Novel metal complexes of mixed piperaquine-acetaminophen and piperaquine-acetylsalicylic acid: Synthesis, characterization and antimicrobial activities

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Yusuf Oloruntoyin Ayipo

2016-11-01

Full Text Available Synthesis of coordination compounds of Zinc(II, Copper(II, Nickel(II, Cobalt(II and Iron(II with mixed piperaquine-acetaminophen and piperaquine-acetylsalicylic acid has been studied. The complexes were characterized via: solubility test, melting point determination, conductivity measurement, Atomic Absorption Spectroscopy, UV-Visible Spectroscopy, FTIR Spectroscopy and magnetic susceptibility. The complexes were proposed to have a stoichiometry ratio of 1:1:1 between each metal salt and the ligands with tetrahedral and octahedral geometry following the reaction pattern of MX.yH2O + L1L2/3 to give ML1L2/3X.yH2O. Biological activities of the synthesized complexes have been evaluated against Escherichia coli and Staphylococcus aureus.

Synthesis, characterization and DFT studies of two new silver(I) complexes with 3,4-lutidine

Science.gov (United States)

Soliman, Saied M.; Assem, Rania; Abu-Youssef, Morsy A. M.; Kassem, Taher S.

2015-04-01

The synthesis, characterization and molecular structure of two new Ag(I) complexes with 3,4-lutidine (34lut) have been reported. The [Ag(34lut)3(OAC)]; 1 and [Ag(34lut)2(TFA)]; 2 complexes, where OAC and TFA are acetate and trifluoroacetate respectively, have been characterized using elemental analysis, FTIR, NMR and mass spectra. Their molecular structures were calculated using DFT quantum chemical calculations. Both 1 and 2 were found to have distorted tetrahedral geometry around the Ag(I). The spectroscopic properties of the studied complexes have been calculated using the same level of theory. The Infrared vibrational frequencies of the COO stretches confirmed that the OAC is monodentate in 1 while the TFA is bidentate in 2. The calculated polarizability (α0) and HOMO-LUMO energy gap (ΔE) values indicated that 1 has higher NLO activity than 2. The electronic spectra of these complexes are calculated using the TD-DFT calculations. The calculated 1H NMR chemical shift values using GIAO approach showed good correlations with the experimental data. The interaction energies using the second order perturbation theory have been used to study the different intramolecular charge transfer interactions in the studied complexes. The NBO calculations indicated that both the Agsbnd O bonds are almost identical in 2 but not in 1.

Synthesis of new nano Schiff base complexes: X-ray crystallography ...

African Journals Online (AJOL)

This study presents synthesis and characterization of new nano uranyl Schiff base complexes. Electrochemistry of these complexes showed a quasireversible redox reaction without any successive reactions. Furthermore, X-ray crystallography exhibited that beside the coordination of tetradentate Schiff base, one solvent ...

Technetium cyanide chemistry: synthesis and characterization of technetium(III) and -(V) cyanide complexes

International Nuclear Information System (INIS)

Trop, H.S.; Jones, A.G.; Davison, A.

1980-01-01

Several new technetium cyanide complexes have been prepared and characterized. The reaction of ammonium hexaiodotechnetate(IV) with potassium cyanide in refluxing aqueous methanol under nitrogen yields potassium heptacyanotechnetate(III) dihydrate, K 4 Tc(CN) 7 .2H 2 O (1). Infrared and Raman measurements indicate that 1 has a pentagonal bipyramidal structure (D/sub 5h/) in both solid and solution. Aqueous solutions of 1 are air sensitive, decomposing to potassium oxopentacyanotechnetate(V) tetrahydrate, K 2 TcO(CN) 5 .4H 2 O (2). This species can also be prepared from the reaction of TcO 2 .xH 2 O with hot aqueous potassium cyanide solutions. Hydrolysis of 2 in water yields potassium trans-dioxo-tetracyanotechnetate(V), K 3 TcO 2 (CN) 4 (3). Preparation of 3 can also be achieved from the treatment of [TcO 2 (Py) 4 ]ClO 4 .2H 2 O with aqueous potassium cyanide. Infrared and Raman measurements on 3 are consistent with the proposed trans-dioxo (D/sub 4h/) structure. Reaction of the oxotetrachlorotechnetate(V) anion, TcOCl 4 , with potassium cyanide in methanol produces trans-oxomethoxytetracyanotechnetate(V). [TcO(OMe)(CN) 4 ] (4). The full details of the synthesis and characterization of these interesting technetium(III) and -(V) complexes, as well as observations on the infrared and Raman spectra of trans-dioxo metal complexes and the hydrolysis of species 2, are presented

Synthesis and characterization of a homogeneous and silica supported homoleptic cationic tungsten(vi) methyl complex: application in olefin metathesis

KAUST Repository

Dey, Raju

2016-08-19

A method for the synthesis of a homogeneous cationic tungsten(VI)penta-methyl complex [(WMe5)(+)(C6F5)(3)BMe-] from neutral tungstenhexamethyl (WMe6) and a silica supported cationic tungstentetramethyl complex [( Si-O-)WMe4+ (C6F5)(3)BMe-] from a neutral silica supported tungstenpentamethyl complex [( Si-O-)WMe5] is described. In both cases a direct demethylation using the B(C6F5)(3) reagent was used. The aforesaid complexes were characterized by liquid or solid state NMR spectroscopy. Interestingly, the homogeneous cationic complex [(WMe5)(+)(C6F5)(3)BMe-] shows moderate activity whereas the supported cationic complex [( Si-O-)WMe4+(C6F5)(3)BMe-] exhibits good activity in olefin metathesis reactions.

Synthesis and characterization of a homogeneous and silica supported homoleptic cationic tungsten(vi) methyl complex: application in olefin metathesis

KAUST Repository

Dey, Raju; Samantaray, Manoja; Poater, Albert; Hamieh, Ali Imad Ali; Kavitake, Santosh Giridhar; Abou-Hamad, Edy; Callens, Emmanuel; Emwas, Abdul-Hamid M.; Cavallo, Luigi; Basset, Jean-Marie

2016-01-01

A method for the synthesis of a homogeneous cationic tungsten(VI)penta-methyl complex [(WMe5)(+)(C6F5)(3)BMe-] from neutral tungstenhexamethyl (WMe6) and a silica supported cationic tungstentetramethyl complex [( Si-O-)WMe4+ (C6F5)(3)BMe-] from a neutral silica supported tungstenpentamethyl complex [( Si-O-)WMe5] is described. In both cases a direct demethylation using the B(C6F5)(3) reagent was used. The aforesaid complexes were characterized by liquid or solid state NMR spectroscopy. Interestingly, the homogeneous cationic complex [(WMe5)(+)(C6F5)(3)BMe-] shows moderate activity whereas the supported cationic complex [( Si-O-)WMe4+(C6F5)(3)BMe-] exhibits good activity in olefin metathesis reactions.

Synthesis, characterization and electrochemical investigation of hetaryl chromium(0) aminocarbene complexes

Czech Academy of Sciences Publication Activity Database

Metelková, R.; Tobrman, T.; Kvapilová, Hana; Hoskovcová, I.; Ludvík, Jiří

2012-01-01

Roč. 82, SI (2012), s. 470-477 ISSN 0013-4686 R&D Projects: GA AV ČR IAA400400813 Institutional support: RVO:61388955 Keywords : Fischer aminocarbene complexes * synthesis * Electrochemical oxidation and reduction Subject RIV: CG - Electrochemistry Impact factor: 3.777, year: 2012

Reactions of zinc hydride and magnesium hydride with pyridine; synthesis and characterization of 1,4-dihydro-1-pyridylzinc and -magnesium complexes

NARCIS (Netherlands)

Koning, A.J. de; Boersma, J.; Kerk, G.J.M. van der

1980-01-01

The synthesis and characterization of 1,4-dihydro-1-pyridylzinc and -magnesium complexes are described. Zinc hydride and magnesium hydride dissolve in and react with pyridine, and the reaction has been studied in detail in the case of zinc hydride. Evaporation of the solvent after 1–2 hours at 0°C

Synthesis and characterization of para-pyridine linked NHC palladium complexes and their studies for the Heck-Mizoroki coupling reaction.

Science.gov (United States)

Liu, Ya-Ming; Lin, Yi-Chun; Chen, Wen-Ching; Cheng, Jen-Hao; Chen, Yi-Lin; Yap, Glenn P A; Sun, Shih-Sheng; Ong, Tiow-Gan

2012-06-28

This paper describes the synthesis of 1-(pyridine-4-ylmethyl) NHC and their Pd(II) and Ag(I) complexes, which are fully characterized. Interestingly, we have also synthesized a Pd complex 3a-CO(3) using a more direct treatment of K(2)CO(3) with PdCl(2). 3a-CO(3) represents the first reported solid structure of a Pd η(2)-carbonato complex stabilized by an NHC framework. 3a-CO(3) can be easily converted to a PdCl(2) derivative by treating it with chloroform. We have found these palladium complexes mediate the Heck-Mizoroki coupling with a low catalyst loading. Furthermore, we also expand such catalytic manifold toward constructing fused polyaromatic substrates, a highly useful class of compounds in optoelectronic chemistry.

Synthesis, characterization, thermal

Directory of Open Access Journals (Sweden)

Selma Bal

2017-09-01

Full Text Available This work explains the synthesis of a new azo-Schiff base compound, derived from condensation between N-ethylcarbazole-3-carbaldehyde and 1,3-diaminopropane, followed by azo coupling reaction with the diazonium salt of 2-amino-4-methyl phenol. The newly synthesized azo-Schiff base was further reacted with the acetate salts of Copper, Cobalt and Nickel to give three coordination compounds. All synthesized compounds have been characterized through spectral analysis. The coordination compounds have been examined for their thermal and catalytic features. Good and moderate yields were obtained for the oxidation of styrene and cyclohexene. Thermal features of the ligand and its complexes have been explained and the results obtained have supported the proposed structures.

Synthesis and Spectral Evaluation of Some Unsymmetrical Mesoporphyrinic Complexes

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Rica Boscencu

2012-06-01

Full Text Available Synthesis and spectral evaluation of new zinc and copper unsymmetrical mesoporphyrinic complexes are reported. Zn(II-5-(4-acetoxy-3-methoxyphenyl-10,15,20-tris-(4-carboxymethylphenylporphyrin, Zn(II-5-[(3,4-methylenedioxyphenyl]-10,15,20-tris-(4-carboxymethylphenylporphyrin, Cu(II-5-(4-acetoxy-3-methoxyphenyl-10,15,20-tris-(4-carboxymethylphenylporphyrin and Cu(II-5-[(3,4-methylenedioxyphenyl]-10,15,20-tris-(4-carboxymethylphenylporphyrin were synthesized using microwave-assisted synthesis. The complexes were characterized by elemental analysis, FT-IR, UV-Vis, EPR and NMR spectroscopy, which fully confirmed their structure. The spectral absorption properties of the porphyrinic complexes were studied in solvents with different polarities. Fluorescence emission and singlet oxygen formation quantum yields were evaluated for the compounds under study, revealing high yields for the zinc derivatives. The copper complexes are not emissive and only display residual capacity for singlet oxygen formation.

Synthesis and characterization of some complexes with imidazole and pyrazole from saccharinate transition ions in oxidation state (II)

International Nuclear Information System (INIS)

Pineda Cedeno, Leslie William

2001-01-01

The synthesis and characterization of metal ions saccharinate of the first serie of transition with the imidazole and pyrazole molecules in water and absolute ethanol were studied. In general, it found that in this series of saccharinate of coordinated water molecules are replaced by imidazole and pyrazole molecules with different substitution patterns, generating neutral complex of molecular formula [M(Sac) 2 (L) n (H 2 O) n-4 ] and cationic complex of molecular formula [M(L) n (H 2 O) 2 ]x2Sac, [M(L) n (H 2 O) 3 ]x2Sac, [M(L) n ]x2Sac, where M = V(II), Cr(II), Mc(II), Fe(II), Co(II), Ni(II) y Zn(II); Sac = saccharinate ion; L = imidazole (imd) and pyrazole (pir) and n = 6,4,3 and 2. These compounds are soluble in DMF and insoluble in all other common solvents. In turn, synthesized compounds in water were characterized by X ray crystallography, where preliminary data of refinement cycles, generate formulas of isostructural type [M(imd) 4 (H 2 O) 2 ]x2Sac and [M(Sac) 2 (pir) 2 (H 2 O) 2 ] where M = Co(II), Ni(II). The imidazole complex crystallize in the triclinic crystal system and space group P-1, while the pyrazole complexes crystallize in the monoclinic crystal system and space group P2 (1)/n. Gradual diminution was observed in the bond distances of M-N (saccharinate ion), M-N (imidazole) and M-N (pyrazole). The complex was characterized by spectroscopic methods, magnetic and electrochemical. (author) [es

Synthesis, Characterization and in Vitro Antibacterial Activities of CdO Nanoparticle and Nano-sheet Mixed-ligand of Cadmium(ІІ Complex

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Zohreh Rashidi Ranjbar

2016-07-01

Full Text Available Here, we report the synthesis of a Schiff-base mixed-ligand complex of cadmium(ІІ in bulk and nano-scales via the precipitation and sonochemical methods, respectively. The complex formula is [Cd(3-bpdh(3-bpdbCl2]n (1, where the ligands are 3-bpdh = 2,5-bis(3-pyridyl-3,4-diaza-2,4-hexadiene and 3-bpdb = 1,4-bis(3-pyridyl-2,3-diaza-1,3-butadiene. The structure of mixed-ligand complex (1 was characterized by IR, 1H NMR and elemental analyses. Cadmium(ІІ oxide nanoparticles were prepared by direct thermolysis from nanosheet of complex (1. The cadmium(ІІ oxide structure was characterized by X-ray Diffraction (XRD and Energy Dispersive X-ray  analyses (EDAX. Size, morphology and structural dispersion of all obtained nanostructures were characterized by Scanning Electron Microscopy (SEM. The Schiff-base ligands, bulk and nano-scales of complex (1 and cadmium(ІІ oxide nanoparticles were analyzed for antibacterial activities against Bacillus alvei (bacteria causing the honey bee European foulbrood disease. The Minimum Inhibitory Concentrations (MIC has been shown moderate antibacterial activities compared with some other standard drugs. Known antibiotics like penicillin and SXT (Trimethoprim/sulfamethoxazole were used as positive control.

Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

International Nuclear Information System (INIS)

Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

2017-01-01

Highlights: • An organic/inorganic hybrid green corrosion inhibitive pigment was synthesized and characterized. • Chemical structure and morphology of the hybrid complex were characterized. • Zinc acetate/Urtica Dioica showed effective inhibition action in saline solution on carbon steel. • The synergistic effect between Zn 2+ cations and inhibitive compounds existed in U.D resulted in protective film deposition on the steel surface. - Abstract: This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV–vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn 2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

Energy Technology Data Exchange (ETDEWEB)

Salehi, E.; Naderi, Reza [School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, P.O. Box 11155-4563, Tehran (Iran, Islamic Republic of); Ramezanzadeh, B., E-mail: ramezanzadeh@aut.ac.ir [Department of Surface Coatings and Corrosion, Institute for Color Science and Technology (ICST), PO 16765-654, Tehran (Iran, Islamic Republic of)

2017-02-28

Highlights: • An organic/inorganic hybrid green corrosion inhibitive pigment was synthesized and characterized. • Chemical structure and morphology of the hybrid complex were characterized. • Zinc acetate/Urtica Dioica showed effective inhibition action in saline solution on carbon steel. • The synergistic effect between Zn{sup 2+} cations and inhibitive compounds existed in U.D resulted in protective film deposition on the steel surface. - Abstract: This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV–vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn{sup 2+} and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

Synthesis of a Benzodiazepine-derived Rhodium NHC Complex by C-H Bond Activation

Energy Technology Data Exchange (ETDEWEB)

Bergman, Roberg G.; Gribble, Jr., Michael W.; Ellman, Jonathan A.

2008-01-30

The synthesis and characterization of a Rh(I)-NHC complex generated by C-H activation of 1,4-benzodiazepine heterocycle are reported. This complex constitutes a rare example of a carbene tautomer of a 1,4-benzodiazepine aldimine stabilized by transition metal coordination and demonstrates the ability of the catalytically relevant RhCl(PCy{sub 3}){sub 2} fragment to induce NHC-forming tautomerization of heterocycles possessing a single carbene-stabilizing heteroatom. Implications for the synthesis of benzodiazepines and related pharmacophores via C-H functionalization are discussed.

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphos Ph Complexes.

Science.gov (United States)

Phanopoulos, Andreas; Long, Nicholas; Miller, Philip

2015-04-10

Herein we report the synthesis of a tridentate phosphine ligand N(CH2PPh2)3 (N-triphos(Ph)) (1) via a phosphorus based Mannich reaction of the hydroxylmethylene phosphine precursor with ammonia in methanol under a nitrogen atmosphere. The N-triphos(Ph) ligand precipitates from the solution after approximately 1 hr of reflux and can be isolated analytically pure via simple cannula filtration procedure under nitrogen. Reaction of the N-triphos(Ph) ligand with [Ru3(CO)12] under reflux affords a deep red solution that show evolution of CO gas on ligand complexation. Orange crystals of the complex [Ru(CO)2{N(CH2PPh2)3}-κ(3)P] (2) were isolated on cooling to RT. The (31)P{(1)H} NMR spectrum showed a characteristic single peak at lower frequency compared to the free ligand. Reaction of a toluene solution of complex 2 with oxygen resulted in the instantaneous precipitation of the carbonate complex [Ru(CO3)(CO){N(CH2PPh2)3}-κ(3)P] (3) as an air stable orange solid. Subsequent hydrogenation of 3 under 15 bar of hydrogen in a high-pressure reactor gave the dihydride complex [RuH2(CO){N(CH2PPh2)3}-κ(3)P] (4), which was fully characterized by X-ray crystallography and NMR spectroscopy. Complexes 3 and 4 are potentially useful catalyst precursors for a range of hydrogenation reactions, including biomass-derived products such as levulinic acid (LA). Complex 4 was found to cleanly react with LA in the presence of the proton source additive NH4PF6 to give [Ru(CO){N(CH2PPh2)3}-κ(3)P{CH3CO(CH2)2CO2H}-κ(2)O](PF6) (6).

Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

Science.gov (United States)

Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

2017-02-01

This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV-vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

Synthesis of samarium complexes with the derivative binder of Schiff Quinolinic base. Characterization and photophysical study

International Nuclear Information System (INIS)

Lucas H, J.

2016-01-01

In this work we determined the metal: binder stoichiometry of the species formed during the UV/Vis spectrophotometric titration of the derivative binder of Schiff quinolinic base, L1 with the samarium nitrate pentahydrate in methanol. Statistical analysis of the data allowed proposing the metal: binder stoichiometry for the synthesis of the complexes which was one mole of samarium salt by 2.5 moles of binder and thus favor the formation of complexes with 1M: 1L and 1M: 2L stoichiometries. They were synthesized in aqueous-organic medium (water-ethanol), isolated and purified two complexes with stoichiometry 1 Sm: 1 L1, complex 1 and 1 Sm: 2 L1, complex 2. The overall yield of the reaction was 76%. The characterization of the formed complexes was performed by visible ultraviolet spectrometry (UV/Vis), nuclear magnetic resonance, X-ray photoelectron spectroscopy (XP S), thermal gravimetric analysis with differential scanning calorimetry (TGA/DSC), and radial distribution function. These complexes were studied by fluorescence and emission phosphorescence at variable temperature. Spectroscopic techniques used in both solution and solid demonstrated the formation and stability of these complexes. In addition XP S indicated that in both complexes the samarium retains its oxidation state 3+. Luminescence studies indicated that there is intra-binding charge transfer which decreases the transfer of light energy from the binder to the samarium. Based on the experimental results, L1 binder molecules and complexes 1 and 2 were modeled that demonstrated the proposed Nc for each complex, as well as allowed to visualize the structural arrangement of the molecules, complexes and binder. (Author)

Synthesis and Characterization of a Heteroleptic Ru(II Complex of Phenanthroline Containing Oligo-Anthracenyl Carboxylic Acid Moieties

Directory of Open Access Journals (Sweden)

Peter A. Ajibade

2010-09-01

Full Text Available In an effort to develop new ruthenium(II complexes, this work describes the design, synthesis and characterization of a ruthenium(II functionalized phenanthroline complex with extended π-conjugation. The ligand were L1 (4,7-bis(2,3-dimethylacrylic acid-1,10-phenanthroline, synthesized by a direct aromatic substitution reaction, and L2 (4,7-bis(trianthracenyl-2,3-dimethylacrylic acid-1,10-phenanthroline, which was synthesized by the dehalogenation of halogenated aromatic compounds using a zero-valent palladium cross-catalyzed reaction in the absence of magnesium-diene complexes and/or cyclooctadienyl nickel (0 catalysts to generate a new carbon-carbon bond (C-C bond polymerized hydrocarbon units. The ruthenium complex [RuL1L2(NCS2] showed improved photophysical properties (red-shifted metal-to-ligand charge-transfer transition absorptions and enhanced molar extinction coefficients, luminescence and interesting electrochemical properties. Cyclic and square wave voltammetry revealed five major redox processes. The number of electron(s transferred by the ruthenium complex was determined by chronocoulometry in each case. The results show that processes I, II and III are multi-electron transfer reactions while processes IV and V involved one-electron transfer reaction. The photophysical property of the complex makes it a promising candidate in the design of chemosensors and photosensitizers, while its redox-active nature makes the complex a potential mediator of electron transfer in photochemical processes.

Synthesis and Characterization of a Triphos Ligand Derivative and the Corresponding Pd ^II Complexes: Triphos Ligand Derivative and Corresponding Pd ^II Complexes

Energy Technology Data Exchange (ETDEWEB)

Miller, Deanna L.; Boro, Brian J.; Grubel, Katarzyna; Helm, Monte L.; Appel, Aaron M.

2015-11-16

The synthesis of the new bis(2-(diphenylphosphino)ethyl)methylhydroxyphosphine tridentate phosphine ligand, LCH2OH/Ph, is reported. The ligand reacts with [Pd(Cl)2(PhCN)2 to form [Pd(LCH2OH/Ph)Cl]Cl. Exchange of the chloride ions for triflate (OTf–) using AgOTf yielded pure [Pd(LCH2OH/Ph)OTf]OTf. In addition to spectral characterization the free ligand, LCH2OH/Ph, and Pd(II) complex, [Pd(LCH2OH/Ph)OTf]OTf, are structurally characterized. This research was supported by the US Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Biosciences, and Geosciences. Pacific Northwest National Laboratory is a multiprogram national laboratory operated by Battelle for DOE.

Synthesis and Characterization of Lanthanum Complexes with Amino Acid Schiff Base

Institute of Scientific and Technical Information of China (English)

张秀英; 张有娟; 杨林

2001-01-01

Six new complexes of lanthanum with amino acid Schiff base ligands, A-F, were prepared in methanol-aqueous solution. The composition and properties of the title complexes were characterized by elemental analysis, molar conductance, infrared, electronic spectra, 1H NMR, thermogravimetric and differential thermal analysis.

Electrochemical synthesis of transition element complexes with carboxyl- and carbonyl-containing ligands

International Nuclear Information System (INIS)

Frolov, V.Yu.; Bolotin, S.N.; Panyushkin, V.T.

2005-01-01

Complexes of d- and f-elements (E = Cu, Ni, Zn, Nd, Tb, Pr, Gd, Er) with carboxyl- and carbonyl-containing ligands were synthesized by the electrochemical method. The products were characterized by elemental analysis, thermal gravimetric analysis and IR spectra. The influence exerted by a number of factors on the process course was studied. The dependence of the electro synthesis parameters on the composition of the forming compounds was established. A new method for anodic synthesis of these compounds was developed [ru

Synthesis and Characterization of Mn 2+ and Fe 2+ Complexes of ...

African Journals Online (AJOL)

The complexes were characterized by infrared and UV visible, while their melting point, solubility and conductivity were investigated. The ligand C=N band appear at 1645 cm-1 while the C=N band infrared absorption vibration appears at 1622 cm-1 and 1626 cm-1 for iron and manganese complexes respectively. The UV ...

Synthesis, Structural Characterization, Antimicrobial Activity, and In Vitro Biocompatibility of New Unsaturated Carboxylate Complexes with 2,2'-Bipyridine.

Science.gov (United States)

Vasile Scăețeanu, Gina; Chifiriuc, Mariana Carmen; Bleotu, Coralia; Kamerzan, Crina; Măruţescu, Luminiţa; Daniliuc, Constantin G; Maxim, Cătălin; Calu, Larisa; Olar, Rodica; Badea, Mihaela

2018-01-12

The synthesis, structural characterization, cytotoxicity, and antimicrobial properties of four new complexes formed by employing acrylate anion and 2,2'-bipyridine are reported herein. X-ray crystallography revealed the trinuclear nature of [Mn₃(2,2'-bipy)₂(C₃H₃O₂)₆] ( 1 ), meanwhile complexes with general formula [M(2,2'-bipy)(C₃H₃O₂)₂(H₂O) x ]∙ y H₂O (( 2 ) M: Ni, x = 1, y = 0; ( 3 ) M: Cu, x = 1, y = 0; ( 4 ) M: Zn, x = 0, y = 1; 2,2'-bipy: 2,2'-bipyridine; C₃H₃O₂: acrylate anion) were shown to be mononuclear. The lowest minimum inhibitory concentration (MIC) of 128 μg mL -1 was recorded for all four tested complexes against Candida albicans , for complex ( 3 ) against Escherichia coli , and for complex ( 4 ) against Staphylocococcus aureus . Compounds ( 3 ) and ( 4 ) were also potent efflux pumps activity inhibitors (EPI), proving their potential for use in synergistic combinations with antibiotics. Complexes ( 1 )-( 4 ) revealed that they were not cytotoxic to HCT-8 cells. They also proved to interfere with the cellular cycle of tumour HCT-8 cells by increasing the number of cells found in the S and G2/M phases. Taken together, these results demonstrate the potential of zinc and copper complexes for use in the development of novel antimicrobial and anti-proliferative agents.

Synthesis, characterization and biodistribution of technetium complexes (99Tc/99mTc) with 2-amino-2-deoxy-D-hexose oximes

International Nuclear Information System (INIS)

Steinmetz, H.J.

1993-05-01

In the present work, the synthesis and isolation of isomeric complexes of technetium ( 99 Tc/ 99m Tc) with the 2-amino-2-deoxy-D-hexoses D-glucose aminoxime, D-galactose aminoxime and D-mannose aminoxime, the characterization of the complexes as 99 Tc compounds, and bio-distribution studies on the analogous 99m Tc complexes have been untertaken. As a first step, the free ligands were synthesized and identified using elemental analysis, infra-red and nuclear magnetic resonance spectroscopy and FAB mass spectroscopy. In the bio-distribution studies on the 99m Tc complexes of D-glucose aminoxime and of D-galactose aminoxime in NMRI mice, significant short-term accumulation of 99m Tc activity in heart muscle could be detected, which may be attributed to a biochemical transport mechanism. Uptake in the lungs and the liver was found, but a more significant uptake was observed in the kidneys, where the complexes were rapidly secreted in proportion to their concentration in the blood plasma. (orig./BBR) [de

Mechanochemical Synthesis, In vivo Anti-malarial and Safety Evaluation of Amodiaquine-zinc Complex

Directory of Open Access Journals (Sweden)

Arise Rotimi Olusanya

2017-09-01

Full Text Available So far, some prospective metal-based anti-malarial drugs have been developed. The mechanochemical synthesis and characterization of Zn (II complex with amodiaquine and its anti-malarial efficacy on Plasmodium berghei-infected mice and safety evaluation were described in this study.

Microwave assisted synthesis, spectral, magnetic and bioevolution of few Mn (II)-amide complexes

Energy Technology Data Exchange (ETDEWEB)

Joshi, Gaurav [Department of Chemistry, Govt. Engineering College, Bikaner (India); Verma, K. K.; Gudesaria, D. D.; Bhojak, N., E-mail: drbhojak@rediffmail.com [GCRC, Department of Chemistry, Govt Dungar College, Bikaner-334003, Rajasthan (India)

2016-05-06

The importance and versatility of amide group containing ligands have promoted the selection of this class of ligands and their complexes for the study. The present work describes the synthesis, spectral and biological investigations on the complexes of amides derived from heterocyclic amines with Mn (II) ions. Four ligands derived 2-aminopyridine and their complexes with Mn (II) have been synthesized. A method for the synthesis of complexes has been developed by the use of microwave irradiation which is in agreement to Green chemistry approach. The complexes have been characterized on the basis of elemental analysis, infrared, electronic, ESR spectra and magnetic susceptibility studies. The diffuse reflectance spectrum of the complexes show bands in the region 20,000 cm{sup −1} to 26,000 cm{sup −1} assignable to {sup 6}A{sub 1g} → {sup 4}T{sub 2g} and {sup 6}A{sub 1g} → {sup 4}E{sub 1g} transitions. These are also typical of tetrahedral environment around the manganese. The magnetic moment (5.80 BM) of the complex indicates high spin tetrahedral environment. The microwave method of synthesis of complexes have been found easier, convenient and ecofriendly. Antimicrobial activities of compounds were also carried out against bacteria and fungi. Further minimal inhibitory concentration (MIC) was also determined for each compound.

A new synthesis route for Os-complex modified redox polymers for potential biofuel cell applications.

Science.gov (United States)

Pöller, Sascha; Beyl, Yvonne; Vivekananthan, Jeevanthi; Guschin, Dmitrii A; Schuhmann, Wolfgang

2012-10-01

A new synthesis route for Os-complex modified redox polymers was developed. Instead of ligand exchange reactions for coordinative binding of suitable precursor Os-complexes at the polymer, Os-complexes already exhibiting the final ligand shell containing a suitable functional group were bound to the polymer via an epoxide opening reaction. By separation of the polymer synthesis from the ligand exchange reaction at the Os-complex, the modification of the same polymer backbone with different Os-complexes or the binding of the same Os-complex to a number of different polymer backbones becomes feasible. In addition, the Os-complex can be purified and characterized prior to its binding to the polymer. In order to further understand and optimize suitable enzyme/redox polymer systems concerning their potential application in biosensors or biofuel cells, a series of redox polymers was synthesized and used as immobilization matrix for Trametes hirsuta laccase. The properties of the obtained biofuel cell cathodes were compared with similar biocatalytic interfaces derived from redox polymers obtained via ligand exchange reaction of the parent Os-complex with a ligand integrated into the polymer backbone during the polymer synthesis. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis, Physical Characterization and Biological Activity of Some Schiff Base Complexes

Directory of Open Access Journals (Sweden)

R. Rajavel

2008-01-01

Full Text Available Structural modification of organic molecule has considerable biological relevance. Further, coordination of a biomolecules to the metal ions significantly alters the effectiveness of the biomolecules. In view of the antimicrobial activity ligand [bis-(2-aminobenzaldehyde] malonoyl dihydrazone], metal complexes with Cu(II, Ni(II, Zn(II and oxovanadium(IV have been synthesized and found to be potential antimicrobial agents. An attempt is also made to correlate the biological activities with geometry of the complexes. The complexes have been characterized by elemental analysis, molar conductance, spectra and cyclicvoltammetric measurements. The structural assessment of the complexes has been carried out based on electronic, infrared and molar conductivity values.

Ni(II, Pd(II and Pt(II complexes with ligand containing thiosemicarbazone and semicarbazone moiety: synthesis, characterization and biological investigation

Directory of Open Access Journals (Sweden)

SULEKH CHANDRA

2008-07-01

Full Text Available The synthesis of nickel(II, palladium(II and platinum(II complexes with thiosemicarbazone and semicarbazone of p-tolualdehyde are reported. All the new compounds were characterized by elemental analysis, molar conductance measurements, magnetic susceptibility measurements, mass, 1H-NMR, IR and electronic spectral studies. Based on the molar conductance measurements in DMSO, the complexes may be formulated as [Ni(L2Cl2] and [M(L2]Cl2 (where M = Pd(II and Pt(II due to their non-electrolytic and 1:2 electrolytic nature, respectively. The spectral data are consistent with an octahedral geometry around Ni(II and a square planar geometry for Pd(II and Pt(II, in which the ligands act as bidentate chelating agents, coordinated through the nitrogen and sulphur/oxygen atoms. The ligands and their metal complexes were screened in vitro against fungal species Alternaria alternata, Aspergillus niger and Fusarium odum, using the food poison technique.

Synthesis, characterization, and reactivity of furan- and thiophene-functionalized bis(n-heterocyclic carbene) complexes of iron(II)

KAUST Repository

Rieb, Julia

2014-09-15

The synthesis of iron(II) complexes bearing new heteroatom-functionalized methylene-bridged bis(N-heterocyclic carbene) ligands is reported. All complexes are characterized by single-crystal X-ray diffraction (SC-XRD), nuclear magnetic resonance (NMR) spectroscopy, and elemental analysis. Tetrakis(acetonitrile)-cis-[bis(o-imidazol-2-ylidenefuran)methane]iron(II) hexafluorophosphate (2a) and tetrakis(acetonitrile)-cis-[bis(o-imidazol-2-ylidenethiophene)methane]iron(II) hexafluorophosphate (2b) were obtained by aminolysis of [Fe{N(SiMe3)2}2(THF)] with furan- and thiophene-functionalized bis(imidazolium) salts 1a and 1b in acetonitrile. The SC-XRD structures of 2a and 2b show coordination of the bis(carbene) ligand in a bidentate fashion instead of a possible tetradentate coordination. The four other coordination sites of these distorted octahedral complexes are occupied by acetonitrile ligands. Crystallization of 2a in an acetone solution by the slow diffusion of Et2O led to the formation of cisdiacetonitriledi[ bis(o-imidazol-2-ylidenefuran)methane]iron(II) hexafluorophosphate (3a) with two bis(carbene) ligands coordinated in a bidentate manner and two cis-positioned acetonitrile molecules. Compounds 2a and 2b are the first reported iron(II) carbene complexes with four coordination sites occupied by solvent molecules, and it was demonstrated that those solvent ligands can undergo ligand-exchange reactions.

Synthesis and characterization of a new complex binuclear of binuclear of Pd(II) containing the antibiotic oxy tetracycline; Sintese e caracterizacao de um novo complexo bimetalico de Pd(II) contendo o antibiotico oxitetraciclina

Energy Technology Data Exchange (ETDEWEB)

Guerra, Wendell [Universidade Federal de Uberlandia (UFU), MG (Brazil). Inst. de Quimica; Fontes, Ana Paula Soares [Universidade Federal de Juiz de Fora (UFJF), MG (Brazil). Dept. de Quimica; Pereira-Maia, Elene Cristina [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Quimica

2010-07-01

This article reports the synthesis and characterization of a new binuclear complex of palladium (II) containing the antibiotic oxytetracycline. The complex was characterized by the usual techniques of analysis. With respect to sites of coordination, the IR spectral data suggests the involvement the oxygen of the amide group and the oxygen of the neighbor hydroxyl group at ring A and to the carbonyl oxygen at C11 and the hydroxyl group at C12. (author)

Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

Energy Technology Data Exchange (ETDEWEB)

Fatimah, Soja Siti, E-mail: soja-sf@upi.edu [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Bahti, Husein H.; Hastiawan, Iwan [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Permanasari, Anna [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia)

2016-02-08

The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, ({sup 1}H, and {sup 13}C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

Science.gov (United States)

Fatimah, Soja Siti; Bahti, Husein H.; Hastiawan, Iwan; Permanasari, Anna

2016-02-01

The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, (1H, and 13C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

Novel polymeric potassium complex: Its synthesis, structural characterization, photoluminescence and electrochemical properties

Energy Technology Data Exchange (ETDEWEB)

Ceyhan, Goekhan [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Tuemer, Mehmet, E-mail: mtumer@ksu.edu.tr [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Koese, Muhammet; McKee, Vickie [Chemistry Department, Loughborough University, LE11 3TU Leicestershire (United Kingdom)

2012-03-15

In this paper, we obtained a novel poly(vanillinato potassium) complex (PVP) as a single crystal and characterized by analytical and spectroscopic methods. A single crystal of the PVP was obtained from the acetone solution. X-ray structural data show that crystals contain polymeric K{sup +} complex of vanillin. Each potassium ion in the polymeric structure is identical and seven-coordinate, bonded to two methoxy, two phenoxy and three aldehyde oxygen atoms from four vaniline molecules. Two aldehyde oxygen atoms are bridging between potassium ions. It crystallizes in the monoclinic system, space group P2{sub 1}/c, with lattice parameters a=9.6215(10) A, b=17.4139(19) A, c=9.6119(10) A, {beta}=100.457(2) Degree-Sign and Z=4. Thermal properties of the PVP were investigated by TGA, DTA and DSC methods. The electrochemical properties of the complex were studied in different solvents and at various scan rates. The luminescence properties of the complex in different solvents and at different pH values have been investigated. The results show that the complex exhibits more efficient luminescence property in CH{sub 3}CN and n-butanol. - Highlights: Black-Right-Pointing-Pointer Novel polymeric potassium complex was prepared and fully characterized. Black-Right-Pointing-Pointer X-ray crystal structure of complex was reported. Black-Right-Pointing-Pointer Electrochemical properties of compound were investigated. Black-Right-Pointing-Pointer Thermal and DSC measurements of complex were examined.

Zinc acetylacetonate hydrate adducted with nitrogen donor ligands: Synthesis, spectroscopic characterization, and thermal analysis

Science.gov (United States)

Brahma, Sanjaya; Shivashankar, S. A.

2015-12-01

We report synthesis, spectroscopic characterization, and thermal analysis of zinc acetylacetonate complex adducted by nitrogen donor ligands, such as pyridine, bipyridine, and phenanthroline. The pyridine adducted complex crystallizes to monoclinic crystal structure, whereas other two adducted complexes have orthorhombic structure. Addition of nitrogen donor ligands enhances the thermal property of these complexes as that with parent metal-organic complex. Zinc acetylacetonate adducted with pyridine shows much higher volatility (106 °C), decomposition temperature (202 °C) as that with zinc acetylacetonate (136 °C, 220 °C), and other adducted complexes. All the adducted complexes are thermally stable, highly volatile and are considered to be suitable precursors for metal organic chemical vapor deposition. The formation of these complexes is confirmed by powder X-ray diffraction, Fourier transform infrared spectroscopy, mass spectroscopy, and elemental analysis. The complexes are widely used as starting precursor materials for the synthesis of ZnO nanostructures by microwave irradiation assisted coating process.

Synthesis and Properties of Chelating N-Heterocyclic Carbene Rhodium(I) Complexes: Synthetic Experiments in Current Organometallic Chemistry

Science.gov (United States)

Mata, Jose A.; Poyatos, Macarena; Mas-Marza, Elena

2011-01-01

The preparation and characterization of two air-stable Rh(I) complexes bearing a chelating N-heterocyclic carbene (NHC) ligand is described. The synthesis involves the preparation of a Ag(I)-NHC complex and its use as carbene transfer agent to a Rh(I) precursor. The so obtained complex can be further reacted with carbon monoxide to give the…

Multifunctional material based on ionic transition metal complexes and gold-silica nanoparticles: synthesis and photophysical characterization for application in imaging and therapy.

Science.gov (United States)

Ricciardi, Loredana; Martini, Matteo; Tillement, Olivier; Sancey, Lucie; Perriat, Pascal; Ghedini, Mauro; Szerb, Elisabeta I; Yadav, Yogesh J; La Deda, Massimo

2014-11-01

A new combination of luminescent ionic transition-metal complexes (M = Ru(II) or Ir(III)) with gold silica-based nanoparticles (GSNPs) gives a promising nanomaterial for application in biomedical fields. Herein we report the synthesis and the photophysical properties of Ru(II) and Ir(III) complexes doped gold core-polysiloxane shell particles prepared by microemulsion method and characterized by Transmission Electron Microscopy, Dynamic Light Scattering and UV-Vis spectroscopy. The cytotoxicity and photodynamic activity of the obtained 50 nm-diameter nanoparticles were evaluated in vitro, providing noteworthy results. Furthermore, their intrinsic phosphorescence allows the localization of the photosensitizing nanoparticles into the cytosol of tumor cells by fluorescence confocal microscope. These valuable features designate them as multifunctional nanoplatforms for theranostic purposes.

Synthesis, structural characterization and cytotoxic activity of two new organoruthenium(II complexes

Directory of Open Access Journals (Sweden)

SANJA GRGURIC-SIPKA

2008-06-01

Full Text Available Two new p-cymene ruthenium(II complexes containing as additional ligands N-methylpiperazine ([(η6-p-cymeneRuCl2(CH3NH(CH24NH]PF6, complex 1 or vitamin K3-thiosemicarbazone ([(η6-p-cymeneRuCl2(K3tsc], complex 2 were synthesized starting from [(η6-p-cymene2RuCl2]2 and the corresponding ligand. The complexes were characterized by elemental analysis, IR, electronic absorption and NMR spectroscopy. The X-ray crystal structure determination of complex 1 revealed “piano-stool” geometry. The differences in the cytotoxic activity of the two complexes are discussed in terms of the ligand present.

Synthesis and structural characterization of lithium

Indian Academy of Sciences (India)

synthesis and characterization of two new iminophos- phonamine ligands ... structures. 2.3 General synthetic method for ligands (1 and 2) ... 2.3b General method for the Synthesis of ligands ...... studies are currently underway in our laboratory.

Synthesis and characterization of some new molybdenum(V) complexes

International Nuclear Information System (INIS)

Kamenar, Boris; Korpar-Choling, Branka; Cindrich, Marina; Matkovich-Chalogovich, Dubravka; Penavich, Maja

1997-01-01

The molybdenium(V) complexes of the types Mo 2 O 3 L 4 (L = acetylacetone or dibenzolymethane), Mo 2 O 4 L 2 L' 2 solvated with L' (L = dibenzolymethane, L' = morpholine or thiomorpholine), and NR-morphH)[Mo 8 O 2 0LL' 3 ] (R = methyl or ethyl, L = dibenzolymethane, L' = NR-morpholine) have been synthesized for the first time. All were characterized by chemical analyses, IR spectra and magnethochemical measurements. Crystal structure of [Mo 2 O 4 (dbm) 2 (morph) 2 ].(morph) has been determined by X-ray diffraction technique. Complex is dinuclear containing the molybdenium atoms in a distorted octahedral geometry. Each molybdenium atom is surrounded by two bridging oxo-oxygen atoms, two oxygen atoms from one bidentately coordinated dibenzolymethane ligand, one nitrogen atom from morpholine molecule and one terminal oxo-oxygen atom. The solvated morpholine molecule is disordered around the diad axis. (author)

Synthesis, characterization and catalytic activity of two novel cis - dioxovanadium(V) complexes: [VO{sub 2}(L)] and [VO{sub 2}(HLox)

Energy Technology Data Exchange (ETDEWEB)

Silva, Natalia M.L.; Chacon, Eluzir P.; Resende, Jackson A.L.C.; Carneiro, Jose Walkimar de M.; Lanznaster, Mauricio, E-mail: mlanz@vm.uff.b [Universidade Federal Fluminense (IQ/UFF), Niteroi, RJ (Brazil). Inst. de Quimica; Pinheiro, Carlos B. [Universidade Federal de Minas Gerais (DF/UFMG), Belo Horizonte (Brazil). Dept. de Fisica; Fernandez, Tatiana L.; Scarpellini, Marciela [Universidade Federal do Rio de Janeiro (IQ/UFRJ), RJ (Brazil). Inst. de Quimica

2011-07-01

Two novel complexes, [VO{sub 2}(L)] (1) and [VO{sub 2}(HLox)] (2), were synthesized and characterized by IV, UV-Vis and NMR spectroscopy, cyclic voltammetry, elemental analysis and X-ray diffraction. The synthesis of a new ligand, H{sub 2}Lox, is also described. Complexes 1 and 2 were obtained by the reaction of [VO(acac){sub 2}] with the ligands HL and H{sub 2}Lox, respectively. Alternatively, 2 was also obtained by the reaction of HL with [VO(acac)2] in the presence of hydroxylamine, and by the reaction of 1 with hydroxylamine. Crystallographic data show that complexes 1 and 2 have similar molecular structures, in which the cis-dioxovanadium(V) center is coordinated to L- or HLox{sup -}, respectively, in a distorted octahedral environment. The catalytic activity of these compounds towards cyclohexane oxidation was evaluated using H{sub 2}O{sub 2} and t-BuOOH as oxidants. Both complexes presented > 70% selectivity for cyclohexylhydroperoxide formation. B3LYP/6.31G(d) calculations were used to confirm the geometry and to help assign the electronic spectra. (author)

Synthesis, Structural Characterization, Antimicrobial Activity, and In Vitro Biocompatibility of New Unsaturated Carboxylate Complexes with 2,2′-Bipyridine

Directory of Open Access Journals (Sweden)

Gina Vasile Scăețeanu

2018-01-01

Full Text Available The synthesis, structural characterization, cytotoxicity, and antimicrobial properties of four new complexes formed by employing acrylate anion and 2,2′-bipyridine are reported herein. X-ray crystallography revealed the trinuclear nature of [Mn3(2,2′-bipy2(C3H3O26] (1, meanwhile complexes with general formula [M(2,2′-bipy(C3H3O22(H2Ox]∙yH2O ((2 M: Ni, x = 1, y = 0; (3 M: Cu, x = 1, y = 0; (4 M: Zn, x = 0, y = 1; 2,2′-bipy: 2,2′-bipyridine; C3H3O2: acrylate anion were shown to be mononuclear. The lowest minimum inhibitory concentration (MIC of 128 μg mL−1 was recorded for all four tested complexes against Candida albicans, for complex (3 against Escherichia coli, and for complex (4 against Staphylocococcus aureus. Compounds (3 and (4 were also potent efflux pumps activity inhibitors (EPI, proving their potential for use in synergistic combinations with antibiotics. Complexes (1–(4 revealed that they were not cytotoxic to HCT-8 cells. They also proved to interfere with the cellular cycle of tumour HCT-8 cells by increasing the number of cells found in the S and G2/M phases. Taken together, these results demonstrate the potential of zinc and copper complexes for use in the development of novel antimicrobial and anti-proliferative agents.

Synthesis, characterization and behavior to gamma radiation of copper (II) complex and l-asparagine

International Nuclear Information System (INIS)

Rodrigues, E.R.

1982-01-01

Synthesis and caracterization of coordination compound formed by interation between l-asparagina (HL) and copper (II) ion are discussed. Elemental analysis, Visible and Ultraviolet electronic Spectroscopy, Infrared Vibrational Spectroscopy, Proton Nuclear Magnetic Resonance and melting and/or decomposition point are made; it is also possible to: a) Synthesize the complex with high degree of purity; b)determine the #betta# sub(max) for absorption in the Visible and Ultraviolet, as well as the molar absorption coefficient; c) determine the probable structure of the complex; d) calculate the kinetic parameters and the break factor by means of radiolysis in ammoniacal aqueous solution of sample submitted by a 60 Co source of #betta#-radiation (Gamma Cell); e) separate the complex from the ionic fractions formed by radiolysis, by means of cromatography in their layers; f) determine the porcentage of Cu in this complex by neutron activation; g) justify the complex resistence in solid phase, to gamma radiation. (A.R.H.) [pt

Synthesis, characterization and biological profile of metal and azo-metal complexes of embelin

Directory of Open Access Journals (Sweden)

R. Aravindhan

2014-12-01

Full Text Available The present study emphasizes synthesis and bioprofiling of embelin, embelin-metal (EM and embelin-azo-metal (EAM complexes in detail. EM complexes were prepared using pure embelin and d-block transition elements, namely Mn, Fe, Co, Ni, Cu, and Zn. Similarly, EAM complexes were synthesized using phenyl azo-embelin with the said transition metals. Embelin, EM, and EAM complexes were subjected to ultra violet visible spectroscopy, Fourier transform infrared spectroscopy, nuclear magnetic resonance, electrospray ionization mass spectrometry, thermogravimetric analysis, carbon hydrogen nitrogen sulfur analysis. With regard to bioprofiling, the test complexes were studied for the antioxidant and antimicrobial activities. Results revealed that the prepared EM and EAM complexes form octahedral complexes with embelin with the yield in the range of 45–75%. All the instrumental analyses authenticate the interaction of metals with bidentate embelin through its enolic and quinonic oxygen atoms as [M(Emb2(H2O2]H2O and [M(Emb-Azo2(H2O2]. The antioxidant profile studies suggested that upon complexation with metals, the free radical scavenging activity of embelin reduced significantly. But, with regard to antimicrobial activity, cobalt and nickel embelin complexes displayed>80% growth inhibition in comparison with embelin alone. The hemolytic activity studies suggested that both embelin and the metal complexes are non-hemolytic. The reason for the reduction in antioxidant and an increase in antimicrobial activities were discussed in detail.

SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ...

African Journals Online (AJOL)

ISSN 1011-3924. © 2018 Chemical Society of Ethiopia and The Authors. Printed in Ethiopia ... SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ACTIVITY OF .... cm−1 to determine the surface functional groups. 10 mg of sample ...

Chiral PEPPSI Complexes: Synthesis, Characterization, and Application in Asymmetric Suzuki–Miyaura Coupling Reactions

KAUST Repository

Benhamou, Laure

2014-01-13

PEPPSI complexes incorporating chiral N-heterocyclic carbene (NHC) ligands based on 2,2-dimethyl-1-(o-substituted aryl)propan-1-amines were synthesized. Two complexes, with one saturated and one unsaturated NHC ligand, were structurally characterized. The chiral PEPPSI complexes were used in asymmetric Suzuki-Miyaura reactions, giving atropisomeric biaryl products in modest to good enantiomeric ratios. © 2013 American Chemical Society.

Chiral PEPPSI Complexes: Synthesis, Characterization, and Application in Asymmetric Suzuki–Miyaura Coupling Reactions

KAUST Repository

Benhamou, Laure; Besnard, Cé line; Kü ndig, E. Peter

2014-01-01

PEPPSI complexes incorporating chiral N-heterocyclic carbene (NHC) ligands based on 2,2-dimethyl-1-(o-substituted aryl)propan-1-amines were synthesized. Two complexes, with one saturated and one unsaturated NHC ligand, were structurally characterized. The chiral PEPPSI complexes were used in asymmetric Suzuki-Miyaura reactions, giving atropisomeric biaryl products in modest to good enantiomeric ratios. © 2013 American Chemical Society.

Synthesis and characterization of rhodium sulfide nanoparticles and thin films

International Nuclear Information System (INIS)

Sosibo, Ndabenhle M.; Revaprasadu, Neerish

2008-01-01

The synthesis and characterization of a rhodium complex, [Rh(S 2 CNEt 2 ) 2 ] is described. The complex was thermolysed at a high temperature (280 deg. C) in the presence of capping agent, hexadecylamine (HDA) to form Rh 2 S 3 nanoparticles. Rod-shaped Rh 2 S 3 nanoparticles with an average length of 26.7 nm and an average breadth of 7.8 nm were synthesized. The complex was also used as a single molecule precursor for the deposition of Rh 2 S 3 thin films on a glass substrate at 350 deg. C and 450 deg. C using the Aerosol Assisted Chemical Vapour Deposition (AACVD) technique. The resultant thin films showed temperature dependent morphologies and showed (0 2 2), (4 1 1) and (6 1 1) lattice planes characteristic of to the orthorhombic Rh 2 S 3 phase. X-ray diffraction and scanning electron microscopy techniques were used to characterize the films

Synthesis and characterization of rhodium sulfide nanoparticles and thin films

Energy Technology Data Exchange (ETDEWEB)

Sosibo, Ndabenhle M. [Department of Chemistry, University of Zululand, Private Bag X1001, KwaDlangezwa 3886 (South Africa); Revaprasadu, Neerish [Department of Chemistry, University of Zululand, Private Bag X1001, KwaDlangezwa 3886 (South Africa)], E-mail: nrevapra@pan.uzulula.za

2008-05-15

The synthesis and characterization of a rhodium complex, [Rh(S{sub 2}CNEt{sub 2}){sub 2}] is described. The complex was thermolysed at a high temperature (280 deg. C) in the presence of capping agent, hexadecylamine (HDA) to form Rh{sub 2}S{sub 3} nanoparticles. Rod-shaped Rh{sub 2}S{sub 3} nanoparticles with an average length of 26.7 nm and an average breadth of 7.8 nm were synthesized. The complex was also used as a single molecule precursor for the deposition of Rh{sub 2}S{sub 3} thin films on a glass substrate at 350 deg. C and 450 deg. C using the Aerosol Assisted Chemical Vapour Deposition (AACVD) technique. The resultant thin films showed temperature dependent morphologies and showed (0 2 2), (4 1 1) and (6 1 1) lattice planes characteristic of to the orthorhombic Rh{sub 2}S{sub 3} phase. X-ray diffraction and scanning electron microscopy techniques were used to characterize the films.

Synthesis and characterization of five-coordinated indium amidinates

Energy Technology Data Exchange (ETDEWEB)

Riahi, Yasaman

2016-07-29

The focus of this work is synthesis, characterization and exploring the reactivity of new indium amidinate compounds of the type R{sub 2}InX (R = R''NCR'NR''; R' = Ph, R'' = SiMe{sub 3}, iPr, dipp; X = Br, Cl) with the coordination number of five and R{sub 3}In (R = Me{sub 3}SiNCPhNSiMe{sub 3}) with the coordination number of six. By using amidinates as chelating ligands the electron deficiency of indium atom will be resolved. Additionally, by using different substituents the study of the different synthesized indium amidinates has become possible. The selected method for the synthesis allows the carbodiimides to react with organolithium compounds to get the corresponding lithium amidinates. Afterwards the resulting lithium amidinates take part in transmetalation reactions with InBr{sub 3} and InCl{sub 3}. The study of the reactivity of indium amidinate complexes including nucleophilic reactions as well as their reduction were also examined. Beside crystal structure analysis, nuclear magnetic resonance spectroscopy as well as elemental analysis has been applied to characterize the compounds.

Synthesis of Cr(III-Morin Complex: Characterization and Antioxidant Study

Directory of Open Access Journals (Sweden)

Qadeer K. Panhwar

2014-01-01

Full Text Available The complex formation between Cr(III and morin was carried out in methanol and confirmed by analytical characterization using UV-Vis, IR, 1H NMR, and TG-DTA. UV-Vis shows significant bathochromic shift in benzoyl upon coordination as well as IR well illustrates the peak shift of C=O group and formation of a O–Cr(III bond. Likewise, 1H NMR studies clarify that Cr(III metal ion replaces the 5OH proton hence; 5-hydroxy-4-keto site is employed by morin in chelation to form six-membered stable ring system out of three available chelating sites. In addition, TG-DTA denotes the presence of coordinated and crystalline water molecules. The melting point of the complex was found to be 389°C by DSC. In addition, Cr(III-morin complex was found to be a more potent antioxidant than morin as evaluated by DPPH• and FRAP methods.

Transition metal complexes of some biologically active ligands; synthesis characterization and bioactivities

International Nuclear Information System (INIS)

Rehman, S.; Ali, N.; Nisar, M.

2009-01-01

Transition/representative transition metals complexes of biologically active chelating agent 1,2-dipyrolodinoethane were synthesized and characterized through spectral and analytical data. The complexes are of the formula (M(L)X/sub 2/). Where (M = Co (II), Ni (II), Cu (II), Zn (II), Hg (II) and Cd (II) and X = CI, Br, NO/sub 3/). Tetrahedral geometry has been proposed to these-metal complexes with the help of magnetic measurements, elemental analysis, chemical stoichiometry and spectroscopic data Antibacterial activity of the ligand and its metal complexes were screened against Eschereschi coli, Klebsiello pneumonia, Proteus mirabilis, Proteus vulhari, Streptococcus pneumonia, Salmonella Iyphi, Bacilh,s anthrax, Streptococcus fecalis and Staphylococcus aureus. Complexes were found to be active against Eschereschi coli, Klebsiella pneumonia, Proteus mirabilis and Proteus vulharis. (author)

Synthesis, characterization and optimization of poly(p-phenylenediamine)-based organoclay composite for Cr(VI) remediation

CSIR Research Space (South Africa)

Mdlalose, L

2017-04-01

Full Text Available of these materials for environmental remediation. We report here the synthesis, characterization and application of a poly(para-phenylenediamine) (poly-pPD) organoclay-based composite for removal of Cr(VI) complexes from wastewater. Adsorption capacity...

Synthesis of magnetite nanoparticles-β-cyclodextrin complex

International Nuclear Information System (INIS)

Cobos Cruz, L.A.; Martinez Perez, C.A.; Monreal Romero, H.A.; Garcia Casillas, P.E.

2008-01-01

In this work, the synthesis and characterization of a magnetite (M) and β-cyclodextrin (CD) complex is presented. The chemical bonding between the magnetite and CD was studied as evidence of host-guest interaction; therefore the CD works like a reactor with the magnetite inside of it, as consequence the growth of the particle is restricted by the electrostatic interaction of M-CD complex. The particle size of the magnetite-cyclodextrin complex (M-CD) decreased 79.1% with 0.5% of CD. The average particle size of the M-CD complex was 10 nm. The saturation magnetization (σ s ) and intrinsic coercivity (H c ) increased 10% and 20%, respectively. In order to understand how the the CD affects the results obtained, the second derivate of remission function was obtained from the ultraviolet-visible spectra (UV-vis). Fourier transform infrared spectroscopy (FTIR) was used to elucidate the interaction between the magnetite and CD. The thermal analysis was measured by thermogravimetric and differential thermal analysis (TGA-DTA). The magnetic properties, intrinsic coercivity (H c ) and the saturation magnetization were determined by vibrating sample magnetometry (VSM); the size and shape of nanoparticles were determined by scanning electron microscopy (SEM). The identification of phases was made by X-ray diffraction

Synthesis, Spectral Characterization and Antioxidant Activity of Tin(II-Morin Complex

Directory of Open Access Journals (Sweden)

Shahabuddin Memon

2012-12-01

Full Text Available The study focuses on the interaction between morin and Tin(II and the resulting complex was characterized through various analytical techniques by comparing it with morin. The complexation was confirmed at first by UV-Vis study, which shows that addition of Tin(II to morin may produce bathochromic shifts indicative of complex formation. IR spectral studies indicated that carbonyl has involved in coordination with Tin(II. Moreover, 1H-NMR studies validated that in conjunction with carbonyl, 3-OH of morin is more appropriate to be involved in complexation by replacement of its proton. Scavenging activities of morin and its Tin(II complex on DPPH• radical showed the inhibitory rates of 65% and 49%, respectively. In addition, the reducing capacity of morin was outstanding at 0.5 and 2.0 mg/ml concentrations relative to Tin(II complex. Overall, the study potentially shows the strong impact in order to design the anticancer drugs jointly from its cytotoxic potential and antioxidant activities, thereby selectively targeting the cancerous cells in result increasing their therapeutic index as well as extra advantages over other anticancer drugs.

Synthesis, characterization and luminescent properties of lanthanide complexes with an unsymmetrical tripodal ligand

Energy Technology Data Exchange (ETDEWEB)

Yan Zhenzhong [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China); Tang Yu [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China)], E-mail: tangyu@lzu.edu.cn; Liu Weisheng; Tan Minyu [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China)

2008-09-15

Solid complexes of lanthanide nitrates with a new unsymmetrical tripodal ligand, bis[(2'-benzylaminoformyl)phenoxyl)ethyl](ethyl)amine (L) have been synthesized and characterized by elemental analysis, infrared spectra and molar conductivity measurements. At the same time, the luminescent properties of the Sm(III), Eu(III), Tb(III) and Dy(III) nitrate complexes in solid state were also investigated. Under the excitation of UV light, these complexes exhibited characteristic emission of central metal ions.

Synthesis, spectroscopic, biological activity and thermal characterization of ceftazidime with transition metals

Science.gov (United States)

Masoud, Mamdouh S.; Ali, Alaa E.; Elasala, Gehan S.; Kolkaila, Sherif A.

2018-03-01

Synthesis, physicochemical characterization and thermal analysis of ceftazidime complexes with transition metals (Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II)) were discussed. It's obtained that ceftazidime act as bidentate ligand. From magnetic measurement and spectral data, octahedral structures were proposed for all complexes except for cobalt, nickel and mercury had tetrahedral structural. Hyper chemistry program confirmed binding sites of ceftazidime. Ceftazidime complexes show higher activity than ceftazidime for some strains. From TG and DTA curves the thermal decomposition mechanisms of ceftazidime and their metal complexes were suggested. The thermal decomposition of the complexes ended with the formation of metal oxides as a final product except in case of Hg complex.

Synthesis and spectroscopic characterization of gallic acid and some of its azo complexes

Science.gov (United States)

Masoud, Mamdouh S.; Hagagg, Sawsan S.; Ali, Alaa E.; Nasr, Nessma M.

2012-04-01

A series of gallic acid and azo gallic acid complexes were prepared and characterized by elemental analysis, IR, electronic spectra and magnetic susceptibility. The complexes were of different geometries: Octahedral, Tetrahedral and Square Planar. ESR was studied for copper complexes. All of the prepared complexes were of isotropic nature. The thermal analyses of the complexes were studied by DTA and DSC techniques. The thermodynamic parameters and the thermal transitions, such as glass transitions, crystallization and melting temperatures for some ligands and their complexes were evaluated and discussed. The entropy change values, ΔS#, showed that the transition states are more ordered than the reacting complexes. The biological activities of some ligands and their complexes are tested against Gram positive and Gram negative bacteria. The results showed that some complexes have a well considerable activity against different organisms.

Synthesis and characterization of six-membered pincer ...

Indian Academy of Sciences (India)

0013167

SUPPORTING INFORMATION. REGULAR ARTICLE. Synthesis and characterization of six-membered pincer nickelacycles and application in alkylation of benzothiazole. †. HANUMANPRASAD PANDIRI,a DIPESH M SHARMA,a RAJESH G GONNADEb and. BENUDHAR PUNJI*,a. aOrganometallic Synthesis and Catalysis ...

Synthesis of new oxovanadium (IV) complexes of potential insulinmimetic activity with coumarin-3-carboxylic acid ligands and substituted derivatives

International Nuclear Information System (INIS)

Salas Fernandez, Paloma; Alvino de la Sota, Nora; Galli Rigo-Righi, Carla

2013-01-01

This work comprises the design and synthesis of four new oxovanadium (IV) complexes, a metal which possesses insulin-mimetic action. Coumarin-3-carboxylic acid and three of its 6 -and 6,8- derivatives were used as ligands. Coumarins are of interest due to their well-known biological properties and pharmacological applications; these include the insulino-sensibilizing effect of certain alcoxy-hydroxy-derivatives which might lead to the eventual existence of a synergetic effect with the active metal center. The synthesis of the vanadyl complexes was preceded by the synthesis of the coumarin-3-carboxylic acid and its 6-bromo- derivative, as well as the syntheses of three derivatives not previously reported: 6-bromo-8-metoxi-, 6-bromo-8-nitro-, and 6-bromo-8-hydroxy-, which were prepared by a Knoevenagel condensation reaction. The complexes, on their part, were prepared by a metathesis reaction between VOSO 4 and the corresponding ligands, on the basis of methods reported for other vanadyl complexes and under strict pH control. The coumarin-3-carboxylic ligands and the derivatives were characterized by 1 H-NMR-, FTIR- and UV-Vis-spectroscopy. In the case of the complexes, their paramagnetic character did not allow for NMR characterization, being thus identified by FT-IR-spectroscopy and by the quantitative determination of their vanadium contents. (author)

Metal complex catalysis in the synthesis of organoaluminium compounds

International Nuclear Information System (INIS)

Dzhemilev, Usein M; Ibragimov, Askhat G

2000-01-01

The published data on the synthesis of organoaluminium compounds involving metal complex catalysts are generalised and systematised. Hydro-, carbo- and cycloalumination reactions of alkenes, conjugated dienes and alkynes catalysed by Ti and Zr complexes are considered in detail. The use of organoaluminium reagents in organic synthesis and novel reactions involving these compounds are discussed. The bibliography includes 240 references.

Complex Hollow Nanostructures: Synthesis and Energy-Related Applications.

Science.gov (United States)

Yu, Le; Hu, Han; Wu, Hao Bin; Lou, Xiong Wen David

2017-04-01

Hollow nanostructures offer promising potential for advanced energy storage and conversion applications. In the past decade, considerable research efforts have been devoted to the design and synthesis of hollow nanostructures with high complexity by manipulating their geometric morphology, chemical composition, and building block and interior architecture to boost their electrochemical performance, fulfilling the increasing global demand for renewable and sustainable energy sources. In this Review, we present a comprehensive overview of the synthesis and energy-related applications of complex hollow nanostructures. After a brief classification, the design and synthesis of complex hollow nanostructures are described in detail, which include hierarchical hollow spheres, hierarchical tubular structures, hollow polyhedra, and multi-shelled hollow structures, as well as their hybrids with nanocarbon materials. Thereafter, we discuss their niche applications as electrode materials for lithium-ion batteries and hybrid supercapacitors, sulfur hosts for lithium-sulfur batteries, and electrocatalysts for oxygen- and hydrogen-involving energy conversion reactions. The potential superiorities of complex hollow nanostructures for these applications are particularly highlighted. Finally, we conclude this Review with urgent challenges and further research directions of complex hollow nanostructures for energy-related applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and Optical Characterization of Mixed Ligands Beryllium Complexes for Display Device Applications

Directory of Open Access Journals (Sweden)

Vandna Nishal

2015-01-01

Full Text Available Synthesis and photoluminescent behaviour of mixed ligand based beryllium complexes with 2-(2-hydroxyphenylbenzoxazole (HPB and 5-chloro-8-hydroxyquinoline (Clq or 5,7-dichloro-8-hydroxyquinoline (Cl2q or 2-methyl-8-hydroxyquinoline (Meq or 8-hydroxyquinoline (q are reported in this work. These complexes, that is, [BeHPB(Clq], [BeHPB(Cl2q], [BeHPB(Meq], and [BeHPB(q], were prepared and their structures were confirmed by elemental analysis, Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, and thermal analysis. The beryllium complexes exhibited good thermal stability up to ~300°C temperature. The photophysical properties of beryllium complexes were studied using ultraviolet-visible absorption and photoluminescence emission spectroscopy. The complexes showed absorption peaks due to π-π∗ and n-π∗ electronic transitions. The complexes emitted greenish blue light with peak wavelength at 496 nm, 510 nm, 490 nm, and 505 nm, respectively, consisting of high intensity. Color tuning was observed with changing the substituents in quinoline ring ligand in metal complexes. The emitted light had Commission Internationale d’Eclairage color coordinates values at x=0.15 and y=0.43 for [BeHPB(Clq], x=0.21 and y=0.56 for [BeHPB(Cl2q], x=0.14 and y=0.38 for [BeHPB(Meq], x=0.17 and y=0.41 for [BeHPB(q]. Theoretical calculations using DFT/B3LYP/6-31G(d,p method were performed to reveal the three-dimensional geometries and the frontier molecular orbital energy levels of these synthesized metal complexes.

Synthesis, radiometric determination of functional groups, complexation

International Nuclear Information System (INIS)

Pompe, S.; Bubner, M.; Schmeide, K.; Heise, K.H.; Bernhard, G.; Nitsche, H.

2000-01-01

The interaction behavior of humic acids with uranium(VI) and the influence of humic substances on the migration behavior of uranium was investigated. A main focus of this work was the synthesis of four different humic acid model substances and their characterization and comparison to the natural humic acid from Aldrich. A radiometric method for the determination of humic acid functional groups was applied in addition to conventional methods for the determination of the functionality of humic acids. The humic acid model substances show functional and structural properties comparable to natural humic acids. Modified humic acids with blocked phenolic OH were synthesized to determine the influence of phenolic OH groups on the complexation behavior of humic acids. A synthesis method for 14 C-labeled humic acids with high specific activity was developed. The complexation behavior of synthetic and natural humic acids with uranium(VI) was investigated by X-ray absorption spectroscopy, laser-induced fluorescence spectroscopy and FTIR spectroscopy. The synthetic model substances show an interaction behavior with uranium(VI) that is comparable to natural humic acids. This points to the fact that the synthetic humic acids simulate the functionality of their natural analogues very well. For the first time the influence of phenolic OH groups on the complexation behavior of humic acids was investigated by applying a modified humic acid with blocked phenolic OH groups. The formation of a uranyl hydroxy humate complex was identified by laserspectroscopic investigations of the complexation of Aldrich humic acid with uranium(VI) at pH 7. The migration behavior of uranium in a sandy aquifer system rich is humic substances was investigated in column experiments. A part of uranium migrates non-retarded through the sediment, bound to humic colloids. The uranium migration behavior is strongly influenced by the kinetically controlled interaction processes of uranium with the humic colloids

Synthesis, characterization and behaviour to gamma radiation of the bis-L-alaninato-copper (II)

International Nuclear Information System (INIS)

Passos, B.F.T.

1985-01-01

The behaviour of coordinated compound obtained from the copper (II) and the L-(+)- alanine to gamma radiation was determined. A study of synthesis and characterization of this complex was made with elementary analysis, ultraviolet and visible electronic spectroscopy, infrared vibrational spectroscopy, proton magnetic resonance spectroscopy and thermo-gravimetric analysis. (C.G.C.)

Synthesis and Spectral Characterization of Antifungal Sensitive Schiff Base Transition Metal Complexes

Science.gov (United States)

Sakthivel, A.; Rajasekaran, K.

2007-01-01

New N2O2 donor type Schiff base has been designed and synthesized by condensing acetoacetanilido-4-aminoantipyrine with 2-aminobenzoic acid in ethanol. Solid metal complexes of the Schiff base with Cu(II), Ni(II), Co(II), Mn(II), Zn(II), VO(IV), Hg(II) and Cd(II) metal ions were synthesized and characterized by elemental analyses, magnetic susceptibility, molar conduction, fast atom bombardment (FAB) mass, IR, UV-Vis, and 1H NMR spectral studies. The data show that the complexes have the composition of ML type. The UV-Vis. and magnetic susceptibility data of the complexes suggest a square-planar geometry around the central metal ion except VO(IV) complex which has square-pyramidal geometry. The in vitro antifungal activities of the compounds were tested against fungi such as Aspergillus niger, Aspergillus flavus, Rhizopus stolonifer, Candida albicans, Rhizoctonia bataicola and Trichoderma harizanum. All the metal complexes showed stronger antifungal activities than the free ligand. The minimum inhibitory concentrations (MIC) of the metal complexes were found in the range of 10~31 µg/ml. PMID:24015086

Synthesis, characterization, DNA binding and cleavage studies of mixed-ligand copper (II complexes

Directory of Open Access Journals (Sweden)

M. Sunita

2017-05-01

Full Text Available New two copper complexes of type [Cu(Bzimpy(LH2O]SO4 (where L = 2,2′ bipyridine (bpy, and ethylene diamine (en, Bzimpy = 2,6-bis(benzimidazole-2ylpyridine have been synthesized and characterized by elemental analyses, molar conductance measurements, magnetic susceptibility measurements, mass, IR, electronic and EPR spectral studies. Based on elemental and spectral studies six coordinated geometries were assigned to the two complexes. DNA-binding properties of these metal complexes were investigated using absorption spectroscopy, fluorescence spectroscopy, viscosity measurements and thermal denaturation methods. Experimental studies suggest that the complexes bind to DNA through intercalation. These complexes also promote the cleavage of plasmid pBR322, in the presence of H2O2.

Synthesis and characterization of iron cobalt (FECO) nanorods ...

African Journals Online (AJOL)

Synthesis and characterization of iron cobalt (FECO) nanorods prepared by simple ... shaped by increasing annealing temperature from room temperature to 800 ... Keywords: FeCo nanoparticles, sodium borohydrid, CTAB, chemical synthesis ...

Materials-by-design: computation, synthesis, and characterization from atoms to structures

Science.gov (United States)

Yeo, Jingjie; Jung, Gang Seob; Martín-Martínez, Francisco J.; Ling, Shengjie; Gu, Grace X.; Qin, Zhao; Buehler, Markus J.

2018-05-01

In the 50 years that succeeded Richard Feynman’s exposition of the idea that there is ‘plenty of room at the bottom’ for manipulating individual atoms for the synthesis and manufacturing processing of materials, the materials-by-design paradigm is being developed gradually through synergistic integration of experimental material synthesis and characterization with predictive computational modeling and optimization. This paper reviews how this paradigm creates the possibility to develop materials according to specific, rational designs from the molecular to the macroscopic scale. We discuss promising techniques in experimental small-scale material synthesis and large-scale fabrication methods to manipulate atomistic or macroscale structures, which can be designed by computational modeling. These include recombinant protein technology to produce peptides and proteins with tailored sequences encoded by recombinant DNA, self-assembly processes induced by conformational transition of proteins, additive manufacturing for designing complex structures, and qualitative and quantitative characterization of materials at different length scales. We describe important material characterization techniques using numerous methods of spectroscopy and microscopy. We detail numerous multi-scale computational modeling techniques that complements these experimental techniques: DFT at the atomistic scale; fully atomistic and coarse-grain molecular dynamics at the molecular to mesoscale; continuum modeling at the macroscale. Additionally, we present case studies that utilize experimental and computational approaches in an integrated manner to broaden our understanding of the properties of two-dimensional materials and materials based on silk and silk-elastin-like proteins.

Pentamethylcyclopentadienyl-rhodium and iridium complexes containing (N^N and N^O) bound chloroquine analogue ligands: synthesis, characterization and antimalarial properties.

Science.gov (United States)

Ekengard, Erik; Kumar, Kamlesh; Fogeron, Thibault; de Kock, Carmen; Smith, Peter J; Haukka, Matti; Monari, Magda; Nordlander, Ebbe

2016-03-07

The synthesis and characterization of twenty new pentamethylcyclopentadienyl-rhodium and iridium complexes containing N^N and N^O-chelating chloroquine analogue ligands are described. The in vitro antimalarial activity of the new ligands as well as the complexes was evaluated against the chloroquine sensitive (CQS) NF54 and the chloroquine resistant (CQR) Dd2 strains of Plasmodium falciparum. The antimalarial activity was found to be good to moderate; although all complexes are less active than artesunate, some of the ligands and complexes showed better activity than chloroquine (CQ). In particular, rhodium complexes were found to be considerably more active than iridium complexes against the CQS NF54 strain. Salicylaldimine Schiff base ligands having electron-withdrawing groups (F, Cl, Br, I and NO2) in para position of the salicyl moiety and their rhodium complexes showed good antiplasmodial activity against both the CQS-NF54 and the CQR-Dd2 strains. The crystal structures of (η(5)-pentamethylcyclopentadienyl){N(1)-(7-chloroquinolin-4-yl)-N(2)-(pyridin-2-ylmethyl)ethane-1,2-diamine)} chlororhodium(III) chloride and (η(5)-pentamethylcyclopentadienyl){(4-chloro-2-(((2-((7-chloroquinolin-4-yl)amino)ethyl)imino)methyl)phenolate)}chlororhodium(III) chloride are reported. The crystallization of the amino-pyridyl complex (η(5)-pentamethylcyclopentadienyl){(N(1)-(7-chloroquinolin-4-yl)-N(2)-(pyridin-2-ylmethyl)ethane-1,2-diamine)}chloroiridium(III) chloride in acetone resulted in the formation of the imino-pyridyl derivative (η(5)-pentamethylcyclopentadienyl){(N1-(7-chloroquinolin-4-yl)-N2-(pyridin-2-ylmethylene)ethane-1,2-diamine)}chloroiridium(III) chloride, the crystal structure of which is also reported.

Bis(pentamethylene)urea complexes of the lanthanide nitrates: synthesis, characterization, properties

International Nuclear Information System (INIS)

Souza, H.K.S. de; Pedrosa, A.M.G.; Marinho, E.P.M.; Batista, M.K.S.; Melo, D.M.A.; Zinner, K.; Zinner, L.B.; Zukerman-Schpector, J.; Vicentini, G.

2003-01-01

Lanthanide nitrate complexes of bis(pentamethylene)urea (BPMU) with general formula Ln(NO 3 ) 3 3BPMU, where Ln: La, Nd, Sm, Eu, Ho and Er have been prepared and characterized based on CHN elemental analyses, lanthanide titration with EDTA, molar conductivity, spectroscopic data and thermal studies. The infrared spectra show that ligands (BPMU) are bonded through the carbonyl oxygen, nitrate counter-ions are bidentate linked to the central ions. The structure of the neodymium complex was determined. The crystal is monoclinic, P2 1/c ,Z=4, with the following parameters: a=10.148(1) A, b=21.879(2), c=19.154(2) A, β=104.11(1) deg., V=4124.3(7) A 3 . The polyhedron is a distorted tricapped trigonal prism, coordination number nine

Hydrothermal synthesis, characterization and luminescent ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 39; Issue 4. Hydrothermal synthesis, characterization and luminescent properties of lanthanide-doped NaLaF 4 nanoparticles. JIGMET LADOL HEENA KHAJURIA SONIKA KHAJURIA ... Keywords. Citric acid; X-ray diffraction; down-conversion emission; energy transfer.

Synthesis and Characterization of Chromium (III) Complexes with L-Glutamic Acid, Glycine and LCysteine

OpenAIRE

Kun Sri Budiasih; Chairil Anwar; Sri Juari Santosa; Hilda Ismail

2013-01-01

Some Chromium (III) complexes were synthesized with three amino acids: L Glutamic Acid, Glycine, and L-cysteine as the ligands, in order to provide a new supplement containing Cr(III) for patients with type 2 diabetes mellitus. The complexes have been prepared by refluxing a mixture of Chromium(III) chloride in aqueous solution with L-glutamic acid, Glycine, and L-cysteine after pH adjustment by sodium hydroxide. These complexes were characterized by Infrared and Uv-Vis s...

Synthesis and characterization of Fe(III-piperazine-derived complexes encapsulated in zeolite Y

Directory of Open Access Journals (Sweden)

Márcio E. Berezuk

2012-01-01

Full Text Available Zeolite-encapsulated complexes have been widely applied in hydrocarbon oxidation catalysis. The "ship-in-a-bottle" encapsulation of iron(III complexes containing piperazine and piperazine-derivative ligands in zeolite-Y is described. The flexible ligand methodology was employed and the efficiency and reproducibility of the procedure was investigated. The catalysts were characterized employing several techniques and the results indicate the presence of coordinated and uncoordinated iron(III ions inside and outside the zeolitic cage.

Synthesis, characterization, antiplasmodial and antitrypanosomal activity of some metal(III complexes of sulfadiazine

Directory of Open Access Journals (Sweden)

P.A. Ajibade

2008-08-01

Full Text Available The Fe(III, Ru(III, Rh(III, and Cr(III complexes of 4-amino-N-(2-pyrimidinylbenzene sulfonamide (sulfadiazine have been synthesized and characterized by elemental analysis, electronic and IR spectroscopy, conductance and room temperature magnetic susceptibility measurements. Sulfadiazine acts as a bidentate ligand through the sulfonamido and the pyrimidinic N-atoms. The compounds are non-electrolytes and the electronic spectra are consistent with the proposed octahedral geometry around the metal ions. The complexes were tested for in vitro activity against cultures of the resistant strains of Plasmodium falciparum, tripamastigotes T. b. rhodesiense and amastigotes L. donovani to determine their antiprotozoal activities. The Fe(III complex is more active than the other complexes against the parasitic protozoa.

Physico-Chemical and In-vitro Microbial Studies of Newly Synthesis Organometallic Complexes

Directory of Open Access Journals (Sweden)

Isam Hussain Al-Karkhi

2014-05-01

Full Text Available Drugs normally synthesized to use as medication to treat diseases like cancer and microbial infections, these synthesized drugs were interested more than naturally-derived drugs which have been shows low activity or not as efficient against diseases. A new ligand 3-methylbenzyl (2Z-2-[1-(pyridin-4-ylethylidene]hydrazine carbodithioate (PE3MBC and its Cd(II, Cu(II, Co(II and Zn(II metal complexes. The new ligand and metal complexes were characterized via various physico-chemical and spectroscopic techniques. Cd(II complex show more activity against microbes and against cancer cell line MCF-7, while other complexes does not shows activity like cadmium complex, all the complexes does not shows any activity against MDAMB-231 cell line. The fatal of the cancer and the microbes cell was due to inhibition of DNA synthesis which was probably due to chelating with metals complexes, or could be referred to lipophilicity, presence of hydrophobic moiety in the complex molecule, also could be due to steric effects and electronic effects.

Synthesis, characterization and anticancer activity of kaempferol-zinc(II) complex.

Science.gov (United States)

Tu, Lv-Ying; Pi, Jiang; Jin, Hua; Cai, Ji-Ye; Deng, Sui-Ping

2016-06-01

According to the previous studies, the anticancer activity of flavonoids could be enhanced when they are coordinated with transition metal ions. In this work, kaempferol-zinc(II) complex (kaempferol-Zn) was synthesized and its chemical properties were characterized by UV-VIS, FT-IR, (1)H NMR, elemental analysis, electrospray mass spectrometry (ES-MS) and fluorescence spectroscopy, which showed that the synthesized complex was coordinated with a Zn(II) ion via the 3-OH and 4-oxo groups. The anticancer effects of kaempferol-Zn and free kaempferol on human oesophageal cancer cell line (EC9706) were compared. MTT results demonstrated that the killing effect of kaempferol-Zn was two times higher than that of free kaempferol. Atomic force microscopy (AFM) showed the morphological and ultrastructural changes of cellular membrane induced by kaempferol-Zn at subcellular or nanometer level. Moreover, flow cytometric analysis indicated that kaempferol-Zn could induce apoptosis in EC9706 cells by regulating intracellular calcium ions. Collectively, all the data showed that kaempferol-Zn might be served as a kind of potential anticancer agent. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis, Spectral, and In Vitro Antibacterial Studies of Organosilicon(IV) Complexes with Schiff Bases Derived from Amino Acids.

Science.gov (United States)

Singh, Har Lal; Singh, Jangbhadur; Mukherjee, A

2013-01-01

The present work stems from our interest in the synthesis, characterization, and antibacterial evaluation of organosilicon(IV) complexes of a class of amino-acid-based Schiff base which have been prepared by the interaction of ethoxytrimethylsilane with the Schiff bases (N OH) in 1 : 1 molar ratio. These complexes have been characterized by elemental analysis, molar conductance, and spectroscopic studies including electronic IR and NMR ((1)H, (13)C, and (29)Si) spectroscopy. The analytical and spectral data suggest trigonal bipyramidal geometry around the silicon atom in the resulting complexes. The ligands and their organosilicon complexes have also been evaluated for in vitro antimicrobial activity against bacteria (Bacillus cereus, Nocardia spp., E. aerogenes, Escherichia coli, Klebsiella spp., and Staphylococcus spp.). The complexes were found to be more potent as compared to the ligands.

Palladium polypyridyl complexes: synthesis, characterization, DNA interaction and biological activity on Leishmania (L.) mexicana

International Nuclear Information System (INIS)

Navarro, Maribel; Betancourt, Adelmo; Hernandez, Clara; Marchan, Edgar

2008-01-01

This paper describes the search for new potential chemotherapeutic agents based on transition metal complexes with planar ligands. In this study, palladium polypyridyl complexes were synthesized and characterized by elemental analysis, NMR, UV-VIS and IR spectroscopies. The interaction of the complexes with DNA was also investigated by spectroscopic methods. All metal-to-ligand charge transfer (MLCT) bands of the palladium polypyridyl complexes exhibited hypochromism and red shift in the presence of DNA. The binding constant and viscosity data suggested that the complexes [PdCl 2 (phen)] and [PdCl 2 (phendiamine)] interact with DNA by electrostatic forces. Additionally, these complexes induced an important leishmanistatic effect on L. (L.) mexicana promastigotes at the final concentration of 10 μmol L -1 in 48 h. (author)

Synthesis, characterization and biological evaluation of ruthenium flavanol complexes against breast cancer

Science.gov (United States)

Singh, Ashok Kumar; Saxena, Gunjan; Sahabjada; Arshad, M.

2017-06-01

Four Ru(II) DMSO complexes (M1R-M4R) having substituted flavones viz. 3-Hydroxy-2-(4-methoxyphenyl)-4H-chromen-4-one (HL1), 3-Hydroxy-2-(4-nitrophenyl)-4H-chromen-4-one (HL2), 3-Hydroxy-2-(4-dimethylaminophenyl)-4H-chromen-4-one (HL3) and 3-Hydroxy-2-(4-chlorophenyl)-4H-chromen-4-one (HL4) were synthesized and characterized by elemental analysis, IR, UV-Vis, 1H NMR spectroscopies and ESI-MS. The molecular structures of the complexes were investigated by integrated spectroscopic and computational techniques (DFT). Both ligands as well as their complexes were screened for anticancer activities against breast cancer cell lines MCF-7. Cytotoxicity was assayed by MTT [3-(4, 5-dimethyl thiazol-2-yl)-2, 5-diphenyl tetrazolium bromide] assay. All ligands and their complexes exhibited significant cytotoxic potential of 5-40 μM concentration at incubation period of 24 h. The cell cytotoxicity increased significantly in a concentration-dependent manner. In this series of compounds, HL2 (IC50 17.2 μM) and its complex M2R (IC50 16 μM) induced the highest cytotoxicity.

Synthesis and characterization of U(VI) and Th(IV) complexes with o-vanillin-p-phenylenediamine

International Nuclear Information System (INIS)

Bi Caifeng; Fan Yuhua

2001-01-01

Two new solid complexes of uranyl nitrate and thorium nitrate with bis-Schiff base o-vanillin-p-phenylenediamine (L) have been synthesized and characterized by elemental analysis, IR, UV, DTA-TG and molar conductance. The compositions of the complexes are confirmed to be [UO 2 LNO 3 ]NO 3 and [ThL(NO 3 ) 2 ](NO 3 ) 2 . Some properties of the complexes are studied

Palladium polypyridyl complexes: synthesis, characterization, DNA interaction and biological activity on Leishmania (L.) mexicana

Energy Technology Data Exchange (ETDEWEB)

Navarro, Maribel [Instituto Venezolano de Investigaciones Cientificas, Caracas (Venezuela). Centro de Quimica; Betancourt, Adelmo [Universidad de Carabobo, Valencia (Venezuela). Facultad Experimental de Ciencia y Tecnologia. Dept. de Quimica; Hernandez, Clara [Universidad de Carabobo Sede Aragua, Maracay (Venezuela). Facultad de Ciencias de la Salud. Dept. de Ciencias Basicas; Marchan, Edgar [Universidad de Oriente, Cumana (Venezuela). Inst. de Investigaciones en Biomedicina y Ciencias Aplicadas. Nucleo de Sucre

2008-07-01

This paper describes the search for new potential chemotherapeutic agents based on transition metal complexes with planar ligands. In this study, palladium polypyridyl complexes were synthesized and characterized by elemental analysis, NMR, UV-VIS and IR spectroscopies. The interaction of the complexes with DNA was also investigated by spectroscopic methods. All metal-to-ligand charge transfer (MLCT) bands of the palladium polypyridyl complexes exhibited hypochromism and red shift in the presence of DNA. The binding constant and viscosity data suggested that the complexes [PdCl{sub 2}(phen)] and [PdCl{sub 2}(phendiamine)] interact with DNA by electrostatic forces. Additionally, these complexes induced an important leishmanistatic effect on L. (L.) mexicana promastigotes at the final concentration of 10 {mu}mol L{sup -1} in 48 h. (author)

Synthesis and characterization of Mn(III) chloro complexes with salen-type ligands

International Nuclear Information System (INIS)

Byun, Jong Chul; Han, Chung Hun; Lee, Nam Ho; Baik, Jong Seok; Park, Yu Chul

2002-01-01

A series of novel salen-type complexes ((Mn(III)(L acn )Cl): n=1∼11) containing Cl - ion were obtained by reactions of the Mn(CH 3 COO) 2 ·4H 2 O with the potentially tetradentate compartmental ligand (H 2 L acn ), prepared by condensation the of one mole of diamine (ethylenediamine, 1,3-propanediamine, o-phenylenediamine, and 2,2-dimethyl-1,3-propanediamine) with two moles of aldehyde (salicylaldehyde, 5-chloro- salicylaldehyde, 3,5-dichlorosalicylal-dehyde, and 3,5-di-tert-butyl-2-hydroxy-benzaldehyde) in a methanol solution . The resulting salen-type ligands and their Mn(III) complexes were identified and characterized by elemental analysis, conductivity, thermogravimetry and UV-VIS, IR, and NMR spectroscopy

Hydrothermal synthesis and characterization of a binuclear complex and a coordination

Directory of Open Access Journals (Sweden)

Reza Mohamadinasab

2010-06-01

Full Text Available Two new copper complexes [(bipy(pydcCu(μ-OCO-pydcCu(bipy(H2O].3.5H¬2O (1 and {[(μ2-C2O4(2,2'-bipyCu].2H2O}n (2 (pydcH2 = pyridine-2,6-dicarboxylilic acid, bipy = 2,2'-bipyridine have been hydrothermally synthesized. Both complexes were characterized by IR spectroscopy, elemental analysis and single crystal X-ray diffraction studies. Complex 1 consists of two independent neutral molecules. In every moiety, metal ion center is in a distorted octahedral geometry. Coordination polymer (2 has been prepared from the reaction of bis-(cyclohexanone-oxal-dihydrazone,2,2'-bipyridine and Cu(NO32 in basic solution and under hydrothermal condition. The results showed that the bis-(cyclohexanone-oxal-dihydrazone was converted to oxalate ion under heating and basic pH. Each metal ion center in 2 is in a distorted octahedral geometry and is coordinated by four oxygen atoms of two bridged oxalate ions and two nitrogen atoms of 2,2'-bipyridine molecules. In the crystal structure of 2, some H-bonds and π-π interaction cause formation of a 3D network.

Copper(II) Complexes of Phenanthroline and Histidine Containing Ligands: Synthesis, Characterization and Evaluation of their DNA Cleavage and Cytotoxic Activity.

Science.gov (United States)

Leite, Sílvia M G; Lima, Luís M P; Gama, Sofia; Mendes, Filipa; Orio, Maylis; Bento, Isabel; Paulo, António; Delgado, Rita; Iranzo, Olga

2016-11-21

Copper(II) complexes have been intensely investigated in a variety of diseases and pathological conditions due to their therapeutic potential. The development of these complexes requires a good knowledge of metal coordination chemistry and ligand design to control species distribution in solution and tailor the copper(II) centers in the right environment for the desired biological activity. Herein we present the synthesis and characterization of two ligands HL1 and H 2 L2 containing a phenanthroline unit (phen) attached to the amino group of histidine (His). Their copper(II) coordination properties were studied using potentiometry, spectroscopy techniques (UV-vis and EPR), mass spectrometry (ESI-MS) and DFT calculations. The data showed the formation of single copper complexes, [CuL1] + and [CuL2], with high stability within a large pH range (from 3.0 to 9.0 for [CuL1] + and from 4.5 to 10.0 for [CuL2]). In both complexes the Cu 2+ ion is bound to the phen unit, the imidazole ring and the deprotonated amide group, and displays a distorted square pyramidal geometry as confirmed by single crystal X-ray crystallography. Interestingly, despite having similar structures, these copper complexes show different redox potentials, DNA cleavage properties and cytotoxic activity against different cancer cell lines (human ovarian (A2780), its cisplatin-resistant variant (A2780cisR) and human breast (MCF7) cancer cell lines). The [CuL2] complex has lower reduction potential (E pc = -0.722 V vs -0.452 V for [CuL1] + ) but higher biological activity. These results highlight the effect of different pendant functional groups (carboxylate vs amide), placed out of the coordination sphere, in the properties of these copper complexes.

Template synthesis of poly aza macrocyclic copper(II) and nickel(II) complexes: Spectral characterization and antimicrobial studies

Energy Technology Data Exchange (ETDEWEB)

Gurumoorthy, P.; Ravichandran, J.; Kaliur Rahiman, A. [The New College, Chennai (India); Karthikeyan, N.; Palani, P. [Univ. of Madras, Chennai (India)

2012-07-15

The template synthesis of copper(II) and nickel(II) complexes derived from 2,6-diformyl-4-methylphenol with diethylenetriamine or 1,2-bis(3-amino propylamino)ethane produce the 12-membered N{sub 3}O and 17-membered N{sub 4}O macrocyclic complexes, respectively. The geometry of the complexes has been determined with the help of electronic and EPR spectroscopic values and found to be five coordinated square pyramidal and, six coordinated distorted tetragonal for 12-membered and 17-membered macrocyclic complexes, respectively. Electrochemical studies of the mononuclear N{sub 3}O and N{sub 4}O copper(II) complexes show one irreversible one electron reduction wave at E{sup pc} = .1.35 and .1.15 V respectively, and the corresponding nickel(II) complexes show irreversible one-electron reduction wave at E{sup pc} = .1.25 and .1.22 V, respectively. The nickel(II) complexes show irreversible one-electron oxidation wave at Epa = +0.84 and +0.82 V, respectively. All the complexes were evaluated for in vitro antimicrobial activity against the human pathogenic bacteria and fungi.

Synthesis of the 99mTc(CO)3-trovafloxacin dithiocarbamate complex and biological characterization in artificially methicillin-resistant Staphylococcus aureus infected rats model

International Nuclear Information System (INIS)

Syed Qaiser Shah; Muhammad Rafiullah Khan

2011-01-01

Synthesis of the 99m Tc(CO) 3 -trovafloxacin dithiocarbamate ( 99m Tc(CO) 3 -TVND) complex and biological characterization in artificially Staphylococcus aureus (S. aureus) infected rats model was assessed. The suitability of the complex was evaluated and compared with 99m TcN-TVND, in terms of radiochemical immovability in saline, in vitro permanence in serum, in vitro binding with S. aureus and biodistribution in Male Sprague-Dawley rats (MSDR). After 30 min of the reconstitution both the complexes showed maximum radiochemical stabilities in saline and remain more than 90% stable up to 120 min. However the 99m Tc(CO) 3 -TVND showed to some extent higher stability than 99m TcN-TVND complex. In serum 1.75% less de-tagging was observed than 99m TcN-TVND complex. Both the complexes showed saturated in vitro binding with S. aureus and no significant difference were observed between the uptakes. Six fold uptakes were noted in the infected muscle as compared to the inflamed and normal muscles of the MDSR. The uptake of the 99m Tc(CO) 3 -TVND in infected muscle of the MSDR was 2.25% high as compared to the 99m TcN-TVND complex. Based on radiochemical stabilities in saline, serum, in vitro binding with MRSA and significantly higher uptake in the infected muscle, we recommend both the complexes for in vivo investigation of the MRSA infection in human. (author)

Synthesis and characterization of Th(IV) and U(VI) complexes with o-vanillin-p-phenylenediamine

International Nuclear Information System (INIS)

Bi Caifeng; Fan Yuhua; Sun Guoxin; Chang Jun

2000-01-01

Two new solid complexes, [ThL(NO 3 ) 2 ](NO 3 ) 2 , [UO 2 L(NO 3 )]NO 3 (L = o-vanillin-p-phenylenediamine) have been synthesized and characterized by elemental analyses, DTA-TG, IR spectra, UV spectra and molar conductance. Possible structures of the two complexes are proposed. (author)

(II) complexes

African Journals Online (AJOL)

activities of Schiff base tin (II) complexes. Neelofar1 ... Conclusion: All synthesized Schiff bases and their Tin (II) complexes showed high antimicrobial and ...... Singh HL. Synthesis and characterization of tin (II) complexes of fluorinated Schiff bases derived from amino acids. Spectrochim Acta Part A: Molec Biomolec.

Synthesis, characterization and comparison of polythiophene ...

Indian Academy of Sciences (India)

38

Synthesis, characterization and comparison of polythiophene-carbon ... b Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol, ..... The scan range was from −0.24 to 1.2 V in reference to.

Mechanically-induced solvent-less synthesis of cobalt and nickel complexes of cimetidine

Directory of Open Access Journals (Sweden)

Adedibu Clement Tella

2011-09-01

Full Text Available Solvent-less synthesis of [Co(CIM2](SO4 and [Ni(CIM2](OAC2 by grinding of CoSO4 and Ni(CH3COO2.4H2O with cimetidine without any solvent is described. The complexes have been characterized by elemental analysis, melting point, AAS, conductivity measurements, TLC, infrared and UV-Vis spectroscopies as well as X-ray powder diffraction. Cimetidine was found to be bidentate or tridentate ligand. Cobalt ion coordinate with cimetidine through the sulphur atom in the thiol group, nitrogen atom of imidazole ring and the nitrogen atom of the secondary amine to give an octahedral geometry with ligand acting as tridentate whereas nickel ion coordinates through the sulphur atom in the thiol group, nitrogen atom of imidazole ring to give tetrahedral structure with ligand acting as bidentate. X-Ray diffraction patterns of the complex were different from that of the ligand suggesting formation of coordination compounds. The method is quick and gives a quantatively yield, without the need for solvents or external heating. Clearly, it can present higher efficiency in terms of materials, energy and time compared to classical solution phase synthesis.

Synthesis and characterization of nano silicon and titanium nitride ...

Indian Academy of Sciences (India)

The characterization techniques indicated ... Scalable synthesis; microwave plasma; chemical synthesis; nanoparticles. 1. Introduction ... used but very few methods are available to produce silicon and titanium ... current (A). (m3/h). 1. Si. 2.1.

Synthesis, characterization, and crystal structures of diruthenium complexes containing bridging salicylato ligands

Energy Technology Data Exchange (ETDEWEB)

Jiang, Mingxuan; Yau, Chun Huan; Hu, Yuxin; Tan, Yong Leng Kelvin [Hwa Chong Institution (Singapore); Li, Yingzhou; Ganguly, Rakesh; Leong, Weng Kee [Division of Chemistry and Biological Chemistry, School of Physical and Mathematical Sciences, Nanyang Technological University (Singapore)

2017-08-03

The thermal reaction of Ru{sub 3}(CO){sub 12} (1) with salicylic acid, in the presence of triphenylphosphine, pyridine, or dimethylsulfoxide, afforded the dinuclear complexes Ru{sub 2}(CO){sub 4}(μ-O{sub 2}CC{sub 6}H{sub 4}OH){sub 2}L{sub 2} (2) [L = PPh{sub 3} (2a). C{sub 5}H{sub 5}N (2b); (CH{sub 3}){sub 2}SO (2c)]. Complex 2b was further reacted with the aromatic dimmines 2,2'-dipyridine or 1,10-phenanthroline to give the cationic diruthenium complexes [Ru{sub 2}(CO){sub 2}(μ-CO){sub 2}(μ-O{sub 2}CC{sub 6}H{sub 4}OH)(N intersection N){sub 2}]{sup +} (3) [(N intersection N) = 2,2'-dipyridine (3a); 1,10-phenanthroline (3b)], which were isolated as their tetraphenylborate salts. All five novel complexes were characterized spectroscopically and analytically. For 2a-2b and 3a-3b, single-crystal X-ray diffraction studies were also carried out. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Synthesis and Characterization of Hexahapto-Chromium Complexes of Single-Walled Carbon Nanotubes

KAUST Repository

Kalinina, Irina

2016-12-17

This chapter employs purified pristine single-walled carbon nanotubes (SWNTs) and octadecylaminefunctionalized-SWNTs. These SWNTs are employed for investigate the potential of the SWNT sidewall to function as a hexahapto ligand for chromium (Cr), with in-depth characterization of the products using some of the techniques, such as thermogravimetric analysis (TGA), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS). Purified electric arc (EA)-produced SWNTs (P2-SWNT) and octadecylaminefunctionalized SWNTs were obtained from Carbon Solutions, Inc. The TEM images show the removal of the Cr particles from the outer surface of the SWNT bundles in the SWNT-Cr complexes after decomplexation; Cr attachment to the surface of the as-prepared complexes (η6-SWNT)Cr(CO)3 and (η6-SWNT-CONH(CH2)17CH3)Cr(CO)3 is clearly evident. The positions of the bands in the Raman spectra of SWNTs are sensitive to doping and thus the chapter examines the effect of complexation of the Cr(CO)3 and Cr(η6-benzene) units on the position of the G and 2D bands in the (η6-SWNT)Cr(CO)3 and (η6-SWNT)Cr(η6-benzene) complexes.

Synthesis, spectroscopic, structural and thermal characterizations of vanadyl(IV) adenine complex prospective as antidiabetic drug agent

Science.gov (United States)

El-Megharbel, Samy M.; Hamza, Reham Z.; Refat, Moamen S.

2015-01-01

The vanadyl(IV) adenine complex; [VO(Adn)2]ṡSO4; was synthesized and characterized. The molar conductivity of this complex was measured in DMSO solution that showed an electrolyte nature. Spectroscopic investigation of the green solid complex studied here indicate that the adenine acts as a bidentate ligand, coordinated to vanadyl(IV) ions through the nitrogen atoms N7 and nitrogen atom of amino group. Thus, from the results presented the vanadyl(IV) complex has square pyramid geometry. Further characterizations using thermal analyses and scanning electron techniques was useful. The aim of this paper was to introduce a new drug model for the diabetic complications by synthesized a novel mononuclear vanadyl(IV) adenine complex to mimic insulin action and reducing blood sugar level. The antidiabetic ability of this complex was investigated in STZ-induced diabetic mice. The results suggested that VO(IV)/adenine complex has antidiabetic activity, it improved the lipid profile, it improved liver and kidney functions, also it ameliorated insulin hormone and blood glucose levels. The vanadyl(IV) complex possesses an antioxidant activity and this was clear through studying SOD, CAT, MDA, GSH and methionine synthase. The current results support the therapeutic potentiality of vanadyl(IV)/adenine complex for the management and treatment of diabetes.

Synthesis, characterization and optical properties of novel N donor ligands-chelated zirconium(IV) complexes

Science.gov (United States)

Shahroosvand, Hashem; Nasouti, Fahimeh; Mohajerani, Ezeddin; Khabbazi, Amir

2012-11-01

Novel zirconium complexes have been synthesized by using a mixture of zirconium nitrate, 1,2,4,5-benzen tetracarboxylic acid (H4btec), 1,10-phenanthroline(phen) and potassium thiocyanate. Monodentate coordination mode of btec acid for all complexes was investigated by FT-IR spectroscopy. The complexes were also characterized by UV-Vis, 1H NMR, CHN, ICP-AES. The reaction details and features were described and discussed. The photoluminescence emission of seven zirconium complexes was shown two series peaks: first, sharp and intense bands from 300 to 500 nm and broadened with less intensity from 650 to 750 nm for the second bands. Each of the zirconium compounds were doped in PVK:PBD blend as host. The ratio of zirconium complexes for each type were modified 8 wt.% in PVK:PBD(100:40). The electroluminescence spectra of zirconium complexes were indicated a red shift rather than PVK:PBD blend. We suggest that the electroplex occurring at PVK-Zr complex interface.

Synthesis, characterization, antimicrobial activity and molecular ...

African Journals Online (AJOL)

Synthesis, characterization, antimicrobial activity and molecular docking studies of combined pyrazol-barbituric acid pharmacophores. Assem Barakat, Bandar M. Al-Qahtani, Abdullah M. Al-Majid, M. Ali Mohammed Rafi Shaik, Mohamed H.M. Al-Agamy, Abdul Wadood ...

Preparation and characterizations of new U(IV) and U(VI) complexes with carboxylate ligands

Energy Technology Data Exchange (ETDEWEB)

Sbrignadello, G; Tomat, G; Battiston, G; Vigato, P A [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi

1978-01-01

The synthesis and characterization of some uranyl(VI) complexes containing glycolate (gly = CH/sub 2/OHCOO/sup -/) and methoxyacetate (MeOAc = CH/sub 3/OCH/sub 2/COO/sup -/) ligands with metal:ligand ratios of 1:1 and 1:2 are reported. In addition, new stable uranium(IV) complexes containing the same ligands, or the oxydiacetate (oda = /sup -/OOCCH/sub 2/OCH/sub 2/COO/sup -/) anion, have been prepared by photolysing aqueous solutions of uranyl(VI) nitrate in the presence of an excess of ligand. The possible structures of these complexes are discussed on the basis of IR results. The photoproduction mechanism of U(IV) complexes is proposed from electronic and spectrofluorimetric spectra and quantum yield data.

Synthesis, characterization, DNA binding and catalytic applications of Ru(III) complexes.

Science.gov (United States)

Shoair, A F; El-Shobaky, A R; Azab, E A

2015-01-01

A new series of azodye ligands 5-chloro-3-hydroxy-4-(aryldiazenyl)pyridin-2(1H)-one (HLn) were synthesized by coupling of 5-chloro-3-hydroxypyridin-2(1H)-one with aniline and its p-derivatives. These ligands and their Ru(III) complexes of the type trans-[Ru(Ln)2(AsPh3)2]Cl were characterized by elemental analyses, IR, (1)H NMR and UV-Visible spectra as well as magnetic and thermal measurements. The molar conductance measurements proved that all the complexes are electrolytes. IR spectra show that the ligands (HLn) acts as a monobasic bidentate ligand by coordinating via the nitrogen atom of the azo group (NN) and oxygen atom of the deprotonated phenolic OH group, thereby forming a six-membered chelating ring and concomitant formation of an intramolecular hydrogen bond. The molecular and electronic structures of the investigated compounds (HLn) were also studied using quantum chemical calculations. The calf thymus DNA binding activity of the ligands (HLn) and their Ru(III) complexes were studied by absorption spectra and viscosity measurements. The mechanism and the catalytic oxidation of benzyl alcohol by trans-[Ru(Ln)2(AsPh3)2]Cl with hydrogen peroxide as co-oxidant were described. Copyright © 2015 Elsevier B.V. All rights reserved.

synthesis and optical characterization of acid-doped polyaniline thin

African Journals Online (AJOL)

HOD

SYNTHESIS AND OPTICAL CHARACTERIZATION OF ACID-DOPED. POLYANILINE THIN .... MATERIALS AND METHODS .... Characterization of Se Doped Polyaniline”,Current. Applied ... with Silver Nanoparticles”, Advances in Materials.

Synthesis, characterization and thermal behavior of antibacterial and antifungal active zinc complexes of bis (3(4-dimethylaminophenyl)-allylidene-1,2-diaminoethane

International Nuclear Information System (INIS)

Montazerozohori, Morteza; Zahedi, Saeedeh; Naghiha, Asghar; Zohour, Mostafa Montazer

2014-01-01

In this work, synthesis of a new series of zinc halide/pseudohalide complexes of a bidentate Schiff base ligand entitled as bis (3-(4-dimethylaminophenyl)-allylidene)-1,2-diaminoethane(L) is described. The ligand and its zinc complexes were characterized by various techniques such as elemental analysis, FT-IR, UV–visible, 1 H and 13 C NMR spectra, cyclic voltammetry, and conductometry. Accordingly ZnLX 2 (X = Cl − , Br − , I − , SCN − and N 3 − ) was suggested as molecular formula of the complexes. Redox behaviors of ligand and its zinc complexes were investigated by cyclic voltammetry method. Furthermore, the ligand and its zinc halide/pseudohalide complexes were tested for their in vitro antibacterial activities against two gram positive bacteria (Staphylococcus aureus and Bacillus subtilis) and two gram negative bacteria (Escherichia coli and Pseudomonas aeruginosa). Also in vitro antifungal activities of them against Candida albicans and Aspergillus niger were investigated. The results indicated that all compounds are antibacterial and antifungal active. Thermal behaviors of ligand and its zinc complexes were studied from room temperature to 1100 °C under argon atmosphere. It was found that the ligand and zinc iodide are decomposed completely via three and four steps respectively while other zinc complexes leave out the metal or organometallic compounds as final residuals after 3–4 decomposition steps at above temperature range. Moreover evaluation of some thermo-kinetic parameters such as activation energy (∆E ⁎ ), enthalpy (∆H ⁎ ), entropy (∆S ⁎ ) and Gibbs free energy change (∆G ⁎ ) of the thermal decomposition steps were performed based on the Coats–Redfern relation. - Highlights: • Some novel complexes of Zn(II) with a bidentate Schiff base ligand have been synthesized. • Redox behavior of ligand and zinc complexes was investigated by cyclic voltammetry. • The ligand and its zinc complexes are antibacterial and

Novel synthesis and characterization of a collagen-based biopolymer initiated by hydroxyapatite nanoparticles.

Science.gov (United States)

Bhuiyan, D; Jablonsky, M J; Kolesov, I; Middleton, J; Wick, T M; Tannenbaum, R

2015-03-01

In this study, we developed a novel synthesis method to create a complex collagen-based biopolymer that promises to possess the necessary material properties for a bone graft substitute. The synthesis was carried out in several steps. In the first step, a ring-opening polymerization reaction initiated by hydroxyapatite nanoparticles was used to polymerize d,l-lactide and glycolide monomers to form poly(lactide-co-glycolide) co-polymer. In the second step, the polymerization product was coupled with succinic anhydride, and subsequently was reacted with N-hydroxysuccinimide in the presence of dicyclohexylcarbodiimide as the cross-linking agent, in order to activate the co-polymer for collagen attachment. In the third and final step, the activated co-polymer was attached to calf skin collagen type I, in hydrochloric acid/phosphate buffer solution and the precipitated co-polymer with attached collagen was isolated. The synthesis was monitored by proton nuclear magnetic resonance, infrared and Raman spectroscopies, and the products after each step were characterized by thermal and mechanical analysis. Calculations of the relative amounts of the various components, coupled with initial dynamic mechanical analysis testing of the resulting biopolymer, afforded a preliminary assessment of the structure of the complex biomaterial formed by this novel polymerization process. Copyright © 2015. Published by Elsevier Ltd.

Synthesis of imine bond containing insoluble polymeric ligand and its transition metal complexes, structural characterization and catalytic activity on esterification reaction.

Science.gov (United States)

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Saribiyik, Oguz Yunus; Yildiz, Emel; Serin, Selahattin

2017-01-01

In this study, synthesis of insoluble polymeric ligand (L) and its transition metal complexes [Cu(L)Cl 2 ]·2H 2 O (1) , [Co(L)Cl 2 (H 2 O) 2 ] (2) and [Ni(L)Cl 2 (H 2 O) 2 ] (3) , having the azomethine groups, were synthesized by the condensation reactions of the diamines and dialdehydes. The structural properties were characterized by the analytical and spectroscopic methods using by elemental analysis, Fourier Transform Infrared, Thermo Gravimetric Analysis, Powder X-ray Diffraction, magnetic susceptibility and Inductively Coupled Plasma. The solubilities of the synthesized polymeric materials were also investigated and found as insoluble some organic and inorganic solvents. Additionally, their catalytic performance was carried out for the esterification reaction of acetic acid and butyl acetate. The highest conversion rate is 75.75% by using catalyst 1 . The esterification of butanol gave butyl acetate with 100% selectivity.

Homodinuclear lanthanide complexes of phenylthiopropionic acid: Synthesis, characterization, cytotoxicity, DNA cleavage, and antimicrobial activity

Science.gov (United States)

Shiju, C.; Arish, D.; Kumaresan, S.

2013-03-01

Lanthanide complexes of La(III), Pr(III), Nd(III), Sm(III), and Ho(III) with phenylthiopropionic acid were synthesized and characterized by elemental analysis, mass, IR, electronic spectra, molar conductance, TGA, and powder XRD. The results show that the lanthanide complexes are homodinuclear in nature. The two lanthanide ions are bridged by eight oxygen atoms from four carboxylate groups. Thermal decomposition profiles are consistent with the proposed formulations. Powder XRD studies show that all the complexes are amorphous in nature. Antimicrobial studies indicate that these complexes exhibit more activity than the ligand itself. The DNA cleavage activity of the ligand and its complexes were assayed on Escherichia coli DNA using gel electrophoresis in the presence of H2O2. The result shows that the Pr(III) and Nd(III) complexes have completely cleaved the DNA. The anticancer activities of the complexes have also been studied towards human cervical cancer cell line (HeLa) and colon cancer cells (HCT116) and it was found that the La(III) and Nd(III) complexes are more active than the corresponding Pr(III), Sm(III), Ho(III) complexes, and the free ligand on both the cancer cells.

Synthesis, Characterization and Spectral Properties of Substituted Tetraphenylporphyrin Iron Chloride Complexes

Directory of Open Access Journals (Sweden)

Kai Li

2011-04-01

Full Text Available A series of substituted tetraphenylporphyrin iron chloride complexes [RTPPFe(IIICl, R=o/p-NO2, o/p-Cl, H, o/p-CH3, o/p-OCH3] were synthesized by a novel universal mixed-solvent method and the spectral properties of free base porphyrins and iron porphyrin compounds were compared with each other. The experimental results showed that the one-pot mixed solvent method was superior to the two-step method in the yields, reaction time and workup of reaction mixtures for the synthesis of iron porphyrin compounds. The highest yields (28.7%-40.4% of RTPPFe(IIICl were obtained in the mixed solvents propionic acid, glacial acetic acid and m-nitrotoluene under reflux for 2 h. A detailed analysis of ultraviolet-visible (UV-vis, infrared (IR and far-infrared (FIR spectra suggested the transformation from free base porphyrins to iron porphyrins. The red shift of the Soret band in ultraviolet-visible spectra due to the presence of p-nitrophenyl substituents and the blue shift of Fe-Cl bond of TPPFeCl in far-infrared spectra were further explained by the electron transfer and molecular planarity in the porphyrin ring.

Synthesis, characterization and use of Ru-Fc intercalation complex as an electrochemical label for the detection of pathogen-DNA

International Nuclear Information System (INIS)

Díaz-Serrano, M; Rosado, A; Guadalupe, A R; Santana, D; Vega, E Z

2013-01-01

This report describes the synthesis of [Ru(Fe-Phen) 2 dppz](PF 6 ) 2 (Ru-Fe complex) for a label-free approach to detect DNA hybridization. The Ru-Fe complex showed oxidation signals at +608 mV and +1192 mV corresponding to the RuII/III and FeII/III centers, respectively. We used the Ru-Fe complex and the Ferrocene covalently attached to the target to monitor the hybridization event of a 70-mer oligo immobilized in 10.3KD NHS-PS-NHS. The lowest target detectable concentration for the DNA fragment was around 0.4 μM.

Synthesis and characterization of metal soaps of lanthanides (III)

International Nuclear Information System (INIS)

Payolla, Filipe Boccato; Ribeiro, Sidney Jose Lima; Massbni, Antonio Carlos

2015-01-01

The present study describes synthesis and partial characterization of Eu"3"+, Nd"3"+, Dy"3"+, Tb"3"+ and Yb"3"+ behenate complexes. The compounds were analyzed using IR-Spectroscopy, TG-DTG, DSC, elemental analysis, XRD, luminescence and SEM. The results show the purity of the compounds. The XRD analysis and the SEM images show the high crystallinity of the complexes. TG-DTG and DSC analyses do not show a liquid crystal behavior, as occurs with other lanthanide metallic soaps. The mass loses until 1000° C show that the compounds lose ligand fragments at specific temperatures. XRD of the residues are compatible with the respective lanthanide oxides. The luminescence analysis shows that the Eu"3"+, Nd"3"+ and Tb"3"+ complexes presents appreciable emission. The Judd-Ofelt parameters obtained are compatible with the values found in the literature. It was not possible to obtain the complexes in a glass-form because it is difficult to prevent the crystallization of the complexes even using liquid nitrogen. The XDR data indicate that one of the complexes axis has 52 Å of length, agreeing with a structure containing behenate-lanthanide ion-behenate. The structures of the complexes were not fully elucidated and more analyses are necessary. The complexes presented a molar ratio of 3:1 (L:M) and were formulated as Bh_3Eu, Bh_3Nd, Bh_3Dy, Bh_3Tb e Bh_3Yb (Bh = behenate anion). (author)

Synthesis, characterization and anticancer activities of two lanthanide(III) complexes with a nicotinohydrazone ligand

Science.gov (United States)

Xu, Zhou-Qin; Mao, Xian-Jie; Jia, Lei; Xu, Jun; Zhu, Tao-Feng; Cai, Hong-Xin; Bie, Hong-Yan; Chen, Ru-Hua; Ma, Tie-liang

2015-12-01

Two isostructural acylhydrazone based complexes, namely [Ce(penh)2(H2O)4](NO3)3·4H2O (1) and [Sm(penh)2(NO3)2](NO3)·C2H5OH (2) (penh = 2-acetylpyridine nicotinohydrazone), have been obtained and characterized by physico-chemical and spectroscopic methods. The ten-coordinated lanthanide metal ion in each complex is surrounded by two independent tridentate neutral acylhydrazones with two ON2 donor sets. The other four coordination oxygen atoms are from four water molecules and two bidentate nitrate anions for complexes 1 and 2, respectively, thus giving distorted bicapped square antiprism geometry. Both complexes have excellent antitumor activity towards human pancreatic cancer (PATU8988), human colorectal cancer (lovo) and human gastric cancer(SGC7901) cell line. Furthermore, the cell apoptosis of complex 1 is detected by AnnexinV/PI flow cytometry.

Photocatalytic semiconductors synthesis, characterization, and environmental applications

CERN Document Server

Hernández-Ramírez, Aracely

2014-01-01

This critical volume examines the different methods used for the synthesis of a great number of photocatalysts, including TiO2, ZnO and other modified semiconductors, as well as characterization techniques used for determining the optical, structural and morphological properties of the semiconducting materials. Additionally, the authors discuss photoelectrochemical methods for determining the light activity of the photocatalytic semiconductors by means of measurement of properties such as band gap energy, flat band potential and kinetics of hole and electron transfer. Photocatalytic Semiconductors: Synthesis, Characterization and Environmental Applications provide an overview of the semiconductor materials from first- to third-generation photocatalysts and their applications in wastewater treatment and water disinfection. The book further presents economic and toxicological aspects in the production and application of photocatalytic materials.

Synthesis, characterization, anti-microbial, DNA binding and cleavage studies of Schiff base metal complexes

Directory of Open Access Journals (Sweden)

Poomalai Jayaseelan

2016-09-01

Full Text Available A novel Schiff base ligand has been prepared by the condensation between butanedione monoxime with 3,3′-diaminobenzidine. The ligand and metal complexes have been characterized by elemental analysis, UV, IR, 1H NMR, conductivity measurements, EPR and magnetic studies. The molar conductance studies of Cu(II, Ni(II, Co(II and Mn(II complexes showed non-electrolyte in nature. The ligand acts as dibasic with two N4-tetradentate sites and can coordinate with two metal ions to form binuclear complexes. The spectroscopic data of metal complexes indicated that the metal ions are complexed with azomethine nitrogen and oxyimino nitrogen atoms. The binuclear metal complexes exhibit octahedral arrangements. DNA binding properties of copper(II metal complex have been investigated by electronic absorption spectroscopy. Results suggest that the copper(II complex bind to DNA via an intercalation binding mode. The nucleolytic cleavage activities of the ligand and their complexes were assayed on CT-DNA using gel electrophoresis in the presence and absence of H2O2. The ligand showed increased nuclease activity when administered as copper complex and copper(II complex behave as efficient chemical nucleases with hydrogen peroxide activation. The anti-microbial activities and thermal studies have also been studied. In anti-microbial activity all complexes showed good anti-microbial activity higher than ligand against gram positive, gram negative bacteria and fungi.

Synthesis, spectroscopic characterization, biological screenings, DNA binding study and POM analyses of transition metal carboxylates

Science.gov (United States)

Uddin, Noor; Sirajuddin, Muhammad; Uddin, Nizam; Tariq, Muhammad; Ullah, Hameed; Ali, Saqib; Tirmizi, Syed Ahmed; Khan, Abdur Rehman

2015-04-01

This article contains the synthesis of a novel carboxylic acid derivative, its transition metal complexes and evaluation of biological applications. Six carboxylate complexes of transition metals, Zn(II) and Hg(II), have been successfully synthesized and characterized by FT-IR and NMR (1H, 13C). The ligand, HL, (4-[(2,6-Diethylphenyl)amino]-4-oxobutanoic acid) was also characterized by single crystal X-ray analysis. The complexation occurs via oxygen atoms of the carboxylate moiety. FT-IR date show the bidentate nature of the carboxylate moiety of the ligand as the Δν value in all complexes is less than that of the free ligand. The ligand and its complexes were screened for antifungal and antileishmanial activities. The results showed that the ligand and its complexes are active with few exceptions. UV-visible spectroscopy and viscometry results reveal that the ligand and its complexes interact with the DNA via intercalative mode of interaction. A new and efficient strategy to identify the pharmacophores and anti-pharmacophores sites in carboxylate derivatives for the antibacterial/antifungal activity using Petra, Osiris and Molinspiration (POM) analyses was also carried out.

Synthesis and characterization of platinum(II) complexes with 2,2'-bipyridine derivative supporting ligands.

Science.gov (United States)

Yang, Kwang Woon; Hwang, Hey Eun; Jung, Hee Sun; Kwak, Chee Hun; Lee, Ji Hoon; Jung, Sang-Chul; Ahn, Ho Geun; Chung, Min Chul

2011-08-01

The reaction of the [Pt(bpy-R)Cl2](bpy-R: R=H (2,2'-bipyridine); R=CH3 (4,4'-dimethyl-2,2'-biypridine (DM-bpy), 3,3'-5,5'-tertamethyl-2,2'-bipyridiyl (TM-bpy)) with 1,4-Bis(5'-2',2"-bipyridine)benzene (bpy-Ph-bpy) affords the following mono- and di-platinum complexes of [(bpy)Pt(bpy-Ph-bpy)][PF6]2 (1), [(bpy)Pt(bpy-Ph-bpy)Pt(bpy)])[PF6]4 (2), [(DM-bpy)Pt(bpy-Ph-bpy)])][PF6]2 (3), and [(TM-bpy)Pt(bpy-ph-bpy)[PF6]2 (4), respectively. These complexes were characterized by NMR, IR, UV/VIS, PL and cyclic voltammetry. The internal quantum yields of these platinum(II) complexes are very high (0.83-0.99) and these complexes emit light at deep blue regions (373-417 nm). The redox behavior of complexes 1 and 2 shows quasi-reversible process.

Combinatorial Strategies for Synthesis and Characterization of Alloy Microstructures over Large Compositional Ranges.

Science.gov (United States)

Li, Yanglin; Jensen, Katharine E; Liu, Yanhui; Liu, Jingbei; Gong, Pan; Scanley, B Ellen; Broadbridge, Christine C; Schroers, Jan

2016-10-10

The exploration of new alloys with desirable properties has been a long-standing challenge in materials science because of the complex relationship between composition and microstructure. In this Research Article, we demonstrate a combinatorial strategy for the exploration of composition dependence of microstructure. This strategy is comprised of alloy library synthesis followed by high-throughput microstructure characterization. As an example, we synthesized a ternary Au-Cu-Si composition library containing over 1000 individual alloys using combinatorial sputtering. We subsequently melted and resolidified the entire library at controlled cooling rates. We used scanning optical microscopy and X-ray diffraction mapping to explore trends in phase formation and microstructural length scale with composition across the library. The integration of combinatorial synthesis with parallelizable analysis methods provides a efficient method for examining vast compositional ranges. The availability of microstructures from this vast composition space not only facilitates design of new alloys by controlling effects of composition on phase selection, phase sequence, length scale, and overall morphology, but also will be instrumental in understanding the complex process of microstructure formation in alloys.

A new myocardial imaging agent: Synthesis, characterization, and biodistribution of gallium-68-BAT-TECH

International Nuclear Information System (INIS)

Kung, H.F.; Liu, B.L.; Mankoff, D.; Kung, M.P.; Billings, J.J.; Francesconi, L.; Alavi, A.

1990-01-01

In order to develop a new myocardial perfusion agent for positron emission tomography (PET), a new lipid-soluble gallium complex was evaluated. Synthesis, radiolabeling, characterization, and biodistribution of a unique gallium complex, [ 67 Ga]BAT-TECH (bis-aminoethanethiol-tetraethyl-cyclohexyl), are described. The complex formation between Ga+3 and BAT-TECH ligand is simple, rapid, and of high yield (greater than or equal to 95%). This process is amenable to kit formulation. The complex has a net charge of +1 and a Ga/ligand ratio of 1:1. Biodistribution in rats shows high uptake in the heart as well as in the liver. When [ 68 Ga] BAT-TECH was injected into a monkey, the heart and liver are clearly delineated by PET imaging, suggesting that this complex may be a possible tracer for myocardial perfusion imaging

Synthesis, Spectroscopic and DFT Characterization of 4â-(4-tert ...

African Journals Online (AJOL)

In this work the synthesis, spectral characterization and non-linear optical properties of metal-free .... following literature methods23–26 The advantage of this method ..... Synthesis of phthalocyanine conjugates with gold nanoparticles and.

Synthesis and characterization of magnetite nanoparticles encapsulated in a bovine hemoglobin microgel

Science.gov (United States)

Mody, Puja J.

This study shows the successful synthesis and characterization of a novel material that is composed of iron oxide particles within a protein gel. During the synthesis, bovine hemoglobin surrounds the forming Fe 3O4 nanoparticles, resulting in a biocompatible hydrogel, which has the potential to be used as a targeted drug delivery vehicle and as an MRI contrast agent. The structure, size, and thermal stability of these hydrogel complexes were analyzed using a range of techniques. Powder x-ray diffraction and infrared spectroscopy indicated the presence of Fe3O 4 and hemoglobin without significant interactions between particles in the solid state. Microscopy analysis determined the average size of these microgel complexes to be 4-9 mum2 in area (˜2-3 mum in diameter), and DSC analysis indicated that none of the microgels exhibited a denaturing or unfolding transition below 54°C regardless of the iron: hemoglobin ratio. Initial testing has been performed on the ability of these materials to act as magnetically activated drug delivery vehicles. Other pertinent tests (for magnetic properties and MRI applicability) are currently proceeding at external labs.

The Synthesis and Characterization of Gold-Core/LDH-Shell Nanoparticles

Science.gov (United States)

Rearick, Colton

In recent years, the field of nanomedicine has progressed at an astonishing rate, particularly with respect to applications in cancer treatment and molecular imaging. Although organic systems have been the frontrunners, inorganic systems have also begun to show promise, especially those based upon silica and magnetic nanoparticles (NPs). Many of these systems are being designed for simultaneous therapeutic and diagnostic capabilities, thus coining the term, theranostics. A unique class of inorganic systems that shows great promise as theranostics is that of layered double hydroxides (LDH). By synthesis of a core/shell structures, e.g. a gold nanoparticle (NP) core and LDH shell, the multifunctional theranostic may be developed without a drastic increase in the structural complexity. To demonstrate initial proof-of-concept of a potential (inorganic) theranostic platform, a Au-core/LDH-shell nanovector has been synthesized and characterized. The LDH shell was heterogeneously nucleated and grown on the surface of silica coated gold NPs via a coprecipitation method. Polyethylene glycol (PEG) was introduced in the initial synthesis steps to improve crystallinity and colloidal stability. Additionally, during synthesis, fluorescein isothiocyanate (FITC) was intercalated into the interlayer spacing of the LDH. In contrast to the PEG stabilization, a post synthesis citric acid treatment was used as a method to control the size and short-term stability. The heterogeneous core-shell system was characterized with scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX), dynamic light scattering (DLS), and powder x-ray diffraction (PXRD). A preliminary in vitro study carried out with the assistance of Dr. Kaushal Rege's group at Arizona State University was to demonstrate the endocytosis capability of homogeneously-grown LDH NPs. The DLS measurements of the core-shell NPs indicated an average particle size of 212nm. The PXRD analysis showed that PEG

Ruthenium(III) Complexes of Heterocyclic Tridentate (ONN) Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

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Ejidike, Ikechukwu P.; Ajibade, Peter A.

2016-01-01

The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III) complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(L)Cl2(H2O)] (where L = tridentate NNO ligands). The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III) compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH) and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radicals, with DPPH scavenging capability in the order: [(PAEBOD)RuCl2] > [(BZEBOD)RuCl2] > [(MOABOD)RuCl2] > [Vit. C] > [rutin] > [(METBOD)RuCl2], and ABTS radical in the order: [(PAEBOD)RuCl2] < [(MOABOD)RuCl2] < [(BZEBOD)RuCl2] < [(METBOD)RuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10), melanoma cancer cell (UACC-62) and breast cancer cell (MCF-7) by SRB assay. PMID:26742030

Ruthenium(III Complexes of Heterocyclic Tridentate (ONN Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

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Ikechukwu P. Ejidike

2016-01-01

Full Text Available The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(LCl2(H2O] (where L = tridentate NNO ligands. The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS radicals, with DPPH scavenging capability in the order: [(PAEBODRuCl2] > [(BZEBODRuCl2] > [(MOABODRuCl2] > [Vit. C] > [rutin] > [(METBODRuCl2], and ABTS radical in the order: [(PAEBODRuCl2] < [(MOABODRuCl2] < [(BZEBODRuCl2] < [(METBODRuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10, melanoma cancer cell (UACC-62 and breast cancer cell (MCF-7 by SRB assay.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

Science.gov (United States)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

Spectroscopic characterization of metal complexes of novel Schiff base. Synthesis, thermal and biological activity studies

Science.gov (United States)

Omar, M. M.; Mohamed, Gehad G.; Ibrahim, Amr A.

2009-07-01

Novel Schiff base (HL) ligand is prepared via condensation of 4-aminoantipyrine and 2-aminobenzoic acid. The ligand is characterized based on elemental analysis, mass, IR and 1H NMR spectra. Metal complexes are reported and characterized based on elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance and thermal analyses (TGA, DrTGA and DTA). The molar conductance data reveal that all the metal chelates are non-electrolytes. IR spectra show that HL is coordinated to the metal ions in a uninegatively tridentate manner with NNO donor sites of the azomethine N, amino N and deprotonated caroxylic-O. From the magnetic and solid reflectance spectra, it is found that the geometrical structures of these complexes are octahedral. The thermal behaviour of these chelates shows that the hydrated complexes losses water molecules of hydration in the first step followed immediately by decomposition of the anions and ligand molecules in the subsequent steps. The activation thermodynamic parameters, such as, E*, ΔH*, ΔS* and ΔG* are calculated from the DrTG curves using Coats-Redfern method. The synthesized ligands, in comparison to their metal complexes also were screened for their antibacterial activity against bacterial species, Escherichia Coli, Pseudomonas aeruginosa, Staphylococcus Pyogones and Fungi (Candida). The activity data show that the metal complexes to be more potent/antibacterial than the parent Shciff base ligand against one or more bacterial species.

Synthesis, photophysical and electrochemical characterization of terpyridine-functionalized dendritic oligothiophenes and their Ru(II complexes

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Amaresh Mishra

2013-05-01

Full Text Available Pd-catalyzed Sonogashira cross-coupling reactions were used to synthesize novel π-conjugated oligothienylene-ethynylene dendrons and their corresponding terpyridine-based ligands. Their complexation with Ru(II led to interesting novel metallodendrimers with rich spectroscopic properties. All new compounds were fully characterized by 1H and 13C NMR, as well as MALDI–TOF mass spectra. Density functional theory (DFT calculations performed on these complexes gave more insight into the molecular orbital distributions. Photophysical and electrochemical studies were carried out in order to elucidate structure–property relationships and the effect of the dendritic structure on the metal complexes. Photophysical studies of the complexes revealed broad absorption spectra covering from 250 to 600 nm and high molar extinction coefficients. The MLCT emission of these complexes were significantly red-shifted (up to 115 nm compared to the parent [Ru(tpy2]2+ complex.

Chromium(III) Complex Obtained from Dipicolinic Acid: Synthesis, Characterization, X-Ray Crystal Structure and Electrochemical Studies

Energy Technology Data Exchange (ETDEWEB)

Ghasemi, Khaled; Rezvani, Ali Reza; Ghasemi, Fatemeh [Univ. of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of); Razak, Ibrahim Abdul; Rosli, Mohd Mustaqim [Universiti Sains Malaysia, Penang (Malaysia)

2013-10-15

The synthesis, X-ray crystallography, spectroscopic (IR, UV-vis), and electrochemical properties of the title compound, [H{sub 3}O][Cr(dipic){sub 2}] [H{sub 3}O{sup +}.Cl{sup -}] (1), (H{sub 2}dipic = 2,6-pyridinedicarboxylic acid), are reported. This complex crystallizes in the monoclinic space group Cc with a = 14.9006(10) A, b = 12.2114(8) A, c = 8.6337(6) A, α = 90.00 .deg., β = 92.7460(10) .deg., γ = 90.00 .deg., and V = 1569.16(18) A3 with Z = 4. The hydrogen bonding and noncovalent interactions play roles in the stabilization of the structure. In order to gain a better understanding of the most important geometrical parameters in the structure of the complex, atoms in molecules (AIM) method at B3LYP/6-31G level of theory has been employed.

Synthesis, characterization and thermal behavior of antibacterial and antifungal active zinc complexes of bis (3(4-dimethylaminophenyl)-allylidene-1,2-diaminoethane

Energy Technology Data Exchange (ETDEWEB)

Montazerozohori, Morteza, E-mail: mmzohori@mail.yu.ac.ir [Department of Chemistry, Yasouj University, Yasouj 75918-74831 (Iran, Islamic Republic of); Zahedi, Saeedeh [Department of Chemistry, Yasouj University, Yasouj 75918-74831 (Iran, Islamic Republic of); Naghiha, Asghar [Department of Animal Sciences, Faculty of Agriculture, Yasouj University, Yasouj (Iran, Islamic Republic of); Zohour, Mostafa Montazer [Genetics of Non-Communicable Disease Research Center, Zahedan University of Medical Sciences, Zahedan (Iran, Islamic Republic of)

2014-02-01

In this work, synthesis of a new series of zinc halide/pseudohalide complexes of a bidentate Schiff base ligand entitled as bis (3-(4-dimethylaminophenyl)-allylidene)-1,2-diaminoethane(L) is described. The ligand and its zinc complexes were characterized by various techniques such as elemental analysis, FT-IR, UV–visible, {sup 1}H and {sup 13}C NMR spectra, cyclic voltammetry, and conductometry. Accordingly ZnLX{sub 2} (X = Cl{sup −}, Br{sup −}, I{sup −}, SCN{sup −} and N{sub 3}{sup −}) was suggested as molecular formula of the complexes. Redox behaviors of ligand and its zinc complexes were investigated by cyclic voltammetry method. Furthermore, the ligand and its zinc halide/pseudohalide complexes were tested for their in vitro antibacterial activities against two gram positive bacteria (Staphylococcus aureus and Bacillus subtilis) and two gram negative bacteria (Escherichia coli and Pseudomonas aeruginosa). Also in vitro antifungal activities of them against Candida albicans and Aspergillus niger were investigated. The results indicated that all compounds are antibacterial and antifungal active. Thermal behaviors of ligand and its zinc complexes were studied from room temperature to 1100 °C under argon atmosphere. It was found that the ligand and zinc iodide are decomposed completely via three and four steps respectively while other zinc complexes leave out the metal or organometallic compounds as final residuals after 3–4 decomposition steps at above temperature range. Moreover evaluation of some thermo-kinetic parameters such as activation energy (∆E{sup ⁎}), enthalpy (∆H{sup ⁎}), entropy (∆S{sup ⁎}) and Gibbs free energy change (∆G{sup ⁎}) of the thermal decomposition steps were performed based on the Coats–Redfern relation. - Highlights: • Some novel complexes of Zn(II) with a bidentate Schiff base ligand have been synthesized. • Redox behavior of ligand and zinc complexes was investigated by cyclic voltammetry. • The

Synthesis and Reactivity of Tripodal Complexes Containing Pendant Bases

Energy Technology Data Exchange (ETDEWEB)

Blacquiere, Johanna M.; Pegis, Michael L.; Raugei, Simone; Kaminsky, Werner; Forget, Amelie; Cook, Sarah; Taguchi, Taketo; Borovik, Andrew S.; Mayer, James M.

2014-09-02

The synthesis of a new tripodal ligand family is reported, with tertiary-amine groups in the second-coordination sphere. The ligands are tris(amido)amine derivatives, with the pendant amines attached via a peptide coupling strategy. They were designed to be used in new catalysts for the oxygen reduction reaction (ORR), in which the pendant acid/base group could improve catalyst performance. Two members of the new ligand family were each metallated with Co(II) and Zn(II) to afford trigonal monopyramidal complexes. Reaction of the cobalt complexes, [Co(L)]-, with dioxygen reversibly generates a small amount of a Co(III)-superoxo species, which was characterized by EPR. Protonation of the zinc complex Zn[N{CH2CH2NC(O)CH2N(CH2Ph)2}3)-– ([Zn(TNBn)]-) with one equivalent of acid occurs with displacement and dissociation of an amide ligand. Addition of excess acid to the any of the complexes [M(L)]- results in complete proteolysis and formation of the ligands H3L. This decomposition limits the use of these complexes as catalysts for the ORR. An alternative ligand with two pyridyl arms was also prepared but could not be metallated. These studies highlight the importance of stability of the primary-coordination sphere of ORR electrocatalysts to both oxidative and acidic conditions. This research was supported as part of the Center for Molecular Electrocatalysis, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences.

Synthesis and spectral properties of europium phthalocyanine complexes

International Nuclear Information System (INIS)

Maksimova, K.N.; Bazyakina, N.L.; Kutyreva, V.V.; Suvorova, O.N.; Domrachev, G.A.

2008-01-01

Synthesis of europium monophthalocyanic complexes with thenoyltrifluroacetonate (tta) and ferrocenoyltrifluoroacetate (fta) ligands has been considered. Spectral characteristics of complexes PcEu(tta)(ttaH) and PcEu(fta)(ftaH) (Pc - phthalocyanine ligand) have been investigated. One of β-diketonate ligand is proposed to bind with europium ion covalently, and the second ligand saturates coordination sphere of europium due to donor-acceptor binding [ru

Synthesis, physico-chemical characterization and biological activity of 2-aminobenzimidazole complexes with different metal ions

Directory of Open Access Journals (Sweden)

Podunavac-Kuzmanović Sanja O.

2004-01-01

Full Text Available Complexes of 2-aminobenzimidazole (L with nitrates of cobalt(II nickel(II, copper (II, zinc(II and silver(I were synthesized. The molar ratio metal:ligand in the reaction of the complex formation was 1:2. It should be noticed, that the reaction of all the metal salts yielded bis(ligand complexes of the general formula M(L2(NO32 × nH2O (M=Co, Ni Cu, Zn or Ag; n=0, 1, 2 or 6. The complexes were characterized by elemental analysis of the metal, molar conductivity, magnetic susceptibility measurements and IR spectra. Co(II, Ni(II and Cu(II complexes behave as non-electrolytes, whilst Zn(II and Ag(I are 1:1 electrolytes. Cu(II complex has a square-planar stereochemistry, Ag(I complex is linear, whilst the Co(II, Ni(II and Zn(II complexes have a tetrahedral configuration. In all the complexes ligand is coordinated by participation of the pyridine nitrogen of the benzimidazole ring. The antimicrobial activity of the ligand and its complexes against Pseudomonas aeruginosa, Bacillus sp. Staphylococcus aureus and Saccharomyces cerevisiae was investigated. The effect of metal on the ligand antimicrobial activity is discussed.

Oligocyclopentadienyl transition metal complexes

Energy Technology Data Exchange (ETDEWEB)

de Azevedo, Cristina G.; Vollhardt, K. Peter C.

2002-01-18

Synthesis, characterization, and reactivity studies of oligocyclopentadienyl transition metal complexes, namely those of fulvalene, tercyclopentadienyl, quatercyclopentadienyl, and pentacyclopentadienyl(cyclopentadienyl) are the subject of this account. Thermal-, photo-, and redox chemistries of homo- and heteropolynuclear complexes are described.

Synthesis and characterization of magnetite nanoparticles coated with lauric acid

Energy Technology Data Exchange (ETDEWEB)

Mamani, J.B., E-mail: javierbm@einstein.br [Instituto do Cérebro-InCe, Hospital Israelita Albert Einstein-HIAE, 05651-901 São Paulo (Brazil); Costa-Filho, A.J. [Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto (Brazil); Cornejo, D.R. [Instituto de Física Universidade de São Paulo, USP, São Paulo (Brazil); Vieira, E.D. [Instituto de Física, Universidade Federal de Goiás, Goiânia (Brazil); Gamarra, L.F. [Instituto do Cérebro-InCe, Hospital Israelita Albert Einstein-HIAE, 05651-901 São Paulo (Brazil)

2013-07-15

Understanding the process of synthesis of magnetic nanoparticles is important for its implementation in in vitro and in vivo studies. In this work we report the synthesis of magnetic nanoparticles made from ferrous oxide through coprecipitation chemical process. The nanostructured material was coated with lauric acid and dispersed in aqueous medium containing surfactant that yielded a stable colloidal suspension. The characterization of magnetic nanoparticles with distinct physico-chemical configurations is fundamental for biomedical applications. Therefore magnetic nanoparticles were characterized in terms of their morphology by means of TEM and DLS, which showed a polydispersed set of spherical nanoparticles (average diameter of ca. 9 nm) as a result of the protocol. The structural properties were characterized by using X-ray diffraction (XRD). XRD pattern showed the presence of peaks corresponding to the spinel phase of magnetite (Fe{sub 3}O{sub 4}). The relaxivities r{sub 2} and r{sub 2}* values were determined from the transverse relaxation times T{sub 2} and T{sub 2}* at 3 T. Magnetic characterization was performed using SQUID and FMR, which evidenced the superparamagnetic properties of the nanoparticles. Thermal characterization using DSC showed exothermic events associated with the oxidation of magnetite to maghemite. - Highlights: • Synthesis of magnetic nanoparticles coated with lauric acid • Characterization of magnetic nanoparticles • Morphological, structural, magnetic, calorimetric and relaxometric characterization.

Synthesis and characterization of rare-earth-doped calcium tungstate nanocrystals

Science.gov (United States)

Suneeta, P.; Rajesh, Ch.; Ramana, M. V.

2018-02-01

In this paper, we report synthesis and characterization of rare-earth-ion-doped calcium tungstate (CaWO4) nanocrystals (NCs). Rare-earth ions, such as gadolinium (Gd), neodymium (Nd), praseodymium (Pr), samarium (Sm) and holmium (Ho), were successfully doped in the CaWO4 NCs by changing the synthesis conditions. The adopted synthesis route was found to be fast and eco-friendly. Structural characterizations, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and compositional analysis, were performed using energy dispersive analysis of X-rays (EDAX) on as-synthesized NCs. The results indicate the size of the NCs ranging between 47 to 68nm and incorporation of rare-earth ions in CaWO4 NCs.

Synthesis and Identification of the Organic Reagent Ereochrom Black T and its Complex with Cobalt (lll

Directory of Open Access Journals (Sweden)

Jassem M. Abd Al Hassein

2017-02-01

Full Text Available The ligand 1–(4–Hydroxy –3–Naphthalene Azo–4–Nitro–8–Hydroxy–6–Sulfonic Naphthalene Acid Sodium Salt was synthesized (by the reaction between 3–amino–4– hydroxyl naphthalene and 3 – nitro – 7 – hydroxyl –5– sulfonic naphthalene acid sodium salt and characterized by FTIR technique, its ionization constants (PKs were determined. Synthesis and spectroscopic investigations of its complex with Co (III in aqueous solution revealed the sole formation of (1: 2 (metal: ligand complex. Specral and magnatic studies of the isolated complex indicates octahedral coordination via the N atoms of the azo groups and the O atoms of the hydroxyl groups. The molar conductivity of the complex was determined in an alcoholic solutions indicates that the complex has high molar conductivity. The magnetic properties were determined by using Gouy balance which indicates diamagnetic complex.

Synthesis and structural characterization of dioxomolybdenum and dioxotungsten hydroxamato complexes and their function in the protection of radiation induced DNA damage.

Science.gov (United States)

Paul, Shiv Shankar; Selim, Md; Saha, Abhijit; Mukherjea, Kalyan K

2014-02-21

The synthesis and structural characterization of two novel dioxomolybdenum(VI) (1) and dioxotungsten(VI) (2) complexes with 2-phenylacetylhydroxamic acid (PAHH) [M(O)2(PAH)2] [M = Mo, W] have been accomplished. The dioxomolybdenum(VI) and dioxotungsten(VI) moiety is coordinated by the hydroxamate group (-CONHO(-)) of the 2-phenylacetylhydroxamate (PAH) ligand in a bi-dentate fashion. In both the complexes the PAHH ligand is coordinated through oxygen atoms forming a five membered chelate. The hydrogen atom of N-H of the hydroxamate group is engaged in intermolecular H-bonding with the carbonyl oxygen of another coordinated hydroxamate ligand, thereby forming an extended 1D chain. The ligand as well as both the complexes exhibit the ability to protect from radiation induced damage both in CTDNA as well as in pUC19 plasmid DNA. As the damage to DNA is caused by the radicals generated during radiolysis, its scavenging imparts protection from the damage to DNA. To understand the mechanism of protection, binding affinities of the ligand and the complex with DNA were determined using absorption and emission spectral studies and viscosity measurements, whereby the results indicate that both the complexes and the hydroxamate ligand interact with calf thymus DNA in the minor groove. The intrinsic binding constants, obtained from UV-vis studies, are 7.2 × 10(3) M(-1), 5.2 × 10(4) M(-1) and 1.2 × 10(4) M(-1) for the ligand and complexes 1 and 2 respectively. The Stern-Volmer quenching constants obtained from a luminescence study for both the complexes are 5.6 × 10(4) M(-1) and 1.6 × 10(4) M(-1) respectively. The dioxomolybdenum(VI) complex is found to be a more potent radioprotector compared to the dioxotungsten(VI) complex and the ligand. Radical scavenging chemical studies suggest that the complexes have a greater ability to scavenge both the hydroxyl as well as the superoxide radicals compared to the ligand. The free radical scavenging ability of the ligand and the

Synthesis, characterization and reactivity of nitrite and nitrosyl derivates of phosphane complexes of tetraamminrethenium (II)

International Nuclear Information System (INIS)

Souza Santos, L. de.

1988-01-01

The substitution reaction: trans-[Ru(NH 3 ) 4 P(III) (H 2 O)] 2+ + NO - 2 K 1 K -1 trans-[Ru(NH 3 ) 4 P(III) (NO 2 ) + + H 2 O. The reaction product has been isolated as trans-[Ru(NH 3 ) 4 P(III) (NO 2 )] (PF 6 ) and characterized by using electronic and infrared spectroscopies and cyclic voltammetry, microanalysis and conductometry techniques. This nitrite complex can be converted into the nitrosyl complex in solution by adding H + , according to: trans-[Ru(NH 3 ) 4 P(III) (NO 2 )] + + 2H + →sup (K)1 trans-[Ru(NH 3 ) 4 P(III) (NO)] 3+ + H 2 O which can be converted back to the nitrite derivative by adding alkali: trans-[Ru(NH 3 ) 4 P(III) (NO)] 3+ + 2 OH - →sup (K)-1 trans-[Ru(NH 3 ) 4 P(III) (NO 2 )] + + H 2 O. The nitrosyl complexes have been synthesized by reaction of NO with trans-[Ru(NH 3 ) 4 P(III) ( 2 O)] 2+ or by reacting the nitrite derivative in acidic solutions, and characterized by eletronic and infrared spetroscopies, cyclic voltametry, microanalysis, eletron paramagnetic resonance (E.P.R.) and nuclear magnetic resonance (N.M.R.) techniques. E.P.R. and N.M.R. data suggest that these complexes are diamagnetic and better formulated as Ru(II)-NO + . (author) [pt

Synthesis of nanosilver on polyamide fabric using silver/ammonia complex

Energy Technology Data Exchange (ETDEWEB)

Montazer, Majid, E-mail: tex5mm@aut.ac.ir [Textile Department, Functional Fibrous Structures and Environmental Enhancement (FFSEE), Amirkabir University of Technology, Hafez Avenue, Tehran (Iran, Islamic Republic of); Shamei, Ali; Alimohammadi, Farbod [Young Researchers Club, Tehran South Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of)

2014-05-01

In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH{sub 3}){sub 2}]{sup +}. The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV–vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. - Highlights: • Novel in situ synthesis of nanosilver on polyamide 6 • Synthesis of nanosilver without using external stabilizing and reducing agent • Synthesis of nanosilver particles within molecular chains of polyamide 6 • Producing antibacterial polyamide 6 using 35 mg/L Ag/ammonia complex • Obtaining durable antibacterial properties on polyamide 6 by this method.

Synthesis of nanosilver on polyamide fabric using silver/ammonia complex

International Nuclear Information System (INIS)

Montazer, Majid; Shamei, Ali; Alimohammadi, Farbod

2014-01-01

In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH 3 ) 2 ] + . The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV–vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. - Highlights: • Novel in situ synthesis of nanosilver on polyamide 6 • Synthesis of nanosilver without using external stabilizing and reducing agent • Synthesis of nanosilver particles within molecular chains of polyamide 6 • Producing antibacterial polyamide 6 using 35 mg/L Ag/ammonia complex • Obtaining durable antibacterial properties on polyamide 6 by this method

Synthesis and Characterization of Organ Tin (IV) Complexes ...

African Journals Online (AJOL)

User

2012-08-21

Aug 21, 2012 ... the reference drug. In addition, within the diorganotin(IV) complexes, monomeric type (3) exhibited a slightly better activity as compared to the organodistannoxane dimer types (1 and 4). Key words: Preliminary in vitro cytotoxic assay, organotin(IV) complexes, comparison study. INTRODUCTION. Although ...

Synthesis and characterization of oxovanadium (IV) dithiocarbamates with pyridine

Energy Technology Data Exchange (ETDEWEB)

Doadrio, Antonio L.; Sotelo, Jose; Fernandez-Ruano, Ana [Universidad Complutense, Madrid (Spain). Facultad de Farmacia. Dept. de Quimica Inorganica y Bioinorganica]. E-mail: antoniov@farm.ucm.es

2002-07-01

We report the synthesis and study of a new series of oxovanadium (IV) dithiocarbamate adducts and derivatives with pyridine and cyclohexyl, di-iso-butyl, di-n-propyl, aniline, morpholine, piperidine and di-iso-propyl amines. The complexes have been characterized by analytical, magneto chemical, IR, visible-UV spectral and thermal studies, and are assigned the formulas [VO(L){sub 2}].py, where L=cyclohexyl, di-iso-butyl, di-n-propyl, aniline dithiocarbamate and [VO(OH)(L)(py){sub 2}] OH.H{sub 2}O (L=morpholine, piperidine and di-iso-propyl dithiocarbamate). The effect of the adduct formation on the p{sub V=0} bound is discussed in terms of the IR (V=O, V-S and V-N stretching frequencies) and electronic spectra (d-d transitions). (author)

Synthesis, characterization and properties of novel amide derivatives based open-chain crown ether and their Tb (III) complexes

International Nuclear Information System (INIS)

Liu, Yanhong; He, Wei; Yang, Zehui; Chen, Yanwen; Wang, Xinwei; Guo, Dongcai

2015-01-01

Six amide-based open-chain crown ether and their solid complexes with terbium nitrates were synthesized. The target complexes were characterized by elemental analysis, mass spectra, EDTA titrimetric analysis, thermal analysis, molar conductivity, infrared spectra and UV–vis spectra. Luminescence properties of the ligands and the corresponding complexes in solid were studied. The results showed that the introduction of electron-donating group to the ligand enhanced the luminescence intensity of the corresponding complex, but electron-withdrawing group conversely. Meanwhile, among all complexes, the luminescence quantum yield of the complex Tb(NO 3 ) 3 Y 1 was highest up to 0.76. Electrochemical properties were also investigated, and the results showed that the introduction of electron-donating group to the ligand enhanced the highest occupied molecular orbit (HOMO) and the lowest unoccupied molecular orbit (LUMO) energy level, but electron-withdrawing group conversely. And these target complexes may possibly be useful for studying in organic light-emitting devices field. - Highlights: • Novel amide derivatives based open-chain crown ether and their Tb (III) complexes were prepared and characterized. • The target complexes presented high thermodynamic stability. • Influence of the substituent on luminescence intensity and electrochemical property were discussed

Novel polymer anchored Cr(III) Schiff base complexes: Synthesis, characterization and antimicrobial properties

Science.gov (United States)

Selvi, Canan; Nartop, Dilek

2012-09-01

New polymer-bound Schiff bases and Cr(III) complexes have been synthesized by the reaction of 4-benzyloxybenzaldehyde, polymer-bound with 2-aminophenol, 2-amino-4-chlorophenol and 2-amino-4-methylphenol. The structure of polymeric-Schiff bases and their Cr(III) complexes have been characterized by elemental analyses, magnetic measurements, IR, UV-Vis, TG-DTA and 1H-NMR. All these compounds have also been investigated for antibacterial activity by the well-diffusion method against Staphylococcus aureus (RSKK-07035), Shigella dysenteria type 10 (RSKK 1036), Listeria monocytogenes 4b(ATCC 19115, Escherichia coli (ATCC 1230), Salmonella typhi H (NCTC 901.8394), Staphylococcus epidermis (ATCC 12228), Brucella abortus (RSKK-03026), Micrococcs luteus (ATCC 93419, Bacillus cereus sp., Pseudomonas putida sp. and for antifungal activity against Candida albicans (Y-1200-NIH).

Charge transfer complex between 2,3-diaminopyridine with chloranilic acid. Synthesis, characterization and DFT, TD-DFT computational studies

Science.gov (United States)

Al-Ahmary, Khairia M.; Habeeb, Moustafa M.; Al-Obidan, Areej H.

2018-05-01

New charge transfer complex (CTC) between the electron donor 2,3-diaminopyridine (DAP) with the electron acceptor chloranilic (CLA) acid has been synthesized and characterized experimentally and theoretically using a variety of physicochemical techniques. The experimental work included the use of elemental analysis, UV-vis, IR and 1H NMR studies to characterize the complex. Electronic spectra have been carried out in different hydrogen bonded solvents, methanol (MeOH), acetonitrile (AN) and 1:1 mixture from AN-MeOH. The molecular composition of the complex was identified to be 1:1 from Jobs and molar ratio methods. The stability constant was determined using minimum-maximum absorbances method where it recorded high values confirming the high stability of the formed complex. The solid complex was prepared and characterized by elemental analysis that confirmed its formation in 1:1 stoichiometric ratio. Both IR and NMR studies asserted the existence of proton and charge transfers in the formed complex. For supporting the experimental results, DFT computations were carried out using B3LYP/6-31G(d,p) method to compute the optimized structures of the reactants and complex, their geometrical parameters, reactivity parameters, molecular electrostatic potential map and frontier molecular orbitals. The analysis of DFT results strongly confirmed the high stability of the formed complex based on existing charge transfer beside proton transfer hydrogen bonding concordant with experimental results. The origin of electronic spectra was analyzed using TD-DFT method where the observed λmax are strongly consisted with the computed ones. TD-DFT showed the contributed states for various electronic transitions.

Functionalized cyclopentadienyl rhodium(III) bipyridine complexes: synthesis, characterization, and catalytic application in hydrogenation of ketones.

Science.gov (United States)

Wang, Wan-Hui; Suna, Yuki; Himeda, Yuichiro; Muckerman, James T; Fujita, Etsuko

2013-07-14

A series of highly functionalized cyclopentadienyl rhodium(III) complexes, [Cp'Rh(bpy)Br](ClO4) (Cp' = substituted cyclopentadienyl), was synthesized from various multi-substituted cyclopentadienes (Cp'H). [Rh(cod)Cl]2 and Cp'H were firstly converted to [Cp'Rh(cod)] complexes, which were then treated with Br2 to give the rhodium(III) dibromides [Cp'RhBr2]2. The novel complexes [Cp'Rh(bpy)Br](ClO4) were obtained readily by the reaction of 2,2'-bipyridine with [Cp'RhBr2]2. These rhodium complexes [Cp'Rh(bpy)Br](ClO4) were fully characterized and utilized in the hydrogenation of cyclohexanone and acetophenone with generally high yields, but they did not exhibit the same reactivity trends for the two substrate ketones. The different activity of these complexes for the different substrates may be due to the influence of the substituents on the Cp' rings.

Tetracarboxylatodirhenium complexes linked by axial cyano bridges to metalpentacarbonyl ligands - synthesis and characterization

International Nuclear Information System (INIS)

Kuehn, F.E.; Wachter, W.; Goncalves, I.S.; Aveiro Univ.; Lopes, A.D.; Lopes, J.P.; Romao, C.C.; Mink, J.; Veszprem Univ.; Hajba, L.; Parola, A.J.; Pina, F.; Sotomayor, J.

1999-01-01

Reaction of Re 2 {μ-O 2 CC(CH 3 ) 3 } 4 Cl 2 with [(CO) 5 M-CN]Na (M=Cr, Mo, W) leads to tetranuclear complexes of formula Re 2 {μ-O 2 CC(CH 3 ) 3 } 4 [-NC-M(CO) 5 ] 2 (M=Cr, Mo, W). These complexes were characterized by 1 H-, 13 C-, and 95 Mo-NMR, IR and Raman spectroscopy, elemental analysis and examined by cyclic voltammetry. The applied methods show the donor capabilities of the [(CO) 5 M-CN] - ligands which shift electron density towards the Re centers weakening the Re-Re quadruple bond. The Re-Re bond lengths and the ν(Re-Re) force constants are estimated based on the FT-IR and Raman examinations. Photchemical examinations and TG/MS experiments have also been conducted. The latter method shows that the product complexes decompose around 100 C, but first loosing their carbonyl substituents; as do the Cr, Mo, W precursor compounds. The dirhenium tetrapivalate unit decomposes only at higher temperatures in a distinct second step. (orig.)

Ultrasound assisted synthesis, characterization and electrochemical study of a tetradentate oxovanadium diazomethine complex

Science.gov (United States)

Merzougui, Moufida; Ouari, Kamel; Weiss, Jean

2016-09-01

The oxovanadium (IV) complex ;VOL; of a tetradentate Schiff base ligand derived from the condensation of diaminoethane and 2-hydroxy-1-naphthaldehyde was efficiently prepared via ultrasound irradiation and the template effect of VO(acac)2. The resulting product was characterized by elemental analysis, infrared, electronic absorption and molar conductance measurement. Single X-ray structure analysis showed that the complex is a monomeric five-coordinate with a distorted square pyramidal geometry. It crystallizes in monoclinic system having unit cell parameters a = 8.3960 (5) Å; b = 12.5533 (8) Å and c = 18.7804 (11) Å; α = γ = 90°; β = 104.843°(2), with P 21/c space group. Cyclic voltammetry of the complex, carried out on a glassy carbon (GC) electrode in DMF, showed reversible cyclic voltammograms response in the potential range 0.15-0.60 V involving a single electron redox wave VV/VIV, the diffusion coefficient is determinedusing GC rotating disk electrode. The Levich plot Ilim = f(ω1/2), was used to calculate the diffusion-convection controlled currents.

Synthesis, Characterization and Thermal Studies of Co(II), Ni(II), Cu ...

African Journals Online (AJOL)

NICO

2010-06-15

Jun 15, 2010 ... metal complexes was confirmed by thermal and IR data of the complexes. KEY WORDS. Synthesis ..... signals deshielded in the spectra of metal complexes, suggests coordination of .... micro analysis data of the complexes.

Validation data supporting the characterization of novel copper complexes as anticancer agents

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Ceyda Acilan

2016-12-01

Full Text Available Three copper(II complexes, Cu(Sal-Gly(phen, Cu(Sal-Glypheamine, Cu(Sal-Glyphepoxy were synthesized and characterized for their anticancer properties and mechanism of action (Acilan et al., in press [1]. Here, we provide supporting data on colon cancer cell lines complementing our previous findings in cervix cells. This paper also contains a data table for the fold changes and p-values of all genes analyzed in this study via a custom RT-qPCR array. All compounds induced DNA damage (based on 8-oxo-guanidine, ɣH2AX staining in cells and apoptosis (based on elevated DNA condensation/fragmentation, Annexin V staining, caspase 3/7 activity and mitochondrial membrane depolarization in HCT-116 colon cancer cells. The increase in oxidative stress was also further confirmed in these cells. Further interpretation of the data presented here can be found in the article entitled “Synthesis, biological characterization and evaluation of molecular mechanisms of novel copper complexes as anticancer agents” (Acilan et al., in press [1].

Synthesis, characterization and biocidal activities of heterobimetallic complexes having tin(IV) as a padlock

Science.gov (United States)

Husain, Ahmad; Nami, Shahab A. A.; Siddiqi, K. S.

2010-04-01

A mononuclear precursor complex, [(CH 3) 2Sn(tpdtc)] and several of its heterobimetallic derivatives of the type, [(CH 3) 2Sn(tpdtc)]MCl 2 have been synthesized by the simple addition reaction of transition metal chlorides, MCl 2· nH 2O where tpdtc = tetraethylenepentamine bis(dithiocarbamate) anion, M = Fe(II), Co(II), Ni(II), Cu(II) and Zn(II). The synthesized complexes have been systematically characterized by the physicochemical and spectroscopic techniques. A square-pyramidal geometry has been proposed for all the transition metal atoms with chloride ions occupying the axial while the three nitrogen atoms occupying the equatorial positions. A symmetrical bidentate coordination has been observed for the dithiocarbamato moiety leading to the formation of 18 member cavity. The thermal studies reveal that the mononuclear complex decomposes in three stages while its heterobimetallic analog exhibits a simple two-stage profile. The conductivity measurement data (1 mmol solution) implies a non-electrolytic behavior for all the complexes as evident by their low conductivity values obtained at room temperature. The heterobimetallic complexes have also been tested against the bacterial ( Escherichia coli and Pseudomonas aeruginosa) and antifungal strains ( Aspergillus niger and Fusarium oxysporum). All the complexes were found to be active against the test organisms and maximum activity was found for [(CH 3) 2Sn(tpdtc)]CuCl 2 complex.

Synthesis, Characterization, and Variable-Temperature NMR Studies of Silver(I) Complexes for Selective Nitrene Transfer.

Science.gov (United States)

Huang, Minxue; Corbin, Joshua R; Dolan, Nicholas S; Fry, Charles G; Vinokur, Anastasiya I; Guzei, Ilia A; Schomaker, Jennifer M

2017-06-05

An array of silver complexes supported by nitrogen-donor ligands catalyze the transformation of C═C and C-H bonds to valuable C-N bonds via nitrene transfer. The ability to achieve high chemoselectivity and site selectivity in an amination event requires an understanding of both the solid- and solution-state behavior of these catalysts. X-ray structural characterizations were helpful in determining ligand features that promote the formation of monomeric versus dimeric complexes. Variable-temperature 1 H and DOSY NMR experiments were especially useful for understanding how the ligand identity influences the nuclearity, coordination number, and fluxional behavior of silver(I) complexes in solution. These insights are valuable for developing improved ligand designs.

Green synthesis, characterization and antibacterial activity of copper ...

African Journals Online (AJOL)

Green synthesis, characterization and antibacterial activity of copper nanoparticles using L -ascorbic ... Journal Home > Vol 10, No 3 (2017) > ... In this study, simple, economical, convenient and environmentally-friendly chemical reduction ...

Synthesis, Characterization and Applications in Catalysis of Polyoxometalate/Zeolite Composites

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Frédéric Lefebvre

2016-05-01

Full Text Available An overview of the synthesis, characterization and catalytic applications of polyoxometalates/zeolites composites is given. The solids obtained by direct synthesis of the polyoxometalate in the presence of the zeolite are first described with their applications in catalysis. Those obtained by a direct mixing of the two components are then reviewed. In all cases, special care is taken in the localization of the polyoxometalate, inside the zeolite crystal, in mesopores or at the external surface of the crystals, as deduced from the characterization methods.

Template synthesis, characterization and antimicrobial activity of some new complexes with isonicotinoyl hydrazone ligands

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LIVIU MITU

2009-09-01

Full Text Available Complexes of Cu(II, Ni(II, Co(II with the 9-anthraldehyde iso-nicotinoyl hydrazone ligand (HL1 and the 3,5-di-tert-butyl-4-hydroxy-benzaldehyde isonicotinoyl hydrazone ligand (H2L2 were synthesized by the template method. The complexes were characterized by analytical analysis, IR, UV-Vis and ESR spectroscopy, magnetic measurements, conductometry and thermal analysis and the two ligands by 1H-NMR spectroscopy. From the elemental analysis, 1:2 (metal:ligand stoichiometry for the complexes of Cu(II, Ni(II with the ligands HL1 and H2L2 and 1:1 (metal:ligand stoichiometry for the complex of Co(II with the ligand HL1 are proposed. The molar conductance data showed that the complexes are non-electrolytes. The magnetic susceptibility results coupled with the electronic and ESR spectra suggested a distorted octahedral geometry for the complexes Ni(II/HL1, Ni(II/H2L2 and Cu(II/H2L2, a tetrahedral stereochemistry for the complex Cu/HL1 and a square-planar geometry for the complex Co/HL1. The IR spectra demonstrated the bidentate coordination of the ligands HL1 and H2L2 by the O=C amide oxygen and the azomethine nitrogen, as well as monodentate coordination of the ligand HL1 by the azomethine nitrogen in the Cu(IIcomplex. The antibacterial activity of the ligands and their metallic complexes were tested against Staphylococcus aureus, Escherichia coli and Klebsiella pneumoniae.

Synthesis, characterization and sup 23 Na NMR shift studies of a novel dysprosium(III) crown ether texaphyrin

Energy Technology Data Exchange (ETDEWEB)

Sessler, J.L.; Mody, T.D. (Texas Univ., Austin, TX (United States). Dept. of Chemistry); Ramasamy, R.; Sherry, A.D. (Texas Univ., Dallas, TX (United States))

1992-05-01

The synthesis and characterization of a novel dysprosium(III) crown-ether texaphyrin (Dy(BCTxp)){sup 2+} is reported. This complex was designed to serve as a ditopic chelate for both dysprosium(III) and sodium cations. {sup 23}Sodium NMR spectroscopic studies indicates that titration of Na{sup +} with increasing concentrations of (Dy(BCTxp)){sup 2+} results in a shift toward higher frequency and gives a net hyperfine shift of 0.86 ppm. Sodium complexation is taking place into the crown subunit in (Dy(BCTxp)){sup 2+} and the degree of complexation is not reduced substantially by the positive charge on the dysprosium(III) portion of this binucleating system.

Synthesis and characterization of transition metal complexes derived from some biologically active furoic acid hydrazones

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P. Venkateswar Rao

2007-04-01

Full Text Available Two new physiologically active ligands, N’-2-[(E-1-hydroxy-4-methyl-2-oxo-2H-8-chromenyl ethylidene-2-furan carbohydrazide (HMCFCH and N’-2-[(Z-1-(4-hydroxy-6-methyl-2-oxo-2H-pyranyl ethylidene]-furan carbohydrazide (HMPFCH and their VO(II, Mn(II, Fe(II, Co(II, Ni(II and Cu(II complexes have been prepared. The ligands and the metal complexes have been characterized by elemental analyses, electrical conductance, magnetic susceptibility measurements, UV-Vis, IR, and ESR spectroscopic data. Basing on the above data, Fe(II and Co(II complexes of HMCFCH and HMPFCH have been assigned a dimeric octahedral geometry. VO(II complexes of HMCFCH and HMPFCH have been assigned sulfate bridged dimeric square pyramidal geometry. Mn(II complex of HMCFCH has been assigned a dimeric octahedral geometry, where as Mn(II complex of HMPFCH has been ascribed to monomeric octahedral geometry. Cu(II and Ni(II complexes of HMCFCH have been ascribed to a polymeric structure. Ni(II complex of HMPFCH has been assigned a dimeric square planar geometry. Cu(II complex of HMPFCH has been proposed an octahedral geometry. The ligands and their metal chelates were screened against S. aureus and P. aeruginosa. The ligands and the metal complexes have been found to be active against these microorganisms. The ligands show more activity than the metal complexes.

Template synthesis and characterization of biologically active transition metal complexes comprising 14-membered tetraazamacrocyclic ligand

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DHARMPAL SINGH

2010-02-01

Full Text Available A novel series of complexes of the type [M(C28H24N4X2], whereM = Co(II, Ni(II, Cu(II, Zn(II and Cd(II, X = Cl–, NO3–, CH3COO– and (C28H24N4 corresponds to the tetradentate macrocyclic ligand, were synthe¬sized by template condensation of 1,8-diaminonaphthalene and diacetyl in the presence of divalent metal salts in methanolic medium. The complexes were characterized by elemental analyses, conductance and magnetic measurements, as well as by UV/Vis, NMR, IR and MS spectroscopy. The low values of the molar conductance indicate non-electrolyte type of complexes. Based on these spectral data, a distorted octahedral geometry may be proposed for all of these complexes. All the synthesized macrocyclic complexes were tested for in vitro antibacterial activity against some pathogenic bacterial strains, viz Bacillus cereus, Salmonella typhi, Escherichia coli and Staphylococcus aureus. The MIC values shown by the complexes against these bacterial strains were compared with the MIC shown by the standard antibiotics linezolid and cefaclor.

Synthesis of complex compounds in the system [ReOG5]2--thiosemicarbazone acetone-Hg-acetone

International Nuclear Information System (INIS)

Amindzhanov, A.A.; Kurbanov, N.M.

1993-01-01

Present article is devoted to synthesis of complex compounds in the system [ReOG 5 ] 2- -thiosemicarbazone acetone-Hg-acetone. The literature data on complex compounds of various metals with thiosemicarbazone was summarized. The synthesis of complex compounds in the system [ReOG 5 ] 2- -thiosemicarbazone acetone-Hg-acetone was conducted. The complex compounds of rhenium with methyl ident thiosemicarbazone were synthesized.

Synthesis, characterization, DFT calculations and antibacterial activity of palladium(II) cyanide complexes with thioamides

Science.gov (United States)

Ahmad, Saeed; Nadeem, Shafqat; Anwar, Aneela; Hameed, Abdul; Tirmizi, Syed Ahmed; Zierkiewicz, Wiktor; Abbas, Azhar; Isab, Anvarhusein A.; Alotaibi, Mshari A.

2017-08-01

Palladium(II) cyanide complexes of thioamides (or thiones) having the general formula PdL2(CN)2, where L = Thiourea (Tu), Methylthiourea (Metu), N,N‧-Dimethylthiourea (Dmtu), Tetramethylthiourea (Tmtu), 2-Mercaptopyridine (Mpy) and 2-Mercaptopyrimidine (Mpm) were prepared by reacting K2[PdCl4] with potassium cyanide and thioamides in the molar ratio of 1:2:2. The complexes were characterized by elemental analysis, thermal and spectroscopic methods (IR, 1H and 13C NMR). The structures of three of the complexes were predicted by DFT calculations. The appearance of a band around 2100 cm-1 in IR and resonances around 120-130 ppm in the 13C NMR spectra indicated the coordination of cyanide to palladium(II). More than one resonances were observed for CN- carbon atoms in 13C NMR indicating the existence of equilibrium between different species in solution. DFT calculations revealed that in the case of the palladium(II) complex of Tmtu, the ionic dinuclear [Pd(Tmtu)4][Pd(CN)4] form was more stable than the dimer of mononuclear complex [Pd(Tmtu)2(CN)2] by 0.91 kcal mol-1, while for the complexes of Tu or Mpy ligands, the nonionic [Pd(L)2(CN)2] forms were more stable than the corresponding [Pd(L)4][Pd(CN)4] complexes by 1.26 and 6.49 kcal mol-1 for L = Tu and Mpy, respectively. The complexes were screened for antibacterial effects and some of them showed significant activities against both gram positive as well as gram negative bacteria.

How students process equations in solving quantitative synthesis problems? Role of mathematical complexity in students’ mathematical performance

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Bashirah Ibrahim

2017-10-01

Full Text Available We examine students’ mathematical performance on quantitative “synthesis problems” with varying mathematical complexity. Synthesis problems are tasks comprising multiple concepts typically taught in different chapters. Mathematical performance refers to the formulation, combination, and simplification of equations. Generally speaking, formulation and combination of equations require conceptual reasoning; simplification of equations requires manipulation of equations as computational tools. Mathematical complexity is operationally defined by the number and the type of equations to be manipulated concurrently due to the number of unknowns in each equation. We use two types of synthesis problems, namely, sequential and simultaneous tasks. Sequential synthesis tasks require a chronological application of pertinent concepts, and simultaneous synthesis tasks require a concurrent application of the pertinent concepts. A total of 179 physics major students from a second year mechanics course participated in the study. Data were collected from written tasks and individual interviews. Results show that mathematical complexity negatively influences the students’ mathematical performance on both types of synthesis problems. However, for the sequential synthesis tasks, it interferes only with the students’ simplification of equations. For the simultaneous synthesis tasks, mathematical complexity additionally impedes the students’ formulation and combination of equations. Several reasons may explain this difference, including the students’ different approaches to the two types of synthesis problems, cognitive load, and the variation of mathematical complexity within each synthesis type.

Synthesis, Characterization, and Thermal and Antimicrobial Activities of Some Novel Organotin(IV: Purine Base Complexes

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Reena Jain

2013-01-01

Full Text Available A new series of organotin(IV complexes with purine bases theophylline (HL1 and theobromine (L2 of the types R3Sn(L1, R2Sn(L1Cl, R3Sn(L2Cl, and R2Sn(L2Cl2 (R = C6H5CH2–; p-ClC6H4CH2– have been synthesized in anhydrous THF. The complexes were characterized by elemental analysis, conductance measurements, molecular weight determinations, UV-vis, IR, 1H, 13C NMR, and mass spectral studies. Various kinetic and thermodynamic parameters of these complexes have also been determined using TG/DTA technique. The thermal decomposition techniques indicate the formation of SnO2 as a residue. The results show that the ligands act as bidentate, forming a five-member chelate ring. All the complexes are 1 : 1 metal-ligand complexes. In order to assess their antimicrobial activity, the ligands and their corresponding complexes have also been tested in vitro against bacteria (E. coli, S. aureus, and P. pyocyanea and fungi (Rhizopus oryzae and Aspergillus flavus. All the complexes exhibit remarkable activity, and the results provide evidence that the studied complexes might indeed be a potential source of antimicrobial agents.

Synthesis, Characterization, Luminescence and Biological Activity of Two Lanthanide Complexes Involving Mixed Ligands

Energy Technology Data Exchange (ETDEWEB)

Ma, Deyun; Guo, Haifu; Qin, Liang [Zhaoqing Univ., Zhaoqing (China); Xu, Jun [Jinan Univ., Guangzhou (China)

2013-09-15

Two new isostructural dinuclear complexes, Ln{sub 2}(4-cpa){sub 6}(bpy){sub 2} (Ln = Eu (1); Tb (2), 4-cpa = 4-chlorophenyl-acetate, bpy = 2,2'-bipyridine), have been hydrothermally synthesized and characterized by IR spectroscopy, elemental analysis, thermogravimetric analysis (TGA), powder X-ray diffraction and single-crystal X-ray diffraction. The lanthanide ions are bridged by two bidentate and two terdentate carboxylate groups to give centrosymmetric dimers with Ln···Ln separations of 3.967(2) and 3.956(3) A, respectively. Each metal atom is nine-coordinate and exhibits a distorted tricapped trigonal prismatic geometry. Three-dimensional fluorescence spectra show that both 1 and 2 emit bright red and green luminescence at room temperature, with long lifetimes of up to 0.369 ms (at 614 nm) and 0.432 ms (at 543 nm), respectively. Moreover, poor luminescence efficiency has been noted for complex 2. The 4-Hcpa ligand and complexes 1-2 have been screened for their phytogrowth-inhibitory activities against Brassica napus L. and Echinochloa crusgalli L., and the results are compared with the activity of quizalofop-P-ethyl.

Copper(II) and palladium(II) complexes with tridentate NSO donor Schiff base ligand: Synthesis, characterization and structures

Science.gov (United States)

Kumar, Sujit Baran; Solanki, Ankita; Kundu, Suman

2017-09-01

Mononuclear copper(II) complex [CuL2] and palladium(II) complexes [Pd(X)L] where X = benzoate(bz) or salicylate(sal) and HL = 2-(methylthio)phenylimino)methyl)phenol, a Schiff base ligand with NSO coordination sites have been synthesized and characterized by microanalyses, IR, UV-Visible spectra, conductivity measurement and magnetic studies. Crystal structures of all the complexes have been solved by single crystal X-ray diffraction studies and showed that there are two molecules in a unit cell in the [CuL2] complex - one molecule has square planar geometry whereas second molecule has distorted square pyramidal geometry and palladium(II) complexes have distorted square planar geometry.

Synthesis, Characterization and Antimicrobial Activities of Transition Metal Complexes of methyl 2-(((E)-(2-hydroxyphenyl)methylidene)amino)benzoate

International Nuclear Information System (INIS)

Ikram, M.; Rehman, S.

2016-01-01

New metal complexes with Schiff base ligand methyl 2-(((E)-(2-hydroxyphenyl)methylidene)amino)benzoate, were synthesized and characterized. Elemental analyses, EI-MS, 1H and 13C(1H)-NMR were used for ligand characterization whereas elemental analyses, EI-MS, IR and UV-Visible spectroscopic techniques were used for the transition metal compounds. All these analyses reveal the bis arrangement of the ligand around the metal centres. The compounds were studied for their antimicrobial activities against different pathogenic microbial species. It was found that the Schiff base ligand was completely inactive in comparison to the transition metal compounds. It was also observed that nickel based metal complex shown good results against Candida albican (25 mm) and zinc based metal complex against Agrobacterium tumefaciens (16 mm). (author)

Synthesis, characterization and mechanistic insights of mycogenic iron oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Bhargava, Arpit; Jain, Navin; Manju Barathi L [Birla Institute of Technology and Science, Centre for Biotechnology, Department of Biological Sciences (India); Akhtar, Mohd Sayeed [Jimma University, Department of Applied Microbiology, College of Natural Sciences (Ethiopia); Yun, Yeoung-Sang [Chonbuk National University, Division of Environmental and Chemical Engineering (Korea, Republic of); Panwar, Jitendra, E-mail: drjitendrapanwar@yahoo.co.in [Birla Institute of Technology and Science, Centre for Biotechnology, Department of Biological Sciences (India)

2013-11-15

In the present study, extracellular synthesis of iron oxide nanoparticles (IONPs) was achieved using Aspergillus japonicus isolate AJP01. The isolate demonstrated its ability to hydrolyze the precursor salt solution, a mixture of iron cyanide complexes, under ambient conditions. Hydrolysis of these complexes released ferric and ferrous ions, which underwent protein-mediated coprecipitation and controlled nucleation resulting in the formation of IONPs. Transmission electron microscopy, selected area electron diffraction pattern, energy dispersive spectroscopy and grazing incidence X-ray diffraction analysis confirmed the mycosynthesis of IONPs. The synthesized particles were cubic in shape with a size range of 60–70 nm with crystal structure corresponding to magnetite. Scanning electron microscopy analysis revealed the absence of IONPs on fungal biomass surface, indicating the extracellular nature of synthesis. Fourier transform infrared spectroscopy confirmed the presence of proteins on as-synthesised IONPs, which may confer their stability. Preliminary investigation indicated the role of proteins in the synthesis and stabilization of IONPs. On the basis of present findings, a probable mechanism for synthesis of IONPs is suggested. The simplicity and versatility of the present approach can be utilized for the synthesis of other nanomaterials.

F-element metalated dipyrrins: synthesis and characterization of a family of uranyl bis(dipyrrinate) complexes.

Science.gov (United States)

Bolotaulo, Duer; Metta-Magaña, Alejandro; Fortier, Skye

2017-03-07

Using an improved, chromatography-free dipyrrin synthesis, the α,β-unsubstituted dipyrrins [RC(C 4 H 2 N) 2 H] (2) (R = tolyl (2toly l ), p-OMe-C 6 H 4 (2anis), mesityl (2mes), ferrocenyl (2Fc)) were isolated in good to excellent yields. Deprotonation of 2 with Na[N(SiMe 3 ) 2 ] gives the alkali metal salts [Na(DME) n ][RC(C 4 H 2 N) 2 ] (3) which reacts with UO 2 Cl 2 (THF) 3 to give the uranyl bis(dipyrrinates) UO 2 [RC(C 4 H 2 N) 2 ] 2 (L) (L = THF (4R-THF); DMAP (4R-DMAP)) (R = tolyl, p-OMe-C 6 H 4 , mesityl, ferrocenyl). The THF adducts, 4R-THF, are unstable in aromatic and nonpolar solvents and rapidly decompose to 2 and an intractable uranium-containing solid. On the other hand, the DMAP adducts, 4R-DMAP, are indefinitely stable in solution. The solid-state structures of 4R-THF and 4R-DMAP reveal distorted trigonal bipyramidal geometries. In the solid-state, the dipyrrinate ligands exhibit significant distortions including bowing and, in some instances, out-of-plane equatorial N-atom coordination, likely as a consequence of steric crowding and interligand repulsion. The complexes, 4R-DMAP, have been fully characterized by NMR, UV/Vis, and fluorescence spectroscopies, and their electrochemical properties have been investigated through cyclic voltammetry. The cyclic voltammograms of 4R-DMAP display several redox features but present a reversible wave at ca. -1.9 V (vs. Fc 0/+ ) attributable to a ligand centred reduction. Fluorescence measurements of all compounds reveal that only the mesityl derivatives 2mes, 3mes, and 4mes fluoresce with modest Stokes shift that ranges from ca. 30-70 nm, with 4mes displaying the greatest relative emission intensity.

Synthesis, characterization and behaviour of trans-bis (argininate) copper (II) to gamma radiation

International Nuclear Information System (INIS)

Pereira, A.B.

1984-01-01

The synthesis, the characterization and the behaviour to gamma radiation of trans-bis (argininate) copper (II) are presented. The synthesis is made from copper sulfate, sodium hydroxide and hydrochloride of L (+) arginine, in aqueous medium, and the characterization by infrared spectroscopy, visible and ultraviolet spectroscopy and elementary analysis. (C.G.C.)

Gd-Complexes of New Arylpiperazinyl Conjugates of DTPA-Bis(amides: Synthesis, Characterization and Magnetic Relaxation Properties

Directory of Open Access Journals (Sweden)

Abdullah O. Ba-Salem

2015-04-01

Full Text Available Two new DTPA-bis(amide based ligands conjugated with the arylpiperazinyl moiety were synthesized and subsequently transformed into their corresponding Gd(III complexes 1 and 2 of the type [Gd(LH2O]·nH2O. The relaxivity (R1 of these complexes was measured, which turned out to be comparable with that of Omniscan®, a commercially available MRI contrast agent. The cytotoxicity studies of these complexes indicated that they are non-toxic, which reveals their potential and physiological suitability as MRI contrast agents. All the synthesized ligands and complexes were characterized with the aid of analytical and spectroscopic methods, including elemental analysis, 1H-NMR, FT-IR, XPS and fast atom bombardment (FAB mass spectrometry.

Synthesis, characterization and study of some physical properties of some lanthanide complexes of salicylaldehyde oxal-dihydrazone

International Nuclear Information System (INIS)

Shrestha, S.; Rao, T.R.; Narang, K.K.; Shrestha, S.P.

2006-05-01

Some Lanthanoid complexes of the type [Ln (L-2H).A.H 2 O] [Ln = Y, La, Nd, Gd, Tb, Dy, A=OAc; and L = Salicyaldehyde oxal di-hydrazone] was synthesized and characterized by various physico- chemical techniques. Dehydration study at two specific temperatures (110 deg. C and 150 deg. C) indicates the presence of water molecules only in co-ordination sphere of the metal ion. IR, electronic spectra, DTA-TG have been recorded to establish the bonding sites of the ligand. All the complexes decomposed above and not melting up to 350 deg. C. The complexes are insoluble in any common organic solvent even in DMF and DMSO. Solid state electrical conductivities at various frequencies show a semiconducting nature of the complexes. Optical band gap measurement of the complex [Dy(SODH-2H).OAc.H 2 O] shows that complex behaves as direct band gap material. No well-defined peaks, except broad humps were observed in X-ray diffractogram of these complexes, indicating an amorphous nature of the complexes. (author)

Synthesis and characterization of organically linked ZnO nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Chory, Christine; Riedel, Ingo; Parisi, Juergen [Energy and Semiconductor Research Laboratory (EHF), University of Oldenburg, Carl-von Ossietzky-Strasse 9-11, 26129 Oldenburg (Germany); Kruska, Carsten; Heimbrodt, Wolfram [Department of Physics and Material Sciences Center, Philipps-University Marburg, Renthof 5, 35032 Marburg (Germany); Feser, Clemens [NEXT ENERGY - EWE Research Centre for Energy Technology e.V., Carl-von Ossietzky-Strasse 15, 26129 Oldenburg (Germany); Beenken, Wichard J.D. [Department of Theoretical Physics I, Ilmenau University of Technology, Weimarer Strasse 25, 98693 Ilmenau (Germany); Hoppe, Harald [Department of Experimental Physics I, Ilmenau University of Technology, Weimarer Strasse 32, 98693 Ilmenau (Germany)

2012-11-15

We report on the solution-based synthesis and characterization of three-dimensional networks of ZnO nanoparticles where the formation of structures is achieved by covalently linking the nanocrystals with bifunctional organic ligands. The colloidal synthesis will be presented with application of two ligands that vary in size and binding sites. Furthermore we report on structural characterization of dried powders and thin films by means of X-ray diffraction and electron microscopy in order to examine the regularity of the structures. We also present first investigations of the optical properties and electrical conductance behavior in lateral direction of the differently linked hybrid ZnO networks. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Synthesis and characterization of organically linked ZnO nanoparticles

International Nuclear Information System (INIS)

Chory, Christine; Riedel, Ingo; Parisi, Juergen; Kruska, Carsten; Heimbrodt, Wolfram; Feser, Clemens; Beenken, Wichard J.D.; Hoppe, Harald

2012-01-01

We report on the solution-based synthesis and characterization of three-dimensional networks of ZnO nanoparticles where the formation of structures is achieved by covalently linking the nanocrystals with bifunctional organic ligands. The colloidal synthesis will be presented with application of two ligands that vary in size and binding sites. Furthermore we report on structural characterization of dried powders and thin films by means of X-ray diffraction and electron microscopy in order to examine the regularity of the structures. We also present first investigations of the optical properties and electrical conductance behavior in lateral direction of the differently linked hybrid ZnO networks. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Synthesis and Characterization of Some Macrocylic Complexes Incorporating Indole and 2,2'-Bipyridine or 1,10-Phenanthroline

Directory of Open Access Journals (Sweden)

Muhammad S. Khan

2015-06-01

Full Text Available Complexes of anionic pentadentate macrocyclic ligands by the template condensation of bis(hydrazino2,2'-bipyridine or 1,10-phenanthroline with an indoledialdehyde have been synthesized. The new Mn(II, Fe(II, Co(II, Ni(II, Cu(II and Zn(II macrocyclic complexes have been characterized by analytical and spectroscopic techniques and by conductivity and magnetic susceptibility measurements.

Synthesis, crystal structure, spectroscopic characterization and nonlinear optical properties of Co(II)- picolinate complex

Energy Technology Data Exchange (ETDEWEB)

Tamer, Ömer, E-mail: omertamer@sakarya.edu.tr; Avcı, Davut; Atalay, Yusuf

2015-11-15

A cobalt(II) complex of picolinate was synthesized, and its structure was fully characterized by the applying of X-ray diffraction method as well as FT-IR, FT-Raman and UV–vis spectroscopies. In order to both support the experimental results and convert study to more advanced level, density functional theory calculations were performed by using B3LYP level. Single crystal X-ray structural analysis shows that cobalt(II) ion was located to the center of distorted octahedral geometry. The C=O, C=C and C=N stretching vibrations were found as highly active and strong peaks, inducing the molecular charge transfer within Co(II) complex. The small energy gap between frontier molecular orbital energies was another indicator of molecular charge transfer interactions within Co(II) complex. The nonlinear optical properties of Co(II) complex were investigated at DFT/B3LYP level, and the hypepolarizability parameter was found to be decreased due to the presence of inversion symmetry. The natural bond orbital (NBO) analysis was performed to investigate molecular stability, hyperconjugative interactions, intramolecular charge transfer (ICT) and bond strength for Co(II) complex. Finally, molecular electrostatic potential (MEP) and spin density distributions for Co(II) complex were evaluated. - Highlights: • Co(II) complex of picolinate was prepared. • Its FT-IR, FT-Raman and UV–vis spectra were measured. • DFT calculations were performed to support experimental results. • Small HOMO-LUMO energy gap is an indicator of molecular charge transfer. • Spin density localized on Co(II) as well as O and N atoms.

Synthesis and characterization of germa[n]pericyclynes.

Science.gov (United States)

Tanimoto, Hiroki; Nagao, Tomohiko; Nishiyama, Yasuhiro; Morimoto, Tsumoru; Iseda, Fumiyasu; Nagato, Yuko; Suzuka, Toshimasa; Tsutsumi, Ken; Kakiuchi, Kiyomi

2014-06-14

The synthesis and characterization of novel pericyclynes comprising germanium atoms and acetylenes, germa[n]pericyclynes, are described. The prepared germa[4]-, [6]-, and [8]pericyclynes were compared by (13)C NMR spectroscopy, X-ray crystallography, cyclic voltammetry, UV-visible spectroscopy, fluorescence emission spectroscopy, Raman spectroscopy, and density functional theory calculation analyses.

Organotin(IV complexes derived from N-ethyl-N-phenyldithiocarbamate: Synthesis, characterization and thermal studies

Directory of Open Access Journals (Sweden)

Jerry O. Adeyemi

2018-05-01

Full Text Available Organotin(IV dithiocarbamate complexes, RSnClL2 and R2SnL2 (R = Me, Bu, Ph, and L = N-ethyl-N-phenyldithiocarbamate, have been synthesized by the reaction of mono- and disubstituted organotin(IV with ammonium dithiocarbamate. The complexes were characterized by elemental analyses, and spectroscopic techniques (1H, 13C NMR and FTIR. The structures of Me2SnL2 and Bu2SnL2 were further established by single crystal X-ray diffraction technique. The crystal structure analysis showed that both complexes (Me2SnL2 and Bu2SnL2 exist as monomers. One of the dithiocarbamate ligands formed a chelate, while the other dithiocarbamate bonded to the central tin atom through one of the sulfur atoms and the second sulfur atom existed as a pendant to form distorted trigonal bipyramidal geometry. The thermal stability of all the complexes was studied using simultaneous thermogravimetry (TG and differential scanning calorimetry (DSC. The TG-DSC results showed that Me2SnL2, BuSnClL2, Bu2SnL2, and PhSnClL2 displayed similar decomposition pathway via isothiocyanate intermediate, while MeSnClL2 and Ph2SnL2 showed decomposition pathways different from the rest of the complexes. All the complexes resulted in SnS as the final product of the thermal decomposition process. Keywords: Organotin, Dithiocarbamate, Crystal structure, Thermal studies

Synthesis and characterization of monomeric and polymeric Cu(II) complexes of 3,4-ethylenedioxythiophene-functionalized with cyclam ligand

International Nuclear Information System (INIS)

Velauthamurty, Kuhamoorthy; Higgins, Simon J.; Rajapakse, R.M. Gamini; Bandara, H.M.N.; Shimomura, Masaru

2010-01-01

A functionalized EDOT derivative with 1,4,8,11-tetraazacyclotetradecane (cyclam) ligand pendant to the ethylene bridge (4) and its complexes [M(4)(BF 4 ) 2 ], where M(II) = Cu(II), was prepared and characterized. Their electrochemical copolymerization with EDOT was studied. The electro-co-polymerized films were characterized by electrochemical methods, X-ray photoelectron spectroscopy and by X-ray fluorescence spectroscopy. The co-polymerization method was found to afford a good control of the metal concentration in the polymer matrix and represents a good technique for preparing electronically conductive polymers containing redox-active metal complexes.

Synthesis, characterization and anti-bacterial activity of divalent transition metal complexes of hydrazine and trimesic acid

Directory of Open Access Journals (Sweden)

K. Kumar

2018-01-01

Full Text Available Transition metal complexes of trimesic acid and hydrazine mixed-ligands with a general formula M(Htma(N2H42, where, M = Mn, Co, Ni, Cu and Zn; H3tma = trimesic acid, have been prepared and characterized by elemental, structural, spectral and thermal analyses. For the complexes, the carboxylate νasym and νsym stretchings are observed at about 1626 and 1367 cm−1 respectively, with Δν between them of ∼260 cm−1, showing the unidentate coordination of each carboxylate group. The hydrazine moieties are present as bridging bidentates. Electronic and EPR spectral studies suggest an octahedral geometry for the complexes. All these complexes show three steps of decomposition in TGA/DTA. SEM images of CuO and MnO residues obtained from the complexes show nano-sized clusters suggesting that the complexes may be used as precursors for nano-CuO and nano-MnO preparation. The antimicrobial activities of the prepared complexes, against four bacteria have been evaluated.

Synthesis, characterization, and reactivity of ruthenium hydride complexes of N-centered triphosphine ligands.

Science.gov (United States)

Phanopoulos, Andreas; Brown, Neil J; White, Andrew J P; Long, Nicholas J; Miller, Philip W

2014-04-07

The reactivity of the novel tridentate phosphine ligand N(CH2PCyp2)3 (N-triphos(Cyp), 2; Cyp = cyclopentyl) with various ruthenium complexes was investigated and compared that of to the less sterically bulky and less electron donating phenyl derivative N(CH2PPh2)3 (N-triphos(Ph), 1). One of these complexes was subsequently investigated for reactivity toward levulinic acid, a potentially important biorenewable feedstock. Reaction of ligands 1 and 2 with the precursors [Ru(COD)(methylallyl)2] (COD = 1,5-cycloocatadiene) and [RuH2(PPh3)4] gave the tridentate coordination complexes [Ru(tmm){N(CH2PR2)3-κ(3)P}] (R = Ph (3), Cyp (4); tmm = trimethylenemethane) and [RuH2(PPh3){N(CH2PR2)3-κ(3)P}] (R = Ph (5), Cyp (6)), respectively. Ligands 1 and 2 displayed different reactivities with [Ru3(CO)12]. Ligand 1 gave the tridentate dicarbonyl complex [Ru(CO)2{N(CH2PPh2)3-κ(3)P}] (7), while 2 gave the bidentate, tricarbonyl [Ru(CO)3{N(CH2PCyp2)3-κ(2)P}] (8). This was attributed to the greater electron-donating characteristics of 2, requiring further stabilization on coordination to the electron-rich Ru(0) center by more CO ligands. Complex 7 was activated via oxidation using AgOTf and O2, giving the Ru(II) complexes [Ru(CO)2(OTf){N(CH2PPh2)3-κ(3)P}](OTf) (9) and [Ru(CO3)(CO){N(CH2PPh2)3-κ(3)P}] (11), respectively. Hydrogenation of these complexes under hydrogen pressures of 3-15 bar gave the monohydride and dihydride complexes [RuH(CO)2{N(CH2PPh2)3-κ(3)P}] (10) and [RuH2(CO){N(CH2PPh2)3-κ(3)P}] (12), respectively. Complex 12 was found to be unreactive toward levulinic acid (LA) unless activated by reaction with NH4PF6 in acetonitrile, forming [RuH(CO)(MeCN){N(CH2PPh2)3-κ(3)P}](PF6) (13), which reacted cleanly with LA to form [Ru(CO){N(CH2PPh2)3-κ(3)P}{CH3CO(CH2)2CO2H-κ(2)O}](PF6) (14). Complexes 3, 5, 7, 8, 11, and 12 were characterized by single-crystal X-ray crystallography.

Synthesis & Characterization of New bis-Symmetrical Adipoyl ...

African Journals Online (AJOL)

Full Title: Synthesis and Characterization of New bis-Symmetrical Adipoyl, Terepthaloyl, Chiral Diimido-di-L-alanine Diesters and Chiral Phthaloyl-L-alanine Ester of Tripropoxy p-tert-Butyl Calix[4]arene and Study of Their Hosting Ability for Alanine and Na+. Bis-symmetrical tripropoxy p-tert-butyl calix[4]arene esters were ...

Synthesis and characterization of monoclinic KGd(WO4)2 particles for non-cubic transparent ceramics

Science.gov (United States)

Thangaraju, D.; Durairajan, A.; Balaji, D.; Moorthy Babu, S.

2013-02-01

Monoclinic KGd(WO4)2 (KGW) particles were synthesized using polymeric metal complex sol-gel synthesis method. The derived particles were made as colloidal suspension form for better rotation of particles to have optimum response for applied magnetic field. The KGW fine particle suspension was prepared using electrostatic repulsion by electrolyte polymer. Prepared suspension was kept at 2 T and particles were settled using electrophoretic sedimentation using pH adjustment. The derived sediment was dried at 100 °C and the properties were characterized using XRD.

Synthesis and structural characterization of a calcium coordination ...

Indian Academy of Sciences (India)

Synthesis and structural characterization of a calcium coordination polymer based on a μ3-bridging. tetradentate binding mode of glycine. SUBRAMANIAN NATARAJAN*a, BIKSHANDARKOIL R. SRINIVASANb , J. KALYANA SUNDARa, K. RAVIKUMARc , R.V. KRISHNAKUMARd , J. SURESHe,. aSchool of Physics, ...

Tridentate hydrazone metal complexes derived from cephalexin and 2-hydrazinopyridine: Synthesis, characterization and antibacterial activity

Science.gov (United States)

Anacona, J. R.; Rincones, Maria

2015-04-01

Metal(II) coordination compounds of a tridentate hydrazone ligand (HL) derived from the condensation of cephalexin antibiotic with 2-hydrazinopyridine were synthesized. The hydrazone ligand and mononuclear [ML(OAc)(H2O)] (M(II) = Mn, Co, Ni, Cu, Zn, Ag) complexes were characterized by several techniques, including elemental and thermal analysis, molar conductance and magnetic susceptibility measurements, electronic, FT-IR, EPR and 1H NMR spectral studies. The cephalexin 2-pyridinylhydrazone ligand HL behaves as a monoanionic tridentate NNO chelating agent. The biological applications of complexes have been studied on three bacteria strains (Escherichia coli, Acinetobacter baumannii and Enterococcus faecalis) by agar diffusion disc method.

Synthesis and characterization of Th(IV) complex of bis-schiff base from o-vanillin and o-phenylene diamine

International Nuclear Information System (INIS)

Fan Yuhua; Bi Caifeng; Bao Meng

1997-01-01

The new solid complex of thorium nitrate with bis-schiff base (L) derived from o-vanillie and o-phenylene diamine has been synthesized and characterized by elemental analysis, DTA-TG, IR, UV and molar conductance analysis. The composition of the complex is confirmed to be ThL(NO 3 ) 4

Solid-phase synthesis of complex and pharmacologically interesting heterocycles

DEFF Research Database (Denmark)

Nielsen, Thomas Eiland

2009-01-01

Efficient routes for the creation of heterocycles continue to be one of the primary goals for solid-phase synthesis. Recent advances in this field rely most notably on transition-metal-catalysis and N-acyliminium chemistry to mediate a range of cyclization processes for the generation of compounds...... with significant structural complexity and diversity. This review describes some of the most systematic solid-phase approaches that are potentially suited for pharmaceutical applications, that is, the methods described are useful for the synthesis of compound collections, and exhibit tunable stereochemistry...

Polypyrrole-silver Nanocomposite: Synthesis and Characterization

OpenAIRE

D. M. Nerkar; S. V. Panse; S. P. Patil; S. E. Jaware; G. G. Padhye

2016-01-01

Polypyrrole-Silver (PPy-Ag) nanocomposite has been successfully synthesized by the chemical oxidative polymerization of pyrrole with iron (III) chloride as an oxidant, in the presence of a colloidal suspension of silver nanoparticles. Turkevich method (Citrate reduction method) was used for the synthesis of silver nanoparticles (Ag NPs). The silver nanoparticles were characterized by UV-Visible spectroscopy which showed an absorption band at 423 nm confirming the formation of nanoparticles. P...

Stimulation of DNA synthesis in bacterial DNA-membrane complexes after low doses of ionizing radiation

Energy Technology Data Exchange (ETDEWEB)

Watkins, D K [Hammersmith Hospital, London (UK). M.R.C. Experimental Radiopathology Unit

1980-09-01

DNA-membrane complexes from three strains of E. coli were irradiated and changes in the rates of DNA synthesis were observed. Doses from 1-10 krad to complexes from W3110 and pol A1 strains gave up to a 100 per cent increase in DNA synthesis; under the same conditions, no change was observed in Bsub(s-1). The degree of stimulation did not depend on the presence of oxygen during irradiation, and a post-irradiation incubation was necessary to achieve activation. The properties of all three complexes were similar when unirradiated. Irradiation of intact organisms under conditions which produced marked, oxygen-dependent inhibition of the Bsub(s-1) complex had no significant effect on those from W3110 and pol A1. Enhanced DNA synthesis is concluded to be due wholly to repair of pre-existing DNA. It is further postulated that DNA synthesis in untreated complexes (E.coli B's,W3110 and pol A1) is mainly of the repair-type and does not necessarily take place at the site of DNA-membrane attachment.

Synthesis and characterization of new mixed ligand complexes of ruthenium(II) containing triphenylphosphine and 2'-hydroxychalcones

International Nuclear Information System (INIS)

Dharmaraj, N.; Natarajan, K.

1994-01-01

A few hexacoordinated ruthenium(II) complexes of the type [RuCl(CO) (HLL')(PPh 3 ) 2 ] and [RuCl(CO)(HLL')(B) (PPh 3 )] (where HLL' 2'-hydroxychalcone, 2'-hydroxy-4-methoxychalcone, 2'-hydroxy-3,4-dimethoxychalcone and B=pyridine(Py), piperidine(Pip), morpholine (Morph)) have been synthesised and characterized on the basis of their analytical and spectral data (IR, electronic and 1 H NMR). In all these complexes, the 2'-hydroxychalcones behave as a uninegative bidentate (OO - ) chelating ligand. (author). 17 refs., 1 tab

Synthesis and characterization of Ru(II) complexes with polyfunctional quinazoline-(3H)-4-ones

International Nuclear Information System (INIS)

Prabhakar, B.; Lingaiah, P.; Laxma Reddy, K.

1991-01-01

Few Ru(II) complexes of the type Ru(O-N-O) 2 with tridentate O-N-O donors and of the type RuCl 2 (O-N) 2 with bidentate O-O and O-N donors have been synthesized and characterized on the basis of analytical, conductivity, thermal, magnetic, IR, electronic and PMR spectral data. The IR and PMR spectral data of the metal complexes indicate that the lignads like 2-methyl/phenyl-3-(2'-hydroxybenzalamino) quinazoline-(3H)-4-one(MHBQ/PHBQ) act as uninegative tridentate, 2-methyl/phenyl-3-(carboxymethyl) quinazoline(3H)-4-one (MCMQ/PCMQ) as uninegative bidentate and 2-methyl/phenyl-3-(furfuralamino) quinazoline-(3H)-4-one (MFQ/PFQ), 2-methyl/phenyl-3-(acetamino) quinazoline-(3H)-4-one (MAQ/PAQ), 2-methyl/phenyl3-(uramino)quinazoline-(3H)-4-one (MUQ/PUQ) and 2-methyl/phenyl-3-thiouramino)quinazoline-(3H)-4-one-(MTUQ/PTUQ) as neutral bidentate ligands. The electronic spectral data of the complexes indicate that the arrangement around Ru(II) is octahedral. (author). 25 refs., 2 tabs

New bioactive silver(I) complexes: Synthesis, characterization, anticancer, antibacterial and anticarbonic anhydrase II activities

Science.gov (United States)

Ozdemir, Ummuhan O.; Ozbek, Neslihan; Genc, Zuhal Karagoz; İlbiz, Firdevs; Gündüzalp, Ayla Balaban

2017-06-01

Silver(I) complexes of alkyl sulfonic acide hydrazides were newly synthesized as homologous series. Methanesulfonic acide hydrazide (L1), ethanesulfonic acide hydrazide (L2), propanesulfonic acide hydrazide (L3) and butanesulfonic acide hydrazide (L4) were used for complexation with Ag(I) ions. The silver complexes obtained in the mol ratio of 1:2 have the structural formula as Ag(L1)2NO3 (I), Ag(L2)2NO3 (II), Ag(L3)2NO3(III), (Ag(L4)2NO3 (IV). The Ag(I) complexes exhibit distorted linear two-fold coordination in [AgL2]+ cations with uncoordinated nitrates. Ligands are chelated with silver(I) ions through unsubstituted primary nitrogen in hydrazide group. Ag(I) complexes were characterized by using elemental analysis, spectroscopic methods (FT-IR, LC-MS), magnetic susceptibility and conductivity measurements. Silver(I) complexes were optimized using PBEPBE/LanL2DZ/DEF2SV basic set performed by DFT method with the Gaussian 09 program package. The geometrical parameters, frontier molecular orbitals (HOMOs and LUMOs) and molecular electrostatic potential (MEP) mapped surfaces of the optimized geometries were also determined by this quantum set. The anticancer activities of silver(I) complexes on MCF-7 human breast cancer cell line were investigated by comparing IC50 values. The antibacterial activities of complexes were studied against Gram positive bacteria; S. aureus ATCC 6538, B. subtilis ATCC 6633, B. cereus NRRL-B-3711, E. faecalis ATCC 29212 and Gram negative bacteria; E. coli ATCC 11230, P. aeruginosa ATCC 15442, K. pneumonia ATCC 70063 by using disc diffusion method. The inhibition activities of Ag(I) complexes on carbonic anhydrase II enzyme (hCA II) were also investigated by comparing IC50 and Ki values. The biological activity screening shows that Ag(I) complex of butanesulfonicacidehydrazide (IV) has the highest activity against tested breast cancer cell lines MCF-7, Gram positive/Gram negative bacteria and carbonic anhydrase II (hCA II) isoenzyme.

Synthesis and Characterization of Chloridobis(dimethylglyoximato4-(2-ferrocenylvinylpyridinecobalt(III: A New Heterobinuclear Cobaloxime

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Sebastián Pizarro

2016-01-01

Full Text Available The synthesis of a new heterobinuclear cobaloxime with 4-(2-ferrocenylvinylpyridine, fcvpy, is reported. The complex [CoCl(dmgH2(fcvpy], where dmgH2 is dimethylglyoxime and dmgH is dimethylglyoximato, has been characterized by 1H-NMR, UV-Vis, cyclic voltammetry, and elemental analysis. The cyclic voltammogram of this complex shows a fc/fc+ reversible wave at +0.58 V versus Ag/AgCl, one irreversible wave, Epc = −0.54 V versus Ag/AgCl, assigned to the reduction of Co(III to Co(II, and two quasireversible processes at −1.02 V and −1.10 V versus Ag/AgCl associated with the reduction of Co(II. The complex showed ferrocene-ligand charge transfer bands at 334 nm and 505 nm. TDDFT/B3LYP/6-31G(d calculations support this assignation.

Synthesis of 3,5-diisopropyl[carboxy-14C]salicylic acid and its 67Cu complex

International Nuclear Information System (INIS)

Chidambaram, M.V.; Epperson, C.E.; Williams, S.; Gray, R.A.; Sorenson, J.R.J.

1991-01-01

The synthesis of 3,5-diisopropyl[carboxy- 14 C]salicylic acid was achieved via Kolbe-Schmitt carboxylation of potassium 2,4-di-isopropylphenolate. The yield of this acid was 81% based upon the weight of the product and 93% based upon radioactivity incorporated into the labeled acid which contains 98% 14 C in the carboxyl group (specific activity = 5.1 μCi/mg). The labeled acid was characterized by ultraviolet spectrophotometry and purity established by thin-layer chromatography, autoradiography, and liquid scintillation counting. A 90% yield of the double labeled 14 C, 67 Cu-complex (specific activity = 4.6 μCi 67 Cu/mg) was obtained using conditions developed with non-radioactive reactants. The presence of 67 Cu in this complex was established using γ-ray emission spectrophometry. (author)

Synthesis and characterization of activated lithium fluoride with silver

International Nuclear Information System (INIS)

Encarnacion E, E. K.; Guerrero S, Z.; Reyes A, J.

2017-10-01

The present work shows part of the results obtained in the development of the research that has been carried out since 2015 entitled -Synthesis and characterization of new thermoluminescent materials for the radiation dosimetry and its applications in health-. In the development of this research, the synthesis of crystals of pure lithium fluoride (LiF) and activated with different concentrations of silver (LiF:Ag); synthesized samples are also presented using different temperatures, as well as varying the concentration of the solvent (water-ethanol). The synthesized materials were characterized through different techniques: scanning electron microscopy and X-ray diffraction. Specifically, the results of the calculation of the size of the LiF crystals are presented using the Scherrer equation. Within the results, a dependence on the size of the crystals is highlighted by means of the following factors: the amount of activator in the sample, the temperature at which the sample was synthesized, as well as the amount of solvent in the synthesis. The samples have a simple cubic crystalline phase. (Author)

Metal–organic coordination architectures of tetrazole heterocycle ligands bearing acetate groups: Synthesis, characterization and magnetic properties

International Nuclear Information System (INIS)

Hu, Bo-Wen; Zheng, Xiang-Yu; Ding, Cheng

2015-01-01

Two new coordination complexes with tetrazole heterocycle ligands bearing acetate groups, [Co(L) 2 ] n (1) and [Co 3 (L) 4 (N 3 ) 2 ·2MeOH] n (2) (L=tetrazole-1-acetate) have been synthesized and structurally characterized. Single crystal structure analysis shows that the cobalt-complex 1 has the 3D 3,6-connected (4 2 .6) 2 (4 4 .6 2 .8 8 .10)-ant topology. By introducing azide in this system, complex 2 forms the 2D network containing the [Co 3 ] units. And the magnetic properties of 1 and 2 have been studied. - Graphical abstract: The synthesis, crystal structure, and magnetic properties of the new coordination complexes with tetrazole heterocycle ligands bearing acetate groups are reported. - Highlights: • Two novel Cobalt(II) complexes with tetrazole acetate ligands were synthesized. • The magnetic properties of two complexes were studied. • Azide as co-ligand resulted in different structures and magnetic properties. • The new coordination mode of tetrazole acetate ligand was obtained.

Novel metallomesogenic polyurethanes: Synthesis, characterization and properties

International Nuclear Information System (INIS)

Senthilkumar, Natarajan; Narasimhaswamy, Tanneru; Kim, Il-Jin

2012-01-01

A series of tetradentate Schiff base metallomesogenic diols were synthesized from two simple dihydroxy benzenes. The metallomesogenic diol was constructed from three ring containing mesogen linked through ester and azomethine with terminal hydroxy group. This upon complexation with copper(II) formed metallomesogenic diol with varying terminal chain length. A series of metallomesogenic polyurethanes were synthesized using these metallomesogenic diols as chain extenders for the prepolymers based on polytetramethylene glycol (PTMG) of varying molecular weight (M n = 650, 2000) and 2,4-toluene diisocyanate (TDI), or 4,4′-methylene bis(phenyl isocyanate) (MDI). The molar ratio of metallomesogenic diol and PTMG were varied in the polyurethane to find their role in liquid crystalline and mechanical properties. Extensive characterization of all metallomesogenic compounds and intermediates were carried out by FT-IR, 1 H and 13 C NMR, EPR, VSM, Mass (EI and FAB) and UV–visible spectroscopy. Hot stage polarizing microscope and differential scanning calorimetry were used to ensure the phase characteristics such as nature of phase, melting and clearing temperatures and phase range. The appearance of enantiotropic smectic A phases indicated high molecular polarizability of the core due to the metal ion. - Highlights: ► Design and synthesis of metallomesogenic diols. ► Metallomesogenic polyurethanes were prepared using these diols as chain extenders. ► Liquid crystalline and mechanical properties were studied. ► A square pyramidal structure for the copper(II) complexes have been proposed. ► Polyurethanes exhibited enantiotropic smectic A phases.

Group 12 dithiocarbamate complexes: Synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites

Science.gov (United States)

Ajibade, Peter A.; Ejelonu, Benjamin C.

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, 1H- and 13C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix.

Novel Organotin(IV) Schiff Base Complexes with Histidine Derivatives: Synthesis, Characterization, and Biological Activity

Science.gov (United States)

Garza-Ortiz, Ariadna; Camacho-Camacho, Carlos; Sainz-Espuñes, Teresita; Rojas-Oviedo, Irma; Gutiérrez-Lucas, Luis Raúl; Gutierrez Carrillo, Atilano; Vera Ramirez, Marco A.

2013-01-01

Five novel tin Schiff base complexes with histidine analogues (derived from the condensation reaction between L-histidine and 3,5-di-tert-butyl-2-hydroxybenzaldehyde) have been synthesized and characterized. Characterization has been completed by IR and high-resolution mass spectroscopy, 1D and 2D solution NMR (1H, 13C  and 119Sn), as well as solid state 119Sn NMR. The spectroscopic evidence shows two types of structures: a trigonal bipyramidal stereochemistry with the tin atom coordinated to five donating atoms (two oxygen atoms, one nitrogen atom, and two carbon atoms belonging to the alkyl moieties), where one molecule of ligand is coordinated in a three dentate fashion. The second structure is spectroscopically described as a tetrahedral tin complex with four donating atoms (one oxygen atom coordinated to the metal and three carbon atoms belonging to the alkyl or aryl substituents), with one molecule of ligand attached. The antimicrobial activity of the tin compounds has been tested against the growth of bacteria in vitro to assess their bactericidal properties. While pentacoordinated compounds 1, 2, and 3 are described as moderate effective to noneffective drugs against both Gram-positive and Gram-negative bacteria, tetracoordinated tin(IV) compounds 4 and 5 are considered as moderate effective and most effective compounds, respectively, against the methicillin-resistant Staphylococcus aureus strains (Gram-positive). PMID:23864839

Synthesis, characterization and anti-fungal evaluation of Ni(II and Cu(II complexes with a derivative of 4-aminoantipyrine

Directory of Open Access Journals (Sweden)

Monika Tyagi

2017-01-01

Full Text Available Transition metal complexes of Ni(II and Cu(II metal ions with the general stoichiometry [M(LX]X and [M(LSO4], where M = Ni(II and Cu(II, L = (1E-N-((5-((E-(2,3-dimethyl-1-phenyl-4-pyrazolineiminomethylthiophen-2-ylmethylene-2,3-dimethyl-1-phenyl-4-pyrazolineamine and X = Cl−, NO3− and SO42−, have been synthesized and characterized. The synthesized ligand and metal complexes were characterized by 1H NMR, IR, mass spectrometry, UV–Vis spectra and EPR. In molecular modelling, the geometries of the Schiff's base and metal complexes were fully optimized with respect to the energy using the 6-31g(d,p basis set. The nickel(II complexes were found to have octahedral geometry, whereas the copper(II complexes were of tetragonal geometry. The covalency factor (β and orbital reduction factor (k suggest the covalent nature of the complexes. To develop broad spectrum new molecules against seed-borne fungi, the minimum inhibitory concentration (MIC of the ligand and its metal complexes was evaluated by the serial dilution method.

Synthesis, Characterization and Antimicrobial Activities of Some ...

African Journals Online (AJOL)

user

of metal ions with vitamin.111: Synthesis and infrared spectra of metal complexes with pyridoxamine and pyridoxine. Inorg. Chim. Acta, 46, 191-197. Gary, J and Adeyemo, A (1981) Interaction of vitamin B1 with Zn(II), Cd (II) and Hg(II) in. Deuterated Dimethyl Sulfoxide. Inorg. Chim. Acta, 55, 93-98. Gohzalez-vergara, E ...

Synthesis and characterization of dioxouranium (VI) complexes of Schiff bases derived from isatin, isovanillin and o-vanillin

International Nuclear Information System (INIS)

Singh, Kavita; Agarwala, B.V.; Naganagowda, G.A.

1996-01-01

Three Schiff bases viz. isatin semicarbazone, isovanillin thiosemicarbazone, o-vanillin para-anisidine and their dioxouranium (VI) complexes have been synthesised and characterized by elemental analysis, IR and NMR spectral studies. (author). 19 refs., 1 tab

Synthesis and characterization of poly(phenylacetylene)s with Ru(II) bis-terpyridine complexes in the side-chain.

Science.gov (United States)

Breul, Alexander M; Kübel, Joachim; Häupler, Bernhard; Friebe, Christian; Hager, Martin D; Winter, Andreas; Dietzek, Benjamin; Schubert, Ulrich S

2014-04-01

An alkyne-functionalized ruthenium(II) bis-terpyridine complex is directly copolymerized with phenylacetylene by alkyne polymerization. The polymer is characterized by size-exclusion chromatography (SEC), (1) H NMR spectroscopy, cyclic voltammetry (CV) measurements, and thermal analysis. The photophysical properties of the polymer are studied by UV-vis absorption spectroscopy. In addition, spectro-electrochemical measurements are carried out. Time-resolved luminescence lifetime decay curves show an enhanced lifetime of the metal complex attached to the conjugated polymer backbone compared with the Ru(tpy)2 (2+) model complex. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and characterization of zinc(II), cadmium(II) and mercury(II) complexes with bis(bidentate) Schiff bases

International Nuclear Information System (INIS)

Das, Mrinal Kanti; Ghosh, Shyamali

1998-01-01

A few Zn(II), Cd(II) and Hg(II) complexes of the bis(bidentate) Schiff bases derived from p-phenylenediamine and salicylaldehyde (H 2 Salpphen), and o-phenylenediamine and o-vanillin (H 2 Vanophen), of the type MCl 2 .H 2 L(H 2 L = H 2 Salpphen or H 2 Vanophen) have been synthesised. The complexes have been characterized by elemental analysis, infrared, 1 H and 13 C NMR and mass spectra. (author)

Synthesis, Characterization and Biological Evaluation of Transition Metal Complexes Derived from N, S Bidentate Ligands

Directory of Open Access Journals (Sweden)

Enis Nadia Md Yusof

2015-05-01

Full Text Available Two bidentate NS ligands were synthesized by the condensation reaction of S-2-methylbenzyldithiocarbazate (S2MBDTC with 2-methoxybenzaldehyde (2MB and 3-methoxybenzaldehyde (3MB. The ligands were reacted separately with acetates of Cu(II, Ni(II and Zn(II yielding 1:2 (metal:ligand complexes. The metal complexes formed were expected to have a general formula of [M(NS2] where M = Cu2+, Ni2+, and Zn2+. These compounds were characterized by elemental analysis, molar conductivity, magnetic susceptibility and various spectroscopic techniques. The magnetic susceptibility measurements and spectral results supported the predicted coordination geometry in which the Schiff bases behaved as bidentate NS donor ligands coordinating via the azomethine nitrogen and thiolate sulfur. The molecular structures of the isomeric S2M2MBH (1 and S2M3MBH (2 were established by X-ray crystallography to have very similar l-shaped structures. The Schiff bases and their metal complexes were evaluated for their biological activities against estrogen receptor-positive (MCF-7 and estrogen receptor-negative (MDA-MB-231 breast cancer cell lines. Only the Cu(II complexes showed marked cytotoxicity against the cancer cell lines. Both Schiff bases and other metal complexes were found to be inactive. In concordance with the cytotoxicity studies, the DNA binding studies indicated that Cu(II complexes have a strong DNA binding affinity.

Synthesis and characterization of reactive dye-cassava mesocarp ...

African Journals Online (AJOL)

The synthesis of triazine based reactive dyes was carried out. The resultant dyes were characterized by thin layers chromatography, molecular weight, infrared and ultra- violet spectroscopy, and used in dyeing cassava mesocarp to produce dye modified cellulosic substrates. The dyed substrates were tested for dye fixation, ...

Synthesis, Characterization and Application of Multiscale Porous Materials

Energy Technology Data Exchange (ETDEWEB)

Hussami, Linda

2010-07-01

This thesis work brings fresh insights and improved understanding of nano scale materials through introducing new hybrid composites, 2D hexagonal in MCM-41 and 3D random interconnected structures of different materials, and application relevance for developing fields of science, such as fuel cells and solar cells. New types of porous materials and organometallic crystals have been prepared and characterized in detail. The porous materials have been used in several studies: as hosts to encapsulate metal-organic complexes; as catalyst supports and electrode materials in devices for alternative energy production. The utility of the new porous materials arises from their unique structural and surface chemical characteristics as demonstrated here using various experimental and theoretical approaches. New single crystal structures and arene-ligand exchange properties of f-block elements coordinated to ligand arene and halogallates are described in Paper I. These compounds have been incorporated into ordered 2D-hexagonal MCM-41 and polyhedral silica nano foam (PNF-SiO{sub 2}) matrices without significant change to the original porous architectures as described in Paper II and III. The resulting inorganic/organic hybrids exhibited enhanced luminescence activity relative to the pure crystalline complexes. A series of novel polyhedral carbon nano foams (PNF-C's) and inverse foams were prepared by nano casting from PNF-SiO{sub 2}'s. These are discussed in Paper IV. The synthesis conditions of PNF-C's were systematically varied as a function of the filling ratio of carbon precursor and their structures compared using various characterization methods. The carbonaceous porous materials were further tested in Paper V and VI as possible catalysts and catalyst supports in counter- and working electrodes for solar- and fuel cell applications

Synthesis and characterization of new optically active poly(amide ...

African Journals Online (AJOL)

Synthesis and characterization of new optically active poly(amide-imide)s based on N -trimellitimido- ... Bulletin of the Chemical Society of Ethiopia ... (DMAc), dimethyl sulfoxide (DMSO) and N-methyl-2-pyrrolidone (NMP) at room temperature.

Synthesis, characterization and biological activity of symmetric dinuclear complexes derived from a novel macrocyclic compartmental ligand

Energy Technology Data Exchange (ETDEWEB)

Mruthyunjayaswamy, B.H.M.; Ijare, Omkar B.; Jadegoud, Y. [Gulbarga University (India). Dept. of Chemistry]. E-mail: bhmmswamy53@rediffmail.com

2005-07-15

A phenol based novel macrocyclic binucleating compartmental ligand N,N-bis(2,6-diiminomethyl-4-methyl-1-hydroxyphenyl)malonoyldicarboxamide was prepared. The complexes were prepared by template method by reacting 2,6-diformyl-4-methylphenol, malonoyl dihydrazide and the metal chlorides of Cu(II), Ni(II), Co(II), Cd(II), Zn(II) and Hg(II) in methanol to get a series of dinuclear complexes. The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibility data, IR, UV-Vis, ESR, NMR and FAB mass spectral data. The dinuclear nature of the complexes was confirmed on the basis of elemental analyses, magnetic susceptibility, ESR and FAB mass spectral data. The ligand as well as Cu(II), Ni(II), Co(II) and Zn(II) complexes were tested for their antibacterial and antifungal properties against Escherichia coli, Staphyloccocus aureus, Aspergillus niger and Fusarium oxysporum. Magnetic susceptibility measurements of Cu(II), Ni(II) and Co(II) complexes reveal that these complexes exhibit antiferromagnetic coupling behavior due to the presence of two metal ions in close proximity. FAB mass spectrum of the Cu(II) complex gave a clear evidence for the dinuclear nature. The ligand and the complexes were found to be less active against the tested bacteria, but the ligand alone was found active against the fungus Fusarium oxysporum. (author)

Synthesis, characterization and biological activity of symmetric dinuclear complexes derived from a novel macrocyclic compartmental ligand

International Nuclear Information System (INIS)

Mruthyunjayaswamy, B.H.M.; Ijare, Omkar B.; Jadegoud, Y.

2005-01-01

A phenol based novel macrocyclic binucleating compartmental ligand N,N-bis(2,6-diiminomethyl-4-methyl-1-hydroxyphenyl)malonoyldicarboxamide was prepared. The complexes were prepared by template method by reacting 2,6-diformyl-4-methylphenol, malonoyl dihydrazide and the metal chlorides of Cu(II), Ni(II), Co(II), Cd(II), Zn(II) and Hg(II) in methanol to get a series of dinuclear complexes. The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibility data, IR, UV-Vis, ESR, NMR and FAB mass spectral data. The dinuclear nature of the complexes was confirmed on the basis of elemental analyses, magnetic susceptibility, ESR and FAB mass spectral data. The ligand as well as Cu(II), Ni(II), Co(II) and Zn(II) complexes were tested for their antibacterial and antifungal properties against Escherichia coli, Staphyloccocus aureus, Aspergillus niger and Fusarium oxysporum. Magnetic susceptibility measurements of Cu(II), Ni(II) and Co(II) complexes reveal that these complexes exhibit antiferromagnetic coupling behavior due to the presence of two metal ions in close proximity. FAB mass spectrum of the Cu(II) complex gave a clear evidence for the dinuclear nature. The ligand and the complexes were found to be less active against the tested bacteria, but the ligand alone was found active against the fungus Fusarium oxysporum. (author)

Synthesis, structural and electrical characterizations of thermally ...

African Journals Online (AJOL)

Synthesis, structural and electrical characterizations of thermally evaporated Cu 2 SnS 3 thin films. ... The surface profilometer shows that the deposited films are rough. The XRD spectra identified the ... The electrical resistivity of the deposited Cu2SnS3 film is 2.55 x 10-3 Ωcm. The conductivity is in the order of 103 Ω-1cm-1.

Synthesis, thermogravimetric, spectroscopic and theoretical characterization of copper(II) complex with 4-chloro-2-nitrobenzenosulfonamide

Science.gov (United States)

Camí, G.; Chacón Villalba, E.; Di Santi, Y.; Colinas, P.; Estiu, G.; Soria, D. B.

2011-05-01

4-Chloro-2-nitrobenzenesulfonamide (ClNbsa) was purified and characterized. A new copper(II) complex, [Cu(ClNbsa) 2(NH 3) 2], has been prepared using the sulfonamide as ligand. The thermal behavior of both, the ligand and the Cu(II) complex, was investigated by thermogravimetric analyses (TG) and differential thermal analysis (DT), and the electronic characteristics analyzed by UV-VIS, FTIR, Raman and 1H NMR spectroscopies. The experimental IR, Raman and UV-VIS spectra have been assigned on the basis of DFT calculations at the B3LYP level of theory using the standard (6-31 + G ∗∗) basis set. The geometries have been fully optimized in vacuum and in modeled dimethylsulfoxide (DMSO) solvent, using for the latter a continuum solvation model that reproduced the experimental conditions of the UV-VIS spectroscopy. The theoretical results converged to stable conformations for the free sulfonamide and for the complex, suggesting for the latter a distorted square planar geometry in both environments.

New Mn(II, Ni(II, Cd(II, Pb(II complexes with 2-methylbenzimidazole and other ligands. Synthesis, spectroscopic characterization, crystal structure, magnetic susceptibility and biological activity studies

Directory of Open Access Journals (Sweden)

Shayma A. Shaker

2016-11-01

Full Text Available Synthesis and characterization of Mn(II, Ni(II, Cd(II and Pb(II mixed ligand complexes of 2-methylbenzimidazole with other ligands have been reported. The structure of the ligands and their complexes was investigated using elemental analysis, IR, UV–Vis, (1H, 13C NMR spectroscopy, molar conductivity and magnetic susceptibility measurements. In all the studies of complexes, the 2-methylbenzimidazole behaves as a neutral monodentate ligand which is coordinated with the metal ions through the N atom. While benzotriazole behaves as a neutral bidentate ligand which is coordinated with the Ni(II ion through the two N atoms. Moreover, the N-acetylglycine behaves as a bidentate ligand which is coordinated with the Mn(II, Ni(II and Pb(II ions through the N atom and the terminal carboxyl oxygen atom. The magnetic and spectral data indicate the tetrahedral geometry for Mn(II complex, irregular tetrahedral geometry for Pb(II complex and octahedral geometry for Ni(II complex. The X-ray single crystal diffraction method was used to confirm a centrosymmetric dinuclear Cd(II complex as each two metal ions are linked by a pair of thiocyanate N = S bridge. Two 2-methylbenzimidazole N-atom donors and one terminal thiocyanate N atom complete a highly distorted square pyramid geometry around the Cd atom. Besides, different cell types were used to determine the inhibitory effect of Mn(II, Ni(II, Cd(II and Pb(II complexes on cell growth using MTT assay. Cd(II complex showed cytotoxic effect on various types of cancer cell lines with different EC50 values.

Synthesis, characterization and reactivity of some lanthanide organometallics

International Nuclear Information System (INIS)

Marchal, N.

1991-12-01

Organo lanthanides with reactive metal-carbon bonds are obtained by direct synthesis of the metal (powder) and a hydrocarbon in ether medium, like with alkali metals. Two types of synthesis are envisaged: formation of covalent bonds by opening cycles, only biphenylene is reactive enough in regard to ytterbium and samarium, these organometallic compounds can also be prepared by the classical way, i.e. reaction of 2.2'-dilithio biphenyl on rare earth halogenides and coupling of 6.6-dimethylfulvene leading to dicyclopentadienyl compounds with Sm and Yb. The reactivity of these complexes is studied by catalysis of ethylene polymerization

Combustion synthesis and structural characterization of Li–Ti mixed

Indian Academy of Sciences (India)

Combustion synthesis and structural characterization of Li–Ti mixed nanoferrites ... were prepared by combustion method at lower temperatures compared to the ... first time at low temperatures, using PEG which acts as a new fuel and oxidant.

Bis(bipyridine)ruthenium(II) complexes with an aliphatic sulfinato donor: synthesis, characterization, and properties.

Science.gov (United States)

Tamura, Motoshi; Tsuge, Kiyoshi; Igashira-Kamiyama, Asako; Konno, Takumi

2011-06-06

Treatment of a thiolato-bridged Ru(II)Ag(I)Ru(II) trinuclear complex, [Ag{Ru(aet)(bpy)(2)}(2)](3+) (aet = 2-aminoethanthiolate; bpy = 2,2'-bipyridine), with NaI in aqueous ethanol under an aerobic condition afforded a mononuclear ruthenium(II) complex having an S-bonded sulfinato group, [1](+) ([Ru(aesi-N, S)(bpy)(2)](+) (aesi = 2-aminoethanesulfinate)). Similar treatment of optically active isomers of an analogous Ru(II)Ag(I)Ru(II) trinuclear complex, Δ(D)Δ(D)- and Λ(D)Λ(D)-[Ag{Ru(d-Hpen-O,S)(bpy)(2)}(2)](3+) (d-pen = d-penicillaminate), with NaI also produced mononuclear ruthenium(II) isomers with an S-bonded sulfinato group, Δ(D)- and Λ(D)-[2](+) ([Ru(d-Hpsi-O,S)(bpy)(2)](+) (d-psi = d-penicillaminesulfinate)), respectively, retaining the bidentate-O,S coordination mode of a d-Hpen ligand and the absolute configuration (Δ or Λ) about a Ru(II) center. On refluxing in water, the Δ(D) isomer of [2](+) underwent a linkage isomerization to form Δ(D)-[3] (+) ([Ru(d-Hpsi-N,S)(bpy)(2)](+)), in which a d-Hpsi ligand coordinates to a Ru(II) center in a bidentate-N,S mode. Complexes [1](+), Δ(D)- and Λ(D)-[2](+), and Δ(D)-[3](+) were fully characterized by electronic absorption, CD, NMR, and IR spectroscopies, together with single-crystal X-ray crystallography. The electrochemical properties of these complexes, which are highly dependent on the coordination mode of sulfinate ligands, are also described. © 2011 American Chemical Society

Synthesis and characterization of natural red dye from Caesalpinia sappan linn

Energy Technology Data Exchange (ETDEWEB)

Mulyanto, Subur, E-mail: subur.mulyanto@poltekba.ac.id [Graduate Program of Mechanical Engineering, SebelasMaret University, Jl. Ir. Sutami 36 A, Surakarta (Indonesia); Department of Mechanical Engineering, State Polytechnic of Balikpapan, Jl. Soekarno-Hatta Km.8 Balikpapan (Indonesia); Suyitno,, E-mail: suyitno@uns.ac.id; Rachmanto, Rendy Adhi, E-mail: rendy.ar@gmail.com; Hidayat, Lullus Lambang Govinda, E-mail: lulus-l@yahoo.com; Hadi, Syamsul, E-mail: syamsulhadi@ft.uns.ac.id [Department of Mechanical Engineering, SebelasMaret University, Jl. Ir. Sutami 36 A, Surakarta (Indonesia); Wibowo, Atmanto Heru, E-mail: aheruwibowo@yahoo.com [Department of Chemistry, SebelasMaret University, Jl. Ir. Sutami 36 A, Surakarta (Indonesia)

2016-03-29

The study reports the synthesis and characterization of natural red dye. The dyes were extracted from woods of Caesalpiniasappanlinn at varied temperatures of 70, 80, 90, and 100°C for three hours. The dry wood chips and water at a ratio of 6:1 were immersed in the reactor of 150 liters. The absorbance spectra of the natural red dyes were measured by ultra-violet-visible spectroscopy. Meanwhile, Fourier transform infrared spectroscopy was used to investigate the functional groups of the natural red dyes. In addition, the basic production cost was calculated and the fastness property towards cotton fabrics was investigated according to the Indonesia national standard of 105-C06:2010, 105-B01:2010, and 0288-2008. The results showed that the functional groups found the extracted red dyes indicated the complex bond of brazilein with peak absorbance at a wavelength of 538-540 nm. The extraction temperature also changed the functional group of brazilein. From the color, the absorbance peak, the functional groups, and the main production cost, the best parameter to synthesize the natural red dyes from Caesalpiniasappanlinn was at a temperature of 80°C for two hours. Moreover, the natural red dyes has the fastness to wash resistance, light resistance, and scrub resistance by 4-5, 4, and 3-4, respectively. However, further studies for synthesis the natural red dyes by using a continuous reactor are required to identify the naturally complex compounds in brazilein for improving the fastness properties and for reducing the cost.

Synthesis and characterization of natural red dye from Caesalpinia sappan linn

International Nuclear Information System (INIS)

Mulyanto, Subur; Suyitno,; Rachmanto, Rendy Adhi; Hidayat, Lullus Lambang Govinda; Hadi, Syamsul; Wibowo, Atmanto Heru

2016-01-01

The study reports the synthesis and characterization of natural red dye. The dyes were extracted from woods of Caesalpiniasappanlinn at varied temperatures of 70, 80, 90, and 100°C for three hours. The dry wood chips and water at a ratio of 6:1 were immersed in the reactor of 150 liters. The absorbance spectra of the natural red dyes were measured by ultra-violet-visible spectroscopy. Meanwhile, Fourier transform infrared spectroscopy was used to investigate the functional groups of the natural red dyes. In addition, the basic production cost was calculated and the fastness property towards cotton fabrics was investigated according to the Indonesia national standard of 105-C06:2010, 105-B01:2010, and 0288-2008. The results showed that the functional groups found the extracted red dyes indicated the complex bond of brazilein with peak absorbance at a wavelength of 538-540 nm. The extraction temperature also changed the functional group of brazilein. From the color, the absorbance peak, the functional groups, and the main production cost, the best parameter to synthesize the natural red dyes from Caesalpiniasappanlinn was at a temperature of 80°C for two hours. Moreover, the natural red dyes has the fastness to wash resistance, light resistance, and scrub resistance by 4-5, 4, and 3-4, respectively. However, further studies for synthesis the natural red dyes by using a continuous reactor are required to identify the naturally complex compounds in brazilein for improving the fastness properties and for reducing the cost.

Synthesis, characterization and magnetic properties of selected Laves and MAX phases

International Nuclear Information System (INIS)

Hamm, Christin Maria

2017-01-01

In this work the rare-earth free Laves phases Ti 2 M 3 Si with M = Mn, Fe, Co, Ni were synthesized by microwave heating and were structurally and magnetically characterized. Furthermore, the solid solution Ti 2 (Co 1-x Fe x ) 3 Si was synthesized by arc melting and spark plasma sintering, as well as their magnetic behavior was studied. In addition to the Laves phases, the focus was on the synthesis and characterization of aluminum-based MAX phases. For the first time the ternary carbides were prepared by microwave heating. The phase-pure representation of MAX phases was particularly challenging for synthetic solid-state chemistry. The susceptor-assisted microwave heating allows the synthesis of high-quality samples, which was shown in this work on M 2 AlC (M = Ti, V, Cr) and V 4 AlC 3 . Furthermore, for the first time, the doping of these materials with Mn and Fe was successful. In addition to the structural characterization of the new phases, the microstructure and magnetic properties are discussed in this work. Using these doped compounds as well as the compound V 4 AlC 3 , it has been shown that field-activated synthesis, particularly susceptor-assisted microwave heating, are a very good synthesis method for compounds which are hard or sometimes not synthesized by conventional methods.

Synthesis, characterization and magnetic properties of novel μ-oxamido heterodinuclear copper(II) - lanthanide(III) complexes

International Nuclear Information System (INIS)

Li, Y.T.; Miao, M.M.; Liao, D.Z.; Jiang, Z.H.; Wang, G.L.

1995-01-01

Six novel μ-oxamido heterobinuclear complexes have been prepared and identified as Cu(oxpn)Ln(L) 2 (ClO 4 ) 3 , where oxpn denotes the N, N'-bis(3-aminopropyl)oxamido dianion, L, 1,10-phenanthroline (phen) and Ln stands for La, Nd, Gd, Tb, Ho, Er. The complexes Cu(oxpn)Gd(oxpn)Gd(phen) 2 (ClO 4 ) 3 were characterized with variable temperature magnetic susceptibility (4-300 K). The exchange integral J (Cu-Gd) was found to be 2.03 cm -1 . The result is commensurate with ferromagnetic interaction between the adjacent metal ions. One plausible mechanism that can cause a ferromagnetic coupling between Gd(III) and Cu(II) is also discussed in terms of spin polarized. (author). 32 refs, 3 figs, 3 tabs

Synthesis, Structural Characterization and Antimicrobial Activity of Cu(II and Fe(III Complexes Incorporating Azo-Azomethine Ligand

Directory of Open Access Journals (Sweden)

Mohammad Azam

2018-04-01

Full Text Available We are reporting a novel azo-azomethine ligand, HL and its complexes with Cu(II and Fe(III ions. The ligand and its complexes are characterized by various physico-chemical techniques using C,H,N analyses, FT-IR, 1H-NMR, ESI-MS and UV-Vis studies. TGA analyses reveal complexes are sufficiently stable and undergo two-step degradation processes. The redox behavior of the complexes was evaluated by cyclic voltammetry. Furthermore, the ligand and its complexes were tested for antimicrobial activity against bacterial and fungal strains by determining inhibition zone, minimal inhibitory concentration (MIC and minimal bactericidal concentration (MBC. The complexes showed moderate antimicrobial activity when tested against Gram +ve and Gram −ve bacterial strains. To obtain insights into the structure of ligand, DFT studies are recorded. The results obtained are quite close to the experimental results. In addition, the energy gap, chemical hardness, softness, electronegativity, electrophilic index and chemical potential were calculated using HOMO, LUMO energy value of ligand.

Synthesis and characterization of tin(II) complexes of fluorinated Schiff bases derived from amino acids.

Science.gov (United States)

Singh, Har Lal

2010-07-01

New tin(II) complexes of general formula Sn(L)(2) (L=monoanion of 3-methyl-4-fluoro-acetophenone phenylalanine L(1)H, 3-methyl-4-fluoro-acetophenone alanine L(2)H, 3-methyl-4-fluoro acetophenone tryptophan L(3)H, 3-methyl-4-fluoro-acetophenone valine L(4)H, 3-methyl-4-fluoro-acetophenone isoleucine L(5)H and 3-methyl-4-fluoro-acetophenone glycine L(6)H) have been prepared. It is characterized by elemental analyses, molar conductance measurements and molecular weight determinations. Bonding of these complexes is discussed in terms of their UV-visible, infrared, and nuclear magnetic resonance ((1)H, (13)C, (19)F and (119)Sn NMR) spectral studies. The ligands act as bidentate towards metal ions, via the azomethine nitrogen and deprotonated oxygen of the respective amino acid. Elemental analyses and NMR spectral data of the ligands with their tin(II) complexes agree with their proposed square pyramidal structures. A few representative ligands and their tin complexes have been screened for their antibacterial activities and found to be quite active in this respect. Copyright 2010 Elsevier B.V. All rights reserved.

Synthesis and Characterization of Pyridino(1,4-Η-cyclohexa-1,3-dieneDerivatives of Iron Tricarbonyl Complexes

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T. I. Odiaka

2011-01-01

Full Text Available In this synthesis, we have been able to show that, the addition of x- substituted pyridines, (X = H, 2- Me, 3- Me 4- Me, 4-NH2 and 4-N(CH32 to the dienyl ring of the organometallic cation, [(Fe(CO3 (1-5- η-2-Me0C3H6]BF4 and [(Fe(CO3(1-5-η-C6H7]BF4 gives ionic substituted diene products, (X C5H4-C6H6Y (Fe(CO3] BF4,Y=H or 2-MeO. The reaction takes place at ordinary room temperature. The resulting products were isolated and characterized.

Synthesis of ultrafine alumina powders using egg white as complexing medium

International Nuclear Information System (INIS)

Salem, R.E.P.; Guilherme, K. A.; Chinelatto, A.S.A.; Chinelatto, A.L.

2011-01-01

Synthesis of alumina powders through chemical methods has been attracting much attention of researchers in the past few years, due to the ability to produce powders in nanometric scale with high degree of purity. In this work, there were synthesized alumina powders through a chemical route, using egg white as a complexing medium and aluminium nitrate as the source of Al 3+ cations. Egg white contains ovalbumin, a protein which acts effectively on the isolation of aluminium cations during the mixing process, enabling the formation of ultrafine alumina powders in a relatively economic and environmentally friendly way. The powders obtained by calcinations of the precursor resin were characterized by X-ray diffraction, specific surface area measurements, infrared spectroscopy and scanning electron microscopy. It was observed that the egg white, present at the reaction medium, allowed obtaining transition alumina powders, with high degree of purity. (author)

Synthesis, crystal structure and computational chemistry research of a Zinc(II complex: [Zn(Pt(Biim2

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Teng Fei

2012-01-01

Full Text Available The title metal-organic coordination complex [Zn(pt(Biim2] (pt=phthalic acid, benzene-1,2-dicarboxylate, Biim=2,2'-biimidazole 1 has been obtained by using hydrothermal synthesis and characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/n with a = 8.5466(15 Å, b = 11.760(2 Å, c = 20.829(4 Å, β = 95.56(2º, V = 2083.5(6 Å3, Mr =497.78, Dc = 1.587 g/cm3, μ(MoKα = 1.226 mm−1, F(000 = 1016, Z = 4, the final R = 0.0564 and wR = 0.1851 for 3656 observed reflections (I > 2σ(I. The elemental analysis, IR, TG and the theoretical calculation were also investigated.

Synthesis and characterization of cadmium doped lead–borate ...

Indian Academy of Sciences (India)

Unknown

Mater. Sci., Vol. 29, No. 1, February 2006, pp. 55–58. © Indian Academy of Sciences. 55. Synthesis and characterization of cadmium doped lead–borate glasses. A A ALEMI*, H SEDGHI†, A R MIRMOHSENI and V GOLSANAMLU. Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.

Synthesis, Characterization, and Antibacterial Studies of Mixed Ligand Dioxouranium Complexes with 8-Hydroxyquinoline and Some Amino Acids

Science.gov (United States)

Patil, Sunil S.; Thakur, Ganesh A.; Shaikh, Manzoor M.

2011-01-01

Mixed ligand complexes of dioxouranium (VI) of the type [UO2(Q)(L)·2H2O] have been synthesized using 8-hydroxyquinoline (HQ) as a primary ligand and amino acids (HL) such as L-threonine, L-tryptophan, and L-isoleucine as secondary ligands. The metal complexes have been characterized by elemental analysis, electrical conductance, magnetic susceptibility measurements, and spectral and thermal studies. The electrical conductance studies of the complexes indicate their nonelectrolytic nature. Magnetic susceptibility measurements revealed diamagnetic nature of the complexes. Electronic absorption spectra of the complexes show intraligand and charge transfer transitions, respectively. Bonding of the metal ion through N- and O-donor atoms of the ligands is revealed by IR studies, and the chemical environment of the protons is confirmed by NMR studies. The thermal analysis data of the complexes indicate the presence of coordinated water molecules. The agar cup and tube dilution methods have been used to study the antibacterial activity of the complexes against the pathogenic bacteria S. aureus, C. diphtheriae, S. typhi, and E. coli. PMID:22389843

Synthesis and self-assembly of complex hollow materials

KAUST Repository

Zeng, Hua Chun

2011-01-01

Hollow materials with interiors or voids and pores are a class of lightweight nanostructured matters that promise many future technological applications, and they have received significant research attention in recent years. On the basis of well-known physicochemical phenomena and principles, for example, several solution-based protocols have been developed for the general preparation of these complex materials under mild reaction conditions. This article is thus a short introductory review on the synthetic aspects of this field of development. The synthetic methodologies can be broadly divided into three major categories: (i) template-assisted synthesis, (ii) self-assembly with primary building blocks, and (iii) induced matter relocations. In most cases, both synthesis and self-assembly are involved in the above processes. Further combinations of these methodologies appear to be very important, as they will allow one to prepare functional materials at a higher level of complexity and precision. The synthetic strategies are introduced through some simple case studies with schematic illustrations. Salient features of the methods developed have been summarized, and some urgent issues of this field have also been indicated. © 2011 The Royal Society of Chemistry.

Synthesis and characterization of a novel meso-porphyrin and its metallo derivatives

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Paulo Cesar Bega

2014-02-01

Full Text Available There has been a growing interest in the properties of substituted meso-tetraarylporphyrins and metallo porphyrins as catalysts for oxidation of hydrocarbons, oxygen detection, among others. This work describes the synthesis of a new porphyrin, 5,10,15,20-tetrakis(4-butoxy-3-methoxyphenylporphyrin, and its metallo complexes. Herein it was used a readily available reactant, vanillin, as starting material which was submitted to alkylation with n-bromobutane affording the synthetic precursor. The desired porphyrin was obtained by reacting the O-alkylated aldehyde with pyrrole in the presence of propionic acid (Alder-Longo method. The purified porphyrin was then subjected to the metallation process using iron (II and manganese (II salts. The synthesized compounds were characterized by IR, UV-Vis, NMR and EPR spectroscopy.

Synthesis, physico-chemical and antimicrobial screening studies on 14 and 16-membered hexaazamacrocyclic complexes bearing pendant amine groups

Directory of Open Access Journals (Sweden)

Shakir Mohammad

2006-01-01

Full Text Available The synthesis and characterization of a series of 14 and 16-membered hexaazamacrocyclic complexes, which were obtained via template condensation of 1,2- diaminoethane or 1,3-diaminopropane, formaldehyde and hydrazine hydrate in the presence of first row transition metal salts are reported. Complexes of the types, [ML¹(NO32]; [CuL¹](NO32 and [ML²Cl2]; [CuL²]Cl2 (where M = Co(II, Ni(II and Zn(II, were obtained. Elemental analyses, IR spectra, ¹H NMR, EPR, UV-Vis, magnetic susceptibility and conductivity measurements have ascertained the overall geometry and stereochemistry of the complexes. An octahedral geometry has been suggested for all the complexes, except for copper compounds, in which the metal centre coordinates to the four nitrogen atoms of macrocyclic ligand in a square planar fashion. These complexes were screened against different fungi and bacteria in vitro and were found to be potentially active in the concentration 5 mg mL-1.

Synthesis, structure, theoretical studies and luminescent properties of a ternary erbium(III) complex with acetylacetone and bathophenanthroline ligands

Energy Technology Data Exchange (ETDEWEB)

Martín-Ramos, Pablo [CEMDRX, Department of Physics, Universidade de Coimbra, Rua Larga, P-3004-516 Coimbra (Portugal); Advanced Materials Laboratory, ETSIIAA, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain); Silva, Pedro S. Pereira, E-mail: psidonio@pollux.fis.uc.pt [CEMDRX, Department of Physics, Universidade de Coimbra, Rua Larga, P-3004-516 Coimbra (Portugal); Chamorro-Posada, Pedro [Higher Technical School of Telecommunications Engineering, Universidad de Valladolid, Campus Miguel Delibes, Paseo Belén 15, 47011 Valladolid (Spain); Silva, Manuela Ramos [CEMDRX, Department of Physics, Universidade de Coimbra, Rua Larga, P-3004-516 Coimbra (Portugal); Milne, Bruce F. [Centre for Computational Physics, Department of Physics, Universidade de Coimbra, P-3004-516 Coimbra (Portugal); Donostia International Physics Centre, Paseo Manuel de Lardizabal 4, 20018 Donostia-San Sebastián (Spain); Nogueira, Fernando [Centre for Computational Physics, Department of Physics, Universidade de Coimbra, P-3004-516 Coimbra (Portugal); Martín-Gil, Jesús [Advanced Materials Laboratory, ETSIIAA, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain)

2015-06-15

A novel erbium(III) complex with acetylacetone (Hacac) and bathophenanthroline (4,7-diphenyl-1,10-phenanthroline, bath) ligands, formulated as [Er(acac){sub 3}(bath)], has been characterized by elemental analysis, X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, absorption and emission spectroscopies. In the theoretical part of this study, semi-empirical quantum chemistry methods using AM1, PM3, PM6 and PM7 models have been employed to predict the structure of the complex, calculate the geometric and crystallographic parameters, and make comparisons with spectroscopic data using INDO/S-CI calculations. Real-time time-dependent density-functional theory (TDDFT) has also been used to calculate the optical absorption spectrum of the complex in the gas phase. - Highlights: • Synthesis and structure of a new erbium(III) β-diketonate complex. • TDDFT used for the first time to calculate the optical absorption spectrum. • Complex show strong near-infrared luminescence at 1.53 µm due to antenna effect.

Synthesis, structure, theoretical studies and luminescent properties of a ternary erbium(III) complex with acetylacetone and bathophenanthroline ligands

International Nuclear Information System (INIS)

Martín-Ramos, Pablo; Silva, Pedro S. Pereira; Chamorro-Posada, Pedro; Silva, Manuela Ramos; Milne, Bruce F.; Nogueira, Fernando; Martín-Gil, Jesús

2015-01-01

A novel erbium(III) complex with acetylacetone (Hacac) and bathophenanthroline (4,7-diphenyl-1,10-phenanthroline, bath) ligands, formulated as [Er(acac) 3 (bath)], has been characterized by elemental analysis, X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, absorption and emission spectroscopies. In the theoretical part of this study, semi-empirical quantum chemistry methods using AM1, PM3, PM6 and PM7 models have been employed to predict the structure of the complex, calculate the geometric and crystallographic parameters, and make comparisons with spectroscopic data using INDO/S-CI calculations. Real-time time-dependent density-functional theory (TDDFT) has also been used to calculate the optical absorption spectrum of the complex in the gas phase. - Highlights: • Synthesis and structure of a new erbium(III) β-diketonate complex. • TDDFT used for the first time to calculate the optical absorption spectrum. • Complex show strong near-infrared luminescence at 1.53 µm due to antenna effect

Synthesis and spectral studies on Cd(II) dithiocarbamate complexes and their use as precursors for CdS nanoparticles

Science.gov (United States)

Sathiyaraj, Ethiraj; Padmavathy, Krishnaraj; Kumar, Chandran Udhaya; Krishnan, Kannan Gokula; Ramalingan, Chennan

2017-11-01

Bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (1) and (2,2‧-bipyridine) bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (2) have been synthesized and characterized by FT-IR, 1HNMR and 13C NMR analyses. For the complex 2, single crystal X-ray diffraction analysis and computational studies (optimized geometry, HOMO-LUMO and MEP) have been executed employing DFT/B3LYP method with LANL 2DZ basic set. The optimized bond lengths and bond angles agree well with the experimental results. The complexes 1 and 2 have been used as single source precursors for the synthesis of ethyleneglycol capped CdS1 and CdS2 nanoparticles, respectively. CdS1 and CdS2 nanoparticles have been synthesized by solvothermal method. PXRD, SEM, Elemental colour mapping, EDAX, TEM and UV-Vis spectroscopy have been used to characterize the as-prepared CdS nanoparticles. The X-ray diffraction pattern confirms both their hexagonal structures.

synthesis and spectra characterization of mixed- ligand complexes

African Journals Online (AJOL)

BARTH EKWUEME

The Schiff base ligand, N-Propylidene-2-methylpyridylamine was obtained from the condensation of 2- aminomethypyridine and propanal.Also, its complexes with Cu(II),Ni(II),Zn(II),Co(II) .... determined with Thomas–Hoover capillary melting apparatus. RESULTS AND DISCUSSION. N-propylidene-2-methylpyridylamine ...

Synthesis and reactivity of triscyclopentadienyl uranium (III) and (IV) complexes

International Nuclear Information System (INIS)

Berthet, J.C.

1992-01-01

The reactions of (RC 5 H 4 ) 3 U with R=trimethylsilylcyclopentadienyl or tertiobutylcyclopentadienyl are studied for the synthesis of new uranium organometallic compounds. Reactions with sodium hydride are first described uranium (III) anionic hydrides obtained are oxidized for synthesis of stable uranium (IV) organometallic hydrides. Stability of these compounds is discussed. Reactivity of these uranium (III) and (IV) hydrides are studied. Formation of new binuclear compounds with strong U-O and U-N bonds is examined and crystal structure are presented. Monocyclooctatetraenylic uranium complexes are also investigated

Physicochemical characterization of functionalized-nanostructured-titania as a carrier of copper complexes for cancer treatment

International Nuclear Information System (INIS)

López, Tessy; Ortiz, Emma; Guevara, Patricia; Gómez, Esteban; Novaro, Octavio

2014-01-01

In the present paper we report the preparation and characterization of functionalized-TiO 2 (F-TiO 2 ) to obtain a biocompatible material to be used as carrier of alternative anticancer agents: copper acetate and copper acetylacetonate. The sol–gel procedure was used to prepare the fuctionalized titania material through hydrolysis and condensation of the titanium's butoxide. Sulfate, amine and phosphate ions served as functional groups which were anchored to the titania's surface. Mineral acids and gamma amine butyric acid were the precursors and they were added at the initial step of the synthesis. The copper complexes were loaded on titania and were also added to the reactor synthesis from the beginning. Infrared and ultraviolet–visible spectroscopies were the principal techniques used to the characterization of F-TiO 2 and copper complexes loaded on titania materials. Transmission Electronic Microscopy (TEM) was used to complement the characterization's studies. The biocompatibility of F-TiO 2 was evaluated by treating different cancer cell lines with increased concentration of this compound. The amine, the sulfate and the phosphate on the titania's surface, as well as the integral structures of the metal complexes on titania were well identified by infrared and ultraviolet–visible spectroscopies. The TEM photographs of Cu(acac) 2 /F-TiO 2 and Cu(Oac) 2 /F-TiO 2 materials showed the formation of nanoparticles, which have sizes ranging from 4 to 10 nm, with no morphology alterations in comparison with F-TiO 2 nanoparticles, suggesting that the presence of low quantities of copper do not affect the structure of the nanoparticles. The Energy Dispersive Spectroscopy (EDS) confirms the presence of copper on the titania's nanoparticles. The biological results indicate that there is more than 90% cell survival, thus suggesting that F-TiO 2 does not cause damage to the cells. Therefore, highly biocompatible titania was obtained by

Recent progress in the direct synthesis of hierarchical zeolites: synthetic strategies and characterization methods

KAUST Repository

Liu, Zhaohui

2017-06-16

Hierarchically structured zeolites combine the merits of microporous zeolites and mesoporous materials to offer enhanced molecular diffusion and mass transfer without compromising the inherent catalytic activities and selectivity of zeolites. This short review gives an introduction to the synthesis strategies for hierarchically structured zeolites with emphasis on the latest progress in the route of ‘direct synthesis’ using various templates. Several characterization methods that allow us to evaluate the ‘quality’ of complex porous structures are also introduced. At the end of this review, an outlook is given to discuss some critical issues and challenges regarding the development of novel hierarchically structured zeolites as well as their applications.

Synthesis and characterization of new ionic liquids

International Nuclear Information System (INIS)

Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S.; Iglesias, M.; Universidad de Santiago de Compostela

2010-01-01

In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

Controlled synthesis of titania using water-soluble titanium complexes: A review

Science.gov (United States)

Truong, Quang Duc; Dien, Luong Xuan; Vo, Dai-Viet N.; Le, Thanh Son

2017-07-01

The development of human society has led to the increase in energy and resources consumption as well as the arising problems of environmental damage and the toxicity to the human health. The development of novel synthesis method which tolerates utilization of toxic solvents and chemicals would fulfill the demand of the society for safer, softer, and environmental friendly technologies. For the past decades, a remarkable progress has been attained in the development of new water-soluble titanium complexes (WSTC) and their use for the synthesis of nanocrystalline titanium dioxide materials by aqueous solution-based approaches. The progress of synthesis of nanocrystalline titanium dioxide using such WSTCs is reviewed in this work. The key structural features responsible for the successfully controlled synthesis of TiO2 are discussed to provide guidelines for the morphology-controlled synthesis. Finally, this review ends with a summary and some perspectives on the challenges as well as new directions in this fascinating research.

Synthesis, Characterization and Antimicrobial Activity of Zirconium (IV) Complexes

Energy Technology Data Exchange (ETDEWEB)

Sharma, Shobhana; Jain, Asha; Saxena, Sanjiv [Univ. of Rajasthan, Jaipur (India)

2012-08-15

Heteroleptic complexes of zirconium (IV) derived from bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic β-diketones of the general formula ZrLL' (where L'H{sub 2}=RCNH(C{sub 6}H{sub 4})SC : C(OH)N(C{sub 6}H{sub 5})N : CCH{sub 3}, R=-C{sub 6}H{sub 5}, -C{sub 6}H{sub 4}Cl(p) and L'H{sub 2}=R'C : (NOH)C : C(OH)N(C{sub 6}H{sub 5})N : CCH{sub 3}, R' = -CH{sub 2}CH{sub 3}, -C{sub 6}H{sub 5}, -C{sub 6}H{sub 4}Cl (p) were prepared by the reactions of zirconium tetrachloride with disodium salts of Schiff bases (L Na{sub 2}) and oximes of heterocyclic β-diketones (L' Na{sub 2}) in 1:1:1 molar ratio in dry refluxing THF. The structures of these monomeric zirconium (IV) complexes were elucidated with the help of elemental analysis, molecular weight measurements, spectroscopic (IR, NMR and mass) studies. A distorted trigonal bipyramidal geometry may be suggested for these heteroleptic zirconium (IV) complexes. The ligands (bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic β-diketones) and their heteroleptic complexes of zirconium (IV) were screened against A. flavus, P. aeruginesa and E. coli.

New 3,4-diaminobenzoic acid Schiff base compounds and their complexes: synthesis, characterization and thermodynamics.

Science.gov (United States)

Mohammadi, Khosro; Niad, Mahmood; Jafari, Tahereh

2014-03-25

Some new tetradentate Schiff base ligands (H3L) were prepared via condensation of 3,4-diaminobenzoic acid with 2-hydroxybenzaldehyde derivatives, such as 3,4-bis((E)-2,4-dihydroxybenzylideneamino)benzoic acid (H3L(1)), 3,4-bis((E)-2-hydroxy-3-methoxybenzylideneamino)benzoic acid (H3L(2)) and 3,4-bis((E)-5-bromo-2-hydroxybenzylideneamino)benzoic acid (H3L(4)). Additionally, a tetradentate Schiff base ligand 3,4-bis((E)-2-hydroxybenzylideneamino)benzoic acid (H3L(3)) and its complexes were synthesized. Their metal complexes of Co(II), Ni(II), Cu(II) and Zn(II) were prepared in good yields from the reaction of the ligands with the corresponding metal acetate. They were characterized based on IR, (1)H NMR, Mass spectroscopy and UV-Vis spectroscopy. Also, the formation constants of the complexes were measured by UV-Vis spectroscopic titration at constant ionic strength 0.1M (NaClO4), at 25 °C in dimethylformamide (DMF) as a solvent. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Synthesis and characterization of a layered double hydroxide containing an intercalated nickel(II) citrate complex

International Nuclear Information System (INIS)

Wang Lianying; Wu Guoqing; Evans, David G.

2007-01-01

The nickel(II) citrate complex anion ([Ni(C 6 H 4 O 7 )] 2- ) may be intercalated into the interlayer galleries of a layered double hydroxide (LDH) host by a process involving ion-exchange with an Mg 2 Al-NO 3 LDH precursor. The powder X-ray diffraction (XRD) pattern confirms that the layered structure is maintained. The thermal decomposition process of the complex anion-intercalated material has been characterized by in situ high temperature powder XRD, thermogravimetry-differential thermal analysis (TG-DTA) and coupled with mass spectrometry (MS). The thermal stability of the nickel(II) citrate complex anion intercalated in LDHs in air is lower than that in the sodium salt. Calcination generates a high degree of nickel(II) oxide dispersion in a matrix of magnesium and aluminium oxide phases which should be an advantage if the materials are used as catalyst precursors. Based on the observed data, a structural model for the [Ni(C 6 H 4 O 7 )] 2- anion intercalated in the galleries of the LDH is proposed

Synthesis and characterization of some metal complexes of a Schiff base derived from ninhydrin and α,L-alanine

Directory of Open Access Journals (Sweden)

Mehabaw Getahun Derebe

2002-06-01

Full Text Available Complexes of Mn(II, Fe(III, Co(II, Ni(II and Zn(II with an intermediate Schiff base derived from ninhydrin and α,L-alanine (indane-1,3-dione-2-imine-N-2-propionate, IDIP were successfully synthesized. All complexes were distinctly colored and were characterized by elemental analysis, molar conductance, magnetic susceptibility, infrared and electronic spectral studies. The ligand (Schiff base was shown to behave as a monobasic tridentate ONO donor. The Mn(II and Fe(III complexes contain only one ligand molecule plus water and chloride(s per metal ion, while all the others contain two ligand molecules per metal ion. An octahedral geometry is proposed for the metal complexes.

Synthesis and characterization of bulk Cu2ZnSnX4 (X: S, Se) via thermodynamically supported mechano-chemical process

International Nuclear Information System (INIS)

Pareek, Devendra; Balasubramaniam, K.R.; Sharma, Pratibha

2015-01-01

Materials with the general formula, Cu 2 ZnSnX 4 (CZTX; X: Group 16 elements), with X being S/Se, have been receiving considerable attention due to their utility as an absorber layer in solar photovoltaics (PV). This paper reports on the synthesis of CZTSe and CZTS nanocrystalline powders at low temperatures, starting from elemental metal and chalcogen powders, via the low cost, scalable technique of ball milling. The prepared samples were well characterized using the different characterization tools. XRD, Raman, SEM and TEM studies confirm the formation of single-phase, stoichiometric, nano-crystalline kesterite CZTS and CZTSe powders. The low temperature phase selection of the complex quaternary compound in this system is seen as a direct consequence of the thermodynamic facilitation, coupled with the capability of mechano-chemical synthesis to aid in overcoming kinetic constraints. The optical bandgap of the various samples of CZTS was observed in the range of 1.4–1.6 eV and corresponding values for CZTSe was observed to be in the range of 1.08–1.18 eV. Our work provides a pathway for developing cheap, scalable, and ink-based techniques for low cost solar PV. - Graphical abstract: Display Omitted - Highlights: • A scalable route for synthesis of near phase pure CZTS/Se nano-crystals has been demonstrated. • Stoichiometric CZTS and CZTSe were synthesized via mechano-chemical synthesis route. • Synthesis at near room temperature is supported by thermodynamic calculations

Fe(II) and Co (II) complexes of (4-(4-bromophenyl)-[2,2'-bipyridine]-6-carboxylic acid) synthesis, characterization and electrochromic studies

International Nuclear Information System (INIS)

Saba, A.; Maqsood, Z.T.; Wasim, A.A.; Basha, F.Z.

2017-01-01

In this study novel complexes of substituted bipyridine (4-(4-bromophenyl)-[2,2'-bipyridine]-6-carboxylic acid) with Fe/sup +2/ and Co/sup +2/ were synthesized and characterized by different physical, analytical and spectral techniques which includes /sup 1/ H-NMR, MALDI-MS, FTIR, UV-VIS Spectrophotometry, CHN analysis and conductometry. Mole ratio method revealed that both complexes satisfied ML2 stoichiometry. Other characterization studies showed that substituted bipyridine acted as a tridentate ligand, with two pyridine N and one carboxylic O atom as binding sites per ligand molecule. The complexes were found octahedral, neutral and possessed fairly high molar absorptivities in visible region. Electrochromic studies revealed that Fe (II) complex had relatively good electrochromic properties with a reversible color change from blue to pale yellow. Co (II) complex, however, did not show significant electrochromic properties in the visible region. (author)

Synthesis, characterization, and photophysical properties of a thiophene-functionalized bis(pyrazolyl) pyridine (BPP) tricarbonyl rhenium(I) complex.

Science.gov (United States)

Lytwak, Lauren A; Stanley, Julie M; Mejía, Michelle L; Holliday, Bradley J

2010-09-07

A bromo tricarbonyl rhenium(I) complex with a thiophene-functionalized bis(pyrazolyl) pyridine ligand (L), ReBr(L)(CO)(3) (1), has been synthesized and characterized by variable temperature and COSY 2-D (1)H NMR spectroscopy, single-crystal X-ray diffraction, and photophysical methods. Complex 1 is highly luminescent in both solution and solid-state, consistent with phosphorescence from an emissive (3)MLCT excited state with an additional contribution from a LC (3)(pi-->pi*) transition. The single-crystal X-ray diffraction structure of the title ligand is also reported.

Synthesis and characterization of Taurine

Directory of Open Access Journals (Sweden)

B Bayarmaa

2014-10-01

Full Text Available Have been obtained 2-aminoethanesulfonic acid (taurine from ethanolamine, sulfuric acid and sodium sulfite during the synthesis in laboratory condition. The process involves two steps of reactions, the first was esterification of ethanolamine with sulfuric acid to produce the intermediate product of 2-aminoethyl ester which than was extended to the second step by sulfonation with sodium sulfite to produce 2-aminoethanesulfonic acid. Resulting product was analyzed using 1H-NMR, IR, FAB-MS analysis and examined purity characterizations of the synthesized products. DOI: http://dx.doi.org/10.5564/mjc.v14i0.200 Mongolian Journal of Chemistry 14 (40, 2013, p57-60

Synthesis and Characterization of Divalent Manganese, Iron, and Cobalt Complexes in Tripodal Phenolate/N-Heterocyclic Carbene Ligand Environments

DEFF Research Database (Denmark)

Käß, Martina; Hohenberger, Johannes; Adelhardt, Mario

2014-01-01

. The complete ligand series offers a convenient way of tuning the electronic and steric environment around the metal center, thus, allowing for control of the complex’s reactivity. This series of divalent complexes of Mn, Fe, and Co was synthesized and characterized by 1H NMR, IR, and UV/vis spectroscopy...... as well as by single-crystal X-ray diffraction studies. Variable-temperature SQUID magnetization measurements in the range from 2 to 300 K confirmed high-spin ground states for all divalent complexes and revealed a trend of increasing zero-field splitting |D| from Mn(II), to Fe(II), to Co(II) complexes...

Synthesis and characterization of a nanostructured matrix hydroxyapatite ceramic bone reconstruction

International Nuclear Information System (INIS)

Correa, P.; Camargo, N.H.A.; Silva, D.F.

2012-01-01

The nanostructured ceramics have been shown promise as biomaterials for bone reconstruction. Among calcium phosphates, hydroxyapatite Ca/P ratio = 1.67 mol stands out because of its crystallographic similarity with the mineral bone phase and biocompatibility. This work was based on synthesis and characterization of a nanostructured hydroxyapatite for use in reconstituting bone tissue. The synthesis method for obtaining the bioceramic powder occurred at process of dissolution/precipitation, involving CaO solid/liquid and phosphoric acid required for forming the composition of Ca/P = 1.67 mole. The material recovered from the synthesis was calcined at 900 ° C/2h, providing the hydroxyapatite powder nanometer. This was subjected to mechanical fragmentation process in mill attritor, providing a hydroxyapatite with modified surface morphology. The results presented relate to morphological characterization studies (SEM), mineralogical (XRD), chemical (FTIR) and particle size distribution, using the laser particle size analysis method. Such results showed the formation of hydroxyapatite phase and morphology satisfactory for use in reconstituting bone tissue

Bis(imidazolin-2-iminato) rare earth metal complexes: synthesis, structural characterization, and catalytic application.

Science.gov (United States)

Trambitas, Alexandra G; Melcher, Daniel; Hartenstein, Larissa; Roesky, Peter W; Daniliuc, Constantin; Jones, Peter G; Tamm, Matthias

2012-06-18

Reaction of anhydrous rare earth metal halides MCl(3) with 2 equiv of 1,3-bis(2,6-diisopropylphenyl)imidazolin-2-imine (Im(Dipp)NH) and 2 equiv of trimethylsilylmethyl lithium (Me(3)SiCH(2)Li) in THF furnished the complexes [(Im(Dipp)N)(2)MCl(THF)(n)] (M = Sc, Y, Lu). The molecular structures of all three compounds were established by single-crystal X-ray diffraction analyses. The coordination spheres around the pentacoordinate metal atoms are best described as trigonal bipyramids. Reaction of YbI(2) with 2 equiv of LiCH(2)SiMe(3) and 2 equiv of the imino ligand Im(Dipp)NH in tetrahydrofuran did not result in a divalent complex, but instead the Yb(III) complex [(Im(Dipp)N)(2)YbI(THF)(2)] was obtained and structurally characterized. Treatment of [(Im(Dipp)N)(2)MCl(THF)(n)] with 1 equiv of LiCH(2)SiMe(3) resulted in the formation of [(Im(Dipp)N)(2)M(CH(2)SiMe(3))(THF)(n)]. The coordination arrangement of these compounds in the solid state at the metal atoms is similar to that found for the starting materials, although the introduction of the neosilyl ligand induces a significantly greater distortion from the ideal trigonal-bipyramidal geometry. [(Im(Dipp)N)(2)Y(CH(2)SiMe(3))(THF)(2)] was used as precatalyst in the intramolecular hydroamination/cyclization reaction of various terminal aminoalkenes and of one aminoalkyne. The complex showed high catalytic activity and selectivity. A comparison with the previously reported dialkyl yttrium complex [(Im(Dipp)N)Y(CH(2)SiMe(3))(2)(THF)(3)] showed no clear tendency in terms of activity.

Lanthanide phosphonates: Synthesis, thermal stability and magnetic characterization

Energy Technology Data Exchange (ETDEWEB)

Amghouz, Z., E-mail: amghouz.uo@uniovi.es [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Garcia, J.R.; Garcia-Granda, S. [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Clearfield, A. [Department of Chemistry, Texas A and M University, College Station, TX 77842-3012 (United States); Rodriguez Fernandez, J.; Pedro, I. de [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

2012-09-25

Highlights: Black-Right-Pointing-Pointer Report of the complete series of lanthanide 1,4-phenylbis(phosphonate). Black-Right-Pointing-Pointer Synthesis under conventional hydrothermal synthesis or microwave-assisted hydrothermal synthesis. Black-Right-Pointing-Pointer Cation size is the key factor for the structural and particles size variations. Black-Right-Pointing-Pointer Thermal behaviour is characterized by unusual very high thermal stability. - Abstract: Series of novel organic-inorganic hybrids materials based on trivalent lanthanides (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and 1,4-phenylbis(phosphonate) obtained under hydrothermal conditions either by oven heat or microwave irradiation. The anhydrous compounds containing La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho, are isostructural. However, the compounds based on Y, Er, Tm, Yb, and Lu are hydrated and their structures have not yet been solved. The series of compounds are characterized by PXRD, TEM, SEM-EDX and thermal analyses (TG-MS and DSC). TEM study show a variable particles size with a minimum mean-particle size of ca. 30 nm. These compounds exhibit unusual very high thermal stability. The size of particles and the thermal stability are depending on lanthanide(III) cation features. All the investigated materials show paramagnetic behaviour. The magnetic susceptibility data follow a Curie-Weiss laws with paramagnetic effective moments in good agreement with those expected for Ln{sup 3+} free ions.

Vinylogous Nicholas reactions in the synthesis of bi- and tricyclic cycloheptynedicobalt complexes.

Science.gov (United States)

Kolodziej, Izabela; Green, James R

2015-11-28

The Lewis acid mediated intramolecular Nicholas reactions of allylic acetate enyne-Co2(CO)6 complexes afford cycloheptenyne-Co2(CO)6 complexes in three manifestations. Electron rich aryl substituted alkyne complexes give tricyclic 6,7,x-benzocycloheptenyne complexes, with x = 5, 6, or 7. Allylsilane substituted complexes afford exo methylene bicyclic x,7-cycloheptenyne complexes (x = 6,7). The allyl acetate function may also be replaced by a benzylic acetate, to afford dibenzocycloheptyne-Co2(CO)6 complexes. Following reductive complexation, the methodology may be applied to the synthesis of the icetexane diterpene carbon framework.

Synthesis and structure of the unligated carbene of chromium

Energy Technology Data Exchange (ETDEWEB)

Billups, W.E.; Souchan Chang; Hauge, R.H.; Margrave, J.L. (Rice Univ., Houston, TX (United States))

1993-04-14

Complexes with metal-carbon double bonds have found applications as intermediates in many important catalytic reactions including cyclopropanation of alkenes by diazoalkanes, Fischer-Tropsch synthesis, olefin metathesis, Ziegler-Natta polymerization, alkane activation, and in the decomposition of transition metal alkyl complexes. However, complexes with the simplest carbene, CH[sub 2], coordinated to the metal center are relatively rare. In this paper the authors report the synthesis and characterization of the simple unligated carbene of chromium by FTIR matrix isolation spectroscopy. 7 refs., 3 figs., 4 tabs.

Synthesis, Properties Characterization and Applications of Various Organobismuth Compounds

Directory of Open Access Journals (Sweden)

Jingfei Luan

2011-05-01

Full Text Available Organobismuth chemistry was emphasized in this review article due to the low price, low toxicity and low radioactivity characteristics of bismuth. As an environmentally-friendly class of organometallic compounds, different types of organobismuth compounds have been used in organic synthesis, catalysis, materials, etc. The synthesis and property characterization of many organobismuth compounds had been summarized. This review article also presented a survey of various applications of organobismuth compounds in organic transformations, as reagents or catalysts. The reactivity, reaction pathways and mechanisms of reactions with organobismuths were discussed. Less common and limiting aspects of organobismuth compounds were also briefly mentioned.

Quantum physics, relativity and complex spacetime towards a new synthesis

CERN Document Server

Kaiser, Gerald

1990-01-01

A new synthesis of the principles of quantum mechanics and Relativity is proposed in the context of complex differential geometry. The positivity of the energy implies that wave functions and fields can be extended to complex spacetime, and it is shown that this complexification has a solid physical interpretation as an extended phase space. The extended fields can be said to be realistic wavelet transforms of the original fields. A new, algebraic theory of wavelets is developed.

SYNTHESIS AND CHARACTERIZATION OF NEW HALOGENATED CURCUMINOIDS

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Eugenio Torres

2013-12-01

Full Text Available In this work a novel procedure of synthesis of compounds analogues to curcumin with halogens atoms in its structure is described, which can increase its solubility and biological activity. Four halogenated curcuminoids were obtained with great pharmacological interest, none of them reported in literature before. Synthesis was carried out by means of the aldol condensation assisted by microwaves of halogenated aromatic aldehydes and acetylacetona, using morpholine as basic catalyst, in absence of solvent, and the reaction just needed 1 min. The products were purified by treatment of the reaction mixture with methanol under ultrasound irradiation, followed by chromatographic column. All obtained compounds were characterized by infrared spectroscopy, nuclear magnetic resonance, quantitative elementary analysis and high resolution mass spectrometry. The RMN-1H data demonstrate in all structures of synthesized curcuminoids the enol form is the most favored.

Synthesis, characterization, and near-infrared luminescent properties of the ternary thulium complex covalently bonded to mesoporous MCM-41

International Nuclear Information System (INIS)

Feng Jing; Song Shuyan; Xing Yan; Zhang Hongjie; Li Zhefeng; Sun Lining; Guo Xianmin; Fan Weiqiang

2009-01-01

The crystal structure of a ternary Tm(DBM) 3 phen complex (DBM=dibenzoylmethane; phen=1, 10-phenanthroline) and the synthesis of hybrid mesoporous material in which the complex covalently bonded to mesoporous MCM-41 are reported. Crystal data: Tm(DBM) 3 phen C 59 H 47 N 2 O 7 Tm, monoclinic, P21/c, a=19.3216(12) A, b=10.6691(7) A, c=23.0165(15) A, α=90 deg., β=91.6330(10) deg., γ=90 deg., V=4742.8(5) A 3 , Z=4. The properties of the Tm(DBM) 3 phen complex and the corresponding hybrid mesoporous material [Tm(DBM) 3 phen-MCM-41] have been studied. The results reveal that the Tm(DBM) 3 phen complex is successfully covalently bonded to MCM-41. Both Tm(DBM) 3 phen complex and Tm(DBM) 3 phen-MCM-41 display typical near-infrared (NIR) luminescence upon excitation at the maximum absorption of the ligands, which contributes to the efficient energy transfer from the ligands to the Tm 3+ ion, an antenna effect. The full width at half maximum (FWHM) centered at 1474 nm in the emission spectrum of Tm(DBM) 3 phen-MCM-41 is 110 nm, which is the potential candidate of broadening amplification band from C band (1530-1560 nm) to S + band (1450-1480 nm) in optical area. - Graphical abstract: The crystal structure of Tm(DBM) 3 phen complex (DBM=dibenzoylmethane; phen=1, 10-phenanthroline). The complex is successfully covalently bonded to MCM-41 (Tm(DBM) 3 phen-MCM-41). After ligand-mediated excitation, the emission spectrum of Tm(DBM) 3 phen-MCM-41 shows the bands 802 and 1474 nm. The FWHM of the 1474-nm band for Tm(DBM) 3 phen-MCM-41 is 110 nm, such a broad spectrum enables a wide gain bandwidth for optical amplification

Synthesis and Spectroscopic Characterization of Two Tetrasubstituted Cationic Porphyrin Derivatives

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Newton M. Barbosa Neto

2011-07-01

Full Text Available An imidazolium tetrasubstituted cationic porphyrin derivative (the free base and its Zn(II complex with five-membered heterocyclic groups in the meso-positions were synthesized using microwave irradiation, and the compounds obtained characterized by 1H-NMR and mass spectrometry. We observed that under microwave irradiation the yield is similar to when the synthesis is performed under conventional heating, however, the time required to prepare the porphyrins decreases enormously. In order to investigate the electronic state of these compounds, we employed UV-Vis and fluorescence spectroscopy combined with quantum chemical calculations. The results reveal the presence, in both compounds, of a large number of electronic states involving the association between the Soret and a blue-shifted band. The Soret band in both compounds also shows a considerable solvent dependence. As for emission, these compounds present low quantum yield at room temperature and no solvent influence on the fluorescence spectra was observed.

Synthesis and characterization of thermally oxidized ZnO films

Indian Academy of Sciences (India)

Administrator

Synthesis and characterization of thermally oxidized ZnO films. A P RAMBU1,* and N IFTIMIE2 .... R. −. Δ. = = (1) where Ra is the sensor resistance in the air and Rg is the .... ple, Aida and coworkers (2006) reported that the total oxidation is ...

Synthesis, characterization and anticancer activity of gold(I) complexes that contain tri-tert-butylphosphine and dialkyl dithiocarbamate ligands

KAUST Repository

Altaf, Muhammad

2015-03-10

Two new gold(I) complexes that contain tri-ter-butylphosphine and dialkyl dithiocarbamate ligands were synthesized and characterized by FTIR, NMR spectroscopy, Cyclic voltammetry, elemental analysis and X-ray diffraction. The in vitro cytotoxicity of both complexes was examined against A549 (lung cancer), MCF7 (breast cancer), and HeLa (cervical cancer) human cancer cell lines. Both complexes exhibit very strong in vitro cytotoxic effects against A549, MCF7 and HeLa cell lines. The screening of the cytotoxic activity based on IC50 data against the A549, MCF7, and HeLa lines shows that the synthesized gold(I) complexes are highly effective, particularly against HeLa cancer cell line. Based on IC50 data, the cytotoxic activity of both complexes is better than well-known commercial anticancer drug cisplatin against all the three cancer lines tested.

Community characterization of heterogeneous complex systems

International Nuclear Information System (INIS)

Tumminello, Michele; Miccichè, Salvatore; Lillo, Fabrizio; Mantegna, Rosario N; Varho, Jan; Piilo, Jyrki

2011-01-01

We introduce an analytical statistical method for characterizing the communities detected in heterogeneous complex systems. By proposing a suitable null hypothesis, our method makes use of the hypergeometric distribution to assess the probability that a given property is over-expressed in the elements of a community with respect to all the elements of the investigated set. We apply our method to two specific complex networks, namely a network of world movies and a network of physics preprints. The characterization of the elements and of the communities is done in terms of languages and countries for the movie network and of journals and subject categories for papers. We find that our method is able to characterize clearly the communities identified. Moreover our method works well both for large and for small communities

Synthesis, Characterization and Spectral Studies of Noble Heterobinuclear Complexes of Transition Metal Ions and their Biological Activity

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Netra Pal Singh

2011-01-01

Full Text Available Some noble heterobinuclear complexes of transition metal ions with bis(salicylaldehydemalonyl-dihydrazone in the presence of 5-nitroindazole Cu(II / Ni(II- chloride of the type [ML1M‘L2Cl2] or [ML1FeL2Cl2]Cl, where M = Ni(II, Cu(II and M' = Mn(II, Co(II, have been prepared. All the complexes have been characterized by IR, UV vis and EPR spectroscopy, elemental analysis, magnetic moment and molar conductance measurement. Spectral studies and magnetic moment measurement in DMF suggest the covalent nature of the complexes, except the [ML1FeL2Cl2]Cl complex which is 1:1 electrolyte. An octahedral geometry is proposed for M‘ and square planer for M for the heterobinuclear complexes. The low value of magnetic moment and overlapping EPR signals are due to spin crossover since both of the metals have unpaired electrons with same molecular symmetry. The lowering of the magnetic moment has been discussed. The biological activity (antifungal and antibacterial of the represented compounds has been studied.

Synthesis, characterization, photoluminescence and cytotoxic properties of novel luminescent Eu(III)complexes based on chromone Schiff base

Science.gov (United States)

Saif, M.; El-Shafiy, Hoda F.; Mashaly, Mahmoud M.; Eid, Mohamed F.; Nabeel, A. I.; Fouad, R.

2018-06-01

Three novel Eu(III) phosphor complexes, [Eu(HL)(OH2)2(C2H5OH)](NO3)2 (1), [Eu(HL)(Bpy)(NO3)2(EtOH)] (2) and [Eu(HL)(Phen)(NO3)2(H2O)] (3) (HL = (11E)-2-hydroxy-N/-((4-oxo-4H-chromen-3-yl)methylene)benzohydrazide; Bpy = 2,2/-bibyridyl and Phen = 1,10-phenanthroline) were prepared. Elemental, thermal, FT-IR and XRD methods were used to characterize their structural configuration. The HL behaves as a monoanionic tridentate ligand. The XRD analysis shows that the ligand and its Eu3+complexes are in nano domain. From fluorescence spectroscopy, all the prepared complexes are highly luminescent, having an impressive visual emission under UV excitation. The H2L and its Eu3+nano-complexes (1-3) were tested for their in vitro cytotoxicity against Ehrlich Ascites Carcinoma cell line (EAC). The Eu(III) nano-complexes (1-3) effectively inhibited EAC growth with IC50 value of 25 μM. The high antitumor activity of the Eu(III) nano-complexes (1-3) were attributed to its chemical structure, and nano size properties.

Synthesis, spectroscopy and antimicrobial activity of vanadium(III) and vanadium(IV) complexes involving Schiff bases derived from tranexamic acid and X-ray structure of Zwitter ion of tranexamic acid

International Nuclear Information System (INIS)

Shahzadi, S.; Ali, S.; Badshah, A.; Parvez, M.; Ahmed, E.; Malik, A.

2007-01-01

The synthesis of six new vanadium complexes of Schiff base derived from Tranexamic acid is reported. All the complexes were characterized by elemental analysis, infrared, electronic spectra, and mass spectrometry. FTIR data reveals that the Schiff base acts as a bidentate and the complexes exhibit the hexa-coordinated geometry in solid state. These complexes were screened for their biological activity against various bacterial and fungal strains. All the ligands show higher activity after complexation. The crystal structure of the Zwitter ion of the Tranexamic acid has been determined by X-ray single crystal diffraction [ru

Physicochemical Characterization of Inclusion Complex of Catechin ...

African Journals Online (AJOL)

with catechin, and characterize the physicochemical properties of the inclusion complex of catechin and ... microscopy (SEM), X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). ... complexes with bioactive compounds.

Synthesis, spectroscopic characterization and antimicrobial activity evaluation of new tridentate Schiff bases and their Co(II complexes

Directory of Open Access Journals (Sweden)

Ganesh More

2017-12-01

Full Text Available A series of Schiff base tridentate ligands and their respective Co(II complexes have been synthesized and characterized by elemental analysis, magnetic susceptibility, IR, NMR and UV–Visible spectra, thermal studies. The IR spectral data suggested that all the ligands acted as monobasic tridentate towards central Co(II ion with an ONO donor atoms sequentially. Analytical data and magnetic susceptibility revealed 1:2 metal to ligand stoichiometry and octahedral geometry for all Co(II complexes. All the prepared compounds were also screened for antimicrobial activity against 5 ESBL (Extended Spectrum β-lactamase and 5 MBL (Metallo β-lactamase producing uropathogens and for antitubercular activity against Mycobacterium tuberculosis (H37Rv strain. Keywords: Schiff base, Antitubercular, Antimicrobial, ESBL, MBL, Metal complex, o-hydroxyl aldehyde, Aminothiophene

Synthesis, characterization and thermal study of some transition metal complexes of an asymmetrical tetradentate Schiff base ligand

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ACHUT S. MUNDE

2010-03-01

Full Text Available Complexes of Cu(II, Ni(II, Co(II, Mn(II and Fe(III with an asymmetric tetradentate Schiff base ligand derived from dehydroacetic acid, 4-methyl-o-phenylenediamine and salicylic aldehyde were synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV–Vis, IR, 1H-NMR spectroscopy, X-ray diffraction analysis of powdered samples and thermal analysis, and screened for antimicrobial activity. The IR spectral data suggested that the ligand behaves as a dibasic tetadentate ligand towards the central metal ion with an ONNO donor atoms sequence. From the microanalytical data, the stoichiometry of the complexes 1:1 (metal:ligand was found. The physico-chemical data suggested square planar geometry for the Cu(II and Ni(II complexes and octahedral geometry for the Co(II, Mn(II and Fe(III complexes. The thermal behaviour (TGA/DTA of the complexes was studied and kinetic parameters were determined by Horowitz–Metzger and Coats–Redfern methods. The powder X-ray diffraction data suggested a monoclinic crystal system for the Co(II, Mn(II and Fe(III complexes. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus niger and Trichoderma viride.

Synthesis, Characterization, and Physicochemical Studies of Mixed Ligand Complexes of Inner Transition Metals with Lansoprazole and Cytosine

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Sarika Verma

2013-01-01

Full Text Available Few complexes of inner transition metals [Th(IV, Ce(IV, Nd(III, Gd(III] have been synthesized by reacting their metal salts with lansoprazole, 2-([3-methyl-4-(2,2,2-trifluoroethoxypyridin-2-yl]methylsulfinyl-1H-benzoimidazole and cytosine. All the complexes were synthesized in ethanolic medium. The yield percentage rangs from 80 to 90%. The complexes are coloured solids. The complexes were characterized through elemental analyses, conductance measurements, and spectroscopic methods (FT IR, FAB Mass, 1H NMR and UV. An IR spectrum indicates that the ligand behaves as bidentate ligands. The metal complexes have been screened for their antifungal activity towards Aspergillus niger fungi. The interaction of inner transition metals with lansoprazole, in presence of cytosine, has also been investigated potentiometrically at two different temperatures 26±1°C and 36±1°C and at 0.1 M (KNO3 ionic strength. The stability constants of ternary complexes indicate the stability order as Th(IV < Ce(IV < Gd(III < Nd(III. logK values obtained are positive and suggest greater stabilization of ternary complexes. The values of thermodynamic parameters (free energy (ΔG, enthalpy (ΔH, and entropy (ΔS are also calculated.

Synthesis and characterization of amorphous cellulose from triacetate of cellulose

International Nuclear Information System (INIS)

Vega-Baudrit, Jose; Sibaja, Maria; Nikolaeva, Svetlana; Rivera A, Andrea

2014-01-01

It was carried-out a study for the synthesis and characterization of amorphous cellulose starting from cellulose triacetate. X-rays diffraction was used in order to obtain the cellulose crystallinity degree, also infrared spectroscopy FTIR was used. (author)

Synthesis, physico-chemical properties and complexing abilities of new amphiphilic ligands from D-galacturonic acid.

Science.gov (United States)

Allam, Anas; Behr, Jean-Bernard; Dupont, Laurent; Nardello-Rataj, Véronique; Plantier-Royon, Richard

2010-04-19

This paper describes a convenient and efficient synthesis of new complexing surfactants from d-galacturonic acid and n-octanol as renewable raw materials in a two-step sequence. In the first step, simultaneous O-glycosidation-esterification under Fischer conditions was achieved. The anomeric ratio of the products was studied based on the main experimental parameters and the activation mode (thermal or microwave). In the second step, aminolysis of the n-octyl ester was achieved with various functionalized primary amines under standard thermal or microwave activation. The physico-chemical properties of these new amphiphilic ligands were measured and these compounds were found to exhibit interesting surface properties. Complexing abilities of one uronamide ligand functionalized with a pyridine moiety toward Cu(II) ions was investigated in solution by EPR titrations. A solid compound was also synthesized and characterized, its relative structure was deduced from spectroscopic data. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Synthesis and X-ray structure of the dysprosium(III) complex derived ...

African Journals Online (AJOL)

Synthesis and X-ray structure of the dysprosium(III) complex derived from the ligand 5-chloro-1 ... Bulletin of the Chemical Society of Ethiopia ... synthesized and its crystal structure determined by single X-ray diffraction at room temperature.

Characterization structural and morphology ZSM-5 zeolite by hydrothermal synthesis

International Nuclear Information System (INIS)

Silva, V.J.; Crispim, A.C.; Queiroz, M.B.; Laborde, H.M.; Rodrigues, M.G.F.; Menezes, R.R.

2009-01-01

Solid acids are catalytic materials commonly used in the chemical industry. Among these zeolites are the most important business processes including water treatment, gas separation, and cracking long hydrocarbon chains to produce high octane gasoline. Its synthesis, characterization and applications have been widely studied. The objective this study was to synthesize the ZSM-5 zeolite for future use in separation processes and catalysis. The zeolite ZSM-5 was prepared by hydrothermal synthesis at 170°C, using silica, deionized water and the director of structures (TPABr - tetrapropylammonium bromide). The materials were characterized by X ray diffraction (XRD), scanning electron microscopy (SEM) and semiquantitative chemical analysis by X ray fluorescence (XRF). According to the XRD was possible to observe the formation of ZSM-5 zeolite, with peaks intense and well defined. The SEM showed the formation of individual particles, clean, rounded shapes. (author)

Polymer Brushes: Synthesis, Characterization, Applications

Science.gov (United States)

Advincula, Rigoberto C.; Brittain, William J.; Caster, Kenneth C.; Rühe, Jürgen

2004-09-01

Materials scientists, polymer chemists, surface physicists and materials engineers will find this book a complete and detailed treatise on the field of polymer brushes, their synthesis, characterization and manifold applications. In a first section, the various synthetic pathways and different surface materials are introduced and explained, followed by a second section covering important aspects of characterization and analysis in both flat surfaces and particles. These specific surface initiated polymerization (SIP) systems such as linear polymers, homopolymers, block copolymers, and hyperbranched polymers are unique compared to previously reported systems by chemisorption or physisorption. They have found their way in both large-scale and miniature applications of polymer brushes, which is covered in the last section. Such 'hairy' surfaces offer fascinating opportunities for addressing numerous problems of both academic and, in particular, industrial interest: high-quality, functional or protective coatings, composite materials, surface engineered particles, metal-organic interfaces, biological applications, micro-patterning, colloids, nanoparticles, functional devices, and many more. It is the desire of the authors that this book will be of benefit to readers who want to "brush-up on polymers".

Preparation and characterizations of Ba0.8Ca0.2TiO3 by complex polymerization method (CPM)

International Nuclear Information System (INIS)

Motta, F.V.; Marques, A.P.A.; Escote, M.T.; Melo, D.M.A.; Ferreira, A.G.; Longo, E.; Leite, E.R.; Varela, J.A.

2008-01-01

Ba 0.8 Ca 0.2 TiO 3 (BCT) was prepared by the complex polymerization method (CPM) using Ba 0.8 Ca 0.2 CO 3 and [Ti[OCH(CH 3 ) 2 ] 4 as starting materials. The powders were crystallized at several temperatures from 400 to 1200 deg. C using different times (from 1 to 8 h). The phase evolution and the physical properties were characterized by X-ray diffraction, Raman and IR spectroscopy. Such results indicate that the precursor Ba 0.8 Ca 0.2 CO 3 used in the synthesis of Ba 0.8 Ca 0.2 TiO 3 promotes an effective complexation of the ions Ca 2+ in the matrix of BaTiO 3 . After heat treatment for 2 h at 600 deg. C the phase BCT was obtained with absence of the CaTiO 3 or BaCO 3 phases. The CPM is an efficient method in the synthesis of the BCT, using small reaction time and low temperature and cost for the preparation of these powders

Physicochemical characterization of functionalized-nanostructured-titania as a carrier of copper complexes for cancer treatment

Energy Technology Data Exchange (ETDEWEB)

López, Tessy [Nanotechnology and Nanomedicine Laboratory, Metropolitan Autonomous University-Xochimilco, Calzada del Hueso 1100, Villa Quietud, Coyoacán, 04960 México D.F. (Mexico); Nanotechnology Laboratory, National Institute of Neurology and Neurosurgery “MVS”, Avenida Insurgentes Sur 3877, La Fama, Tlalpan, 14269 México D.F. (Mexico); Department of Chemical and Biomolecular Engineering, Tulane University, 6823 St. Charles Avenue, New Orleans (United States); Ortiz, Emma, E-mail: emma170@hotmail.com [Nanotechnology Laboratory, National Institute of Neurology and Neurosurgery “MVS”, Avenida Insurgentes Sur 3877, La Fama, Tlalpan, 14269 México D.F. (Mexico); Guevara, Patricia [Neuroimmunology Laboratory, National Institute of Neurology and Neurosurgery “MVS”, Insurgentes Sur 3877, La Fama, Tlalpan, 14269 México D.F. (Mexico); Gómez, Esteban [Nanotechnology Laboratory, National Institute of Neurology and Neurosurgery “MVS”, Avenida Insurgentes Sur 3877, La Fama, Tlalpan, 14269 México D.F. (Mexico); Novaro, Octavio [Institute of Physics-UNAM, Circuito de la Investigación Científica Ciudad Universitaria, CP 04510 México D.F. (Mexico)

2014-07-01

In the present paper we report the preparation and characterization of functionalized-TiO{sub 2} (F-TiO{sub 2}) to obtain a biocompatible material to be used as carrier of alternative anticancer agents: copper acetate and copper acetylacetonate. The sol–gel procedure was used to prepare the fuctionalized titania material through hydrolysis and condensation of the titanium's butoxide. Sulfate, amine and phosphate ions served as functional groups which were anchored to the titania's surface. Mineral acids and gamma amine butyric acid were the precursors and they were added at the initial step of the synthesis. The copper complexes were loaded on titania and were also added to the reactor synthesis from the beginning. Infrared and ultraviolet–visible spectroscopies were the principal techniques used to the characterization of F-TiO{sub 2} and copper complexes loaded on titania materials. Transmission Electronic Microscopy (TEM) was used to complement the characterization's studies. The biocompatibility of F-TiO{sub 2} was evaluated by treating different cancer cell lines with increased concentration of this compound. The amine, the sulfate and the phosphate on the titania's surface, as well as the integral structures of the metal complexes on titania were well identified by infrared and ultraviolet–visible spectroscopies. The TEM photographs of Cu(acac){sub 2}/F-TiO{sub 2} and Cu(Oac){sub 2}/F-TiO{sub 2} materials showed the formation of nanoparticles, which have sizes ranging from 4 to 10 nm, with no morphology alterations in comparison with F-TiO{sub 2} nanoparticles, suggesting that the presence of low quantities of copper do not affect the structure of the nanoparticles. The Energy Dispersive Spectroscopy (EDS) confirms the presence of copper on the titania's nanoparticles. The biological results indicate that there is more than 90% cell survival, thus suggesting that F-TiO{sub 2} does not cause damage to the cells. Therefore

[Synthesis and Characterization of a Sugar Based Electrolyte for Thin-film Polymer Batteries

Science.gov (United States)

1998-01-01

The work performed during the current renewal period, March 1,1998 focused primarily on the synthesis and characterization of a sugar based electrolyte for thin-film polymer batteries. The initial phase of the project involved developing a suitable sugar to use as the monomer in the polymeric electrolyte synthesis. The monomer has been synthesized and characterized completely. Overall the yield of this material is high and it can be produced in relatively large quantity easily and in high purity. The scheme used for the preparation of the monomer is outlined along with pertinent yields.

Synthesis,Characterization and Application of Benzyl-substituted Cyclopentadienyl lanthanide Complexes as Catalyst Precursors for the Syndiotactic Polymerization of Methyl Methacrylate

Institute of Scientific and Technical Information of China (English)

QIAN,Yan-Long(钱延龙); BALA,Muhammad D.; XIE,Xiao-Min(谢小敏); HUANG,Ji-Ling(黄吉玲)

2004-01-01

Benzyl-substituted cyclopentadienyl lanthanide complexes were synthesized and characterized by elemental analysis, MS and IR spectroscopy. The analytical data point out the formation of monomeric, unsolvated complexes.In conjunction with Al(Et)3 as co-catalyst, the title complexes are efficient catalysts for the syndiotactic polymerization of methyl methacrylate. For the complex (C6H5CH2C5H4)2YCI, under the optimum polymerization conditions (60 ℃, n(MMA):n(catalyst):n(co-catalyst)= 1000:1:10), a predominantly syndiotactic (rr=66%) polymer of high molecular weight (Mη = 105000) was obtained.

Template synthesis, characterization and antimicrobial activity of the complex combinations of some transitional metals with isonicotinoylhydrazone -2,4,6- trimethylbenzaldehyde

International Nuclear Information System (INIS)

Mitu, L.ITU; Imran, M.

2011-01-01

The complexes of Cu(II), Ni(II), Co(II), Mn(II), and Zn(II) with isonicotinoyl-hydrazone -2,4,6-trimethylbenzaldehyde (INHTB) are reported. The complexes have been characterized by analytical data, IR, UV-Vis, NMR spectra, magnetic susceptibility, thermal analysis and for the Cu(II) complex the ESR spectrum has been recorded. The anti-bacterial activity of these complexes were investigated against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Salmonella enteritidis, Shigella flexneri bacteria. The INHTB ligand is coordinated at the metallic ions by oxygen amide (O=C) and the azomethine nitrogen. (author)

Synthesis characterization and biological evaluation of a novel mixed ligand 99mTc complex as potential brain imaging agent

International Nuclear Information System (INIS)

Rey, A.; Manta, E.; Leon, A.; Papadopoulos, M.; Pirmettis, Y.; Raptopoulou, C.; Chiotellis, E.; Leon, E.; Mallo, L.

1998-01-01

One approach in the design of neutral oxotechnetium complexes is based on the simultaneous substitution of a tridentate dianionic ligand and a monodentate monoanionic coligand on a [Tc(V)O] +3 precursor. Following this ''mixed ligand'' concept, a novel 99m Tc complex with N,N-bis(2-mercaptoethyl)-N'N'-diethylethylenediamine as ligand and 1-octanethiol as coligand is prepared and evaluated as potential brain radiopharmaceutical. Preparation of the complex at tracer level was accomplished by using 99m Tc-glucoheptonate as precursor. The substitution was optimized and a coligand/ligand ratio of 5 was selected. Under this conditions the labeling yield was over 80% and a major product (with radiochemical purity > 80%) was isolated by HPLC methods and used for biological evaluation. Chemical characterization at carrier level was developed using the corresponding rhenium complex as structural model. The Re complex was also prepared by substitution method and isolated as a crystalline product. The crystals were characterized by UV-vis and IR spectra and elemental analysis. Results were consistent with the expected ReOLC structure. X ray crystallographic study demonstrated that the complex adopts a distorted trigonal bipyramidal geometry. The basal plane is defined by the SS atoms of the ligand and the oxo group, while the N of the ligand and the S of the colligand occupy the two apical positions. All sulphur atoms underwent ionization leading to the formation of a neutral compound. 99 Tc complex was also prepared. Although it was not isolated due to the small amount of reagents employed, the HPLC profile was identical to the one observed for the rhenium complex suggesting the same chemical structure. Biodistribution in mice demonstrated early brain uptake, fast blood clearance, excretion through hepatobiliary system and a brain/blood ratio that increased significantly with time. (author)

Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

KAUST Repository

Al-Bloushi, Mohammed

2013-05-01

Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

Synthesis and characterization of strontium molybdate doped with copper, cobalt and zinc for purposes photocatalytic

International Nuclear Information System (INIS)

Dutra, F.B.; Silva, M.M.S.; Moriyama, A.L.L.; Souza, C.P.

2016-01-01

The broad concerns of contemporary society with environmental problems requires legislation and more effective techniques for wastewater treatment. In recent years, ceramic materials that have properties such as high melting points and high stability have been receiving great emphasis in several studies in particular heterogeneous photocatalysis, rapid and efficient method for the complete mineralization of contaminants. In this context, the present work deals with the synthesis and characterization of molybdate Strontium (SrMoO4) doped with copper, cobalt and zinc for the purpose of photocatalytic studies. The compounds were synthesized by complexation method EDTA / Citrate basic medium. The powders were characterized by Thermogravimetric Analysis (TG), X-Ray Diffraction (XRD), Particle size distribution by laser diffraction, Spectroscopy in the UV-Visible region, Energy Dispersive Spectroscopy (EDS) and Scanning Electron Microscopy (SEM), showing promising results as the crystalline phase of development and potential uses for the purpose of heterogeneous photocatalysis. (author)

N-BUTYL SUBSTITUTED N-HETEROCYCLIC CARBENE-PD(II-PYRIDINE (PEPPSI COMPLEXES: SYNTHESIS, CHARACTERIZATION AND CATALYTIC ACTIVITY IN THE SUZUKI-MIYAURA REACTION

Directory of Open Access Journals (Sweden)

Rukiye Fırıncı

2016-08-01

Full Text Available A series of N-butyl substituted imidazolium salts, (1a-c and their pyridine enhanced precatalyst preparation stabilization and initiation (PEPPSI themed palladium N-heterocyclic carbene complexes (2a-c were synthesized and characterized. Pd-NHC complexes were fully determined by elemental analysis and spectroscopic. The synthesized complexes were tested in Suzuki-Miyaura cross-coupling reaction. These complexes were found to be efficient catalysts for the Suzuki-Miyaura reaction of phenylboronic acid with aryl bromides.

Synthesis and characterization of ligands and bifunctional chelating agents by modification of cysteine for complexation studies with 99mTc

International Nuclear Information System (INIS)

Pillai, M.R.A.; Kothari, K.; Banerjee, S.; Samuel, G.; Suresh, M.; Sarma, H.D.

1998-01-01

The synthesis of four novel ligands using the amino-acid cysteine and its ethyl carboxylate derivative is described. The synthetic method involves a two-step procedure, wherein the intermediate Schiff base formed by the condensation of the amino group of the cysteine substrate and salicylaldehyde is reduced to give the target ligands. The intermediates and the final products are characterised by high resolution NMR spectroscopy. Complexation studies of the ligands with 99m Tc are standardised using stannous tartrate as the reducing agent at varying reaction conditions. The complexes are characterised using standard quality control techniques such as TLC, paper electrophoresis and PC. Lipophilicities of the complexes are estimated by solvent extraction into chloroform. Substantial changes in net charge and lipophilicity in the 99m Tc complexes are observed on substituting the carboxylic acid residue in ligand I and II with the ethyl carboxylate groups (ligands III and IV). All the ligands formed complexes in high yield. While the complexes of ligand I and II are observed to be hydrophilic in nature and are not extractable into CHCl 3 , ligands III and IV gave neutral and lipophilic complexes. Though the distribution ratios of the complexes of ligands III and IV in CHCl 3 /saline system are observed to be very high, considerable differences in lipophilicities are also observed as evidenced by the difference in their respective extractabilities in chloroform. On storage, the complex of ligand III exhibit a tendency to get converted to a hydrophilic and non-extractable species. The bio-distribution of the complexes of ligands I and II showed that they have predominantly renal clearances whereas the complexes of ligands III and IV exhibited a significant hepatobiliary uptake and did not show much uptake in brain in spite of its favourable properties such as neutrality, lipophilicity and conversion into a hydrophilic species. (author)

Synthesis and characterization of mixed ligand complexes of Zn(II ...

Indian Academy of Sciences (India)

Unknown

the total % weight loss is 60⋅73%, and the weight loss at 891°C was 54⋅24%, which corresponds to a weight loss of molecular weight of 179 units. The. TGA curve of 3 complex showed sudden weight loss at 300°C, indicating the absence of water molecules in the coordination sphere of the complex. The total weight loss ...

Synthesis and Characterization of Novel Magnetite Nanoparticle Block Copolymer Complexes

OpenAIRE

Zhang, Qian

2007-01-01

Superparamagnetic Magnetite (Fe3O4) nanoparticles were synthesized and complexed with carboxylate-functionalized block copolymers, and aqueous dispersions of the complexes were investigated as functions of their chemical and morphological structures. The block copolymer dispersants possessed either poly(ethylene oxide), poly(ethylene oxide-co-propylene oxide), or poly(ethylene oxide-b-propylene oxide) outer blocks, and all contained a polyurethane center block with pendant carboxylate functi...

Synthesis of sp3-rich scaffolds for molecular libraries through complexity-generating cascade reactions

DEFF Research Database (Denmark)

Flagstad, Thomas; Min, Geanna; Bonnet, K.

2016-01-01

An efficient strategy for the synthesis of complex small molecules from simple building blocks is presented. Key steps of the strategy include tandem Petasis and Diels–Alder reactions, and divergent complexity-generating cyclization cascades from a key dialdehyde intermediate. The methodology...

Synthesis and characterization of innovative insulation materials

Directory of Open Access Journals (Sweden)

Skaropoulou Aggeliki

2018-01-01

Full Text Available Insulation elements are distinguished in inorganic fibrous and organic foamed materials. Foamed insulation materials are of great acceptance and use, but their major disadvantage is their flammability. In case of fire, they tend to transmit the flame producing toxic gases. In this paper, the synthesis and characterization of innovative inorganic insulation materials with properties competitive to commercial is presented. Their synthesis involves the mixing of inorganic raw material and water with reinforcing agent or/and foaming agent leading to the formation of a gel. Depending on raw materials nature, the insulation material is produced by freeze drying or ambient drying techniques of the gel. The raw material used are chemically benign and abundantly available materials, or industrial by-products and the final products are non-toxic and, in some cases, non-flammable. Their density and thermal conductivity was measured and found 0.02-0.06 g/cm3 and 0.03-0.04 W/mK, respectively.

Characterization of the inclusion complex ropivacaine: β-cyclodextrin

International Nuclear Information System (INIS)

Fraceto, Leonardo Fernandes; Moraes, Carolina Morales; Araujo, Daniele Ribeiro de; Zanella, Luciana; Paula, Eneida de; Pertinhez, Thelma de Aguiar

2007-01-01

Ropivacaine (RVC) is a widely used local anesthetic. The complexation of RVC with β-cyclodextrin (β-CD) is of great interest for the development of more efficient local anesthetic formulations. The present work focuses on the characterization of the RVC:β-CD complex by nuclear magnetic resonance (NMR). The stoichiometry of the complex is 1:2 RVC:β-CD. DOSY-NMR shows that the association constant is 55.5 M -1 . Longitudinal relaxation time results show that RVC changes its mobility in the presence of β-CD. This study is focused on the physicochemical characterization of inclusion complexes that are potentials options for pain treatment. (author)

Synthesis, characterization, antimicrobial and antitumor reactivity of new palladium(II) complexes with methionine and tryptophane coumarine derivatives

Science.gov (United States)

Stojković, Danijela Lj; Jevtić, Verica V.; Vuković, Nenad; Vukić, Milena; Čanović, Petar; Zarić, Milan M.; Mišić, Milena M.; Radovanović, Dragče M.; Baskić, Dejan; Trifunović, Srećko R.

2018-04-01

In reaction of 3-acetyl-4-hydroxy coumarine with methionine methyl ester hydrochloride and tryptophane methyl ester hydrochloride the corresponding enamine ligands were obtained. Palladium (II) complexes were prepared in reaction of potassium-tetrachloridopalladate (II) and corresponding enamine. All compounds were characterized by microanalysis, infrared, 1H and 13C NMR spectroscopy. In vitro antitumor activity of the mentioned ligands and corresponding palladium (II) complexes, as well as me-Gly and me-Val ligands and [Pd (me-Gly)]Cl and [Pd (me-Val)2] complexes was determined by MTT assay against two leukemia cell lines (JVM-13 and MOLT-4) and against primary leukemic cells isolated from chronic lymphocytic leukemia (CLL) patients. Antimicrobial activity of the tested compound was evaluated by determining the minimum inhibitory concentration (MIC) and minimum microbicidal concentration (MMC) against three reference bacterial strains: E. faecalis, P. aeruginosa, S. aureus and one clinical isolate of yeast: Candida spp.

Ru/Fe bimetallic complexes: Synthesis, characterization, cytotoxicity and study of their interactions with DNA/HSA and human topoisomerase IB.

Science.gov (United States)

Takarada, Jessica E; Guedes, Adriana P M; Correa, Rodrigo S; Silveira-Lacerda, Elisângela de P; Castelli, Silvia; Iacovelli, Federico; Deflon, Victor Marcelo; Batista, Alzir Azevedo; Desideri, Alessandro

2017-12-15

Three ruthenium/iron-based compounds, 1: [Ru(MIm)(bipy)(dppf)]PF 6 (MIm = 2-mercapto-1-methylimidazole anion), 2: [RuCl(Im)(bipy)(dppf)]PF 6 (Im = imidazole), and 3: [Ru(tzdt)(bipy)(dppf)]PF 6 (tzdt = 1,3-thiazolidine-2-thione anion) (dppf = 1,1'-bis(diphenylphosphine)ferrocene and bipy = 2,2'-bipyridine), were synthesized, and characterized by elemental analyses, conductivity, UV/Vis, IR, 1 H, 13 C and 31 P{1H} NMR spectroscopies, and by electrochemical technique. The complex 3 was also characterized by single-crystal X-ray. The three ruthenium(II) complexes show cytotoxicity against DU-145 (prostate carcinoma cells) and A549 (lung carcinoma cells) tumor cells. The free ligands do not exhibit any cytotoxic activity, such as evident by the IC 50 values higher than 200 μM. UV/Vis and viscosity experiments showed that the complexes interact weakly with the DNA molecule, via electrostatic forces. The interaction of the complexes 1-3 with the HSA is moderate, with K b values in range of 10 5 -10 7  M -1 , presenting a static mechanism of interaction stabilized by hydrophobic. Complexes 2 and 3 showed high affinity for the FA7 HSA site as evidenced by fluorescence spectroscopy and molecular docking. Complexes 1-3 were tested as potential human Topoisomerase IB inhibitors by analysing the different steps of the enzyme catalytic cycle. The results indicate that all compounds efficiently inhibit the DNA relaxation and the cleavage reaction, in which the effect increases upon pre-incubation. Complexes 1 and 2 are also able to slow down the religation reaction. Copyright © 2017 Elsevier Inc. All rights reserved.

Synthesis and Characterization of Two New p-tert-Butylcalix[4]-arene Schiff Bases

Directory of Open Access Journals (Sweden)

Saeed Taghvaee Ganjali

2001-03-01

Full Text Available Synthesis and characterization of two new Schiff bases of p-tertbuthylcalix[4]arene (H2L1 and HL2 is described. The synthesis of H2L1 and HL2 has been achieved by the condensation of salicylaldehyde with the amine group of upper rim monoamine p-tert-butylcalix[4]arene in ethanol. These compounds have been characterized on the basis of elemental analysis and spectral data. Solvatochromicity and fluorescence properties were observed and measured for H2L1 and HL2. Solvatochromicity of these ligands indicates their potential for NLO applications.

Room temperature synthesis of protonated layered titanate sheets using peroxo titanium carbonate complex solution.

Science.gov (United States)

Sutradhar, Narottam; Sinhamahapatra, Apurba; Pahari, Sandip Kumar; Bajaj, Hari C; Panda, Asit Baran

2011-07-21

We report the synthesis of peroxo titanium carbonate complex solution as a novel water-soluble precursor for the direct synthesis of layered protonated titanate at room temperature. The synthesized titanates showed excellent removal capacity for Pb(2+) and methylene blue. Based on experimental observations, a probable mechanism for the formation of protonated layered dititanate sheets is also discussed.

Unprecedented Carbonato Intermediates in Cyclic Carbonate Synthesis Catalysed by Bimetallic Aluminium(Salen) Complexes.

Science.gov (United States)

Castro-Osma, José A; North, Michael; Offermans, Willem K; Leitner, Walter; Müller, Thomas E

2016-04-21

The mechanism by which [Al(salen)]2 O complexes catalyse the synthesis of cyclic carbonates from epoxides and carbon dioxide in the absence of a halide cocatalyst has been investigated. Density functional theory (DFT) studies, mass spectrometry and (1) H NMR, (13) C NMR and infrared spectroscopies provide evidence for the formation of an unprecedented carbonato bridged bimetallic aluminium complex which is shown to be a key intermediate for the halide-free synthesis of cyclic carbonates from epoxides and carbon dioxide. Deuterated and enantiomerically-pure epoxides were used to study the reaction pathway. Based on the experimental and theoretical results, a catalytic cycle is proposed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis, properties and reactivity of intramolecular hypercoordinate silicon complexes

International Nuclear Information System (INIS)

Nikolin, A A; Negrebetsky, V V

2014-01-01

The state of the art of the chemistry of hypercoordinate silicon compounds is analyzed. Published data on the current top-priority approaches to the preparative synthesis of these compounds and on their properties, structures and reactivity are summarized and generalized. Relying on the results obtained by modern physicochemical methods, the possible mechanisms of stereodynamic processes occurring in the coordination units of hypercoordinate silicon complexes are discussed. The bibliography includes 157 references

Graphene optoelectronics synthesis, characterization, properties, and applications

CERN Document Server

bin M Yusoff, Abdul Rashid

2014-01-01

This first book on emerging applications for this innovative material gives an up-to-date account of the many opportunities graphene offers high-end optoelectronics.The text focuses on potential as well as already realized applications, discussing metallic and passive components, such as transparent conductors and smart windows, as well as high-frequency devices, spintronics, photonics, and terahertz devices. Also included are sections on the fundamental properties, synthesis, and characterization of graphene. With its unique coverage, this book will be welcomed by materials scientists, solid-

Synthesis, Crystal structure and Characterization of a New Oxalate ...

Indian Academy of Sciences (India)

in a slightly distorted octahedral environment, by two O atoms from two water molecules and four O atoms of two oxalate anions acting as chelating ligands. ... component for building up supramolecular systems and for participating in hydrogen bonding ... heating rate of 10◦C min−1. 2.2 Synthesis of the complex. Aqueous ...

Synthesis and characterization of functionalized CNTs using soya and milk protein

Science.gov (United States)

saxena, Sanjay; ranu, Rachana; Hait, Chandan; Priya, Shruti

2014-10-01

Nanotechnology is the study of the phenomenon and manipulation of matter at atomic and molecular scale to enhance their older property and generate several new properties. Carbon nanotubes (CNTs) are one of the most commonly mentioned building blocks of nanotechnology. CNTs are very prevalent in today's world of medical research and are being highly researched in the fields of efficient drug delivery and bio sensing methods for disease treatment and health monitoring. There are number of methods for synthesizing CNTs. This is a biological method for synthesis of CNTs in which protein is used as carbon source and amino acids present in protein form complex with metal salt. The CNTs synthesized are then characterized and functionalized using techniques such as transmission electron microscopy, Fourier transform infra-red, nuclear magnetic resonance, ultra-violet visible spectroscopy, X-ray diffraction, etc. The properties of the synthesized CNTs are studied with the help of techniques such as thermo-gravimetric analysis, differential thermal analysis, and vibrating sample magnetometer, etc.

Synthesis and characterization of triangulene

Science.gov (United States)

Pavliček, Niko; Mistry, Anish; Majzik, Zsolt; Moll, Nikolaj; Meyer, Gerhard; Fox, David J.; Gross, Leo

2017-05-01

Triangulene, the smallest triplet-ground-state polybenzenoid (also known as Clar's hydrocarbon), has been an enigmatic molecule ever since its existence was first hypothesized. Despite containing an even number of carbons (22, in six fused benzene rings), it is not possible to draw Kekulé-style resonant structures for the whole molecule: any attempt results in two unpaired valence electrons. Synthesis and characterization of unsubstituted triangulene has not been achieved because of its extreme reactivity, although the addition of substituents has allowed the stabilization and synthesis of the triangulene core and verification of the triplet ground state via electron paramagnetic resonance measurements. Here we show the on-surface generation of unsubstituted triangulene that consists of six fused benzene rings. The tip of a combined scanning tunnelling and atomic force microscope (STM/AFM) was used to dehydrogenate precursor molecules. STM measurements in combination with density functional theory (DFT) calculations confirmed that triangulene keeps its free-molecule properties on the surface, whereas AFM measurements resolved its planar, threefold symmetric molecular structure. The unique topology of such non-Kekulé hydrocarbons results in open-shell π-conjugated graphene fragments that give rise to high-spin ground states, potentially useful in organic spintronic devices. Our generation method renders manifold experiments possible to investigate triangulene and related open-shell fragments at the single-molecule level.

Synthesis and studies of novel high metal content organic aerogels obtained from a polymerizable titanium complex

International Nuclear Information System (INIS)

Cadra, S.

2010-01-01

Inertial Confinement Fusion (ICF) is a technique widely studied by the French atomic commission (CEA). Experiments will be performed within the Laser Megajoule (LMJ). They require innovative materials like organic aerogels that constitute laser targets. Such polymeric material must provide both a high porosity and a significant titanium percentage (1 atom %). Moreover, the monomers developed must be compatible with the synthesis procedure already in use. According to these specifications, a new polymerizable titanium complex was synthesized and fully characterized. This air and moisture-stable monomer provides a high metal percentage. Its free-radical cross-linked copolymerization affords several titanium-containing polymers. These gels were dried under supercritical conditions and organic aerogels were obtained. The chemical compositions of these materials were investigated by NMR, IR and elemental analysis while their structure was characterized by MEB-EDS, MET, N 2 adsorption/desorption isotherms measurements and SAXS. The data collected fit the specification requirements. Moreover, the mechanisms responsible of the foam nano-structure formation were discussed. (author) [fr

Nickel(II) and palladium(II) triphenylphosphine complexes incorporating tridentate Schiff base ligands: Synthesis, characterization and biocidal activities

Science.gov (United States)

Shabbir, Muhammad; Akhter, Zareen; Ashraf, Ahmad Raza; Ismail, Hammad; Habib, Anum; Mirza, Bushra

2017-12-01

Nickel(II) and palladium(II) triphenylphosphine complexes incorporating tridentate Schiff bases have been prepared and characterized by elemental analysis as well as by spectroscopic techniques (FTIR & NMR). The synthesized compounds were assessed to check their potential biocidal activity by using different biological assays (brine shrimp cytotoxicity, antimicrobial, antioxidant, antitumor and drug-DNA interaction). Results of brine shrimp cytotoxicity assay showed that ligand molecules are more bioactive than metal complexes with LD50 as low as 12.4 μg/mL. The prominent antitumor activity was shown by nickel complexes while the palladium complexes exhibited moderate activity. The synthesized compounds have shown high propensity for DNA binding either through intercalation or groove binding which represents the mechanism of antitumor effect of these compounds. Additionally, ligand molecules and nickel metal complexes showed significant antioxidant activity with IC50 values as low as 3.1 μg/mL and 18.9 μg/mL respectively while palladium complexes exhibited moderate activity. Moreover, in antimicrobial assays H2L1, Ni(L1)PPh3 and H2L3 showed dual inhibition against bacterial and fungal strains while for the rest of the compounds varying degree of activity was recorded against different strains. Overall comparison of results suggests that the synthesized compounds can be promising candidate for drug formulation and development.

Synthesis, structural characterization and photoluminescence properties of rhenium(I) complexes based on bipyridine derivatives with carbazole moieties.

Science.gov (United States)

Li, Hong-Yan; Wu, Jing; Zhou, Xin-Hui; Kang, Ling-Chen; Li, Dong-Ping; Sui, Yan; Zhou, Yong-Hui; Zheng, You-Xuan; Zuo, Jing-Lin; You, Xiao-Zeng

2009-12-21

Three N,N-bidentate ligands, 5,5'-dibromo-2,2-bipyridine (L1) and two carbazole containing ligands of 5-bromo-5'-carbazolyl-2,2-bipyridine (L2), 5,5'-dicarbazolyl-2,2'-bipyridine (L3), and their corresponding rhenium Re(CO)3Cl(L) complexes (ReL1-ReL3) have been successfully synthesized and characterized by elemental analysis, 1H NMR and IR spectra. Their photophysical properties and thermal analysis, along with the X-ray crystal structure analysis of L3 and complexes ReL1 and ReL3 are also described. In CH2Cl2 solution at room temperature, all complexes display intense absorption bands at ca. 220-350 nm, which can be assigned to spin-allowed intraligand (pi-->pi*) transitions, and the low energy broad bands in the 360-480 nm region are attributed to the metal to ligand charge-transfer d(Re)-->pi* (diimine) (MLCT). The introduction of carbazole moieties improves the MLCT absorption and molar extinction coefficient of these complexes. Upon excitation at the peak maxima, all complexes show strong emissions around 620 nm, which are assigned to d(Re)-->pi* (diimine) MLCT phosphorescence. The photoluminescence lifetime decay of Re(I) complexes were measured and the quantum efficiencies of the rhenium(I) complexes were calculated by using air-equilibrated [Ru(bpy)3]2+ x 2 Cl- aqueous solution as standard (phi(std) = 0.028). The complexes with appended carbazole moieties exhibit enhanced luminescence performances relative to ReL1.

The synthesis of complex molecules in interstellar clouds

Science.gov (United States)

Huntress, W. T., Jr.; Mitchell, G. F.

1979-01-01

The abundances of polyatomic molecules that may be formed by CH3(+) radiative association reactions in dense interstellar molecular clouds are reevaluated. The formation of a number of complex interstellar molecules via radiative association reactions involving ionic precursors other than CH3(+) is also investigated; these additional precursors include CH3O(+), CH3CO(+), CH5(+), HCO(+), NO(+), H2CN(+), C2H2(+), and NH3(+). The results indicate that the postulated gas-phase ion-molecule radiative association reactions could potentially explain the synthesis of most of the more complex species observed in dense molecular clouds such as Sgr B2. It is concluded, however, that in order to be conclusive, laboratory data are needed to show whether or not these reactions proceed at the required rates at low temperatures.

Synthesis and spectroscopic behavior of highly luminescent Eu 3+-dibenzoylmethanate (DBM) complexes with sulfoxide ligands

Science.gov (United States)

Niyama, E.; Brito, H. F.; Cremona, M.; Teotonio, E. E. S.; Reyes, R.; Brito, G. E. S.; Felinto, M. C. F. C.

2005-09-01

In this paper the synthesis, characterization and photoluminescent behavior of the [RE(DBM) 3L 2] complexes (RE = Gd and Eu) with a variety of sulfoxide ligands; L = benzyl sulfoxide (DBSO), methyl sulfoxide (DMSO), phenyl sulfoxide (DPSO) and p-tolyl sulfoxide (PTSO) have been investigated in solid state. The emission spectra of the Eu 3+-β-diketonate complexes show characteristics narrow bands arising from the 5D 0 → 7F J ( J = 0-4) transitions, which are split according to the selection rule for C n, C nv or C s site symmetries. The experimental Judd-Ofelt intensity parameters ( Ω2 and Ω4), radiative ( Arad) and non-radiative ( Anrad) decay rates, and R02 for the europium complexes have been determined and compared. The highest value of Ω2 (61.9 × 10 -20 cm 2) was obtained to the complex with PTSO ligand, indicating that Eu 3+ ion is in the highly polarizable chemical environment. The higher values of the experimental quantum yield ( q) and emission quantum efficiency of the emitter 5D 0 level ( η) for the Eu-complexes with DMSO, DBSO and PTSO sulfoxides suggest that these complexes are promising Light Conversion Molecular Devices (LCMDs). The lower value of quantum yield ( q = 1%), for the hydrated complex [Eu(DBM) 3(H 2O)], indicates that the luminescence quenching occurs via multiphonon relaxation by coupling with the OH-oscillators from water molecule coordinated to rare earth ion. The pure red emission of the Eu-complexes has been confirmed by ( x, y) color coordinates.

Synthesis, spectroscopic characterization and catalytic oxidation ...

Indian Academy of Sciences (India)

were characterized by infrared, electronic, electron paramagnetic resonance ... The catalytic oxidation property of ruthenium(III) complexes were also ... cies at room temperature. ..... aldehyde part of Schiff base ligands, catalytic activ- ity of new ...

Fluorido complexes of technetium

International Nuclear Information System (INIS)

Mariappan Balasekaran, Samundeeswari

2013-01-01

Fluorine chemistry has received considerable interest during recent years due to its significant role in the life sciences, especially for drug development. Despite the great nuclear medicinal importance of the radioactive metal technetium in radiopharmaceuticals, its coordination chemistry with the fluorido ligand is by far less explored than that of other ligands. Up to now, only a few technetium fluorides are known. This thesis contains the synthesis, spectroscopic and structural characterization of novel technetium fluorides in the oxidation states ''+1'', ''+2'', ''+4'' and ''+6''. In the oxidation state ''+6'', the fluoridotechnetates were synthesized either from nitridotechnetic(VI) acid or from pertechnetate by using reducing agent and have been isolated as cesium or tetraethylammonium salts. The compounds were characterized spectroscopically and structurally. In the intermediate oxidation state ''+4'', hexafluoridotechnetate(IV) was known for long time and studied spectroscopically. This thesis reports novel and improved syntheses and solved the critical issues of early publications such as the color, some spectroscopic properties and the structure of this key compound. Single crystal analyses of alkali metal, ammonium and tetramethylammonium salts of hexafluoridotechnetate(IV) are presented. In aqueous alkaline solutions, the ammonium salt of hexafluoridotechnetate(IV) undergoes hydrolysis and forms an oxido-bridged dimeric complex. It is the first step hydrolysis product of hexafluoridotechnetate(IV) and was characterized by spectroscopic and crystallographic methods. Low-valent technetium fluorides with the metal in the oxidation states of ''+2'' or ''+1'' are almost unknown. A detailed description of the synthesis and characterization of pentafluoridonitrosyltechnetate(II) is presented. The complex was isolated as alkali metal salts, and spectroscopic as well as structural features of the complexes are presented. Different salts of the trans

Synthesis and evaluation of complexing and extracting properties of diamides for the U(VI)/Pu(IV) partitioning

International Nuclear Information System (INIS)

Wahu, S.

2012-01-01

This work concerns the synthesis and evaluation of new diamides for co-extraction of U(VI) and Pu(IV) from spent nuclear fuels in concentrated nitric acid medium and the subsequent selective back-extraction of Pu(IV) at lower nitric acidity. Thus, three diamides series, namely R 2 NOC(CH 2 ) n CONR 2 , RR'NOC(CH 2 ) n CONRR' and R 2 NOC(CH 2 CHR')CONR 2 (series 1, 2 and 3, respectively) were synthesized and studied in the expectation to establish a structure-activity relationship regarding the extraction properties of such compounds towards actinides. Extraction tests showed that these diamides can effectively and selectively extract U(VI) and Pu(IV) from Am(III) at high acidity. In addition, it was found that the selective back-extraction of Pu(IV) from U(VI) can be achieved, as expected, merely by changing the acidity, when the nitrogen atoms of these diamides are substituted by branched alkyl chains. The mode of coordination of actinides by the above diamides has also been studied through the use of short chain diamides model compounds, allowing the crystallization of the actinide complexes and, thus, their characterization by X-ray diffraction. EXAFS investigation suggested that the uranium coordination sphere in the complexes formed with long chain diamides and extracted into the organic phase is identical to the one observed in U(VI) complexes obtained with short chain diamides model compounds. However, the stoichiometry of model complexes is 1:1, UO 2 (NO 3 ) 2 TEDA, whereas extracted U(VI) complexes exhibit 1:2 stoichiometry, UO 2 (NO 3 ) 2 (TEHDA) 2 . Finally, Th (IV) complexes were also prepared and characterized and further compared to U(VI) complexes. (author) [fr

Ruthenium(II) arene complexes with chelating chloroquine analogue ligands: Synthesis, characterization and in vitro antimalarial activity†

Science.gov (United States)

Glans, Lotta; Ehnbom, Andreas; de Kock, Carmen; Martínez, Alberto; Estrada, Jesús; Smith, Peter J.; Haukka, Matti; Sánchez-Delgado, Roberto A.; Nordlander, Ebbe

2012-01-01

Three new ruthenium complexes with bidentate chloroquine analogue ligands, [Ru(η6-cym)(L1)Cl]Cl (1, cym = p-cymene, L1 = N-(2-((pyridin-2-yl)methylamino)ethyl)-7-chloroquinolin-4-amine), [Ru(η6-cym)(L2)Cl]Cl (2, L2 = N-(2-((1-methyl-1H-imidazol-2-yl)methylamino)ethyl)-7-chloroquinolin-4-amine) and [Ru(η6-cym)(L3)Cl] (3, L3 = N-(2-((2-hydroxyphenyl)methylimino)ethyl)-7-chloroquinolin-4-amine) have been synthesized and characterized. In addition, the X-ray crystal structure of 2 is reported. The antimalarial activity of complexes 1–3 and ligands L1, L2 and L3, as well as the compound N-(2-(bis((pyridin-2-yl)methyl)amino)ethyl)-7-chloroquinolin-4-amine (L4), against chloroquine sensitive and chloroquine resistant Plasmodium falciparum malaria strains was evaluated. While 1 and 2 are less active than the corresponding ligands, 3 exhibits high antimalarial activity. The chloroquine analogue L2 also shows good activity against both the choloroquine sensitive and the chloroquine resistant strains. Heme aggregation inhibition activity (HAIA) at an aqueous buffer/n-octanol interface (HAIR50) and lipophilicity (D, as measured by water/n-octanol distribution coefficients) have been measured for all ligands and metal complexes. A direct correlation between the D and HAIR50 properties cannot be made because of the relative structural diversity of the complexes, but it may be noted that these properties are enhanced upon complexation of the inactive ligand L3 to ruthenium, to give a metal complex (3) with promising antimalarial activity. PMID:22249579

Synthesis and characterization of the Rhodium (II) citrate complex

International Nuclear Information System (INIS)

Najjar, R.; Santos, F.S. dos; Seidel, W.

1987-01-01

The preparation and characterization of the rhodium (II) citrate is described. Rhodium citrate was prepared by reacting citric acid trihydrated (3,4 g, 16 mmols) with anhydrous rhodium acetate (0,44 g, 1 mmol). Th electronic instruments, thermogravimetric curve and spectrum of rhodium (II) citrate are analysed. (M.J.C.) [pt

DOE complex buried waste characterization assessment

International Nuclear Information System (INIS)

Kaae, P.S.; Holter, G.M.; Garrett, S.M.K.

1993-01-01

The work described in this report was conducted by Pacific Northwest Laboratory to provide information to the Buried Waste Integrated Demonstration (BWID) program. The information in this report is intended to provide a complex-wide planning base for th.e BWID to ensure that BWID activities are appropriately focused to address the range of remediation problems existing across the US Department of Energy (DOE) complex. This report contains information characterizing the 2.1 million m 3 of buried and stored wastes and their associated sites at six major DOE facilities. Approximately 85% of this waste is low-level waste, with about 12% TRU or TRU mixed waste; the remaining 3% is low-level mixed waste. In addition, the report describes soil contamination sites across the complex. Some of the details that would be useful in further characterizing the buried wastes and contaminated soil sites across the DOE complex are either unavailable or difficult to locate. Several options for accessing this information and/or improving the information that is available are identified in the report. This document is a companion to Technology Needs for Remediation: Hanford and Other DOE Sites, PNL-8328 (Stapp 1993)

Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

International Nuclear Information System (INIS)

Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

2009-01-01

Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

Synthesis, physico-chemical characterization and biological activity of copper(ii and nickel(ii complexes with l-benzoyl-2-methylbenzimidazole derivatives

Directory of Open Access Journals (Sweden)

Podunavac-Kuzmanović Sanja O.

2002-01-01

Full Text Available Chlorides of copper(II and nickel(ll react with 1-benzoyl-2-methylbenzimidazole or 1-(4-chlorobenzoyl-2-methylbenzimidazole to give complexes of the type [M(LnCln(H20∙Cln (M = Cu or Ni; L = (1-benzoyl-2-methylbenzimidazole or 1-(4-chlorobenzoyl-2-methylbenzimidazole; n=O, 1 or 2. The complexes were synthesized and characterized by elemental analysis, molar conductivity magnetic susceptibility measurements and IR spectra. These studies suggest that all the complexes possess an octahedral stereochemistry. The antibacterial activity of (1-benzoyl-2-methylbenzimidazole or 1-(4-chlorobenzoyl-2-methylbenzimidazole and their complexes was evaluated against Escherichia coli and Bacillus sp.

Synthesis, characterization and biocidal activity of new organotin complexes of 2-(3-oxocyclohex-1-enyl)benzoic acid.

Science.gov (United States)

Vieira, Flaviana T; de Lima, Geraldo M; Maia, José R da S; Speziali, Nivaldo L; Ardisson, José D; Rodrigues, Leonardo; Correa, Ary; Romero, Oscar B

2010-03-01

The reaction of 1,3-cyclohexadione with 2-aminobenzoic acid has produced the 2-(3-oxocyclohex-1-enyl)benzoic acid (HOBz). Subsequent reactions of the ligand with organotin chlorides led to [Me(2)Sn(OBz)O](2) (1), [Bu(2)Sn(OBz)O](2) (2), [Ph(2)Sn(OBz)O](2) (3), [Me(3)Sn(OBz)] (4), [Bu(3)Sn(OBz)] (5) and [Ph(3)Sn(OBz)] (6). All complexes have been fully characterized. In addition the structure of complexes (2) and (4) have been authenticated by X-ray crystallography. The biological activity of all derivatives has been screened against Cryptococcus neoformans and Candida albicans. In addition we have performed toxicological testes employing human kidney cell. The complexes (3), (5) and (6) displayed the best values of inhibition of the fungus growing, superior to ketoconazole. Compound (5) presented promising results in view of the antifungal and cytotoxicity assays. Copyright (c) 2009 Elsevier Masson SAS. All rights reserved.

DNA-membrane complex restoration in Micrococcus radiodurans after X-irradiation: relation to repair, DNA synthesis and DNA degradation

Energy Technology Data Exchange (ETDEWEB)

Dardalhon-Samsonoff, M; Averbeck, D [Institut du Radium, 75 - Paris (France). Lab. Curie

1980-07-01

The DNA-membrane complex in Micrococcus radiodurans was shown to be essentially constituted of proteins, lipids and DNA. The complex was dissociated immediately after X-irradiation of cells and restored during post-incubation in complete medium. In X-irradiated protoplasts some DNA remained associated with the complex. Restoration of the complex during post-incubation was only seen in a medium favouring DNA polymerase and ligase activities. Under this condition no DNA synthesis occurred, suggesting that complex restoration may involve ligase activity. The complex restoration in the wild type and the X-ray sensitive mutant UV17 of M. radiodurans was strictly dependent on the X-ray dose. It was correlated with survival and DNA degradation but always preceded the onset of DNA synthesis after X-irradiation. At the same dose the complex restoration was about 2 fold lower in mutant than in wild type cells indicating that the restoration of the complex is related to repair capacity. The results are consistent with the idea that the complex protects X-irradiated DNA of M. radiodurans from further breakdown and, subsequently, permits DNA synthesis and repair to occur.

Electronic, electrical and magnetic ceramics synthesis and characterization

International Nuclear Information System (INIS)

Calix, V.S.; Saligan, P.P.; Naval, P.C.

1989-01-01

This paper describes the research and development activities of the Philippine Nuclear Research Institute (PNRI) on the synthesis and characterization of soft and hard ferrites and some beta alumina type superionic conductor materials. XRD, XRF and Moessbauer effect spectrometry are used to determine the structure phases, compositions and some magnetic properties of the materials. Effects of composition and preparation methods on the bulk electronic and magnetic properties are also discussed. (Auth.). 6 figs.; 3 tabs

Palladium complexes with simple iminopyridines as catalysts for polyketone synthesis.

Science.gov (United States)

Rosar, V; Dedeic, D; Nobile, T; Fini, F; Balducci, G; Alessio, E; Carfagna, C; Milani, B

2016-10-07

Four iminopyridines (N-N') differing in the nature of the substituents on the iminic carbon and on the ortho positions of the aryl ring (H or CH3) on the iminic nitrogen were used for the synthesis of neutral and monocationic palladium(ii) complexes of general formulae [Pd(CH3)Cl(N-N')] and [Pd(CH3)(NCCH3)(N-N')][PF6]. The detailed NMR characterization in solution highlighted that: (i) for both series of complexes, the Pd-CH3 signal is progressively shifted to a lower frequency on increasing the number of methyl groups on the ligand skeleton; (ii) for the neutral derivatives, the chemical shift of the (15)N NMR signals, determined through {(1)H,(15)N}-HMBC spectra, is significantly affected by the coordination to palladium; (iii) the coordination induced shift (CIS) of the nitrogen atom trans to the CH3 ligand is smaller than the other. The structure in the solid state for the neutral derivatives with all the four ligands was solved, pointing out that: (iv) the Pd-C bond distance increases with the basicity of the nitrogen-donor ligand; (v) the Pd-N bond distance correlates well with the CIS value. The combining of the solution and solid state structural features allows stating that: (vi) the Pd-CH3 singlet is a good probe for the electron donor capability of the ligand; (vii) the CIS value might be used as a probe for the strength of the Pd-N bond. All monocationic complexes generated active catalysts for the CO/vinyl arene copolymerization, leading to prevailingly syndiotactic polyketones. The catalyst performances, both in terms of catalyst productivity and polymer molecular weight, correlate well with the precatalyst structural features.

Synthesis, characterization, photoluminescent properties and antimicrobial activities of two novel polymeric silver(I) complexes with diclofenac

Science.gov (United States)

Hamamci Alisir, Sevim; Sariboga, Bahtiyar; Caglar, Sema; Buyukgungor, Orhan

2017-02-01

Two novel silver(I) complexes with diclofenac, ({2-(2,6-dicholoroanilino)phenylacetic acid} = dicl) namely [Ag(dicl)]n (1) and [Ag(dicl)(bipy)]n (2) (bipy: 4,4'-bipyridine), have been synthesized and characterized by elemental analysis, IR spectroscopy, thermal analysis and single-crystal X-ray diffraction. X-ray crystallographic data of 1 revealed that dicl anion adopts a μ3-η1,η2 coordinated mode link three Ag atoms generate 1D infinite chain structure. In 2, dicl ligand plays crucial role to form double-ladder chain structure, clamping two neighboring [Ag(μ-bipy)]∞ chains by using carboxylate oxygen atoms (O1, O2). The most interesting structural feature of 2 is the presence of strong π···π interactions between aromatic phenyl rings of dicl placed in the adjacent 1D chains, leads to forming 2D slab structure. The coordination modes of dicl in the title complexes are supported by using IR spectroscopy. Thermal stabilities of 1 and 2 have been determined by TG/DTA/DTG techniques. The luminescent properties of complex 1 and 2 have been investigated in the solid state at room temperature. Furthermore, the title complexes have been tested for their in vitro antibacterial activities and are determined to be highly effective for antibacterial activity against Gram(+) and Gram(-) pathogenic bacteria cells. 1 and 2 showed activity on Fungi, as well.

Synthesis, characterization and serum albumin binding studies of vitamin K3 derivatives.

Science.gov (United States)

Suganthi, Murugesan; Elango, Kuppanagounder P

2017-01-01

Synthesis, characterization and bovine serum albumin (BSA) binding properties of three derivatives of vitamin K3 have been described. Results of UV-Vis and fluorescence spectra indicate complexation between BSA and the ligands with conformational changes in protein, which is strongly supported by synchronous and three dimensional fluorescence studies. Addition of the ligands quenches the fluorescence of BSA which is accompanied by reduction in quantum yield (Ф) from 0.1010 to 0.0775-0.0986 range. Thermodynamic investigations reveal that hydrophobic interaction is the major binding force in the spontaneous binding of these ligands with BSA. The binding constants obtained depend on the substituent present in the quinone ring, which correlates linearly with the Taft's field substituent constant (σ F ). The results show that compound with strong electron withdrawing nitro-group forms relatively stronger complex with BSA than amino and thioglycolate substituted ones. Circular dichroism studies show that the α-helical content of the protein, upon complexation with the ligands, decreases in the case of amino and nitro substituted vitamin K3 while increases in thioglycolate substituted compound. Molecular docking studies indicated that the vitamin K3 derivatives are surrounded by hydrophobic residues of the BSA molecule, which is in good agreement with the results of fluorescence spectral and thermodynamic studies. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of composites of mixed oxides of iron ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 34; Issue 4. Synthesis and characterization of composites of mixed oxides of iron and neodymium in polymer matrix of aniline–formaldehyde. Sajdha H N Sheikh B L Kalsotra N Kumar S Kumar. Volume 34 Issue 4 July 2011 pp 843-851 ...

Novel acridone-modified MCM-41 type silica: Synthesis, characterization and fluorescence tuning

Directory of Open Access Journals (Sweden)

Maximilian Hemgesberg

2011-06-01

Full Text Available A Mobil Composition of Matter (MCM-41 type mesoporous silica material containing N-propylacridone groups has been successfully prepared by co-condensation of an appropriate organic precursor with tetraethyl orthosilicate (TEOS under alkaline sol–gel conditions. The resulting material was fully characterized by means of X-ray diffraction (XRD, N2-adsorption–desorption, transmission electron microscopy (TEM, IR and UV–vis spectroscopy, as well as 29Si and 13C CP-MAS NMR techniques. The material features a high inner surface area and a highly ordered two-dimensional hexagonal pore structure. The fluorescence properties of the organic chromophore can be tuned via complexation of its carbonyl group with scandium triflate, which makes the material a good candidate for solid state sensors and optics. The successful synthesis of highly ordered MCM materials through co-condensation was found to be dependent on the chemical interaction of the different precursors.

Synthesis of New Benzocoumaryl Oxadiazolyls as Strong Blue ...

African Journals Online (AJOL)

NICO

complexes in DSSCs.5 Beside this, in support of our investiga- ... synthesis and fluorescent studies on benzocoumarins12 and development of new heterocyclic ..... characterized by elemental analysis and spectroscopic data. 3.1. UV-visible ...

Microplasma synthesis on aluminum with additions of iron and nickel soluble complexes in electrolyte

Energy Technology Data Exchange (ETDEWEB)

Rogov, A.B., E-mail: alex-lab@bk.ru [Nikolaev Institute of Inorganic Chemistry. 3, Acad. Lavrentiev Ave, Novosibirsk, 630090 (Russian Federation); Mironov, I.V.; Terleeva, O.P.; Slonova, A.I. [Nikolaev Institute of Inorganic Chemistry. 3, Acad. Lavrentiev Ave, Novosibirsk, 630090 (Russian Federation)

2012-10-01

Highlights: Black-Right-Pointing-Pointer Alkaline homogeneous electrolyte with transition metals complexes. Black-Right-Pointing-Pointer Coatings contain metallic iron, nickel and their oxides in alumina-silica matrix. Black-Right-Pointing-Pointer Effect of Fe/Ni ratio on coatings properties and process characteristics. - Abstract: The microplasma synthesis of coatings containing iron and nickel from homogeneous electrolytes has been studied. For stabilization of transition metals in solution, it is proposed to use chelation. It was found that the synthesis of coatings using alternating current leads to the formation of metallic iron and nickel particles in addition to oxide phases. The iron and nickel complexes concentrations ratio in the electrolyte correlates with the coatings composition. Obtained coatings have been studied by scanning electron microscopy with X-ray microanalyser and by X-ray diffraction with Cu and Mo radiation. The metal content in the coating was determined spectrophotometrically from the absorption of iron thiocyanate complexes and nickel dimethylglyoxime complex.

Synthesis, characterization and biological activities of semicarbazones and their copper complexes.

Science.gov (United States)

Venkatachalam, Taracad K; Bernhardt, Paul V; Noble, Chris J; Fletcher, Nicholas; Pierens, Gregory K; Thurecht, Kris J; Reutens, David C

2016-09-01

Substituted semicarbazones/thiosemicarbazones and their copper complexes have been prepared and several single crystal structures examined. The copper complexes of these semicarbazone/thiosemicarbazones were prepared and several crystal structures examined. The single crystal X-ray structure of the pyridyl-substituted semicarbazone showed two types of copper complexes, a monomer and a dimer. We also found that the p-nitrophenyl semicarbazone formed a conventional 'magic lantern' acetate-bridged dimer. Electron Paramagnetic Resonance (EPR) of several of the copper complexes was consistent with the results of single crystal X-ray crystallography. The EPR spectra of the p-nitrophenyl semicarbazone copper complex in dimethylsulfoxide (DMSO) showed the presence of two species, confirming the structural information. Since thiosemicarbazones and semicarbazones have been reported to exhibit anticancer activity, we examined the anticancer activity of several of the derivatives reported in the present study and interestingly only the thiosemicarbazone showed activity while the semicarbazones were not active indicating that introduction of sulphur atom alters the biological profile of these thiosemicarbazones. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis and physicochemical characterization of rhenium (V) complexes with bisbenzoylthiosemicarbazones

International Nuclear Information System (INIS)

Gagieva, S.Ch.; Gutnova, N.A.; Tsaloev, A.T.; Khubulov, A.B.; Arutyunyants, A.A.; Galimov, Yu.B.

2003-01-01

Rhenium (V) complexing with mono- and bis-benzoylthiosemicarbazones is studied in dependence on hydrohalic acids concentration changes. It is determined that in media with high concentration of hydrohalic acids (6 mol/l HCl, 7 mol/l HBr) in dependence on reaction conditions stable complexes with bi- and tridentate coordination of thiosemicarbazone are formed. In the case of hydrohalic acid concentration decreasing stable binuclear and oxohydroxycomplexes are formed. Composition and structure of the compounds obtained are determined by the methods of element analysis, IR spectroscopy, conductometry. Thermal investigations of the compounds obtained are done [ru

An unsymmetrical porphyrin and its metal complexes: synthesis, spectroscopy, thermal analysis and liquid crystal properties

Directory of Open Access Journals (Sweden)

CHANGFU ZHUANG

2009-09-01

Full Text Available The synthesis and characterization of a new unsymmetrical porphyrin liquid crystal, 5-(4-stearoyloxyphenylphenyl-10,15,20-triphenylporphyrin (SPTPPH2 and its transition metal complexes (SPTPPM, M(II = Zn, Fe, Co, Ni, Cu or Mn are reported. Their structure and properties were studied by elemental analysis, and UV–Vis, IR, mass and 1H-HMR spectroscopy. Their luminescent properties were studied by excitation and emission spectroscopy. The quantum yields of the S1 ® S0 fluorescence were measured at room temperature. According to thermal studies, the complexes have a higher thermal stability (no decomposition until 200 °C. Differential scanning calorimetry (DSC data and an optical textural photograph, obtained using a polarizing microscope (POM, indicate that the porphyrin ligand had liquid crystalline character and that it exhibited more than one mesophase and a low-lying phase transition temperature, with transition temperatures of 19.3 and 79.4 °C; the temperature range of the liquid crystal (LC phase of the ligand was 70.1 °C.

Synthesis and characterization of the [Te(SCN2H4)4] (SO4)2 complex. Application to the separation of 99Mo from fission products

International Nuclear Information System (INIS)

Mestnik, S.A.C.; Silva, C.P.G. da.

1988-10-01

Thiourea reacts with tellurium-IV ions, in sulfuric medium, to form cationic complex which is strongly retained on cationic ion exchanger. The method was applied to separate 99 Mo from 132 Te obtained in the fission of 235 U since molybdenum does not form such complex and passes throught the cationic exchanger column in the molibdate form. In this paper, the procedure of the tellurium-thiourea complex preparation and its characterization are described. Elemental analysis, ultraviolet and infra-red absorption spectrophotometry as well as thermogravimetry were used to characterize the complex. (author) [pt

Synthesis and characterization of novel Cu(II) complex coated Fe3O4@SiO2 nanoparticles for catalytic performance

Science.gov (United States)

Nasrollahzadeh, Mahmoud; Sajjadi, Mohaddeseh; Khonakdar, Hossein Ali

2018-06-01

In this study, a convenient method for the synthesis of arylaminotetrazoles has been developed using a copper (II)-aminotetrazole complex immobilized on silica-coated Fe3O4 (Fe3O4@SiO2) nanoparticles (Fe3O4@SiO2-aminotet-Cu(II)) as a novel and efficient magnetically catalyst. The constructed superparamagnetic core-shell nanoparticles were successfully prepared, as proven using different spectroscopic techniques such as fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscope (TEM), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), thermogravimetry and differential thermogravimetry (TG-DTG) and vibrating sample magnetometer (VSM) analysis. The applicability of Fe3O4@SiO2-aminotet-Cu(II) magnetic catalyst allows the efficient synthesis of a variety of arylaminotetrazoles from the reaction between various arylcyanamides with sodium azide in high yields. The effect of catalyst loading was investigated. In addition, the reaction mechanism for the synthesis of arylaminotetrazoles was reasonably proposed. Results show that the 1-aryl-5-amino-1H-tetrazole (B isomer) and 5-arylamino-1H-tetrazole (A isomer) can be obtained from the arylcyanamides carrying electron-donating and electron-withdrawing substituents, respectively. This procedure offers a simple methodology, relatively short reaction times, easy work-up, high yields of the products and a cleaner reaction with elimination of hydrazoic acid (HN3). Moreover, catalyst can be conveniently recovered through the use of external magnet and reused for at least 6 times without any significant loss of its activity.

Synthesis and characterization of NiO nanoparticles by thermal decomposition of nickel linoleate and their optical properties

Energy Technology Data Exchange (ETDEWEB)

Kalam, Abul, E-mail: abul_k33@yahoo.com [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia); Al-Sehemi, Abdullah G.; Al-Shihri, Ayed S. [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia); Du Gaohui [Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Institute of Physical Chemistry, Zhejiang Normal University, Jinhua 321004 (China); Ahmad, Tokeer [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India)

2012-06-15

Well dispersed nickel oxide nanoparticles have been synthesized successfully by direct calcination of nickel linoleate. The structure, morphology and properties of the nanoparticles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy and ultraviolet-visible spectroscopy. Transmission electron microscopic studies show that nickel oxide nanoparticles are uniform with an average size of 14-20 nm. The optical band gap of 3.8 eV is obtained using UV-Visible spectroscopy which exhibits the red shift compared with the bulk counterpart. - Highlights: Black-Right-Pointing-Pointer Synthesis of metal oxide nanoparticles by using metal complexes as precursors. Black-Right-Pointing-Pointer Characterization of isolated nanoparticles using XRD, FTIR, SEM, TEM and HRTEM data. Black-Right-Pointing-Pointer The expected optical properties of these nanoparticles are clarified.

The Synthesis, Characterization and Catalytic Reaction Studies of Monodisperse Platinum Nanoparticles in Mesoporous Oxide Materials

Energy Technology Data Exchange (ETDEWEB)

Rioux, Robert M. [Univ. of California, Berkeley, CA (United States)

2006-01-01

A catalyst design program was implemented in which Pt nanoparticles, either of monodisperse size and/or shape were synthesized, characterized and studied in a number of hydrocarbon conversion reactions. The novel preparation of these materials enables exquisite control over their physical and chemical properties that could be controlled (and therefore rationally tuned) during synthesis. The ability to synthesize rather than prepare catalysts followed by thorough characterization enable accurate structure-function relationships to be elucidated. This thesis emphasizes all three aspects of catalyst design: synthesis, characterization and reactivity studies. The precise control of metal nanoparticle size, surface structure and composition may enable the development of highly active and selective heterogeneous catalysts.

Synthesis, Characterization and Antimicrobial Studies of a New Mannich Base N-[Morpholino(phenylmethyl]acetamide and Its Cobalt(II, Nickel(II and Copper(II Metal Complexes

Directory of Open Access Journals (Sweden)

L. Muruganandam

2012-01-01

Full Text Available A new Mannich base N-[morpholino(phenylmethyl]acetamide (MBA, was synthesized and characterized by spectral studies. Chelates of MBA with cobalt(II, nickel(II and copper(II ions were prepared and characterized by elemental analyses, IR and UV spectral studies. MBA was found to act as a bidentate ligand, bonding through the carbonyl oxygen of acetamide group and CNC nitrogen of morpholine moiety in all the complexes. Based on the magnetic moment values and UV-Visible spectral data, tetracoordinate geometry for nitrato complexes and hexacoordinate geometry for sulphato complexes were assigned. The antimicrobial studies show that the Co(II nitrato complex is more active than the other complexes.

Oxovanadium (iv) complexes with n/o- and o-donor ligands: their synthesis, characterization, semiempirical study and alkaline phosphatase activity (abstract)

International Nuclear Information System (INIS)

Munawar, K.S.; Ali, S.; Khan, A.N.

2011-01-01

Various N/O- and O-donor ligands and their oxovanadium complexes have been synthesized and characterized by different techniques such as FTIR, elemental analysis, thermogravimetery and conductometry. The IR data show the bidentate nature of the ligands and reveals hexa-coordinated geometry in the solid state which is also confirmed by semi-empirical study. Conductance measurements reveal the non-electrolytic nature of the complexes. These complexes have been checked for their alkaline phosphatase activity in the presence and absence of inhibitor which shows that by the addition of inhibitor the activity of enzyme decreases and at higher concentration it is completely inhibited. (author)

Synthesis and characterization of energetic thermoplastic elastomers for propellant formulations

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Aparecida M. Kawamoto

2009-01-01

Full Text Available Synthesis and characterization of energetic ABA-type thermoplastic elastomers for propellant formulations has been carried out. Following the working plan elaborated, the synthesis and characterization of Poly 3- bromomethyl-3-methyl oxetane (PolyBrMMO, Poly 3- azidomethyl-3-methyl oxetane (PolyAMMO, Poly 3,3-bis-azidomethyl oxetane (PolyBAMO and Copolymer PolyBAMO/AMMO (by TDI end capping has been successfully performed. The thermoplastic elastomers (TPEs were synthesized using the chain elongation process PolyAMMO, GAP and PolyBAMO by diisocyanates. In this method 2.4-toluene diisocyanate (TDI is used to link block A (hard and mono- functional to B (soft and di-functional. For the hard A-block we used PolyBAMO and for the soft B-block we used PolyAMMO or GAP.This is a joint project set up, some years ago, between the Chemistry Division of the Institute of Aeronautics and Space (IAE - subordinated to the Brazilian Ministry of Defense - and the Fraunhofer Institut Chemische Technologie (ICT, in Germany. The products were characterized by different techniques as IR- and (1H,13CNMR spectroscopies, elemental and thermal analyses. New methodologies based on FT-IR analysis have been developed as an alternative for the determination of the molecular weight and CHNO content of the energetic polymers.

DFT predictions, synthesis, stoichiometric structures and anti-diabetic activity of Cu (II) and Fe (III) complexes of quercetin, morin, and primuletin

Science.gov (United States)

Jabeen, Erum; Janjua, Naveed Kausar; Ahmed, Safeer; Murtaza, Iram; Ali, Tahir; Masood, Nosheen; Rizvi, Aysha Sarfraz; Murtaza, Gulam

2017-12-01

The current study is aimed at the synthesis of Cu (II) and Fe (III) complexes of three flavonoids {morin (mor), quercetin (quer) and primuletin (prim)} and characterization through UV-Vis spectroscopy, cyclic voltammetry, FTIR, and thermal analysis. Structure prediction through DFT calculation was supported by experimental data. Benesi-Hildebrand equation was modified to function for 1:2 Cu-flavonoid and 1:3 Fe-flavonoid complexes. DFT predictions revealed that out of poly chelation sites present in morin and quercetin, 3-OH site was utilized as preferable chelation site while primuletin chelated through 5-OH position. In-vivo trials revealed the complexes to have better anti-diabetic potential than respective flavonoid. Fls/M-Fls proved as antagonistic to Alloxan induced diabetes and also retained anti-diabetic activity even in the presence of (2-hydroxypropyl)-β-cyclodextrin (HPβCD).

Synthesis and characterization of an iron complex bearing a cyclic tetra-N-heterocyclic carbene ligand: An artifical heme analogue?

KAUST Repository

Anneser, Markus R.

2015-04-20

An iron(II) complex with a cyclic tetradentate ligand containing four N-heterocyclic carbenes was synthesized and characterized by means of NMR and IR spectroscopies, as well as by single-crystal X-ray structure analysis. The iron center exhibits an octahedral coordination geometry with two acetonitrile ligands in axial positions, showing structural analogies with porphyrine-ligated iron complexes. The acetonitrile ligands can readily be substituted by other ligands, for instance, dimethyl sulfoxide, carbon monoxide, and nitric oxide. Cyclic voltammetry was used to examine the electronic properties of the synthesized compounds. © 2015 American Chemical Society.

Hierarchical modeling and robust synthesis for the preliminary design of large scale complex systems

Science.gov (United States)

Koch, Patrick Nathan

Large-scale complex systems are characterized by multiple interacting subsystems and the analysis of multiple disciplines. The design and development of such systems inevitably requires the resolution of multiple conflicting objectives. The size of complex systems, however, prohibits the development of comprehensive system models, and thus these systems must be partitioned into their constituent parts. Because simultaneous solution of individual subsystem models is often not manageable iteration is inevitable and often excessive. In this dissertation these issues are addressed through the development of a method for hierarchical robust preliminary design exploration to facilitate concurrent system and subsystem design exploration, for the concurrent generation of robust system and subsystem specifications for the preliminary design of multi-level, multi-objective, large-scale complex systems. This method is developed through the integration and expansion of current design techniques: (1) Hierarchical partitioning and modeling techniques for partitioning large-scale complex systems into more tractable parts, and allowing integration of subproblems for system synthesis, (2) Statistical experimentation and approximation techniques for increasing both the efficiency and the comprehensiveness of preliminary design exploration, and (3) Noise modeling techniques for implementing robust preliminary design when approximate models are employed. The method developed and associated approaches are illustrated through their application to the preliminary design of a commercial turbofan turbine propulsion system; the turbofan system-level problem is partitioned into engine cycle and configuration design and a compressor module is integrated for more detailed subsystem-level design exploration, improving system evaluation.

Synthesis and Characterization of Poly(Amidoamine Dendrimers Encapsulatd 198Au Nanoparticles

Directory of Open Access Journals (Sweden)

R. Ritawidya1,2

2012-12-01

Full Text Available Brachytherapy or internal radiotherapy is one of many methods used for treatment of cancer. This modality requires an agent with radionuclides that emits  or β particle with a proper energy. 198Au (99% β max = 0.96 MeV and t1/2 = 2.69 days is one of radionuclides that has been considered to be effective for the above-mentioned purpose. The purpose of this research was to synthesis and characterize poly(amidoamine (PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles as a new brachytherapy agent. PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles was successfully synthesized by a bottom-up method using sodium borohydride as a reductor. Purification was then performed by a size exclusion chromatography in order to separate large Au nanoparticles that were formed outside the cavity of PAMAM G3.0 dendrimers. Prior to the synthesis of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles, the synthetic procedure was first established by using a non-radioactive Au. The PAMAM G3.0 dendrimers encapsulated Au nanoparticles produced was then characterized by using an UV-Vis spectroscopy, a transmission electron microscopy (TEM, particle size analyzer (PSA, and an atomic absorption spectroscopy (AAS. Characterization results revealed that PAMAM G3.0 dendrimers encapsulated Au nanoparticles that were prepared from a reaction mixture of PAMAM G3.0 dendrimers and Au HAuCl4 with mol ratio of 2.8, was found to be a proper formula. It produced PAMAM G3.0 dendrimers encapsulated Au nanoparticles with diameter of 1.743 nm, spheris, uniform and drug loading value of 26.34%. This formula was then used in synthesis using radioactive Au, 198Au. Characterization results of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles gave a radiochemical purity of 99.4% and zero charge.

Copper(II Complexes with Ligands Derived from 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one: Synthesis and Biological Activity

Directory of Open Access Journals (Sweden)

Raluca Cernat

2006-11-01

Full Text Available The synthesis of Cu(II complexes derived from Schiff base ligands obtainedby the condensation of 2-hydroxybenzaldehyde or terephtalic aldehyde with 4-amino-antipyrine (4-amino-2,3-dimethyl-1-phenyl-3-pyrazolin-5-one is presented. The newlyprepared compounds were characterized by 1H-NMR, UV-VIS, IR and ESRspectroscopy. The determination of the antimicrobial activity of the ligands and of thecomplexes was carried out on samples of Escherichia coli, Klebsiella pneumoniae,Acinetobacter boumanii, Pseudomonas aeruginosa, Staphylococcus aureus and Candidasp. The qualitative and quantitative antimicrobial activity test results proved that all theprepared complexes are very active, especially against samples of Ps. aeruginosa, A.Boumanii, E. coli and S. aureus.

Synthesis and antileishmanial activity of antimony (V) complexes of hydroxypyranone and hydroxypyridinone ligands.

Science.gov (United States)

Sheikhmoradi, Vafa; Saberi, Sedigheh; Saghaei, Lotfollah; Pestehchian, Nader; Fassihi, Afshin

2018-04-01

A novel series of antimony (V) complexes with the hydroxypyranone and hydroxypyridinone ligands were synthesized and characterized by 1 HNMR, FT-IR and electron spin ionization mass spectroscopic (ESI-MS) techniques. The synthesis process involved protection of hydroxyl group followed by the reaction of the intermediate with primary amines and finally deprotection. All compounds were evaluated for in vitro activities against the amastigote and promastigote forms of Leishmania major . Most of the synthesized compounds exhibited good antileishmanial activity against both forms of L. major . IC 50 values of the most active compounds; 9d , 9d and 9e , after 24, 48 and 72 h against amastigote model were 15, 12.5 and 5.5 μg/mL, respectively. 9e , 11 and 9e inhibited the promastigote form of parasite after 24, 48 and 72 h with IC 50 values of 10, 2 and 1 μg/mL, respectively.

Synthesis of praseodymium allyl iodide complex and its use in piperilene polymerization

International Nuclear Information System (INIS)

Gajlyunas, G.A.; Biktimirov, R.Kh.; Khajrullina, R.M.; Marina, N.G.; Manakov, Yu.B.; Tolstikov, G.A.

1987-01-01

Synthesis, structure and catalytic properties of tetrahydrofuran praseodymium allyl iodine complex (1) are described and studied. Complex 1 is formed during interaction of allyl iodine with metal praseodymium (the molar ratio is 2:1) in THF at room temperature with 97% yield. It represents the solid powder-like substance of the light-brown colour with a pale green shade, being sensitive to moisture and oxygen and decomposing at temperature >120 deg. On the basis of the IR-spectroscopy data the supposition about the dimeric (or n-dimensional) complex structure is made. The complex prepared in combination with tributyl aluminium during piperylene polymerization gives a high-stereoregular and high-molecular polypiperylene

Asymmetric Ruthenium(II and Osmium(II Complexes with New Bidentate Polyquinoline Ligands. Synthesis and NMR Characterization

Directory of Open Access Journals (Sweden)

Antonino Mamo

2010-03-01

Full Text Available A series of Ru(II and Os(II tris-chelate complexes with new bidentate 2-pyridylquinoline ligands have been synthesized and fully characterized by EA,1H-NMR and FAB-MS techniques. The new ligands are: L1 = 4-p-methoxyphenyl-6-bromo-2-(2′- pyridylquinoline (mphbr-pq and L2 = 4-p-hydroxyphenyl-6-bromo-2-(2′-pyridyl-quinoline (hphbr-pq. The complexes studied are: [Ru(bpy2L1](PF62 (C1, [Ru(bpy2L2](PF62 (C2, [Os(bpy2L1](PF62 (C3, [Os(bpy2L2](PF62 (C4 (bpy = 2,2′-bipyridine, [Ru(dmbpy2L1](PF62 (C5, [Ru(dmbpy2L2](PF62 (C6, [Os(dmbpy2L1](PF62 (C7, and [Os(dmbpy2L2](PF62 (C8 (dmbpy = 4,4′-dimethyl-2,2′-bipyridine. Moreover, new functionalized complexes C9-C12 were obtained by the basecatalyzed direct alkylation of C2, C4, C6, and C8 with 6-bromo-1-hexene. The complete assignment of the 1H-NMR spectra for the two new ligands (L1 and L2, and their Ru(II or Os(II complexes has been accomplished using a combination of one- and two-dimensional NMR techniques. The JH,H values have been determined for the majority of the resonances.

Synthesis, characterization, antibacterial and antifungal studies of some transition and rare earth metal complexes of N-benzylidene-2-hydroxybenzohydrazide

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T.K. Chondhekar

2011-12-01

Full Text Available The solid complexes of Cu(II, Co(II, Mn(II, La(III and Ce(III were prepared from bidentate Schiff base, N-benzylidene-2-hydroxybenzohydrazide. The Schiff base ligand was synthesized from 2-hyhdroxybenzohydrazide and benzaldehyde. These metal complexes were characterized by molar conductivity, magnetic susceptibility, thermal analysis, X-ray diffraction, FTIR, 1H-NMR, UV-Vis and mass spectroscopy. The analytical data of these metal complexes showed metal:ligand ratio of 1:2. The physico-chemical study supports the presence of square planar geometry around Cu(II and octahedral geometry around Mn(II, Co(II, La(III and Ce(III ions. The IR spectral data reveal that the ligand behaves as bidentate with ON donor atom sequence towards central metal ion. The molar conductance values of metal complexes suggest their non-electrolyte nature. The X-ray diffraction data suggest monoclinic crystal system for these complexes. Thermal behavior (TG/DTA and kinetic parameters calculated by Coats-Redfern method are suggestive of more ordered activated state in complex formation. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus niger and Trichoderma.

Mixed Metal Complexes of Isoniazid and Ascorbic Acid: Chelation ...

African Journals Online (AJOL)

HP

these ligands and their metal complexes have revealed the bi-dentate coordination of isoniazid ligand to ... of the drugs on coordination with a metal is enhanced ..... James, O.O., Nwinyi, C.O. and. Allensela, M.A. (2008). Cobalt(II) complexes of mixed antibiotics: Synthesis,. Characterization, antimicrobial potential and their.

Synthesis and spectral studies of some lanthanide(III) complexes ...

African Journals Online (AJOL)

... compounds were characterized through various physico-chemical studies. The coordinating ligand DABAAPS behave as tridentate N,N,O-donors. The central metal ion displays the coordination number nine in these complexes. Thermal stabilities of these complexes were also studied through thermogravimetric analysis.

Synthesis and characterization of dental composites

Science.gov (United States)

Djustiana, Nina; Greviana, Nadia; Faza, Yanwar; Sunarso

2018-02-01

During the last few decades, the increasing demands in esthetic dentistry have led to the development of dental composites material that provide similar appearance to the natural teeth. Recently, esthetic trend was an issue which increase the demand for teeth restorations that is similar with the origin. The esthetics of dental composite are more superior compared to amalgam, since its color look similar with natural teeth. Various dental composites have been developed using many type of fillers such as amorphous silica, quartz), borosilicate, Li-Sr-Ba-Al glass and oxide: zirconia and alumina. Researchers in Faculty of Dentistry University of Padjadjaran have prepared dental composites using zirconia-alumina-silica (ZAS) system as the filler. The aim is to improve the mechanical properties and the esthetic of the dental composites. The ZAS was obtained from chemical grade purity chemicals and Indonesia's natural sand as precursors its characterization were also presented. This novel method covers the procedure to synthesis and characterize dental composites in Padjadjaran University and some review about dental composites in global research.

Synthesis and characterization of nickel(II), cobalt(II), copper(II), manganese(II), zinc(II), zirconium(IV), dioxouranium(VI) and dioxomolybdenum(VI) complexes of a new Schiff base derived from salicylaldehyde and 5-methylpyrazole-3-carbohydrazide

International Nuclear Information System (INIS)

Syamal, A.; Maurya, M.R.

1986-01-01

Synthesis of a new Schiff base derived from salicylaldehyde and 5-methylpyrazole-3-carbohydrazide, and its coordination compounds with nickel(II), cobalt(II), copper(II), manganese(II), zinc(II), zirconium(IV), dioxouranium(VI) and dioxomolybdenum(VI) are described. The ligand and the complexes have been characterized on the basis of analytical, conductance, molecular weight, i.r., electronic and n.m.r. spectra and magnetic susceptibility measurements. The stoichiometries of the complexes are represented as NiL . 3H 2 O, CoL . 2H 2 O, CuL, MnL . 2H 2 O, ZnL . H 2 O, Zr(OH) 2 (LH) 2 , Zr(OH) 2 L . 2MeOH, UO 2 L . MeOH and MoO 2 L . MeOH (where LH 2 =Schiff base). The copper(II) complex shows a subnormal magnetic moment due to antiferromagnetic exchange interaction while the nickel(II), cobalt(II) and manganese(II) complexes show normal magnetic moments at room temperature. The i.r. and n.m.r. spectral studies show that the Schiff base behaves as a dibasic and tridentate ligand coordinating through the deprotonated phenolic oxygen, enolic oxygen and azomethine nitrogen. (orig.)

4,4′-Bipyridine-aided synthesis and characterization of Zn(II) and Cd(II) 2-sulfoterephthalate complexes

International Nuclear Information System (INIS)

Xiao, Shan-Shan; Li, Xin-Xin; Zheng, Xiang-Jun; Jia, Tian-Jing; Jin, Lin-Pei

2013-01-01

Six d 10 complexes, [Zn 1.5 (stp)(bpy) 0.5 (H 2 O) 2 ]·0.5H 2 O (1), Cd 1.5 (stp)(bpy) 0.5 (H 2 O) 2 (2), [Cd 1.5 (stp)(bpy)(H 2 O)]·H 2 O (3), [Zn 0.5 (bpy) 0.5 (H 2 O) 2 ][Zn(stp)(bpy)(H 2 O)]·0.5H 2 O (4), Cd 3 (stp) 2 (bpy) 3 (H 2 O) 3 (5), Hbpy·[Zn 0.5 (bpy)(H 2 O) 2 ][Zn 0.5 (stp)(H 2 O)]·H 2 O (6) based on 2-sulfoterephthalate (stp 3− ) and 4,4′-bipyridine (bpy) have been synthesized under hydro/solvo-thermal conditions and structurally characterized. Complex 1 exhibits a three-fold interpenetrated 3D porous architecture. Complexes 2 and 3 possess helices with different chirality arranging alternately. 4 and 6 are addition compounds, which compose of complex cation and complex anion. Complex 5 features a 3D layer-pillar framework in which a (4, 4) grid layer is constructed by stp 3− ligands and Cd(II) ions, and the layers are further connected by bpy pillars. The solid-state luminescent properties of the coordination polymers have also been investigated. - Graphical abstract: Display Omitted - Highlights: • Complexes 1–3 possess helices with different chirality arranging alternately. • The structural diversity can be attributed to various coordination modes of ligands. • The formation of helical structure is related to the adjacent carboxyl and sulfonate groups. • Bpy exhibits three roles: bridge, hydrogen bonding acceptor, and template

Synthesis characterization and toxicity of lanthanide complexes with schiff bases derived from S-benzoyl dithiocarbazate and aldehydes

Energy Technology Data Exchange (ETDEWEB)

Siddiqi, K S; Tabassum, S; Zaidi, S A.A.; Kureshy, R I; Khan, N H [Aligarh Muslim Univ. (India). Dept. of Chemistry

1989-12-01

New O:N:S and N:S donor ligands namely, S-benzoyl-N-(o-hydroxybenzaldehyde) dithiocarbazate, S-benzoyl-N-(N,N-dimethylaminobenzaldehyde ) dithiocarbazate, S-benzoyl-N(N-thiophene-2-aldehyde) dithiocarbazate and their complexes with La(III), Ce(III), Pr(III), Nd(III), Sm(III), Gd(III), Tb(III), Dy(III), Ho(III), Er(III), Yb(III), and Lu(III) have been synthesized and characterized on the basis of elemental analysis, IR, NMR and electronic spectroscopy. The nephelauxetic effect(1-{beta}overlined), bonding parameter, {beta}overlined, bsup(1/2) and Sinha covalency parameter {delta}, have been calculated. Their positive values indicate covalent nature of metal-ligand bond which is also supported by their molar conductances measured in nitrobenzene. Magnetic moment values exhibit paramagnetic nature of the complexes. Log K,{Delta}G, {Delta}H and {Delta}S values have also been ca lculated. Toxicity of the compounds has been evaluated against cockroaches and fungi(Aspergillus flavus and A. niger). The LD{sub 50} and % inhibition values demonstrate greater efficacy of the complexes than that of the free bases. (author). 4 tabs., 12 refs.

Synthesis characterization and toxicity of lanthanide complexes with schiff bases derived from S-benzoyl dithiocarbazate and aldehydes

International Nuclear Information System (INIS)

Siddiqi, K.S.; Tabassum, S.; Zaidi, S.A.A.; Kureshy, R.I.; Khan, N.H.

1989-01-01

New O:N:S and N:S donor ligands namely, S-benzoyl-N-(o-hydroxybenzaldehyde) dithiocarbazate, S-benzoyl-N-(N,N-dimethylaminobenzaldehyde ) dithiocarbazate, S-benzoyl-N(N-thiophene-2-aldehyde) dithiocarbazate and their complexes with La(III), Ce(III), Pr(III), Nd(III), Sm(III), Gd(III), Tb(III), Dy(III), Ho(III), Er(III), Yb(III), and Lu(III) have been synthesized and characterized on the basis of elemental analysis, IR, NMR and electronic spectroscopy. The nephelauxetic effect(1-βoverlined), bonding parameter, βoverlined, bsup(1/2) and Sinha covalency parameter δ, have been calculated. Their positive values indicate covalent nature of metal-ligand bond which is also supported by their molar conductances measured in nitrobenzene. Magnetic moment values exhibit paramagnetic nature of the complexes. Log K,ΔG, ΔH and ΔS values have also been ca lculated. Toxicity of the compounds has been evaluated against cockroaches and fungi(Aspergillus flavus and A. niger). The LD 50 and % inhibition values demonstrate greater efficacy of the complexes than that of the free bases. (author). 4 tabs., 12 refs

Mononuclear Pd(II) complex as a new therapeutic agent: Synthesis, characterization, biological activity, spectral and DNA binding approaches

Science.gov (United States)

Saeidifar, Maryam; Mirzaei, Hamidreza; Ahmadi Nasab, Navid; Mansouri-Torshizi, Hassan

2017-11-01

The binding ability between a new water-soluble palladium(II) complex [Pd(bpy)(bez-dtc)]Cl (where bpy is 2,2‧-bipyridine and bez-dtc is benzyl dithiocarbamate), as an antitumor agent, and calf thymus DNA was evaluated using various physicochemical methods, such as UV-Vis absorption, Competitive fluorescence studies, viscosity measurement, zeta potential and circular dichroism (CD) spectroscopy. The Pd(II) complex was synthesized and characterized using elemental analysis, molar conductivity measurements, FT-IR, 1H NMR, 13C NMR and electronic spectra studies. The anticancer activity against HeLa cell lines demonstrated lower cytotoxicity than cisplatin. The binding constants and the thermodynamic parameters were determined at different temperatures (300 K, 310 K and 320 K) and shown that the complex can bind to DNA via electrostatic forces. Furthermore, this result was confirmed by the viscosity and zeta potential measurements. The CD spectral results demonstrated that the binding of Pd(II) complex to DNA induced conformational changes in DNA. We hope that these results will provide a basis for further studies and practical clinical use of anticancer drugs.

New porphyrin-polyoxometalate hybrid materials: synthesis, characterization and investigation of catalytic activity in acetylation reactions.

Science.gov (United States)

Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

2012-10-14

New hybrid complexes based on covalent interaction between 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatozinc(II) and 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatotin(IV) chloride, and a Lindqvist-type polyoxometalate, Mo(6)O(19)(2-), were prepared. These new porphyrin-polyoxometalate hybrid materials were characterized by (1)H NMR, FT IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided several spectral data for synthesis of these compounds. Cyclic voltammetry showed the influence of the polyoxometalate on the redox process of the porphyrin ring. The catalytic activity of tin(IV)porphyrin-hexamolybdate hybrid material was investigated in the acetylation of alcohols and phenols with acetic anhydride. The reusability of this catalyst was also investigated.

Synthesis, characterization and antibacterial activity of a new calcium complex using sodium 2-mercaptobenzothiazole and 1, 10-phenanthroline as ligands

Science.gov (United States)

Gulab, Hussain; Shah, Zarbad; Mahmood, Mazhar; Shah, Syed Raza; Ali, Sajid; Iqbal, Muhammad; Khan, Muhammad Naeem; Flörke, Ulrich; Khan, Shahid Ali

2018-02-01

A new Ca-complex (Ca (H2 O)4 (C12 H8 N2)2)(C7 H4 N S2)2 has been synthesized by the reaction of calcium chloride, sodium 2-mercaptobenzothiazole and 1,10-phenanthroline. The complex was characterized by using X-ray crystallography and FT-IR spectroscopy. The complex was tested against different bacterial strains i.e. Staphylococcus aureus, Escherichia coli, Acinetobacter baumanni, Providencia stuartii and Pseudomonas aeruginosa. The complex was found to exhibit remarkable anti-bacterial activity against Pseudomonas aeruginosa with an inhibition zone of 25 mm and good anti-bacterial activity against Acinetobacter baumanni with a zone of inhibition of 16 mm comparable to the Levofloxacin standard (zone of inhibition of 25 mm).

Synthesis, characterization and gas sensing performance of SnO2 ...

Indian Academy of Sciences (India)

Synthesis, characterization and gas sensing performance of SnO2 thin films prepared by spray pyrolysis. GANESH E PATIL, D D KAJALE, D N CHAVAN†, N K PAWAR††, P T AHIRE, S D SHINDE#,. V B GAIKWAD# and G H JAIN. ∗. Materials Research Laboratory, Arts, Commerce and Science College, Nandgaon 423 106, ...

Low-level waste characterization plan for the WSCF Laboratory Complex

International Nuclear Information System (INIS)

Morrison, J.A.

1994-01-01

The Waste Characterization Plan for the Waste Sampling and Characterization Facility (WSCF) complex describes the organization and methodology for characterization of all waste streams that are transferred from the WSCF Laboratory Complex to the Hanford Site 200 Areas Storage and Disposal Facilities. Waste generated at the WSCF complex typically originates from analytical or radiological procedures. Process knowledge is derived from these operations and should be considered an accurate description of WSCF generated waste. Sample contribution is accounted for in the laboratory waste designation process and unused or excess samples are returned to the originator for disposal. The report describes procedures and processes common to all waste streams; individual waste streams; and radionuclide characterization methodology

Synthesis and Characterization of Electroresponsive Materials with Applications In: Part I. Second Harmonic Generation. Part II. Organic-Lanthanide Ion Complexes for Electroluminescence and Optical Amplifiers.

Science.gov (United States)

Claude, Charles

1995-01-01

Materials for optical waveguides were developed from two different approaches, inorganic-organic composites and soft gel polymers. Inorganic-organic composites were developed from alkoxysilane and organically modified silanes based on nonlinear optical chromophores. Organically modified silanes based on N-((3^' -trialkoxysilyl)propyl)-4-nitroaniline were synthesized and sol-gelled with trimethoxysilane. After a densification process at 190^circC with a corona discharge, the second harmonic of the film was measured with a Nd:YAG laser with a fundamental wavelength of 1064nm, d_{33} = 13pm/V. The decay of the second harmonic was expressed by a stretched bi-exponential equation. The decay time (tau _2) was equal to 3374 hours, and was comparable to nonlinear optical systems based on epoxy/Disperse Orange 1. The processing temperature of the organically modified silane was limited to 200^circC due to the decomposition of the organic chromophore. Soft gel polymers were synthesized and characterized for the development of optical waveguides with dc-electrical field assisted phase-matching. Polymers based on 4-nitroaniline terminated poly(ethylene oxide-co-propylene oxide) were shown to exhibit second harmonic generation that were optically phase-matched in an electrical field. The optical signals were stable and reproducible. Siloxane polymers modified with 1-mercapto-4-nitrobenzene and 1-mercapto-4-methylsulfonylstilbene nonlinear optical chromophores were synthesized. The physical and the linear and nonlinear optical properties of the polymers were characterized. Waveguides were developed from the polymers which were optically phase -matched and had an efficiency of 8.1%. The siloxane polymers exhibited optical phase-matching in an applied electrical field and can be used with a semiconductor laser. Organic lanthanide ion complexes for electroluminescence and optical amplifiers were synthesized and characterized. The complexes were characterized for their thermal and

Materials Research Society Symposium Proceedings Volume 635. Anisotropic Nanoparticles - Synthesis, Characterization and Applications

National Research Council Canada - National Science Library

Lyon, L

2000-01-01

This volume contains a series of papers originally presented at Symposium C, "Anisotropic Nanoparticles Synthesis, Characterization and Applications," at the 2000 MRS Fall Meeting in Boston, Massachusetts...

Synthesis, characterization, biological and electrical conductivity ...

African Journals Online (AJOL)

All the complexes have been characterized on the basis of elemental analyses, magnetic susceptibility measurement, electronic and IR spectra and thermogravimetric analysis. The IR spectral data suggested that the ligands behave as dibasic tridentate moiety towards the central metal ion coordinating through phenolic ...

Nano-/micro metallic wire synthesis on Si substrate and their characterization

International Nuclear Information System (INIS)

Kaur, Jaskiran; Kaur, Harmanmeet; Singh, Surinder; Kanjilal, Dinakar; Chakarvarti, Shiv Kumar

2014-01-01

Nano-/micro wires of copper are grown on semiconducting Si substrate using the template method. It involves the irradiation of 8 um thick polymeric layer coated on Si with150 MeV Ni ion beam at a fluence of 2E8. Later, by using the simple technique of electrodeposition, copper nano-/micro wires were grown via template synthesis. Synthesized wires were morphologically characterized using SEM and electrical characterization was carried out by finding I-V plot

Synthesis of ruthenium (III) complexes with benzimidazole derivatives

International Nuclear Information System (INIS)

Vyas, P.C.; Chahar, Yogesh K.; Garg, Yajula; Seth, Gita

2003-01-01

Complexes of ruthenium with biologically important benzimidazole derivatives, viz. 2-(2'-hydroxyphenyl) benzimidazole (HOPBI), 2-2'- mercaptophenyl) benzimidazole (HSPBI), 2- (2'-hydroxynaphthyl) benzimidazole (HONBI) have been synthesized and characterized. (author)

Synthesis, characterization and antibacterial screening of 2,4 ...

African Journals Online (AJOL)

Air stable silver Ag(I) complexes of pyrimethamine and trimethoprim drugs have been synthesized and characterized by elemental analysis, Fourier transform infrared (FTIR) and ultraviolet visible (UV-Vis) spectroscopy, and conductivity measurement. The metal complexes formed a three and four coordinate geometry with ...

Synthesis and complexation of acyclic dithiolate ligands

International Nuclear Information System (INIS)

Ashford, L.

1999-11-01

-[N,N'-bis(p-nitro-o-mereaptobenzyliden)propylenediaminate, Copper- [N,N'-bis(p-nitro-o-mercaptobenzyliden)propylenediaminate and Nickel-[N,N'-bis(o-mercaptobenzyliden)propylenediaminate] are analysed. Comparison of the data of the Ni(II) species show the major effects of the para-nitro group arise from electron withdrawal from the thiolate donors. The synthesis and complexation of the (2-mercaptomethyl)thiophenolato series of ligands, via the corresponding (2-hydroxymethyl)thiophenolato compounds, is detailed. Removal of β-elimination pathways by use of an o-xylyl linker allows the synthesis of α,α'-di[(2-mercaptomethyl)thiophenolato]-o-xylene. Reaction of α,α'-di[(2-mercaptomethyl)thiophenolato]-o-xylene with Group 10 metal ions Ni(II) and Pd(ll) monomers and a Pt(ll) trinuclear complex. Potential causes of the broad and featureless resonances in the 1 H NMR spectra of the complexes are investigated. The Ni(II) and Pd(ll) monomers are reacted with Pt(ll) salts to give trinuclear species. (author)

Iron complexes of pharmaceutical interest: Antianemics

Directory of Open Access Journals (Sweden)

Cakić Milorad D.

2003-01-01

Full Text Available Preparations based on different compounds of bi- and trivalent iron are curently used for the prevention and therapy of sideropenic anemia in human and veterinary medicine. The application of preparations based on dextran started about 1950. Up to now, synthesis and production of preparations were performed with the purpose of improving pharmacological performance by using dextran oligosaccharides with different weight - average molar masses and their oxidized and hydrogenated derivatives. Synthesis of polynuclear iron(lll complexs with other oligosaccharides (inulin and pullulan and their derivatives was developed, with potential or valid pharmacological activity for sideropenic anemia treatment.A Review of iron(lll complexes with different oligosaccharides, their physico-chemical characterization pharmaco-biological performance, global structure, further research and possible applications of then complexes, are presented in this paper.

Zinc(II) halide complexes with 2-methoxyaniline ligand: Synthesis, characterization, thermal analyses, crystal structure determination and luminescent properties

Science.gov (United States)

Amani, Vahid

2018-03-01

Three new mononuclear zinc(II) complexes, [Zn(2-MeO-C6H4NH2)2X2] (X is Cl in 1, Br in 2 and I in 3), were prepared from the reactions of ZnX2 with 2-methoxyaniline (2-MeO-C6H4NH2) ligand in methanol. Suitable crystals of these complexes were obtained for X-ray diffraction measurements by slow evaporation of methanol solution at room temperature. The three complexes were thoroughly characterized by thermogravimetric analysis, elemental analysis (CHNO), spectral methods (IR, UV-Vis, 13C{1H}NMR, 1H NMR and luminescence), and single crystal X-ray diffraction. The X-ray structural analysis indicated that in the structures of these complexes, the zinc(II) cation is four-coordinated in a distorted tetrahedral configuration by two N atoms from two 2-methoxyanyline ligands and two halide anions. Also, in these complexes intermolecular interactions, for example Nsbnd H⋯X hydrogen bonds (in 1-3), Csbnd H⋯X hydrogen bonds (in 3), Csbnd H⋯π interactions (in 1 and 2) and π⋯π interactions (in 3), are effective in the stabilization of the crystal structures. In addition, the luminescence spectra of all complexes in methanolic solution show that the intensity of their emission bands is stronger than that for free 2-methoxyaniline ligand.

Synthesis and characterization of poly aniline for electrochemical biosensor construction

International Nuclear Information System (INIS)

Magalhaes, Gleice S.L.; Southgate, Erica F.; Alhadeff, Eliana M.; Guimaraes, Maria Jose O.C.

2011-01-01

Conductors polymers have many attractive interests to the industry due their highly technological applications. This work treats specially of polyaniline because it's large electrical conductivity, electrochemical properties, associate to the chemical stability in environmental conditions and synthesis facility. The main of this work is the application in a construction of an electrochemical biosensor for ethanol detection and quantification. Different conditions of synthesis of the conductor emeraldine polyaniline form were studied, investigated the influence of the dopant agent and the reactional environment conditions temperature on the reaction yield and conductivities. The polyaniline that showed the best conductivity were characterized by differential and thermal gravimetric analysis, infrared spectroscopy, X ray diffraction, and cycle voltammetry, comparing with the commercial polyaniline. (author)

Synthesis and characterization of Au incorporated Alq3 nanowires

Science.gov (United States)

Khan, Mohammad Bilal; Ahmad, Sultan; Parwaz, M.; Rahul, Khan, Zishan H.

2018-05-01

We report the synthesis and characterization of pure and Au incorporated Alq3 nanowires. These nanowires are synthesized using thermal vapor transport method. The luminescence intensity of Au incorporated Alq3 nanowires are recorded to be higher than that of pure Alq3 nanowires, which is found to increase with the increase in Au concentration. Fluorescence quenching is also observed when Au concentration is increased beyond the certain limit.

Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

Science.gov (United States)

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-03-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

Design, synthesis and characterization of a highly luminescent Eu-complex monomer featuring thenoyltrifluoroacetone and 5-acryloxyethoxymethyl-8-hydroxyquinoline

Energy Technology Data Exchange (ETDEWEB)

Xu Cunjin [State Key Laboratory of Chemical Engineering, Department of Chemical and Biochemical Engineering, Zhejiang University, Hangzhou 310027 (China); College of Material, Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036 (China); Li Bogeng, E-mail: bgli@zju.edu.cn [State Key Laboratory of Chemical Engineering, Department of Chemical and Biochemical Engineering, Zhejiang University, Hangzhou 310027 (China); Wan Jintao; Bu Zhiyang [State Key Laboratory of Chemical Engineering, Department of Chemical and Biochemical Engineering, Zhejiang University, Hangzhou 310027 (China)

2011-08-15

A multi-functional ligand, 5-acryloxyethoxymethyl-8-hydroxyquinoline (Hamq), was synthesized, which contained a polymerizable C=C double bond for the copolymerization with other vinyl monomers and acted as photon antenna able to transfer energy to Eu{sup 3+} ions effectively. The triplet state energy of Hamq was determined to be 22,370 cm{sup -1} via the phosphorescence spectra of Hamq and its gadolinium complex. The title complex monomer Eu(tta){sub 2}(amq) was prepared by coordination reaction of Hamq with europium isopropoxide and 2-thenoyltrifluoroacetone (Htta) in dry organic solvents under argon atmosphere and characterized by elemental analysis and IR spectrum. The photophysical properties of the complex were studied in detail with UV-vis, luminescence spectra, luminescence lifetime and quantum yield. The complex exhibited nearly monochromatic red emission at 612 nm, a remarkable luminescence quantum yield at room temperature (30.6%) upon ligand excitation and a long {sup 5}D{sub 0} lifetime (389 {mu}s), which indicated that the ligand Hamq could sensitize the luminescence of Eu(III) ion efficiently in Eu(tta){sub 2}(amq), resulting in a strong luminescence of its copolymer poly[MMA-co-Eu(TTA){sub 2}(amq)] under UV excitation. The excellent luminescence properties of the complex made it not only a promising light-conversion molecular device but also an excellent luminescent monomer. - Highlights: >iWe designed and synthesized a highly luminescent Eu-complex monomer. > Quantum yield and lifetime of the complex are 30.6% and 389 {mu}s, respectively. > Excellent luminescence of the complex made it an excellent luminescent monomer.

Synthesis and characterization of variable-architecture thermosensitive polymers for complexation with DNA.

Science.gov (United States)

Pennadam, Sivanand S; Ellis, James S; Lavigne, Matthieu D; Górecki, Dariusz C; Davies, Martyn C; Alexander, Cameron

2007-01-02

Copolymers of N-isopropylacrylamide with a fluorescent probe monomer were grafted to branched poly(ethyleneimine) to generate polycations that exhibited lower critical solution temperature (LCST) behavior. The structures of these polymers were confirmed by spectroscopy, and their phase transitions before and after complexation with DNA were followed using ultraviolet and fluorescence spectroscopy and light scattering. Interactions with DNA were investigated by ethidium bromide displacement assays, while temperature-induced changes in structure of both polymers and polymer-DNA complexes were evaluated by fluorescence spectroscopy, dynamic light scattering, laser Doppler anemometry, and atomic force microscopy (AFM) in water and buffer solutions. The results showed that changes in polymer architecture were mirrored by variations in the architectures of the complexes and that the overall effect of the temperature-mediated changes was dependent on the graft polymer architecture and content, as well as the solvent medium, concentrations, and stoichiometries of the complexes. Furthermore, AFM indicated subtle changes in polymer-DNA complexes at the microstructural level that could not be detected by light scattering techniques. Uniquely, variable-temperature aqueous-phase AFM was able to show that changes in the structures of these complexes were not uniform across a population of polymer-DNA condensates, with isolated complexes compacting above LCST even though the sample as a whole showed a tendency for aggregation of complexes above LCST over time. These results indicate that sample heterogeneities can be accentuated in responsive polymer--DNA complexes through LCST-mediated changes--a factor that is likely to be important in cellular uptake and nucleic acid transport.

Synthesis, characterization, DNA interaction and antimicrobial screening of isatin-based polypyridyl mixed-ligand Cu(II and Zn(II complexes

Directory of Open Access Journals (Sweden)

NATARAJAN RAMAN

2010-06-01

Full Text Available Several mixed ligand Cu(II/Zn(II complexes using 3-(phenyl-imino-1,3-dihydro-2H-indol-2-one (obtained by the condensation of isatin and aniline as the primary ligand and 1,10-phenanthroline (phen/2,2’-bipyridine (bpy as an additional ligand were synthesized and characterized analytically and spectroscopically by elemental analyses, magnetic susceptibility and molar conductance measurements, as well as by UV–Vis, IR, NMR and FAB mass spectroscopy. The interaction of the complexes with calf thymus (CT DNA was studied using absorption spectra, cyclic voltammetric and viscosity measurements. They exhibit absorption hypochromicity, and the specific viscosity increased during the binding of the complexes to calf thymus DNA. The shifts in the oxidation–reduction potential and changes in peak current on addition of DNA were shown by CV measurements. The Cu(II/Zn(II complexes were found to promote cleavage of pUC19 DNA from the supercoiled form I to the open circular form II and linear form III. The complexes show enhanced antifungal and antibacterial activities compared with the free ligand.

Synthesis, characterization and antibacterial activity of aspirin and ...

African Journals Online (AJOL)

Dr J. T. Ekanem

Novel complexes of Co (11), Ni (11) and Fe (111) with aspirin and paracetamol have synthesized and characterized using infrared, electronic and Hnmr spectral, melting point and conductivity measurements. The two ligands have been found to act as bidentate chelating agents. Aspirin complexes coordinate through the ...

Green synthesis and characterization of graphene nanosheets

Energy Technology Data Exchange (ETDEWEB)

Tavakoli, Farnosh [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

2015-03-15

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

Green synthesis and characterization of graphene nanosheets

International Nuclear Information System (INIS)

Tavakoli, Farnosh; Salavati-Niasari, Masoud; Badiei, Alireza; Mohandes, Fatemeh

2015-01-01

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products

Scaling up complex interventions: insights from a realist synthesis.

Science.gov (United States)

Willis, Cameron D; Riley, Barbara L; Stockton, Lisa; Abramowicz, Aneta; Zummach, Dana; Wong, Geoff; Robinson, Kerry L; Best, Allan

2016-12-19

Preventing chronic diseases, such as cancer, cardiovascular disease and diabetes, requires complex interventions, involving multi-component and multi-level efforts that are tailored to the contexts in which they are delivered. Despite an increasing number of complex interventions in public health, many fail to be 'scaled up'. This study aimed to increase understanding of how and under what conditions complex public health interventions may be scaled up to benefit more people and populations.A realist synthesis was conducted and discussed at an in-person workshop involving practitioners responsible for scaling up activities. Realist approaches view causality through the linkages between changes in contexts (C) that activate mechanisms (M), leading to specific outcomes (O) (CMO configurations). To focus this review, three cases of complex interventions that had been successfully scaled up were included: Vibrant Communities, Youth Build USA and Pathways to Education. A search strategy of published and grey literature related to each case was developed, involving searches of relevant databases and nominations from experts. Data extracted from included documents were classified according to CMO configurations within strategic themes. Findings were compared and contrasted with guidance from diffusion theory, and interpreted with knowledge users to identify practical implications and potential directions for future research.Four core mechanisms were identified, namely awareness, commitment, confidence and trust. These mechanisms were activated within two broad scaling up strategies, those of renewing and regenerating, and documenting success. Within each strategy, specific actions to change contexts included building partnerships, conducting evaluations, engaging political support and adapting funding models. These modified contexts triggered the identified mechanisms, leading to a range of scaling up outcomes, such as commitment of new communities, changes in relevant

Novel synthesis on poly (vinyl alcohol): characterization, complexation a biological activity

International Nuclear Information System (INIS)

El-Sawy, N.M.; Elassar, A.Z.; Al-Fulaij, O.

2002-01-01

Poly(vinyl alcohol), PVA, readily condensed with phenyl hydrazine and malononitrile in basic medium to give the hydrazone and pyran derivatives, respectively. PVA reacted with chloroacetonitrile, biuet and thiophene carbonyl chloride to give modified polymeric materials. While addition of PVA to acrylonitrile and phenyl isothiocyanate gives the ether and thiocarbamate ester derivatives, respectively. Hydroxylamine hydrochloride reacted with the modified, carbonitrile containing, polymer to give the amidoxime derivative. The amidoximated products of PVA and carbamate ester of polymeric material were complexed with CUCL2 solution. The complex materials were confirmed by using UV and ESDS measurements. The morphology of PVA and complex with CUII was observed by SEM. Biological activity of some of the prepared compounds was investigated toward bacteria and fungi

Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

Science.gov (United States)

Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

2015-07-01

Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis, characterization, cytotoxic and antitubercular activities of new gold(I) and gold(III) complexes containing ligands derived from carbohydrates.

Science.gov (United States)

Chaves, Joana Darc Souza; Damasceno, Jaqueline Lopes; Paula, Marcela Cristina Ferreira; de Oliveira, Pollyanna Francielli; Azevedo, Gustavo Chevitarese; Matos, Renato Camargo; Lourenço, Maria Cristina S; Tavares, Denise Crispim; Silva, Heveline; Fontes, Ana Paula Soares; de Almeida, Mauro Vieira

2015-10-01

Novel gold(I) and gold(III) complexes containing derivatives of D-galactose, D-ribose and D-glucono-1,5-lactone as ligands were synthesized and characterized by IR, (1)H, and (13)C NMR, high resolution mass spectra and cyclic voltammetry. The compounds were evaluated in vitro for their cytotoxicity against three types of tumor cells: cervical carcinoma (HeLa) breast adenocarcinoma (MCF-7) and glioblastoma (MO59J) and one non-tumor cell line: human lung fibroblasts (GM07492A). Their antitubercular activity was evaluated as well expressed as the minimum inhibitory concentration (MIC90) in μg/mL. In general, the gold(I) complexes were more active than gold(III) complexes, for example, the gold(I) complex (1) was about 8.8 times and 7.6 times more cytotoxic than gold(III) complex (8) in MO59J and MCF-7 cells, respectively. Ribose and alkyl phosphine derivative complexes were more active than galactose and aryl phosphine complexes. The presence of a thiazolidine ring did not improve the cytotoxicity. The study of the cytotoxic activity revealed effective antitumor activities for the gold(I) complexes, being more active than cisplatin in all the tested tumor cell lines. Gold(I) compounds (1), (2), (3), (4) and (6) exhibited relevant antitubercular activity even when compared with first line drugs such as rifampicin.

Synthesis of nanosilver on polyamide fabric using silver/ammonia complex.

Science.gov (United States)

Montazer, Majid; Shamei, Ali; Alimohammadi, Farbod

2014-05-01

In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH3)2](+). The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV-vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and characterization of some metal complexes of a Schiff ...

African Journals Online (AJOL)

KEY WORDS: Metal complexes, Schiff base, Ninhydrin, α,L-Alanine, .... Buck Scientific Infrared Spectrophotometer Model 500 in the range of 4000 .... Assignments based on Nakamoto [35], ν - stretching vibration, δ - bending or deformation.

Synthesis and study of dioxouranium (6) carboxylate complexes with ammonia

International Nuclear Information System (INIS)

Spitsyn, V.I.; Mazo, G.N.; Dunaev, K.M.; Santalova, N.A.

1980-01-01

Heterophase synthesis of a series of ammonia complexes of dioxouranium (6) carboxylates namely, UO 2 (HCOO) 2 x2NH 3 , UO 2 (CH 3 COO) 2 x2NH 3 , UO 2 (CH 3 CH 2 OO) 2 x2NH 3 is presented and their properties and structure are studied. Comparison of infrared spectra of dioxouranium (6) carboxylates and their ammonia complexes has shown that NH 3 molecule introduction changes in principle the coordination of azidoligand turning out bridge carboxylate groups into island ones and weakening their bonds with central cations. In spectra of all diammiacates the shift of bands of deformational and valent oscillations of N-H bond in comparison with spectrum of pure ammonia tells about NH 3 coordination with metal. Complexes thermolysis has been studied under iso- and polythermal conditions. General diagram of thermal decay is presented [ru

Characterization of complex networks : Application to robustness analysis

NARCIS (Netherlands)

Jamakovic, A.

2008-01-01

This thesis focuses on the topological characterization of complex networks. It specifically focuses on those elementary graph measures that are of interest when quantifying topology-related aspects of the robustness of complex networks. This thesis makes the following contributions to the field of

Synthesis of samarium complexes with the derivative binder of Schiff Quinolinic base. Characterization and photophysical study; Sintesis de complejos de samario con el ligante derivado de base de Schiff Quinolinica. Caracterizacion y estudio fotofisico

Energy Technology Data Exchange (ETDEWEB)

Lucas H, J.

2016-07-01

In this work we determined the metal: binder stoichiometry of the species formed during the UV/Vis spectrophotometric titration of the derivative binder of Schiff quinolinic base, L1 with the samarium nitrate pentahydrate in methanol. Statistical analysis of the data allowed proposing the metal: binder stoichiometry for the synthesis of the complexes which was one mole of samarium salt by 2.5 moles of binder and thus favor the formation of complexes with 1M: 1L and 1M: 2L stoichiometries. They were synthesized in aqueous-organic medium (water-ethanol), isolated and purified two complexes with stoichiometry 1 Sm: 1 L1, complex 1 and 1 Sm: 2 L1, complex 2. The overall yield of the reaction was 76%. The characterization of the formed complexes was performed by visible ultraviolet spectrometry (UV/Vis), nuclear magnetic resonance, X-ray photoelectron spectroscopy (XP S), thermal gravimetric analysis with differential scanning calorimetry (TGA/DSC), and radial distribution function. These complexes were studied by fluorescence and emission phosphorescence at variable temperature. Spectroscopic techniques used in both solution and solid demonstrated the formation and stability of these complexes. In addition XP S indicated that in both complexes the samarium retains its oxidation state 3+. Luminescence studies indicated that there is intra-binding charge transfer which decreases the transfer of light energy from the binder to the samarium. Based on the experimental results, L1 binder molecules and complexes 1 and 2 were modeled that demonstrated the proposed Nc for each complex, as well as allowed to visualize the structural arrangement of the molecules, complexes and binder. (Author)

Use of collagen hydrolysate as a complex nitrogen source for the synthesis of penicillin by Penicillium chrysogenum.

Science.gov (United States)

Leonhartsberger, S; Lafferty, R M; Korneti, L

1993-09-01

Optimal conditions for both biomass formation and penicillin synthesis by a strain of Penicillium chrysogenum were determined when using a collagen-derived nitrogen source. Preliminary investigations were carried out in shaken flask cultures employing a planned experimental program termed the Graeco-Latin square technique (Auden et al., 1967). It was initially determined that up to 30% of a conventional complex nitrogen source such as cottonseed meal could be replaced by the collagen-derived nitrogen source without decreasing the productivity with respect to the penicillin yield. In the pilot scale experiments using a 30 l stirred tank type of bioreactor, higher penicillin yields were obtained when 70% of the conventional complex nitrogen source in the form of cottonseed meal was replaced by the collagen hydrolysate. Furthermore, the maximum rate of penicillin synthesis continued for over a longer period when using collagen hydrolysate as a complex nitrogen source. Penicillin synthesis rates were determined using a linear regression.

Synthesis and characterization of lanthanum complex (5-choloro-8-hydroxy quinoline) bis (2-2'bipyridine) lanthanum La(Bpy)2(5-Clq)

Science.gov (United States)

Kumar, Rahul; Soam, Ankur; Bhargava, Parag

2017-05-01

Lanthanum complex, (5-choloro 8-hydroxy quinoline) bis (2-2'bipyridine) has been synthesized and characterized by different techniques. Lanthanum complex, La(Bpy)2(5-Clq) was characterized for structural, thermal and photoluminescence analysis. Structural analysis of this material was done by Fourier transformed infrared spectroscopy (FTIR) and mass spectroscopy. Thermal analysis of this material was done by thermal gravimetric analysis (TGA) and material shows the thermal stability up to 400°C. Absorption and emission spectra of the material was measured by UV-visible spectroscopy and photoluminescence spectroscopy. Solution of this material La(Bpy)2(5-Clq) in ethanol showed absorption peak at 332 nm, which may be attributed due to (π - π*) transitions. The photoluminescence spectra of La(Bpy)2(5-Clq) in ethanol solution showed intense peak at 505 nm.

Synthesis quality control and biodistribution of technetium-99m triamcinolone (99mTc-TA) complex: An inflammation tracer agent

International Nuclear Information System (INIS)

Rizvii, Faheem Askari; Naqvi, Syed Ali Raza; Mehdi, Muhammad; Roohi, Samina; Zahoor, Ameer Fawad; Khan, Zulfiqar Ali; Sohaib, Muhammad; Rasheed, Rashid

2017-01-01

In present study synthesis of 99m Tc-triamcinolone acetonide ( 99m Tc-TA) complex and its stability using set of quality control parameters such as ligand concentration, reducing agent concentration, pH, temperature and reaction time was assessed. 99m Tc-TA complex was characterized in terms of percent (%) yield, stability in saline and serum using chromatographic procedures. Radiochemically the 99m Tc-TA complex was found quite stable in saline and serum. After 30 min of reaction the complex showed maximum radiochemical yield of 96.32% which decreased to 96.25 % after 4 h incubation period. In serum, the % yield of radiochemical was remained same up to 2 h which decreased to 93.5% at 24 h time point. Normal biodistribution pattern in Sprague-Dawley rats revealed liver, stomach and kidneys as areas of high 99m Tc-TA complex uptake (8.44 ±1.32, 8.75 ± 1.03 and 12.67 ± 1.21%, respectively) at 1 h post injection time point. Scintigraphy of 99m Tc-TA in rabbits showed similar eco as observed in biodistribution study. Based on the promising results obtained in context of in vitro and in vivo stability and biodistribution, 99m Tc-TA complex could be further studied to identify the inflammation based diseases

Fluorido complexes of technetium

Energy Technology Data Exchange (ETDEWEB)

Mariappan Balasekaran, Samundeeswari

2013-07-04

Fluorine chemistry has received considerable interest during recent years due to its significant role in the life sciences, especially for drug development. Despite the great nuclear medicinal importance of the radioactive metal technetium in radiopharmaceuticals, its coordination chemistry with the fluorido ligand is by far less explored than that of other ligands. Up to now, only a few technetium fluorides are known. This thesis contains the synthesis, spectroscopic and structural characterization of novel technetium fluorides in the oxidation states ''+1'', ''+2'', ''+4'' and ''+6''. In the oxidation state ''+6'', the fluoridotechnetates were synthesized either from nitridotechnetic(VI) acid or from pertechnetate by using reducing agent and have been isolated as cesium or tetraethylammonium salts. The compounds were characterized spectroscopically and structurally. In the intermediate oxidation state ''+4'', hexafluoridotechnetate(IV) was known for long time and studied spectroscopically. This thesis reports novel and improved syntheses and solved the critical issues of early publications such as the color, some spectroscopic properties and the structure of this key compound. Single crystal analyses of alkali metal, ammonium and tetramethylammonium salts of hexafluoridotechnetate(IV) are presented. In aqueous alkaline solutions, the ammonium salt of hexafluoridotechnetate(IV) undergoes hydrolysis and forms an oxido-bridged dimeric complex. It is the first step hydrolysis product of hexafluoridotechnetate(IV) and was characterized by spectroscopic and crystallographic methods. Low-valent technetium fluorides with the metal in the oxidation states of ''+2'' or ''+1'' are almost unknown. A detailed description of the synthesis and characterization of pentafluoridonitrosyltechnetate(II) is presented. The

Mononuclear mercury(II) complexes containing bipyridine derivatives and thiocyanate ligands: Synthesis, characterization, crystal structure determination, and luminescent properties

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Amani, Vahid; Alizadeh, Robabeh; Alavije, Hanieh Soleimani; Heydari, Samira Fadaei; Abafat, Marzieh

2017-08-01

A series of mercury(II) complexes, [Hg(Nsbnd N)(SCN)2] (Nsbnd N is 4,4‧-dimethyl-2,2‧-bipyridine in 1, 5,5‧-dimethyl-2,2‧-bipyridine in 2, 6,6‧-dimethyl-2,2‧-bipyridine in 3 and 6-methyl-2,2‧-bipyridine in 4), were prepared from the reactions of Hg(SCN)2 with mentioned ligands in methanol. Suitable crystals of these complexes were obtained for X-ray diffraction measurement by methanol diffusion into a DMSO solution. The four complexes were thoroughly characterized by spectral methods (IR, UV-Vis, 13C{1H}NMR, 1H NMR and luminescence), elemental analysis (CHNS) and single crystal X-ray diffraction. The X-ray structural analysis indicated that in the structures of these complexes, the mercury(II) cation is four-coordinated in a distorted tetrahedral configuration by two S atoms from two thiocyanate anions and two N atoms from one chelating 2,2‧-bipyridine derivative ligand. Also, in these complexes intermolecular interactions, for example Csbnd H⋯N hydrogen bonds (in 1-4), Csbnd H⋯S hydrogen bonds (in 1, 2 and 4), π … π interactions (in 2-4), Hg⋯N interactions (in 2) and S⋯S interactions (in 4), are effective in the stabilization of the crystal structures and the formation of the 3D supramolecular complexes. Furthermore, the luminescence spectra of the title complexes show that the intensity of their emission bands are stronger than the emission bands for the free bipyridine derivative ligands.

Synthesis, characterization and fluorescence studies of a novel europium complex based sensor

International Nuclear Information System (INIS)

Li Bin; Chen Qiuyun; Wang Yachen; Huang Jing; Li Yang

2010-01-01

A novel europium(III) complex was synthesized using TTA (α-thenoyltrifluoroacetone) as the first ligand and H 2 bpdc (2,2'-bipyridine-3,3'-dicarboxylate) as the second ligand. Elemental analysis, thermal analysis, IR and UV-vis spectrum and fluorescence spectrum of the europium(III) complex were carried out. A characteristic Eu 3+ fluorescence emission was observed in ethanol-water (1:1) solution, indicating that the complex is stable in solution and the emission of Eu(III) ions was not influenced by the water molecules. The fluorescence emission of the complex was quenched completely by the Co 2+ and Fe 3+ ions, but the quenched emission was recovered in the presence of glycine. Moreover, the Eu 3+ emission was very sensitive to pH, so the complex can be used as pH-dependent fluorescence probe or chemosensors.

Synthesis, spectroscopic characterization, crystallographic studies and antibacterial assays of new copper(II) complexes with sulfathiazole and nimesulide

Science.gov (United States)

Nunes, Julia Helena Bormio; de Paiva, Raphael Enoque Ferraz; Cuin, Alexandre; da Costa Ferreira, Ana Maria; Lustri, Wilton Rogério; Corbi, Pedro Paulo

2016-05-01

New ternary copper(II) complexes of sulfathiazole (SFT, C9H8N3O2S2) or nimesulide (NMS, C13H11N2O5S) and 2,2‧-bipyridine (bipy) were synthesized, and characterized by chemical and spectroscopic techniques. Elemental analyses indicated a 2:1:1 sulfonamide/copper/bipy composition for both complexes. Mass spectrometric measurements permitted identifying the molecular ions [Cu(SFT)2(bipy)+H]+ and [Cu(NMS)2(bipy)+H]+ at m/z 728 and 835, respectively, confirming the proposed compositions. Crystal structure of the [Cu(SFT)2(bipy)] complex was solved by powder X-ray diffraction analysis (PXRD), attesting that the Cu(II) ion is hexacoordinated in a distorted octahedral geometry. Each SFT molecule coordinates to the metal ion by the nitrogen atoms of the SO2-N group and of the heterocyclic ring. The coordination sphere is completed by a bipyridine. Electronic paramagnetic resonance (EPR) studies were carried out for the [Cu(NMS)2(bipy)] complex, indicating a tetragonal environment around the metal ion. It was suggested that NMS coordinates to Cu(II) by the nitrogen and oxygen atoms of the SO2-N group, which was confirmed by infrared spectroscopic studies. Biological studies showed the antibacterial activity of both Cu-SFT and Cu-NMS complexes, with the minimum inhibitory concentration (MIC) values ranging from 0.10 to 0.84 mmol L-1 against Gram-negative bacteria for [Cu(SFT)2(bipy)], and from 1.50 to 3.00 mmol L-1 against Gram-positive and -negative bacteria for [Cu(NMS)2(bipy)].

Synthesis, Characterization and Antibacterial Studies of N-(Benzothiazol-2-yl)-4-chlorobenzenesulphonamide and Its Neodymium(III) and Thallium(III) Complexes.

Science.gov (United States)

Obasi, Lawrence Nnamdi; Oruma, Uchechukwu Susan; Al-Swaidan, Ibrahim Abdulrazak; Ramasami, Ponnadurai; Ezeorah, Chigozie Julius; Ochonogor, Alfred Ezinna

2017-02-22

N -(Benzothiazol-2-yl)-4-chlorobenzenesulphonamide (NBTCS) was synthesized by condensation reaction of 4-chlorobenzenesulphonyl chloride and 2-aminobenzothiazole in acetone under reflux. Neodymium(III) and thallium(III) complexes of the ligand were also synthesized. Both ligand and metal complexes were characterized using UV-Vis, IR, ¹H- and 13 C-NMR spectroscopies, elemental analysis and molar conductance measurement. IR studies revealed that the ligand is tridentate and coordinates to the metal ions through nitrogen and oxygen atoms of the sulphonamide group and nitrogen atom attached to benzothiazole ring. The neodymium(III) complex displays a coordination number of eight while thallium(III) complex displays a coordination number of six. The ligand and its complexes were screened in vitro for their antibacterial activities against Escherichia coli strains ( E. coli 6 and E. coli 13 ), Proteus species, Staphylococcus aureus and Pseudomonas aeruginosa using the agar well diffusion technique. The synthesized compounds were found to be more active against the microorganisms screened relative to ciprofloxacin, gentamicin and co-trimoxazole.

Synthesis, characterization and antimicrobial activities of a Schiff ...

African Journals Online (AJOL)

Complexes of Cu(II), Ni(II) and Mn(II) with a Schiff base derived from condensation reaction of phenylalanine and acetylacetone have been synthesized and characterized analytically and spectroscopically. Melting point of the Schiff base was 188oC and the complexes decompose within a temperature range of 210-242oC.

New aminoporphyrins bearing urea derivative substituents: synthesis, characterization, antibacterial and antifungal activity

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Gholamreza Karimipour

2015-06-01

Full Text Available This work studied the synthesis of 5,10,15-tris(4-aminophenyl-20-(N,N-dialkyl/diaryl-N-phenylurea porphyrins (P1-P4 with alkyl or aryl groups of Ph, iPr, Et and Me, respectively and also the preparation of their manganese (III and cobalt (II complexes (MnP and CoP. The P1-P4 ligands were characterized by different spectroscopic techniques (1H NMR, FTIR, UV-Vis and elemental analysis, and metalated with Mn and Co acetate salts. The antibacterial and antifungal activities of these compounds in vitro were investigated by agar-disc diffusion method against Escherichia coli (-, Pseudomonas aeruginosa (-, Staphylococcus aureus(+, Bacillus subtilis (+ and Aspergillus oryzae and Candida albicans. Results showed that antibacterial and antifungal activity of the test samples increased with increase of their concentrations and the highest activity was obtained when the concentration of porphyrin compounds was 100 µg/mL. The activity for the porphyrin ligands depended on the nature of the urea derivative substituents and increased in the order P1 > P2 > P3 >P4, which was consistent with the order of their liposolubility. MnP and CoP complexes exhibited much higher antibacterial and antifungal activity than P1-P4ligands. Further, the growth inhibitory effects of these compounds was generally in the order CoP complexes > MnP complexes > P1-P4 ligands. Among these porphyrin compounds, CoP1displayed the highest antibacterial and antifungal activity, especially with a concentration of 100 µg/mL, against all the four tested bacteria and two fungi, and therefore it could be potential to be used as drug.

Synthesis and characterization of chiral thorium(IV) and uranium(IV) benzamidinate complexes

Energy Technology Data Exchange (ETDEWEB)

Schoene, Sebastian; Maerz, Juliane; Kaden, Peter; Patzschke, Michael; Ikeda-Ohno, Atsushi [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Chemistry of the F-Elements

2017-06-01

Two chiral benzamidinate complexes of tetravalent actinides (Th(IV) and U(IV)) were synthesized using a salt metathesis reaction of the corresponding actinide(IV) tetrachlorides and the potassium salt of the chiral benzamidine (S,S)-N,N-Bis-(1-phenylethyl)-benzamidine ((S)-HPEBA). The structure of the complexes was determined with single crystal X-ray diffraction. These are the first examples of chiral amidinate complexes of actinides.

Synthesis, physical characterization, antibacterial activity and ...

African Journals Online (AJOL)

Some five-coordinated cobalt(III) complexes were synthesized and characterized using elemental analysis, 1H NMR and IR spectra. The formation constants and the thermodynamic parameters were measured spectrophotometrically for the 1:1 adduct formation of [Co(Chel)(PBu3)]ClO4.H2O where Chel = cd3OMesalen, ...

Boron-based nanostructures: Synthesis, functionalization, and characterization

Science.gov (United States)

Bedasso, Eyrusalam Kifyalew

Boron-based nanostructures have not been explored in detail; however, these structures have the potential to revolutionize many fields including electronics and biomedicine. The research discussed in this dissertation focuses on synthesis, functionalization, and characterization of boron-based zero-dimensional nanostructures (core/shell and nanoparticles) and one-dimensional nanostructures (nanorods). The first project investigates the synthesis and functionalization of boron-based core/shell nanoparticles. Two boron-containing core/shell nanoparticles, namely boron/iron oxide and boron/silica, were synthesized. Initially, boron nanoparticles with a diameter between 10-100 nm were prepared by decomposition of nido-decaborane (B10H14) followed by formation of a core/shell structure. The core/shell structures were prepared using the appropriate precursor, iron source and silica source, for the shell in the presence of boron nanoparticles. The formation of core/shell nanostructures was confirmed using high resolution TEM. Then, the core/shell nanoparticles underwent a surface modification. Boron/iron oxide core/shell nanoparticles were functionalized with oleic acid, citric acid, amine-terminated polyethylene glycol, folic acid, and dopamine, and boron/silica core/shell nanoparticles were modified with 3-(amino propyl) triethoxy silane, 3-(2-aminoethyleamino)propyltrimethoxysilane), citric acid, folic acid, amine-terminated polyethylene glycol, and O-(2-Carboxyethyl)polyethylene glycol. A UV-Vis and ATR-FTIR analysis established the success of surface modification. The cytotoxicity of water-soluble core/shell nanoparticles was studied in triple negative breast cancer cell line MDA-MB-231 and the result showed the compounds are not toxic. The second project highlights optimization of reaction conditions for the synthesis of boron nanorods. This synthesis, done via reduction of boron oxide with molten lithium, was studied to produce boron nanorods without any

Synthesis, characterization, electrochemical studies and X-ray structures of mixed-ligand polypyridyl copper(II complexes with the acetate

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Adekunle Oluwafunmilayo F.

2016-01-01

Full Text Available [Cu(phen2(CH3COO](ClO4.2H2O (1 and [Cu(bipy2(CH3COO]-(ClO4.H2O (2 {phen = 1,10-phenanthroline, bipy = 2,2’-bipyridine}were synthesized and characterized. The complexes were characterized by employying elemental analyses, infrared and UV-Visible spectroscopy, room temperature magnetic measurements and the crystal structures elucidated using X-ray diffraction experiment. The redox properties of the complexes were also investigated. Both structures have a square pyramidal CuN4O chromophore which exhibit significant distortions due to long Cu-O [2.217(3 Å for (1 and 2.179 (1 for (2] and Cu-N [2.631(2 Å for (1 and 2.714(1 Å for (2] bonds. This distortion if further shown by the O-Cu-N bond angles [147.71(8 o for (1 and 153.40(5 o for (2]. The elemental analyses further support the structural details unveiled by the single crystal X-ray diffraction analysis. The infrared spectra shows the acetate vibrational frequencies at 1587 cm-1,1428 cm-1, 1314 cm-1 for (1 and 1571 cm-1, 1441 cm-1, 1319c m-1 for (2 and the perchlo-rate bands at 1059 cm-1, 720 cm-1 (1 and 1080 cm-1,768 cm-1 (2. The broad d-d bands for the copper ion at 14,514 cm-1(1 and 14,535 cm-1(2 support the adoption of square pyramid geometries. The magnetic moments for the two complexes are 1.83 B.M for (1 and 1.72 B.M for (2. The peak to peak values of the two complexes show that the electrode reactions are quasi-reversibile with ΔEp = 0.023V (1 and 0.025V for (2. In both structures, there are π-π intermolecular interactions in addition to hydrogen bonding between the units.

Synthesis, purification and characterization of [3,5 - T] p-aminobenzoic acid

International Nuclear Information System (INIS)

Corol-Cucu, Delia-Irina; Chiper, Diana; Mihaila, V.; Negoita, N.

2000-01-01

This paper refers to the synthesis, purification and characterization of [3,5-T] p-aminobenzoic acid (PAB,H' vitamine). The p-aminobenzoic acid is used in the treatment of rheumatic arthritis and dermatological affections. The advantage of tritium labelling of p-aminobenzoic acid is that some biomedical important aspects of collagen's behaviour are made clear. The PAB stimulate the grow of intestinal bacteria so necessary to synthesis of some vitamins (bio tine, pantothenic acid). Tritium is the only radioactive isotope of hydrogen. Several steps have to be carried out in the synthesis of the final product as well as to study its biological behavior. For the labelling of PAB one prefers the substitution of bromine from PAB-3,5-Br with tritium because of simplicity of reaction and the easy synthesis of halogen compound. The first step in synthesis is the protection of NH 2 group through acetylation of PAB. After that PAB is bromated into the 3 and 5 position with elementary bromine. The raw compound is purified and recrystallized and characterized through thin layer chromatography.The tritium labelling is performed through substitution of bromine from bromate derivative, using Pd/C (10% Pd) as catalyst and low basic conditions for the neutralization of HBr resulting from reaction. After the separation of PAB-3,5-T through filtration, the catalyst remains on the filter paper and the labelled compound goes in aqueous solution. PAB-3,5-T is purified through thin layer chromatography with the solvent system n-BuOH:NH 4 OH(25%):H 2 O:EtOH (8:1:2:2,5, v/v) with silica gel GF 254 as support. The determination of activity is carried out with LSC (Liquid Scintillation Counter). A 98% purity was determined through TLC in the same conditions while determination of activity distribution was performed with a 2π Berthold scanner with gas running and without window. The chemical concentration has been measured through UV spectrophotometry and by comparing extinction with

Characterization and complexation of humic acid

International Nuclear Information System (INIS)

Kim, J.I.; Buckau, G.; Klenze, R.; Rhee, D.S.; Wimmer, H.

1990-05-01

This paper summarizes the research contributions to the CEC project MIRAGE II, particularly the research area: complexation and colloids (COCO). The first part of the paper comprises the characterization of humic and fulvic acids from different origins: a commercial product from Aldrich Co. used as a reference humic acid and site specific humic acids from Gorleben (FRG), Boom Clay (B) and Fanay Augeres (F) aquifer systems. The second part includes the complexation of trivalent actinides: Am(III) and Cm(III) with various humic acids. A number of different methods have been applied for the complexation study: spectrophotometry, ultrafiltration, laser-indused photoacoustic spectroscopy (LPAS) and time resolved laser fluorescence spectroscopy (TRLFS). The evaluation process of complexation constant is discussed extensively and the well consolidated results are presented, which can be directly used for the geochemical modelling of the radionuclide migration. (orig.)

Mitochondrial complex III defects contribute to inefficient respiration and ATP synthesis in the myocardium of Trypanosoma cruzi-infected mice.

Science.gov (United States)

Wen, Jian-Jun; Garg, Nisha Jain

2010-01-01

In this study, we conducted a thorough analysis of mitochondrial bioenergetic function as well as the biochemical and molecular factors that are deregulated and contribute to compromised adenosine triphosphate (ATP) production in the myocardium during Trypanosoma cruzi infection. We show that ADP-stimulated state 3 respiration and ATP synthesis supported by pyruvate/malate (provides electrons to complex I) and succinate (provides electrons to complex II) substrates were significantly decreased in left ventricular tissue and isolated cardiac mitochondria of infected mice. The decreased mitochondrial ATP synthesis in infected murine hearts was not a result of uncoupling between the electron-transport chain and oxidative phosphorylation and decreased availability of the intermediary metabolites (e.g., NADH). The observed decline in the activities of complex-I, -IV, and -V was not physiologically relevant and did not contribute to compromised respiration and ATP synthesis in infected myocardium. Instead, complex III activity was decreased above the threshold level and contributed to respiratory-chain inefficiency and the resulting decline in mitochondrial ATP synthesis in infected myocardium. The loss in complex III activity occurred as a consequence of cytochrome b depletion. Treatment of infected mice with phenyl-alpha-tert-butyl nitrone (PBN, antioxidant) was beneficial in preserving the mtDNA-encoded cytochrome b expression, and subsequently resulted in improved complex III activity, mitochondrial respiration, and ATP production in infected myocardium. Overall, we provide novel data on the mechanism(s) involved in cardiac bioenergetic inefficiency during T. cruzi infection.

Sol – Gel synthesis and characterization of magnesium peroxide nanoparticles

International Nuclear Information System (INIS)

Jaison, J; Chan, Y S; Ashok raja, C; Balakumar, S

2015-01-01

Magnesium peroxide is an excellent source of oxygen in agriculture applications, for instance it is used in waste management as a material for soil bioremediation to remove contaminants from polluted underground water, biological wastes treatment to break down hydrocarbon, etc. In the present study, sol-gel synthesis of magnesium peroxide (MgO 2 ) nanoparticles is reported. Magnesium peroxide is odourless; fine peroxide which releases oxygen when reacts with water. During the sol-gel synthesis, the magnesium malonate intermediate is formed which was then calcinated to obtain MgO 2 nanoparticles. The synthesized nanoparticles were characterized using Thermo gravimetric -Differential Thermal Analysis (TG- DTA), X-Ray Diffraction studies (XRD) and High Resolution Transmission Electron Microscope (HRTEM). Our study provides a clear insight that the formation of magnesium malonate during the synthesis was due to the reaction between magnesium acetate, oxalic acid and ethanol. In our study, we can conclude that the calcination temperature has a strong influence on particle size, morphology, monodispersity and the chemistry of the particles. (paper)

Synthesis and characterization of divalent metal complexes with ligand derived from the reaction of 3-aminopyridine and biacetyl

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RAMESH KUMAR

2006-09-01

Full Text Available Divalent cobalt, nickel and copper salts reacted in situ with 3-aminopyridine and biacetyl to form complexes of the type: [M(Ap2biac2X2], where Ap2biac is the ligand and X=Cl, Br, NO3 or NCS. The complexes were analysed and characterized as distorted octahedral by conductance, molecular weight, magnetic, electronic and IR spectral studies. The electronic spectra were interpreted and tentative aassignments made. The infrared spectral studies revealed that two molecules of 3-aminopyridine were joined by molecules of biacetyl through a two carbon atom bridge and that the ligand coordinated through azomethine nitrogen atoms, whereas the pyridine nitrogen does not participate in the coordination. In the far infrared spectra, various metal–ligand vibrations were observed and are discussed.

Anticancer Activity of Polyoxometalate-Bisphosphonate Complexes: Synthesis, Characterization, In Vitro and In Vivo Results.

Science.gov (United States)

Boulmier, Amandine; Feng, Xinxin; Oms, Olivier; Mialane, Pierre; Rivière, Eric; Shin, Christopher J; Yao, Jiaqi; Kubo, Tadahiko; Furuta, Taisuke; Oldfield, Eric; Dolbecq, Anne

2017-07-03

We synthesized a series of polyoxometalate-bisphosphonate complexes containing Mo VI O 6 octahedra, zoledronate, or an N-alkyl (n-C 6 or n-C 8 ) zoledronate analogue, and in two cases, Mn as a heterometal. Mo 6 L 2 (L = Zol, ZolC 6 , ZolC 8 ) and Mo 4 L 2 Mn (L = Zol, ZolC 8 ) were characterized by using single-crystal X-ray crystallography and/or IR spectroscopy, elemental and energy dispersive X-ray analysis and 31 P NMR. We found promising activity against human nonsmall cell lung cancer (NCI-H460) cells with IC 50 values for growth inhibition of ∼5 μM per bisphosphonate ligand. The effects of bisphosphonate complexation on IC 50 decreased with increasing bisphosphonate chain length: C 0 ≈ 6.1×, C 6 ≈ 3.4×, and C 8 ≈ 1.1×. We then determined the activity of one of the most potent compounds in the series, Mo 4 Zol 2 Mn(III), against SK-ES-1 sarcoma cells in a mouse xenograft system finding a ∼5× decrease in tumor volume than found with the parent compound zoledronate at the same compound dosing (5 μg/mouse). Overall, the results are of interest since we show for the first time that heteropolyoxomolybdate-bisphosphonate hybrids kill tumor cells in vitro and significantly decrease tumor growth, in vivo, opening up new possibilities for targeting both Ras as well as epidermal growth factor receptor driven cancers.

Synthesis and Characterization of Block Copolymers with Unique Chemical Functionalities and Entropically-Hindering Moieties

Science.gov (United States)

2017-08-14

methanol as a function of chemistry , morphology and hydration levels. Accomplishments: This section is included in the "upload" section. Training...Copolymer Blend Membranes.” In Press, Polymer Engineering and Science, DOI: 10.1002 /pen.24508, 2017. 5. M. Pérez-Pérez and D. Suleiman. “Synthesis and...Synthesis and Characterization of Sulfonated Amine Block Copolymers for Energy Efficient Applications". Chemical Engineering Symposium, University of

Synthesis of (2-[{sup 11}C]Methoxy)rotenone, a marker of mitochondrial complex I activity

Energy Technology Data Exchange (ETDEWEB)

Charalambous, A; Mangner, T J; Kilbourn, M R

1995-01-01

Recent studies suggest that defects in the function of the complexes of the electron transport chain might be involved in the pathology of neurological diseases such as mitochondrial encephalopathies, Parkinson's Huntington's and Alzheimer's disease. Rotenone is a potent reversible competitive inhibitor of complex I (NADH-CoQ reductase). To study the possible involvement of complex I in such diseases, we synthesized (2-[{sup 11}C]methoxy)rotenone by [{sup 11}C]alkylation of 2-O-desmethyl rotenone methyl enol ether followed by hydrolysis of the enol ether to the ketone using aqueous trifluoroacetic acid. (2-[{sup 11}C]Methoxy)rotenone was purified by high pressure liquid chromatography (silica gel) and was obtained in 7-10% yields decay corrected to end of bombardment in synthesis times typically shorter than 48 min. Radiochemical purities were over 95% and specific activities averaged 1000 Ci/mmol at end of synthesis.

Synthesis and characterization of Ni(II, Cu(II and Co(III complexes with polyamine-containing macrocycles bearing an aminoethyl pendant arm

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K. S. SIDDIQI

2004-09-01

Full Text Available Reaction of [M(ppn2]X2 (where M = Cu(II, Ni(II, Co(II and ppn = 1,3-diaminopropane with formaldehyde and ethylenediamine in methanol results in the ready formation of a 16-membered macrocyclic complex. The complexes were characterized by elemental anlysis, IR, EPR, electronic spectral data, magnetic moments and conductance measurements. The Cu(II, Ni(II and Co(III complexes are coordinated axially with both pendant groups of the hexadentate macrocycle. These pendant donors are attached to the macrocycle by a carbon chain. The electrical conductivities of the Cu(II and Ni(II chelates indicated them to be 1:2 electrolytes whilst those of Co(III is a 1:3 electrolyte in DMSO. The EPR spectrum of the copper complex exhibited G at 3.66, which indicates a considerable exchange interaction in the complex. Spectroscopic evidence suggests that in all of the complexes the metal ion is in an octahedral environment.

Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

Science.gov (United States)

Destiarti, Lia; Wahyuni, Nelly; Prawatya, Yopa Eka; Sasri, Risya

2017-03-01

Synthesis and characterization of mangan oxide coated sand from quartz sand fraction of Capkala kaolin has been conducted. There were two methods on synthesis of Mangan Oxide Coated Sand (MOCS) from Capkala Kaolin compared in this research. Characterization of MOCS was done by using Scanning Electron Microscope/Energy Dispersive X-Ray Spectrometer (SEM/EDX) and X-Ray Diffraction (XRD). The MOCS was tested to reduce phosphate in laundry waste. The result showed that the natural sand had bigger agregates and a relatively uniform structural orientation while both MOCS had heterogen structural orientation and manganese oxide formed in cluster. Manganese in first and second methods were 1,93% and 2,63%, respectively. The XRD spectrum showed clear reflections at 22,80°, 36,04°, 37,60° and a broad band at 26,62° (SiO2). Based on XRD spectrum, it can be concluded that mineral constituents of MOCS was verified corresponding to pyrolusite (MnO2). The former MOCS could reduce almost 60% while the later could reduce 70% phosphate in laundry waste.

Synthesis, Spectroscopy, Theoretical, and Electrochemical Studies of Zn(II, Cd(II, and Hg(II Azide and Thiocyanate Complexes of a New Symmetric Schiff-Base Ligand

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Morteza Montazerozohori

2013-01-01

Full Text Available Synthesis of zinc(II/cadmium(II/mercury(II thiocyanate and azide complexes of a new bidentate Schiff-base ligand (L with general formula of MLX2 (M = Zn(II, Cd(II, and Hg(II in ethanol solution at room temperature is reported. The ligand and metal complexes were characterized by using ultraviolet-visible (UV-visible, Fourier transform infrared (FT-IR, 1H- and 13C-NMR spectroscopy and physical characterization, CHN analysis, and molar conductivity. 1H- and 13C-NMR spectra have been studied in DMSO-d6. The reasonable shifts of FT-IR and NMR spectral signals of the complexes with respect to the free ligand confirm well coordination of Schiff-base ligand and anions in an inner sphere coordination space. The conductivity measurements as well as spectral data indicated that the complexes are nonelectrolyte. Theoretical optimization on the structure of ligand and its complexes was performed at the Becke’s three-parameter hybrid functional (B3 with the nonlocal correlation of Lee-Yang-Parr (LYP level of theory with double-zeta valence (LANL2DZ basis set using GAUSSIAN 03 suite of program, and then some theoretical structural parameters such as bond lengths, bond angles, and torsion angles were obtained. Finally, electrochemical behavior of ligand and its complexes was investigated. Cyclic voltammograms of metal complexes showed considerable changes with respect to free ligand.

Synthesis, characterization and interaction of N,N'-dipyridoxyl (1,4-butanediamine) Co(III) salen complex with DNA and HSA

Science.gov (United States)

Janati Fard, F.; Mashhadi Khoshkhoo, Z.; Mirtabatabaei, H.; Housaindokht, M. R.; Jalal, R.; Eshtiagh Hosseini, H.; Bozorgmehr, M. R.; Esmaeili, A. A.; Javan Khoshkholgh, M.

2012-11-01

Co(III) salen complex with N,N'-dipyridoxyl (1,4-butanediamine) Schiff-base ligand as tetradentate ligand was synthesized and characterized by the elemental and spectroscopic analysis. The interaction of this complex with calf thymus DNA (ct DNA) has been investigated in vitro using UV absorption, fluorescence spectroscopy, thermal denaturation and gel electrophoresis techniques. The binding constant has been estimated to be 1 × 104 M-1 using UV absorption. The addition of ct DNA to Co(III) salen solution resulted in a fluorescence quenching. The binding constant and site size binding have been calculated in connection with other experimental observations show that the interactive model between Co(III) salen and ct DNA is an intercalative one. The interaction between plasmid DNA (pTZ57R DNA) and this complex is confirmed by gel electrophoresis studies. Furthermore, the interaction between HSA and Co(III) salen complex was investigated by UV absorption, fluorescence spectroscopy and molecular modeling. The binding constant for the interaction of this complex with HSA were found to be 3.854 × 104 M-1 using UV absorption, which was in good agreement with the binding constant obtained from fluorescence method (3.866 × 104 M-1). The binding distance between HSA and this complex was estimated to be 2.48 nm according to Förster theory of non-radioactive energy transfer. Molecular modeling studies suggested that hydrophobic interaction was the predominant intermolecular forces stabilizing Co(III) complex-HSA system.

Synthesis, Characterization and Antibacterial Activity of Novel 1,3-Diethyl-1,3-bis(4-nitrophenylurea and Its Metal(II Complexes

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Hoda Pasdar

2017-12-01

Full Text Available A bioactive ligand and its dinuclear metal(II complexes were synthesized and characterized by Fourier-transform infrared spectroscopy (FT-IR, ultraviolet-visible (UV-Visible, nuclear magnetic resonance (1H-NMR, mass spectroscopy and molar conductance measurements. The ligand has been crystalized in the monoclinic system with a P21/c space group. The biological activities of metal complexes were evaluated using disc diffusion and broth dilution methods. In vitro antibacterial activities of the ligand and their metal complexes were examined against two Gram-positive bacteria (Bacillus subtilis and Staphylococcus aureus and two Gram-negative bacteria (Escherichia coli and Serratia marcescens and compared to the standard drugs. It was found that metal complexes displayed much higher antibacterial activities and better inhibitory effects than that of the ligand and standard drugs. Among these complexes, the compound having Zn-metal showed greater antibacterial activity against all four tested bacteria and was more effective against Serratia marcescens with the zone inhibition diameter of 26 mm and MIC value of 31.25 µg/mL.

Synthesis, Characterization and Antibacterial Studies of N-(Benzothiazol-2-yl-4-chlorobenzenesulphonamide and Its Neodymium(III and Thallium(III Complexes

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Lawrence Nnamdi Obasi

2017-02-01

Full Text Available N-(Benzothiazol-2-yl-4-chlorobenzenesulphonamide (NBTCS was synthesized by condensation reaction of 4-chlorobenzenesulphonyl chloride and 2-aminobenzothiazole in acetone under reflux. Neodymium(III and thallium(III complexes of the ligand were also synthesized. Both ligand and metal complexes were characterized using UV-Vis, IR, 1H- and 13C-NMR spectroscopies, elemental analysis and molar conductance measurement. IR studies revealed that the ligand is tridentate and coordinates to the metal ions through nitrogen and oxygen atoms of the sulphonamide group and nitrogen atom attached to benzothiazole ring. The neodymium(III complex displays a coordination number of eight while thallium(III complex displays a coordination number of six. The ligand and its complexes were screened in vitro for their antibacterial activities against Escherichia coli strains (E. coli 6 and E. coli 13, Proteus species, Staphylococcus aureus and Pseudomonas aeruginosa using the agar well diffusion technique. The synthesized compounds were found to be more active against the microorganisms screened relative to ciprofloxacin, gentamicin and co-trimoxazole.

Synthesis and characterization of anisotropic magnetic hydrogels

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Hinrichs, Stephan, E-mail: stephan.hinrichs@chemie.uni-hamburg.de; Nun, Nils; Fischer, Birgit, E-mail: birgit.fischer@chemie.uni-hamburg.de

2017-06-01

Multiresponsive hydrogels are an interesting new class of materials. They offer the advantage, that they respond to different stimuli like temperature, pH and magnetic fields. By this they can change their properties which makes the hydrogels ideal candidates for many applications in the technical as well as medical field. Here we present the synthesis and characterization of hydrogels - micro- as well as macrogels - which consist of an iron oxide core, varying in phase and morphology, embedded in a thermoresponsive polymer, consisting of poly N-isopropylacrylamide. By using dynamic light scattering we investigated the thermoresponsive properties. In addition we were able to follow the formation of the macrogel by monitoring the shear viscosity.

Synthesis and characterization of μ-hydroxido- and μ-polycarboxylato-bridged iron(III complexes with 2,2’-bipyridine

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Tasić Nikola

2014-01-01

Full Text Available Four novel polymeric iron(III complexes with 2,2’-bipyridine (bipy and different aromatic polycarboxylato ligands as anions of phthalic (pht, isophthalic (ipht, terephthalic (tpht and pyromellitic (pyr acid were synthesized by ligand exchange reaction. The complexes were characterized by elemental and TG/DSC analysis, FTIR and diffuse reflectance UV-VIS-NIR spectroscopy and magnetic susceptibility measurements. Based on analytical and spectral data the formulae of the complexes are {[Fe4(bipy2 (H2O2(OH6(pht3]•2H2O}n (1, {[Fe4(bipy2(Hipht2(ipht2(OH6]•4H2O}n (2, {[Fe4(bipy2(Htpht2(OH6(tpht2]•4H2O}n (3 and {[Fe4(bipy(H2O8(OH4 (pyr2]•H2O}n (4. All complexes are red brown and low-spin with a distorted octahedral geometry and FeO6 or FeN2O4 chromophore. Polycarboxylato ligands have a bridging role in all cases, whereas monodentate COO groups are present in 2 and 3, bridging and chelate COO groups are established in 1 and 4. The thermal behaviour of 1-4 was investigated in detail and the molar dehydration enthalpies were calculated. According to the all those results, the structural formulae of the complexes 1-4 were proposed. [Projekat Ministarstva nauke Republike Srbije, br. III45007