-3,4-diaza-2,4-hexadiene} were prepared and characterized by elemental analyses and IR spectroscopy. Compound 3 was structurally characterized by single-crystal X-ray diffraction and is one-dimensional polymer with coordination environments of distorted octahedral, ZnN₂O₄. The thermal stabilities of compounds 1–3 were studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Direct calcination of the compounds 1–3 at 600 °C under air atmospheres yields different morphologies of nano-sized ZnO.     

Synthesis and characterization of Cu(II), Co(II) and Ni(II) coordination polymers containing bis(imidazolyl) ligands

Two structurally related flexible imidazolyl ligands, bis(N-imidazolyl)methane (L₁) and 1,4-bis(N-imidazolyl)butane (L₂), were reacted with Cu(II), Co(II) and Ni(II) salts of aliphatic/aromatic dicarboxylic acids resulting in the formation of a number of novel metal–organic coordination architectures, [CuB₂(ox)₂(L₁)₂(H₂O)₂] · 4H₂O (1) (ox = oxalate), [Cu(pdc)(L₂)_1.5] · 4H₂O (2, pdc = pyridine-2,6-dicarboxylate), [Co(L)₂(H₂O)₂](tp) · 4H₂O (3, tp = terephthalate), [Ni(L₁)₂(H₂O)₂](ip) · 5H₂O (4, ip = isophthalate), [Cu₂(L₁)₄(H₂O)₄](tp)₂ · 7H₂O (5), [Co(mal)(L₁)(H₂O)] · 0.5MeOH (6, mal = malonate), [Co(pdc)(L₁)(H₂O)] (7). All the complexes have been structurally characterized by X-ray diffraction analysis. The different coordination modes of the dicarboxylate anions, due to their chain length, rigidity and diimidazolyl functionality, lead to a wide range of different coordination structures. The coordination polymers exhibit 1D single chain, ladder, 2D sheet and 2D network structures. The aliphatic and aromatic dicarboxylates can adopt chelating μ₂ and chelating-bridging μ₃ coordination modes, or act as uncoordinated counter anions. The central metal ions are coordinated in N₂O₄, N₄O₂, N₂O₃ and N₃O₃ fashions, depending on the ancillary ligands. The topology of 1 gives rise to macrocycles which are connected through hydrogen bonds to form 1D chains, whereas compound 2 exhibits a 1D polymeric ladder in which the carboxylate acts as a pincer ligand. Compounds 3–5 show doubly bridged 1D chains, and the dicarboxylate groups are not coordinated but form 2D corrugated sheets with water molecules intercalated between the cationic layers. Compound 6 has a 2D network sheet structure in which each metal ion links three neighboring Co atoms by the bis(N-imidazolyl)methane ligand. The cobalt compound 7, with a 2D polymeric double sheet structure, is built from pincer carboxylate (pdc) and 1,4-bis(N-imidazolyl)methane ligands.     

Cadmium(II) nano-dimensional square grid polymers based on bis(imidazol-1-yl-methyl)benzene: synthesis,characterization, and photoluminescence

Two new nano-dimensional square grid metal–organic polymers, {[Cd(1,3-bix)₂(H₂O)₂](NO₃)₂} _n (1) and [Cd(1,3-bix)₂(NO₃)₂] _n (2) (1,3–bix?=?1,3-bis(imidazol-1-yl-methyl)benzene), have been synthesized and structurally characterized by single-crystal X-ray crystallography and FT-IR spectroscopy. Polymers 1 and 2 are 2-D layer structures consisting of nano-dimensional square grid units. The photoluminescent properties of 1 and 2 were investigated.     

Tuning the topological net of two new copper(II) coordination polymers based on a paddle-wheel secondary building unit via altering the auxiliary ligands

Two new coordination polymers, [Cu(BDC)(L₁)_0.5]_n (1) and [Cu(BDC)(L₂)_0.5]_n (2) [H₂BDC=5-methyl-1,3-benzenedicarboxylic acid, L₁=1,4-bis(2-methyl-imidazol-1-yl) butane and L₂=1,4-bis(1-imidazol-yl)-2,5-dimethylbenzene], were synthesized from Cu(II), H₂BDC, and L₁/L₂. The carboxylate groups in 1 and 2 are bis-monodentate. By changing the N-donor ligands, 1 and 2 exhibit different topologies from a rob topological net to a twofold interpenetrating pcu net; however, they possess the same paddle-wheel secondary building unit in which Cu(II) has square-pyramidal geometry. The thermal stabilities of 1 and 2 are investigated.     

Treatment effects and mechanisms of Cu(II) coordination polymer in hypotension after anesthesia

A Cu(II) coordination polymer (CP) (that is, [Cu₂(OH)(H₂O)₂(cbca)·2H₂O]_n (1)) has been obtained with the reaction between Cu(II) salt and 4′-(1-carboxyethoxy)-[1,1′-biphenyl]-3,5-dicarboxylic acid (H₃cbca), a semi-rigid tricarboxylic acid ligand under the hydrothermal reaction condition. Prevention activity of the new compound on hypotension after anesthesia surgery was evaluated and the related mechanism was researched at the same time. The noninvasive blood pressure monitor was firstly conducted to measure the blood pressure of the animal after compound treatment. Besides, the real time RT-PCR assay was also used to determine theα receptor relative expression on vascular endothelial cells after compound treatment.     

Synthesis,structure and electrochemical properties of a zinc(II) coordination polymer based on ferrocenyl-substituted carboxylate and bis (benzimidazolyl)pentane ligands

By reaction of two ligands, Na(o-OOCC₆H₄COFc) (Fc?=?(η⁵–C₅H₅)Fe(η⁵–C₅H₄)) and 1,1′–(1,5–pentamethylene)bis-1H-benzimidazole (pbbm), with Zn(OAc)₂?·?2H₂O in methanol solution, we have synthesized a zinc(II) coordination polymer [Zn(o-OOCC₆H₄COFc)₂(pbbm)] _n . The polymer was characterized by X-ray single crystal diffraction, IR spectroscopy, and elemental analysis. Each Zn atom was connected by two pbbm ligands, leading to an infinite one-dimensional chain. Two monodentate o-FcCOC₆H₄COO^? anions completed the coordination sphere of the central Zn(II) ion. The polymer's electrochemical properties were investigated in DMF solution.     

Thermal,spectroscopic, X-ray powder diffraction,and structural studies on a new Cd(II) mixed-ligand coordination polymer

A new coordination polymer derived from Cd(II) with both rigid and flexible spacer ligands trans-1,2-bis(4-pyridyl)ethane (bpa) and 4,4′-bipyridine (4, 4′-bipy), {[Cd(μ-bpa)(4, 4′-bipy)₂(H₂O)₂] · (ClO₄)₂} _n has been synthesized and characterized by elemental analysis, IR-, ¹H NMR spectroscopy and studied by thermal analyses as well as X-ray crystallography. The single crystal X-ray analysis shows that the complex is a 1-D polymer as a result of bridging 1,3-di(4-pyridyl)propane (bpa). The 1-D chains are further self-assembled into a 3-D network via hydrogen bonding and π–π stacking. In this structure the perchlorates fill the voids. Thermal studies of this polymer show step to step separating of ligands and counter ion at different temperatures.     

Spectroscopic,thermal and structural studies of a new mercury(II) one-dimensional coordination polymer, [Hg(3-bpo)2(SCN)2], 3-bpo = 2,5- bis (3-pyridyl)-1,3,4-oxadiazole

A new mercury(II)-organic polymeric complex generated from 2,5-bis(3-pyridyl)-1,3,4-oxadiazole (3-bpo) as an angular dipyridyl derivative ligand, [Hg(3-bpo)₂(SCN)₂], was prepared from reactions of ligand 3-bpo with mercury(II) thiocyanate. The compound was characterized by elemental analysis, IR-, ¹H NMR-, ¹³C NMR-spectroscopy and structurally determined by X-ray single crystal diffraction. The thermal stability of [Hg(3-bpo)₂(SCN)₂] was studied by thermal gravimetric (TG) and differential thermal analyses (DTA).