Silver(I) complexes of N-methylbenzothiazole-2-thione: Synthesis, structures and antibacterial activity

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Aslanidis, P., E-mail: aslanidi@chem.auth.gr [Laboratory of Inorganic Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki (Greece); Hatzidimitriou, A.G.; Andreadou, E.G. [Laboratory of Inorganic Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki (Greece); Pantazaki, A.A., E-mail: natasa@chem.auth.gr [Laboratory of Biochemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki (Greece); Voulgarakis, N. [Department of Logistics, Alexander Technological Educational Institute, GR-60100 Katerini (Greece)

2015-05-01

Three silver(I) complexes containing N-methylbenzothiazole-2-thione (mbtt) have been prepared and structurally characterized by X-ray single-crystal analysis. Silver(I) nitrate, and silver(I) triflate react with mbtt to give homoleptic complexes of formula [(mbtt){sub 2}Ag(μ-mbtt){sub 2}Ag(mbtt){sub 2}](NO{sub 3}){sub 2} (1) and [Ag(mbtt){sub 3}](CF{sub 3}SO{sub 3}) (2) respectively, while silver(I) chloride gives the binuclear halide-bridged [(mbtt){sub 2}Ag(μ{sub 2}-Cl){sub 2}Ag(mbtt){sub 2}] (3). In the binuclear complex 1 the two metal ions, separated by 3.73 Å from each other, are doubly bridged by the exocyclic S-atoms of two mbtt ligands, with the tetrahedral environment around each silver ion being completed by the S-atoms of two terminally bonded mbtt units. Compound 2 is mononuclear with the metal ion surrounded by the exocyclic S-atoms of three mbtt ligands in a nearly ideal trigonal planar arrangement. The new complexes showed significant in vitro antibacterial activity against certain Gram-positive and Gram-negative bacterial strains.

Design, Synthesis, Fluorescence Properties and Antibacterial Activities of New 8-Chloro-3-Alkyl-3H-Pyrazolo[4,3-a]acridine-11-Carbonitriles

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Rahmani, Zeynab; Pordel, Mehdi; Davoodnia, Abolghasem [Islamic Azad Univ., Mashhad (Iran, Islamic Republic of)

2014-02-15

The treatment of alkylated nitro derivatives of indazole with 2-(4-chlorophenyl)acetonitrile under basic conditions gave the new 8-chloro-3-alkyl-3H-pyrazolo[4,3-a]acridine-11-carbonitriles via the nucleophilic substitution of hydrogen which proceeds at room temperature with concomitant cyclisation in fairly good yields. The structures of all newly synthesized compounds were confirmed by IR, {sup 1}H NMR, {sup 13}C NMR and mass spectral data. Fluorescence experimental results of all newly synthesized compounds revealed remarkable photoluminescence properties and strong green fluorescence properties. Also, the new compounds exhibited potent antibacterial activity and their antibacterial activity (MIC) against Gram positive (Staphylococcuse aureus methicillin resistant S. aureus and Bacillus subtilis) and negative bacterial (Pseudomonas aeruginosa and Escherichia coli) species were determined.

Modification of benzoxazole derivative by bromine-spectroscopic, antibacterial and reactivity study using experimental and theoretical procedures

Science.gov (United States)

Aswathy, V. V.; Alper-Hayta, Sabiha; Yalcin, Gözde; Mary, Y. Sheena; Panicker, C. Yohannan; Jojo, P. J.; Kaynak-Onurdag, Fatma; Armaković, Stevan; Armaković, Sanja J.; Yildiz, Ilkay; Van Alsenoy, C.

2017-08-01

N-[2-(2-bromophenyl)-1,3-benzoxazol-5-yl]-2-phenylacetamide (NBBPA) was synthesized in this study as an original compound in order to evaluate its antibacterial activity against representative Gram-negative and Gram-positive bacteria, with their drug-resistant clinical isolate. Microbiological results showed that this compound had moderate antibacterial activity. Study also encompassed detailed FT-IR, FT-Raman and NMR experimental and theoretical spectroscopic characterization and assignation of the ring breathing modes of the mono-, ortho- and tri-substituted phenyl rings is in agreement with the literature data. DFT calculations were also used to identify specific reactivity properties of NBBPA molecule based on the molecular orbital, charge distribution and electron density analysis, which indicated the reactive importance of carbonyl and NH2 groups, together with bromine atom. DFT calculations were also used for investigation of sensitivity of the NBBPA molecules towards the autoxidation mechanism, while molecular dynamics (MD) simulations were used to investigate the influence of water. The molecular docking results suggest that the compound might exhibit inhibitory activity against GyrB complex.

Electron transfer reactions in some complexes of V+2, Co+3 and Eu+3

International Nuclear Information System (INIS)

Lellis, F.T.P.

1983-01-01

The stability constants β 1 , β 2 , β 3 for the mono-,bis-and tris-substituted complexes from vanadium (III) ions with the pyridine-2-carboxilate liquid are determined potentiometrically. The tris-substituted complex in aqueous solutions by electronic spectra and reversible cyclic voltammetry using gold electrodes is extensively characterized. In the investigation of electron tranfer kinetics involving mild oxidizing complexes, such as Co(NH 3 ) 3+ 6 , Co(en) 3+ 3 , Co(en) 2 gly 2+ , Co (histidinate) + 2 , Ru(NH 3 ) 3+ 6 and Eu 3+ ions, the tris (picolinate) vanadate (III) complex is used. Electron transfer kinetics for the Eu 3+ / 2+ couple in terms of a pseudo-first order process is analysed. The results, in terms of a tunneling mechanism, involving a set of similar, nuclear coordinates for the reactants and products, are explained. (M.J.C.) [pt

Synthesis, characterization, structure and properties of heterobimetallic complexes [CuNi(μ-OAc) (μ-OH) (μ-OH2) (bpy)2] (BF4)2 and [CuNi(bz)3(bpy)2] ClO4 from 2,2‧ bipyridine

Science.gov (United States)

Kurbah, Sunshine D.; Kumar, A.; Syiemlieh, I.; Dey, A. K.; Lal, R. A.

2018-02-01

Heterobimetallic complexes of the composition [CuNi(bpy)2 (μ-OAc) (μ-OH) (μ-OH2)](BF4)2 (1) and [CuNi(bz)3 (bpy)2]ClO4 (2) were synthesized in moderate yield through solid state reaction and have been characterized by elemental analyses, molar conductance, mass spectra, magnetic moment, EPR, UV-Vis, IR spectroscopies and cyclic voltammetry. The ground state in complex (1) is doublet while that in complex (2), the ground state is a mixture of doublet and quartet, respectively. The structure of the complexes has been established by X-ray crystallography. The electron transfer reactions of the complexes have been investigated by cyclic voltammetry.

Aspartic protease inhibitory and nematocidal activity of phenyl-4-(2-phenylhydrazonohexahydrofuro[3,2-c]pyridazin-7-ol (Percival dianhydroosazone

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El Sayed H. El Ashry

2014-04-01

Full Text Available We synthesized Phenyl-4-(2-phenylhydrazonohexahydrofuro[3,2-c]pyridazin-7-ol (compound 3. The structure compound 3 was elucidated with IR, 1H NMR, 13C NMR and EIMS spectra. Compound 3 showed potent inhibitory activity against aspartic proteases, human cathepsin D and Plasmodium falciparum plasmepsin-II with IC50 = 20 μM. Enzyme-inhibitor complexes were predicted to stabilize by electrostatic and hydrophobic interactions between the side chains of amino acid residues at the active center and compound 3. Moreover, compound 3 displayed good nematocidal activity against all developmental stages of C. elegans.

A Comparative Study of the Inclusion Complexes of 2-[5'-benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole and 2-[5'-(p-N,N-dimethylamino- benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole withβ-Cyclodextrin

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S. Panda

2011-01-01

Full Text Available The compounds 2-[5'-benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole and 2-[5'-(p-N,N-dimethylamino- benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole have been synthesized in their purest forms starting from 2-aminobenzothiazole. The inclusion complexes of the above compounds have been prepared with β-cyclodextrin to increase their solubility and bioaccessibility in polar medium. The formation of inclusion complexes have been ascertained by study of spectral characteristic before and after inclusion complex formation. The stability of inclusion complexes and nature of interaction between the host and guest are known from the determination of thermodynamic parameters. Further the antibacterial and antifungal activities of the compounds are determined which is found to increase significantly after inclusion complex formation

Chemical functionalization of crystalline silicon surface with complexes of type (M3 (Dpa) 4X2) for the development of electronic devices

International Nuclear Information System (INIS)

Sanchez Zamora, Maria Alejandra

2012-01-01

New surfaces on crystalline silicon (100) diamines have been developed. The diamines 4-aminopyridine, 4-aminomethylpyridine and 1,12-dodecildiame, and self-assembled surfaces Si-diamine-metallic complexes, with cooper (II) acetate and trimetal Cu 3 (dpa) 4 CI 2 were studied. These surfaces are characterized with X-ray photoelectron spectroscopy (XPS), chemical force microscopy (CFM), by contact angle and cyclic voltammetry (CV). The XPS has suggested the formation of diamines monolayers with covalent binding to crystalline silicon, and modification of these surfaces, with metal complexes by coordination chemistry. The CFM has confirmed that surfaces are modified with diamines and cooper (II) acetate, and that were determined different chemical forces according to the change. The contact angle has been suggested that the functionalized surface with 4-aminomethylpyridine has had similar basicity to 1,12-dodecildiame, and more than 4-aminopyridine. This implies that the coordination with metallics complexes is benefited with 4-aminopyridine, which in turn is reflected with electrochemical data. Cyclic voltammetry analysis have showed that silicon surfaces with 4-aminomethylpyridine and 4-aminopyridine with cooper (II) acetate and trimetal have been electrochemically active. Thus, the surfaces could to have interesting applications in molecular electronics. (author) [es

Synthesis, Characterization, Crystal Structure and Antibacterial Activities of Transition Metal(II Complexes of the Schiff Base 2-[(4-Methylphenyliminomethyl]-6-methoxyphenol

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Guo-Liang Zhao

2009-05-01

Full Text Available Five transition metal(II complexes, [ML2Cl2] 1~5, were synthesized from the reaction of MCl2·nH2O (M = Mn, Co, Ni, Cu, Cd and the Schiff base ligand 2-[(4-methylphenyliminomethyl]-6-methoxyphenol (C15H15NO2, L, obtained by condensation of o-vanillin (2-hydroxy-3-methoxybenzaldehyde with p-toluidine. They were characterized by elemental analysis, molar conductance, FT-IR spectra, thermal analysis. The structure of complex 1 was determined by single-crystal X-ray diffraction. Its crystal structure is of monoclinic system, space group P21/c with a = 9.0111(18 Å, b = 11.222(2 Å, c =28.130 (6 Å, α = 90 º, β = 92.29(3 º, γ = 90 º, V = 2867.6(10 Å3, Z = 4. The Mn atom is six-coordinate and displays distorted octahedral geometry.The Schiff base ligand and its complexes have been tested in vitro to evaluate their antibacterial activity against bacteria, viz., Escherichia coli, Staphylococcus aureus and Bacillus subtilis. It has been found that the complexes have higher activity than the corresponding free Schiff base ligand against the same bacteria.

1-(2-Chlorobenzyloxy-3-[1,2,3]triazol-1-yl-propan-2-ol Derivatives: Synthesis, Characterization, and DFT-Based Descriptors Analysis

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Eloisa Román-Maldonado

2017-01-01

Full Text Available A novel series of 1-(2-chlorobenzyloxy-3-[1,2,3]triazol-1-yl-propan-2-ol derivatives was designed and synthesized using copper catalyzed alkyne-azide cycloaddition in the key step. Theoretical investigation of molecular and electronic properties by means of global and local reactivity indexes of the synthetized compounds was carried out, using DFT (Density Functional Theory at PBEPBE/6-31++G⁎⁎ level.

Influence of Exciplex formation on the electroluminescent properties of dimeric Zn (II) bis-2-(2'-hydroxyphenyl) benzoxazole complex and monomeric Zn (II) 2-(1'-hydroxynaphthyl) benzothiazole complex

Science.gov (United States)

Prakash, Sattey; Anand, R. S.; Manoharan, S. Sundar

2011-10-01

In this paper we present the factors affecting electroluminescent properties of Zinc complexes of oxazole & thiazole derivatives. Electroluminescent spectra of the Zinc (II) complex of bis-[2-(2'-hydroxyphenyl) benzoxazole], [Zn (HPBO)2]2 and 2-(1'-hydroxynaphthyl) benzothiazole [Zn (HNBT)2] show unusual broadening and shows structural and photophysical similarity with [Zn (HPBT)2]2, a dimeric complex. The [Zn (HPBO)2]2 complex as an emissive layer in the device structure ITO /PEDOT:PSS /TPD (30nm) /[Zn (HPBO)2]2 (60nm) /BCP (6nm) /Ca (3nm) /Al (200nm) shows a broad bluish green emission, with a full width at half maxima (FWHM1˜70nm). The EL spectra is much broader compared to the PL spectra because of exciplex formation at the interfacial region between the emissive layer (EML) & hole transport layer (HTL). We also show the device performance of Zinc 2-(1'-hydroxynaphthyl) benzothiazole [Zn (HNBT)2] complex as emissive layer. Distinctly this device shows a broad greenish yellow emission with a peak maxima at 535nm and 690nm, owing to the exciplex formation between electron transport layer (ETL) and emissive layer (EML), which is in sharp contrast to the exciplex formation across the HTL-EML interface observed for the [Zn (HPBO)2]2 complex.

99mTc complexes of benzimidazole and benzoxazole ligands and their biodistribution studies

International Nuclear Information System (INIS)

Kothari, K.; Manju, S.; Pillai, M.R.A.; Rath, N.; Dash, K.C.; Sarma, H.D.

1997-01-01

Complexation studies of 2 (2' -hydroxyphenyl)benzimidazole (HPBI) and 2(2' -pyridyl)benzoxazole (PBO) with 99m Tc were carried out. The complexes were characterised by TLC, paper electrophoresis and solvent extraction. The ligand HPBI forms complex in high yield (>90%). Biodistribution studies carried out with 99m Tc-HPBI complex in Swiss Albino mice showed rapid clearance of the complex from blood and excretion of the activity through hepatobiliary system. (author). 2 refs., 1 fig., 3 tabs

Screening the DNA interaction ability and antimicrobial activity of a few novel bioactive complexes tethering N-((2-aminophenyl)(phenyl)methylene)-4-nitroaniline

Energy Technology Data Exchange (ETDEWEB)

Muniyandi, Vellaichamy; Raman, Natarajan, E-mail: ramchem1964@gmail.com

2016-11-01

Few novel transition metal complexes having N-((2-aminophenyl)(phenyl)methylene)-4-nitroaniline were synthesized and characterized by elemental analyses, IR, {sup 1}H and {sup 13}C NMR, electronic, EPR and mass spectra, conductivity and magnetic susceptibility measurements. All the metal complexes adopted square planar geometrical arrangements. The DNA-binding properties of the metal(II) complexes have been investigated by electronic absorption, fluorescence, CD spectra, cyclic voltammetry, differential pulse voltammogram and viscosity measurements. The results obtained indicate that these complexes bind to DNA via an intercalation binding mode. DNA cleavage activities indicate that the metal complexes exhibit greater activity than the ligand. The antimicrobial screening reveals that all the metal complexes exhibit better activity than the free ligand. - Highlights: • The newly synthesized mixed-ligand metal complexes act as persistent intercalators. • These mixed-ligand metal complexes display better chemical nuclease activity. • They exhibit potential antimicrobial activity. • Novel DNA targeting metal complexes are synthesized.

Synthesis and antibacterial activity of some derivatives of 1,3,4-thia-dia-zol[3,2-a]pyrimidine

International Nuclear Information System (INIS)

Sangov, Z.G.

2004-01-01

The purpose of this work is direct synthesis of derivatives of 1,3,4-thia-dia-zol[3,2-a]pyrimidine containing functional groups in second and sixth position of cycle, studying antibacterial activity obtained compounds on culture fungus, typical for this region and searching for new high-effective biologically active matters with low toxicity which let wide assortment of medicinal preparations

Cyclic voltammetric study of the reduction of U(III) to uranium metal in molten LiCl-NaCl-CaCl2-BaCl2-UCl3

International Nuclear Information System (INIS)

Poa, D.S.; Tomczuk, Z.; Steunenberg, R.K.

1986-01-01

Cyclic voltammetry was used to investigate the electrochemistry of the reduction of UCl 3 to uranium metal in molten LiCl-NaCl-CaCl 2 -BaCl 2 (49.7-8.0-26.5-15.8 mol %) containing dissolved UCl 3 . The purpose of the study was to obtain information on the kinetics of the reaction, which will be used in the design of electrorefining equipment for the reprocessing of core and blanket fuel discharged from the Integral Fast Reactor (IFR). The electrorefining operation employs the above salt as the electrolyte and a liquid cadmium pool as the anode

Transition metal complexes of 5-bromosalicylidene-4-amino-3-mercapto-1,2,4-triazine-5-one: Synthesis, characterization, catalytic and antibacterial studies

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AYALOOR SUBRAMANIAN RAMASUBRAMANIAN

2011-01-01

Full Text Available Transition metal complexes of 5-bromosalicylidene-4-amino-3-mercapto-1,2,4-triazine-5-one with metal precursors, such as Cu(II, Ni(II, Co(II and Pd(II, were synthesized and characterized by physico–chemical and spectroscopic techniques. All the complexes are of the ML type. Based on analytical, spectral data and magnetic moments, the Co(II and Ni(II complexes were assigned octahedral geometries, while the Cu (II and Pd(II complexes square planar. A study on the catalytic oxidation of benzyl alcohol, cyclohexanol, cinnamyl alcohol, 2-propanol and 2-methyl-1-propanol was performed with N-methylmorpholine-N-oxide (NMO as co-oxidant. All the complexes and their parent organic moiety were screened for their biological activity on several pathogenic bacteria and were found to possess appreciable bactericidal properties.

Synthesis, structure characterization and biological studies on a new aromatic hydrazone, 5-(2-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)hydrazono)-2,2-dimethyl-1,3-dioxane-4,6-dione, and its transition metal complexes

Science.gov (United States)

Kumar, Shubha S.; Biju, S.; Sadasivan, V.

2018-03-01

A new aromatic hydrazone 5-(2-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)hydrazono)-2,2-dimethyl-1,3-dioxane-4,6-dione has been synthesized by Japp-Klingemann reaction from diazotized 4-aminoantipyrine and Meldrum's acid. A few 3d-metal ion complexes of this hydrazone were synthesized. The compound and its complexes were characterized by UV-Visible, 1H NMR, ESR, Mass spectral, molar conductance and magnetic susceptibility measurements. The compound was found to exist in hydrazone form in solid state and solution from SXRD and 1H NMR study. The influence of pH on the molecule was studied and found that it shows azo/enol-hydrazone tautomerism in solution. This molecule act as a univalent tridentate ligand and the complexes were assigned to have a 1:2 stoichiometry (M:L). The antioxidant properties of the compounds were explored by DPPH assay and found that the ligand possesses better free radical scavenging effect than the complexes. Antimicrobial activities of these compounds were investigated and were found to be active.

Diazadienes in chemistry of lanthanides: latest view on old ligands. Synthesis, structure and properties of complexes {[(R)CNC6H3Pr2i]2}Lu(THF)2(μ-Cl)2Li(THF2 (R=CH3, CH2)

International Nuclear Information System (INIS)

Makhrova, T.V.; Fukin, G.K.; Cherkasov, A.V.; Trifonov, A.A.

2008-01-01

Reaction of dianion derivative [DADLi 2 ] (DAD -1,4-bis(2,6-diisopropylphenyl)-2,3-dimethyl-1,4-diaza-1,3-butadiene) prepared in situ by the reduction of corresponding DAD by the excess of metal lithium in THF with anhydrous LuCl 3 (1:1) results in the formation of the metal cyclic complex {[(R)CNC 6 H 3 Pr 2 i ] 2 }Lu(THF) 2 (μ-Cl) 2 Li(THF) 2 (1) containing the fragment N-C(Me)=C(Me)-N. DAD Treatment by two equivalents BuLi in the mixture ether-hexane (20 Deg C) results in the activation of the C-H bond of methyl substitutes at imine carbon. By the reaction of dilithium derivative [DAD - 2 H Li 2 ] formed in situ with LuCl 3 in THF the complex {[(CH 2 )CNC 6 H 3 Pr 2 i ] 2 }Lu(THF) 2 (μ-Cl) 2 Li(THF) 2 (2) with diamide ligand N-C(=CH 2 )-C(=CH 2 )-N was prepared. Structures of 1 and 2 complexes have been established by X-ray structure analysis [ru

Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes

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Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M. Arif

2016-05-01

We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica.

Antibacterial evaluation of some Schiff bases derived from 2-acetylpyridine and their metal complexes.

Science.gov (United States)

Gwaram, Nura Suleiman; Ali, Hapipah Mohd; Khaledi, Hamid; Abdulla, Mahmood Ameen; Hadi, A Hamid A; Lin, Thong Kwai; Ching, Chai Lay; Ooi, Cher Lin

2012-05-18

A series of Schiff bases derived from 2-acetylpyridne and their metal complexes were characterized by elemental analysis, NMR, FT-IR and UV-Vis spectral studies. The complexes were screened for anti-bacterial activity against Methicillin-resistant Staphylococcus aureus (MRSA), Acinetobacter baumanni (AC), Klebsiella pneumonie (KB) and Pseudomonas aeruginosa (PA) using the disc diffusion and micro broth dilution assays. Based on the overall results, the complexes showed the highest activities against MRSA while a weak antibacterial activity was observed against A. baumanii and P. aeruginosa.

Diastereoisomers of 2-benzyl-2, 3-dihydro-2-(1H-inden-2-yl)-1H-inden-1-ol: potential anti-inflammatory agents.

Science.gov (United States)

Sheridan, Helen; Walsh, John J; Cogan, Carina; Jordan, Michael; McCabe, Tom; Passante, Egle; Frankish, Neil H

2009-10-15

The synthesis and biological activity of the novel diastereoisomers of 2-benzyl-2,3-dihydro-2-(1H-inden-2-yl)-1H-inden-1-ol is reported. The 2,2-coupled indane dimers were synthesised by coupling of the silyl enol ether of 1-indanone with the dimethyl ketal of 2-indanone. The coupled product was directly alkylated to give the racemic ketone which was reduced to the diastereoisomeric alcohols. The alcohols were separated and their relative stereochemistry was established by X-ray crystallography. These molecules demonstrate significant anti-inflammatory activity in vivo and in vitro and may represent a new class of anti-inflammatory agent.

Synthesis, screening and QSAR studies of 3-benzoyl-2-oxo/thioxo-1,2,3,4-tetrahydro-pyrimidine analogues as antibacterial agents

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Ramesh L. Sawant

2008-12-01

Full Text Available The purpose of this study was to synthesize several 3-benzoyl-5-acyl-6-methyl-4-substituted-2-oxo/thioxo-1,2,3,4-tetrahydropyrimidines, evaluate them for their antibacterial activity and to establish correlation between the activity and physicochemical properties. 5-Acyl-6-methyl-4-substituted-2-oxo/thioxo-1,2,3,4-tetrahydropyrimidines (A were synthesized by cyclocondensation reaction between appropriate aldehyde, acetoacetate and urea/thiourea in presence of aluminium chloride and hydrochloric acid which upon treatment with benzoyl chloride in presence of pyridine in benzene furnish the title compounds (1-28. The structures of all title compounds have been confirmed on the basis of their analytical, IR and NMR spectral data. The title compounds have been tested for antibacterial activity against Staphylococcus aureus. The compounds were divided into training and test sets. A quantitative structure activity relationship study was made using various descriptors. Several statistical expressions were developed using stepwise multiple linear regression analysis. The best quantitative structure activity relationship model was further cross validated. The study revealed that total positive partial charge (PC+ and total polar negative Van der Waals surface area (Q_VSA_PNEG contributes negatively where as contribution of Van der Waals surface area to molar refractivity (SMR_VSA7 contributes positively to the antibacterial activity. The compounds with improved antibacterial potential can be successfully designed with selected quantitative structure activity relationship model.

Synthesis, thermodynamic properties and antibacterial activities of lanthanide complexes with 3,5-dimethoxybenzoic acid and 1,10-phenanthroline

Energy Technology Data Exchange (ETDEWEB)

Zheng, Jun-Ru [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Ren, Shu-Xia [Material Science and Engineering School, Shijiazhuang Tiedao University, Shijiazhaung 050043 (China); Ren, Ning [Department of Chemistry, Handan College, Handan 056005 (China); Zhang, Jian-Jun, E-mail: jjzhang6@126.com [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Zhang, Da-Hai [Department of Chemistry, Handan College, Handan 056005 (China); Wang, Shu-Ping [College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China)

2013-11-20

Graphical abstract: Four novel complexes ([Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} (Ln = Tb(1), Dy(2), Er(3), Yb(4); 3,5-DmeoxBA = 3,5-dimethoxybenzoic acid; phen = 1,10-phenanthroline))were synthesized and characterized by elemental analysis, IR and TG/DSC-FTIR technology. Heat capacities of the four complexes were measured by differential scanning calorimetry (DSC). The antibacterial action of the four complexes on bacteria and fungus such as Escherichia coli, Staphylococcus aureus and Candida albicans were studied by filter paper approach. - Highlights: • Four novel complexes ([Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} were synthesized and characterized. • The thermal decomposition processes of the title complexes were studied using the TG/DSC–FTIR coupling techniques. • The heat capacities of the complexes were measured by (DSC). • The antibacterial action of the four complexes on Escherichia coli, Staphylococcus aureus and Candida albicans were studied. - Abstract: Four lanthanide complexes with a general formula [Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} (Ln = Tb(1), Dy(2), Er(3), Yb(4); 3,5-DmeoxBA = 3,5-dimethoxybenzoic acid; phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, infrared spectra (IR), and thermogravimetric, differential scanning calorimetry techniques, combined with Fourier transform infrared (TG/DSC–FTIR) technology. The thermal decomposition processes of the four complexes were investigated by TG/DSC–FTIR techniques. Heat capacities were measured by DSC. The values of the experimental heat capacities were fitted to a polynomial equation with the least-squares method. Based on the fitted polynomial, the smoothed heat capacities and thermodynamic functions (H{sub T} − H{sub 298.15} {sub K}), (S{sub T} − S{sub 298.15} {sub K}), and (G{sub T} − G{sub 298.15} {sub K}) were calculated. The antibacterial action of the four complexes on bacteria and fungus such as Escherichia coli, Staphylococcus aureus and

Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes.

Science.gov (United States)

Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M Arif

2016-05-15

We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica. Copyright © 2016 Elsevier B.V. All rights reserved.

Metal Fe3+ ions assisted synthesis of highly monodisperse Ag/SiO2 nanohybrids and their antibacterial activity

International Nuclear Information System (INIS)

Zhang, Nianchun; Xue, Feng; Yu, Xiang; Zhou, Huihua; Ding, Enyong

2013-01-01

Graphical abstract: TEM images of the Ag/SiO 2 -2 nanohybrids. The homogeneous and more mono-disperse Ag nanoparticles deposit on SiO 2 spheres. Through this method, Ag nanoparticles are easily formed on the surface of SiO 2 compared to other methods. Highlights: ► We prepared homogeneous and mono-dispersed Ag/SiO 2 -2 nanohybrids by adding Fe 3+ ions. ► The Ag/SiO 2 -2 nanohybrids had core(SiO 2 )-shell(Ag) structure. ► The Ag/SiO 2 -2 nanohybrids exhibited excellent antibacterial activity against bacteria. ► The reaction temperature was lower and the yield of Ag/SiO 2 -2 nanohybrids were higher. - Abstract: Highly monodispersed Ag/SiO 2 nanohybrids with excellent antibacterial property were synthesized by using DMF as a reducing agent and employing an additional redox potential of metal Fe 3+ ion as a catalytic agent. The obtained Ag/SiO 2 -2 nanohybrids of about 240 nm were highly monodispersity and uniformity by adding trace Fe 3+ ions into the reaction which Ag + reacted with N,N-dimethyl formamide (DMF) at 70 °C. Compared to the conventional techniques, which need long time and high temperature for silica coating of Ag nanoparticles, this new method was capable of synthesizing monodispersed, uniform, high yield Ag/SiO 2 nanohybrids. The electron was transferred from the Fe 2+ ion to the Ag + ion to accelerate the nucleation of silver nanoparticles. The chemical structures, morphologies and properties of the Ag/SiO 2 nanohybrids were characterized by X-ray diffraction (XRD), (High-resolution, Scanning transmission) transmission electron microscopy (TEM, HRTEM and STEM), and X-ray photoelectron spectroscopy (XPS), and UV–vis spectroscopy (UV–vis) and test of antibacterial. The results demonstrated that the silver nanoparticles supported on the surface of SiO 2 spheres in Ag/SiO 2 -2 nanohybrids structure, the Ag nanoparticles were homogeneous and monodispersed. The results also indicated that the Ag/SiO 2 -2 nanohybrid had excellent antibacterial.

Synthesis, antioxidant and antibacterial activities of 3-nitrophenyl ferrocene

Science.gov (United States)

Benabdesselam, S.; Izza, H.; Lanez, T.; Guechi, E. K.

2018-03-01

The current work aims in its first part to synthesize 3-nitrophenylferrocene after diazotizing nitroaniline in the meta position by the sodium nitrite and the formation of the corresponding diazonium salt: 3-nitrobenzendiazonium sulfate, then the salt in solution was added to the ferrocene for the purpose of introducing the nitrophenyl moiety thereon (arylation) and the formation of 3-nitrophenylferrocene. The second part is devoted to the study of the antioxidant activity of 3-NPF by applying the trapping test of superoxide radical using cyclic voltammetry, the free radical DPPH trapping test by spectrophotometry. The results showed that 3-nitrophenylferrocene has a scavenging effect of DPPH radical with IC50 = 1.44mg/ml, superoxide radical with IC50=5.38mg/ml. The third part is devoted to the study of antibacterial activity of the synthesized compound tested on four strains of bacteria: Escherichia coli, Pseudomonas aeruginosa, Enterococcus faecalis and Klebsiella pneumoniae. The obtained results clearly showed that 3-nitrophenylferrocene has low activities on the four bacterial strains with diameters of inhibition zones do not exceeding 17 mm at concentrations of 25mg/ml.

Synthesis, urease inhibition, antioxidant and antibacterial studies of some 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones and their 3,6-disubstituted 1,2,4-triazolo[3,4-b]1,3,4-thiadiazole derivatives

International Nuclear Information System (INIS)

Hanif, Muhammad; Saleem, Muhammad; Rama, Nasim Hasan; Hussain, Muhammad Tahir; Zaib, Sumera; Aslam, Muhammad Adil M.; Iqbal, Jamshed; Jones, Peter G.

2012-01-01

A new series of 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones, bearing various methoxybenzyl- and methoxyphenethyl groups, was synthesized by refluxing potassium hydrazinecarbodithioate salts in dilute aqueous solution of hydrazine hydrate. These salts were formed by the reaction of acid hydrazides and carbon disulfide in methanolic potassium hydroxide solution at 0-5 deg C. 4-Amino- 5-aryl-3H-1,2,4-triazole-3-thiones were condensed with different substituted aromatic acids to yield 3,6-disubstituted-1,2,4-triazolo[3,4-b]1,3,4-thiadiazoles. The structures of the synthesized compounds were characterized by infrared (IR), 1 H and 13 C nuclear magnetic resonance (NMR), elemental analysis and mass spectrometric (MS) studies. All the synthesized compounds were screened for their urease inhibition, antioxidant and antibacterial activities. Some compounds showed excellent urease inhibition activity, more than the standard drug. Others exhibited potent antioxidant activity. All the compounds showed significant antibacterial activities as compared to the standard drug. (author)

Antibacterial Evaluation of Some Schiff Bases Derived from 2-Acetylpyridine and Their Metal Complexes

Directory of Open Access Journals (Sweden)

Thong Kwai Lin

2012-05-01

Full Text Available A series of Schiff bases derived from 2-acetylpyridne and their metal complexes were characterized by elemental analysis, NMR, FT-IR and UV-Vis spectral studies. The complexes were screened for anti-bacterial activity against Methicillin-resistant Staphylococcus aureus (MRSA, Acinetobacter baumanni (AC, Klebsiella pneumonie (KB and Pseudomonas aeruginosa (PA using the disc diffusion and micro broth dilution assays. Based on the overall results, the complexes showed the highest activities against MRSA while a weak antibacterial activity was observed against A. baumanii and P. aeruginosa.

Indolo[3,2-c]cinnolines with antiproliferative, antifungal, and antibacterial activity.

Science.gov (United States)

Barraja, P; Diana, P; Lauria, A; Passannanti, A; Almerico, A M; Minnei, C; Longu, S; Congiu, D; Musiu, C; La Colla, P

1999-08-01

A series of indolo[3,2-c]cinnoline derivatives was prepared and tested to evaluate their biological activity. Most of them inhibited the proliferation of leukemia, lymphoma and solid tumor-derived cell lines at micromolar concentrations, whereas none of the compounds were active against HIV-1. With the exception of 7g, all title compounds showed antibacterial activity against gram-positive bacteria, being up to 200 times more potent than the reference drug streptomycin. Some of the indolo[3,2-c]cinnolines were also endowed with good antifungal activity, particularly against Criptococcus neoformans.

A Recyclable Palladium-Catalyzed Synthesis of 2-Methylene-2,3-Dihydrobenzofuran-3-ols by Cycloisomerization of 2-(1-Hydroxyprop-2-ynylphenols in Ionic Liquids

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Bartolo Gabriele

2013-09-01

Full Text Available A recyclable palladium-catalyzed synthesis of 2-methylene-2,3-dihydrobenzofuran-3-ols 2 by heterocyclization of 2-(1-hydroxyprop-2-ynylphenols 1 in an ionic liquid medium (BmimBF4 is presented. The process takes place under relatively mild conditions (100 °C, 5 h in the presence of catalytic amounts (2 mol % of PdI2 in conjunction with KI (5 equiv with respect to PdI2 and an organic base, such as morpholine (1 equiv with respect to 1, to give 2 in high yields (70%–86%. The PdI2-KI catalytic system could be recycled up to six times without appreciable loss of activity. Moreover, products 2 could be easily converted in a one-pot fashion into 2-hydroxymethylbenzofurans 3 (52%–71%, based on 1 and 2-methoxymethylbenzofurans 4 (52%–80%, based on 1 by acid-catalyzed allylic isomerization or allylic nucleophilic substitution.

Rhodium, iridium and nickel complexes with a 1,3,5-triphenylbenzene tris-MIC ligand. Study of the electronic properties and catalytic activities

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Carmen Mejuto

2015-12-01

Full Text Available The coordination versatility of a 1,3,5-triphenylbenzene-tris-mesoionic carbene ligand is illustrated by the preparation of complexes with three different metals: rhodium, iridium and nickel. The rhodium and iridium complexes contained the [MCl(COD] fragments, while the nickel compound contained [NiCpCl]. The preparation of the tris-MIC (MIC = mesoionic carbene complex with three [IrCl(CO2] fragments, allowed the estimation of the Tolman electronic parameter (TEP for the ligand, which was compared with the TEP value for a related 1,3,5-triphenylbenzene-tris-NHC ligand. The electronic properties of the tris-MIC ligand were studied by cyclic voltammetry measurements. In all cases, the tris-MIC ligand showed a stronger electron-donating character than the corresponding NHC-based ligands. The catalytic activity of the tri-rhodium complex was tested in the addition reaction of arylboronic acids to α,β-unsaturated ketones.

Highly Fluorescent Group 13 Metal Complexes with Cyclic, Aromatic Hydroxamic Acid Ligands

Energy Technology Data Exchange (ETDEWEB)

Seitz, Michael; Moore, Evan G.; Raymond, Kenneth N.

2008-02-11

The neutral complexes of two ligands based on the 1-oxo-2-hydroxy-isoquinoline (1,2-HOIQO) motif with group 13 metals (Al, Ga, In) show bright blue-violet luminescence in organic solvents. The corresponding transition can be attributed to ligand-centered singlet emission, characterized by a small Stokes shifts of only a few nm combined with lifetimes in the range between 1-3 ns. The fluorescence efficiency is high, with quantum yields of up to 37% in benzene solution. The crystal structure of one of the indium(III) complexes (trigonal space group R-3, a = b = 13.0384(15) {angstrom}, c = 32.870(8) {angstrom}, ? = {beta} = 90{sup o}, {gamma} = 120{sup o}, V = 4839.3(14) {angstrom}{sup 3}, Z = 6) shows a six-coordinate geometry around the indium center which is close to trigonal-prismatic, with a twist angle between the two trigonal faces of 20.7{sup o}. Time-dependent density functional theory (TD-DFT) calculations (Al and Ga: B3LYP/6-31G(d)); In: B3LYP/LANL2DZ of the fac and mer isomers with one of the two ligands indicate that there is no clear preference for either one of the isomeric forms of the metal complexes. In addition, the metal centers do not have a significant influence on the electronic structure, and as a consequence, on the predominant intraligand optical transitions.

Synthesis, photophysical property study of novel fluorescent 4-(1,3 ...

Indian Academy of Sciences (India)

Some of the benzoxazole derivatives exhibit diverse ... NSC-693638 and antibacterial agents;13 some exam- ples are UK-1, ..... 1H NMR (D2O Exchange of Comp .... test material in 10% (v/v) DMSO (usually a stock con- .... Refractive index of solvent for standard .... synthesis B M Trost, and I Flemming (eds) New York:.

Synthesis, characterization, electrochemical investigation and antioxidant activities of a new hybrid cyclohexaphosphate: Cu1.5Li(C2H10N2)P6O18·7H2O

Science.gov (United States)

Sleymi, Samira; Lahbib, Karima; Rahmouni, Nihed; Rzaigui, Mohamed; Besbes-Hentati, Salma; Abid, Sonia

2017-09-01

A new organic-inorganic hybrid transition metal phosphate, Cu1.5Li(C2H10N2)P6O18·7H2O, has been prepared and characterized by X-ray diffraction, spectroscopy (infrared, Raman, diffuse reflectance and UV-Vis) and thermal analysis (TG). In addition, its electrochemical behaviors, as well as its antioxidant and antibacterial activities, have been investigated. Its structure is built up by the alternate linkages between copper and phosphate polyhedra, forming puckered layers with intersecting 12-membered rings, in which the ethylenediammonium cations reside. This compound is the first framework structure constructed from cyclohexaphosphates and three distinct copper cations. Cyclic voltammetry study in an acetonitrile solution reveals the facile anodic oxidation of its organic part on a platinum disk and a progressive growing of a thin film, though the repetitive cycling of potential. The title compound was tested for its in vitro antioxidant activities by 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2‧-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), Ferrous chelating ability (FIC) and Ferric Reducing Power (FRP) methods. The antioxidant activity of Cu1.5Li(C2H10N2)P6O18·7H2O was analyzed simultaneously with its antibacterial capacity against Escherichia coli, Salmonella typhimurium, Staphylococus aureus, Enterococcus feacium, Streptococcus agalactiae and Candida albicans. The tested compound showed significant antioxidant activities with low antibacterial properties.

Spectroscopic studies and antibacterial activities of some new 16-membered octaazamacrocyclic complexes derived from thiocarbohydrazide and pentane-2,4-dione

Science.gov (United States)

Singh, D. P.; Kumar, Krishan; Chopra, Rimpi Mehani ne'e.

2011-02-01

A series of macrocyclic complexes of the type [M(C 12H 20N 8S 2)X 2]; where M = Co(II), Ni(II), Cu(II), Zn(II); X = Cl -, NO 3-, CH 3COO - has been synthesized by template condensation of thiocarbohydrazide and pentane-2,4-dione in the presence of divalent metal salts in methanolic medium. The complexes have been characterized with the help of elemental analyses, conductance measurements, magnetic measurements, electronic, NMR, IR, EPR and MS spectral studies. The low value of molar conductance indicates them to be non-electrolytes. On the basis of various studies a distorted octahedral geometry may be proposed for all of these complexes. These metal complexes were also tested for their in vitro antibacterial activities against some Gram-positive bacterial strains, i.e., Bacillus subtilis, Bacillus stearothermophilus and two Gram-negative bacterial strains, i.e., Escherichia coli, Pseudomonas putida. The results obtained were compared with standard antibiotics, Chloramphenicol and Streptomycin and found that some of the synthesized complexes show good antibacterial activities as compared to the standard antibiotics.

Synthesis and Antibacterial Activity of 1,3,4-Oxadiazole and 1,2,4 ...

African Journals Online (AJOL)

NJD

The antibacterial activities of the starting materials, the synthetic intermediates and the products were tested and are reported below. 2. Results and Discussion. 2.1. Synthesis. The final products 4, 6, 8 and 9 have been synthesized by a common pathway as summarized in Scheme 1. The methyl salicylate 2 was synthesized ...

Synthesis and biological characterization of (3R,4R)-4-(2-(benzhydryloxy)ethyl)-1-((R)-2-hydroxy-2-phenylethyl)-piperidin-3-ol and its stereoisomers for monoamine transporters

Science.gov (United States)

Kharkar, Prashant S.; Batman, Angela M.; Zhen, Juan; Beardsley, Patrick M.; Reith, Maarten E. A.

2012-01-01

In this report we describe synthesis and biological evaluation of a series of asymmetric 4-(2-(benzhydryloxy)ethyl)-1-((R)-2-hydroxy-2-phenylethyl)-piperidin-3-ol based dihydroxy compounds where the hydroxy groups are located both on the piperidine ring and also on the N-phenylethyl side chain exo-cyclically. In vitro uptake inhibition data indicates high affinity of these molecules for the dopamine transporter (DAT) in addition to their moderate to high affinity for the norepinephrine transporter (NET). Interestingly, compounds 9b and 9d exhibited affinities for all three monoamine transporters with highest potency at DAT and NET and moderate potency at the serotonin transporter (SERT) (Ki 2.29, 78.4 and 155 nM for 9b and 1.55, 14.1 and 259 nM for 9d, respectively). Selected compounds, 9a, 9d and 9d’ were tested for their locomotor activity effects in mice, and for their ability to occasion the cocaine discriminative stimulus in rats. These test compounds generally exhibited a much longer duration of action than cocaine for elevating locomotor activity, and dose-dependently completely generalized the cocaine discriminative stimulus. PMID:19449323

Speed of sound in saturated aliphatic alcohols (propan-2-ol, butan-2-ol, and 2-methylpropan-1-ol) and alkanediols (ethane-1,2-diol, propane-1,2- and -1,3-diol) at temperature between 253.15 K and 353.15 K and pressures up to 30 MPa

International Nuclear Information System (INIS)

Dávila, María J.; Gedanitz, Holger; Span, Roland

2016-01-01

Highlights: • Speed of sound measurements were made in aliphatic alcohols and alkanediols. • Speeds of sound were measured in a wide temperature and pressure range. • A pulse-echo method with a double path type sensor operating at 8 MHz was employed. • A double polynomial equation was used to fit the experimental speed of sound data. • The accurate results were compared with available literature sources. - Abstract: Speeds of sound have been measured in three saturated aliphatic alcohols (propan-2-ol, butan-2-ol, and 2-methylpropan-1-ol) and three alkanediols (ethane-1,2-diol, propane-1,2- and -1,3-diol) in the temperature range from (253.15 to 353.15) K and pressures up to 30 MPa by use of a pulse-echo method with a double path type sensor operating at 8 MHz. The expanded overall uncertainties (k = 2) in the speed of sound measurements are estimated to be 0.013% for propan-2-ol, 0.019% for butan-2-ol, 0.01% for 2-methylpropan-1-ol, 0.009% for ethane-1,2-diol, 0.02% for propane-1,2-diol, and 0.07% for propane-1,3-diol. Experimental speeds of sound data were correlated with the temperature and pressure with an empirical double polynomial equation. Our results were also compared with the available literature data and a satisfactory agreement was found.

Synthesis and Biological Activities on Metal Complexes of 2,5-Diamino-1,3,4-thiadiazole Derived from Semicarbazide Hydrochloride

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Matthew A. Adebayo

2011-07-01

Full Text Available A bioactive ligand, 2,5-diamino-1,3,4-thiadiazole (L, derived from semicarbazide hydrochloride, and its metal complexes were prepared and characterized. The complexes were characterized using elemental, infra-red, ultraviolet/visible, magnetic moment, atomic absorption, thin layer chromatography and molar conductance measurements. The IR data revealed that the ligand (L behaved as a tridentate neutral ligand. It coordinated to the metal ion via sulphur and nitrogen of the amines. The molar conductance data reveal that the chelates are non-electrolytes. From the Ultraviolet/Visible spectra and magnetic moment data, the complexes were found to have octahedral geometrical structure. In vivo evaluation of the antimicrobial activities of the metal complexes and the ligands showed greater activity against some micro-organisms when compared to the parent compounds. The chelates do not show toxicity against the activities of enzymes from homogenates of liver, kidney and serum in experimental rats.

Synthesis and properties of complexes of 1-phenyl-2,3-dimetylpyrazolone-5-thione with metals

International Nuclear Information System (INIS)

Bikkulova, A.T.; Kapina, A.P.; Medvedeva, E.A.

1985-01-01

Cadmium complexes with thiopyrine (1-phenyl-2.3-dimethylpyrazolone-5-thione) (R) of the composition CdR 2 X 2 are obtained by precipitation from hydrochloric acid solutions at pH=1 and at chloride and bromide (X) excess. The formation of coordination bond of a metal through the sulphur atom is established by the IR- and NMR-spectroscopy methods. Fungicidal activity of the compositions obtained is detected

Formation of ternary CaUO2(CO3)3(2-) and Ca2UO2(CO3)3(aq) complexes under neutral to weakly alkaline conditions.

Science.gov (United States)

Lee, Jun-Yeop; Yun, Jong-Il

2013-07-21

The chemical behavior of ternary Ca-UO2-CO3 complexes was investigated by using time-resolved laser fluorescence spectroscopy (TRLFS) in combination with EDTA complexation at pH 7-9. A novel TRLFS revealed two distinct fluorescence lifetimes of 12.7 ± 0.2 ns and 29.2 ± 0.4 ns for uranyl complexes which were formed increasingly dependent upon the calcium ion concentration, even though nearly indistinguishable fluorescence peak shapes and positions were measured for both Ca-UO2-CO3 complexes. For identifying the stoichiometric number of complexed calcium ions, slope analysis in terms of relative fluorescence intensity versus calcium concentration was employed in a combination with the complexation reaction of CaEDTA(2-) by adding EDTA. The formation of CaUO2(CO3)3(2-) and Ca2UO2(CO3)3(aq) was identified under given conditions and their formation constants were determined at I = 0.1 M Na/HClO4 medium, and extrapolated to infinitely dilute solution using specific ion interaction theory (SIT). As a result, the formation constants for CaUO2(CO3)3(2-) and Ca2UO2(CO3)3(aq) were found to be log β113(0) = 27.27 ± 0.14 and log β213(0) = 29.81 ± 0.19, respectively, providing that the ternary Ca-UO2-CO3 complexes were predominant uranium(vi) species at neutral to weakly alkaline pH in the presence of Ca(2+) and CO3(2-) ions.

Synthesis, spectral and antimicrobial activity of [3-(4-chloro-phenoxy-2,4-diisopropyl-2,3,4,5-tetrahydro-1H-3l5-benzo[e][1,3,2]diazaphosphepin-3-ylidene]-alkyl-amine

Directory of Open Access Journals (Sweden)

R. Usha Nagalakshmi

2009-11-01

Full Text Available 3-(4-chlorophenoxy-2,4-diisopropyl-2,3,4,5-tetrahydro-1H-benzo[e][1,3,2]diaza-phosphepine was synthesized starting from 1,2-bis(bromomethylbenzene by reacting with 2 equimolar isopropyl amine, one equimolar PBr3 and then one equimolar 4-chlorophenol, respectively. The Staudinger reaction of the diazaphphosphine with a series of alkyl azides gave the corresponding iminophosphoranes. Antibacterial activities of the synthesized iminophosphoranes were screened

New coordination polymers from 1D chain, 2D layer to 3D framework constructed from 1,2-phenylenediacetic acid and 1,3-bis(4-pyridyl)propane flexible ligands

International Nuclear Information System (INIS)

Xin Lingyun; Liu Guangzhen; Wang Liya

2011-01-01

The hydrothermal reactions of Cd, Zn, or Cu(II) acetate salts with H 2 PHDA and BPP flexible ligands afford three new coordination polymers, including [Cd(PHDA)(BPP)(H 2 O)] n (1), [Zn(PHDA)(BPP)] n (2), and [Cu 2 (PHDA) 2 (BPP)] n (3) (H 2 PHDA=1,2-phenylenediacetic acid, BPP=1,3-bis(4-pyridyl)propane). The single-crystal X-ray diffractions reveal that all three complexes feature various metal carboxylate subunits extended further by the BPP ligands to form a diverse range of structures, displaying a remarked structural sensitivity to metal(II) cation. Complex 1 containing PHDA-bridged binuclear cadmium generates 1D double-stranded chain, complex 2 results in 2D→2D interpenetrated (4,4) grids, and complex 3 displays a 3D self-penetrated framework with 4 8 6 6 8 rob topology. In addition, fluorescent analyses show that both 1 and 2 exhibit intense blue-violet photoluminescence in the solid state. - Graphical Abstract: We show diverse supramolecular frameworks based on the same ligands (PHDA and BPP) and different metal acetate salts including 1D double-stranded chain, 2D → 2D twofold interpenetrated layer, and 3D self-penetration networks. Highlights: → Three metal(II = 2 /* ROMAN ) coordination polymers were synthesized using H 2 PHDA and BPP. → The diversity of structures show a remarked sensitivity to metal(II) center. → Complexes show the enhancement of fluorescence compared to that of free ligand.

Fused 1,2,3-Dithiazoles: Convenient Synthesis, Structural Characterization, and Electrochemical Properties

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Lidia S. Konstantinova

2016-05-01

Full Text Available A new general protocol for synthesis of fused 1,2,3-dithiazoles by the reaction of cyclic oximes with S2Cl2 and pyridine in acetonitrile has been developed. The target 1,2,3-dithiazoles fused with various carbocycles, such as indene, naphthalenone, cyclohexadienone, cyclopentadiene, and benzoannulene, were selectively obtained in low to high yields. In most cases, the hetero ring-closure was accompanied by chlorination of the carbocyclic moieties. With naphthalenone derivatives, a novel dithiazole rearrangement (15→13 featuring unexpected movement of the dithiazole ring from α- to β-position, with respect to keto group, was discovered. Molecular structure of 4-chloro-5H-naphtho[1,2-d][1,2,3]dithiazol-5-one 13 was confirmed by single-crystal X-ray diffraction. Electrochemical properties of 13 were studied by cyclic voltammetry and a complex behavior was observed, most likely including hydrodechlorination at a low potential.

Electrochemistry of TiF4 in 1-butyl-2,3-dimethylimidazolium tetrafluoroborate

International Nuclear Information System (INIS)

Andriyko, Yuriy; Andriiko, Alexander; Babushkina, Olga B.; Nauer, Gerhard E.

2010-01-01

Electrochemical behaviour of Ti(IV) species in the ionic liquid (IL) 1-butyl-2,3-dimethylimidazolium tetrafluoroborate (BMMImBF 4 ) was studied by means of chronopotentiometry (CP) and cyclic voltammetry (CV) in melts with different concentrations of TiF 4 (2-35 mol%) within a temperature range of 65-180 deg. C. The electrochemical reduction of Ti(IV) was suggested to proceed via the sequence of one-electron steps with the formation of poorly soluble low valence intermediates (LVI). LVIs undergo further solid-state electrochemical reduction to Ti metal. Thin Ti coatings on a Pt substrate were thus obtained and characterized by ESEM method. FTIR spectroscopy was used for identification of the electrochemical active species of Ti(IV). The reaction 2BF 4 - + TiF 4 ↔ TiF 6 2- + 2BF 3 ↑ takes place in the concentrated solutions of TiF 4 at elevated temperatures.

Synthesis, characterization and initial evaluation of 5-nitro-1-(trifluoromethyl-3H-1λ3,2-benziodaoxol-3-one

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Nico Santschi

2014-01-01

Full Text Available The synthesis of 5-nitro-1-(trifluoromethyl-3H-1λ3,2-benziodaoxol-3-one (3, a hypervalent-iodine-based electrophilic trifluoromethylating reagent, is described. Whereas considerations based on cyclic voltammetry and X-ray structural properties would predict an inferior reactivity when compared to the non-nitrated derivative 2, 19F NMR kinetic studies showed that this new derivative is almost one order of magnitude more reactive. Furthermore, differential scanning calorimetry measurements indicated that, in addition, it is also safer to handle.

Synthesis and distribution of tritiated N,N`-dibenzoyl-1,3-diaminopropan-2-ol

Energy Technology Data Exchange (ETDEWEB)

Lambert, D.M.; Gallez, Bernard [Universite Catholique de Louvain, Dept. des Sciences Pharmaceutiques, Bruxelles (Belgium)

1996-10-01

Tritiated N,N`-dibenzoyl-1,3-diaminopropan-2-ol, a compound mimicking a diacylglycerol moiety used as a lipid drug carrier was prepared from N,N`-dibenzoyl-1,3-diaminopropan-2-ol by isotopic exchange in the presence of rhodium chloride. Preliminary preparation of the deuterated analog was made in order to assess the position of the substitution. A biodistribution study was carried out in mice after intravenous administration. Five minutes after administration, the level found in the brain was about 9% of the injected dose per g organ. This value decreases to 1 % 3 hours after administration while at the same time radioactive levels measured in the urine increased. (author).

Synthesis, structural and antibacterial study of new silver complex with 3-acetyl-2H chromene-2-one

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Z. Ali

2017-01-01

Full Text Available A new silver complex [Ag(C11H8O32]NO3 was synthesized by the reaction of silver nitrateand coumarin based ligand (3-acetyl-2H-chromene-2-one through solution method. The product was characterized using different analytical techniques like melting point, Infrared spectroscopy, Raman spectroscopy, powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, atomic absorption spectroscopy and mass spectrometry. An antibacterial study of the complex was also studied for its possible use in medical treatment.

Synthesis, 2D NMR, electrochemistry and luminescence of ruthenium (II) complexes with 2,2-bipyridine and 5-(ω-bromoalkylamido)-1, 10-phenanthroline

International Nuclear Information System (INIS)

Peng Wang; Xiangping Wang, Guoyi Zhu; Xiaoyan Jing; Jun Wang

2000-01-01

The efficient synthesis of 5-(5-bromovaleramido)-1, 10-phenanthroline, 5-(6-bromohexanamido)-1,10-phenanthroline, and 5-(11-bromoundecanamido)-1, 10-phenanthroline are described, which reacted with cis-Ru(bpy) 2 Cl 2 .2H 2 O and sodium hexafluorophosphate to form Ru(bpy) 2 [phen-NHCO(CH 2 ) n Br](PF 6 ) 2 (n=4, 5 or 10; phen=1,10-phenanthroline). The intricate 1 H NMR spectra at low field of these complexes were completely assigned in virtue of 1 H- 1 H COSY technique. Cyclic voltammetry was used to study electrochemical behaviours of these complexes, and their luminescent properties were investigated with fluorescent spectra. (author)

Synthesis and biological characterization of (3R,4R)-4-(2-(benzhydryloxy)ethyl)-1-((R)-2-hydroxy-2-phenylethyl)-piperidin-3-ol and its stereoisomers for activity toward monoamine transporters.

Science.gov (United States)

Kharkar, Prashant S; Batman, Angela M; Zhen, Juan; Beardsley, Patrick M; Reith, Maarten E A; Dutta, Aloke K

2009-07-01

A novel series of optically active molecules based on a 4-(2-(benzhydryloxy)ethyl)-1-((R)-2-hydroxy-2-phenylethyl)-piperidin-3-ol template were developed. Depending on stereochemistry, the compounds exhibit various degrees of affinity for three dopamine, serotonin, and norepinephrine transporters. These molecules have the potential for treating several neurological disorders such as drug abuse, depression, and attention deficit hyperactivity disorder.Herein we describe the synthesis and biological evaluation of a series of asymmetric 4-(2-(benzhydryloxy)ethyl)-1-((R)-2-hydroxy-2-phenylethyl)-piperidin-3-ol-based dihydroxy compounds in which the hydroxy groups are located on both the piperidine ring and the N-phenylethyl side chain. In vitro uptake inhibition data of these molecules indicate high affinity for the dopamine transporter (DAT) in addition to moderate to high affinity for the norepinephrine transporter (NET). Interestingly, compounds 9 b and 9 d exhibit affinities for all three monoamine transporters, with highest potency at DAT and NET, and moderate potency at the serotonin transporter (SERT) (K(i): 2.29, 78.4, and 155 nM for 9 b and 1.55, 14.1, and 259 nM for 9 d, respectively). Selected compounds 9 a, 9 d, and 9 d' were tested for their locomotor activity effects in mice and for their ability to occasion the cocaine-discriminative stimulus in rats. These test compounds generally exhibit a much longer duration of action than cocaine for elevating locomotor activity, and completely generalize the cocaine-discriminative stimulus in a dose-dependent manner.

Homoleptic diphosphacyclobutadiene complexes [M(η(4)-P2C2R2)2]x- (M = Fe, Co; x = 0, 1).

Science.gov (United States)

Wolf, Robert; Ehlers, Andreas W; Khusniyarov, Marat M; Hartl, František; de Bruin, Bas; Long, Gary J; Grandjean, Fernande; Schappacher, Falko M; Pöttgen, Rainer; Slootweg, J Chris; Lutz, Martin; Spek, Anthony L; Lammertsma, Koop

2010-12-27

The preparation and comprehensive characterization of a series of homoleptic sandwich complexes containing diphosphacyclobutadiene ligands are reported. Compounds [K([18]crown-6)(thf)(2)][Fe(η(4)-P(2)C(2)tBu(2))(2)] (K1), [K([18]crown-6)(thf)(2)][Co(η(4)-P(2)C(2)tBu(2))(2)] (K2), and [K([18]crown-6)(thf)(2)][Co(η(4)-P(2)C(2)Ad(2))(2)] (K3, Ad = adamantyl) were obtained from reactions of [K([18]crown-6)(thf)(2)][M(η(4)-C(14)H(10))(2)] (M = Fe, Co) with tBuC[triple bond]P (1, 2), or with AdC[triple bond]P (3). Neutral sandwiches [M(η(4)-P(2)C(2)tBu(2))(2)] (4: M = Fe 5: M = Co) were obtained by oxidizing 1 and 2 with [Cp(2)Fe]PF(6). Cyclic voltammetry and spectro-electrochemistry indicate that the two [M(η(4)-P(2)C(2)tBu(2))(2)](-)/[M(η(4)-P(2)C(2)tBu(2))(2)] moieties can be reversibly interconverted by one electron oxidation and reduction, respectively. Complexes 1-5 were characterized by multinuclear NMR, EPR (1 and 5), UV/Vis, and Mössbauer spectroscopies (1 and 4), mass spectrometry (4 and 5), and microanalysis (1-3). The molecular structures of 1-5 were determined by using X-ray crystallography. Essentially D(2d)-symmetric structures were found for all five complexes, which show the two 1,3-diphosphacyclobutadiene rings in a staggered orientation. Density functional theory calculations revealed the importance of covalent metal-ligand π bonding in 1-5. Possible oxidation state assignments for the metal ions are discussed.

Lipase Catalyzed Kinetic Resolution of rac-2-(3-Methoxy-4-methylphenyl) propan-1-ol and rac-2-(3-Hydroxy-4-methylphenyl)propyl propanoate for S-(+)-Xanthorrhizol

International Nuclear Information System (INIS)

Shafioul, Azam Sharif Mohammed; Cheong, Chan Seong

2012-01-01

Xanthorrhizol is a bisabolane type of natural sesquiterpene, the major component of essential oils of Curcuma xanthorrhiza. 2-(3-Methoxy-4-methylphenyl)propan-1-ol and 2-(3-hydroxy-4-methyl phenyl)propan-1-ol could be essential building block for enantioselective synthesis of xanthorrhizol. Enantioselective (c = 53%, E = 80 ± 3) for R-(+)-2-(3-hydroxy-4-methylphenyl) propan-1-ol and (c = 58%, E = 27 ± 1) for R-(+)-2-(3- methoxy-4-methylphenyl) propan-1-ol resolution processes were developed via lipase-catalyzed reaction. We found lipase Aspergillus oryzae (AOL) and Porcine pancreas (PPL) are selective to transesterification and hydrolysis in organic and aqueous phase. Modified demethylated substrate is appropriate for enantioselective hydrolysis reaction without any additives. Enantiopure chiral alcohol was crystallized from ethyl acetate/ n-hexane co-solvent system. Gram scale resolved chiral intermediate will facilitate the synthesis of the unnatural S-(+)-xanthorrhizol, the corresponding isomer of the natural one

Lipase Catalyzed Kinetic Resolution of rac-2-(3-Methoxy-4-methylphenyl) propan-1-ol and rac-2-(3-Hydroxy-4-methylphenyl)propyl propanoate for S-(+)-Xanthorrhizol

Energy Technology Data Exchange (ETDEWEB)

Shafioul, Azam Sharif Mohammed [University of Science and Technology, Daejeon (Korea, Republic of); Cheong, Chan Seong [Korea Institute of Science and Technology, Seoul (Korea, Republic of)

2012-02-15

Xanthorrhizol is a bisabolane type of natural sesquiterpene, the major component of essential oils of Curcuma xanthorrhiza. 2-(3-Methoxy-4-methylphenyl)propan-1-ol and 2-(3-hydroxy-4-methyl phenyl)propan-1-ol could be essential building block for enantioselective synthesis of xanthorrhizol. Enantioselective (c = 53%, E = 80 ± 3) for R-(+)-2-(3-hydroxy-4-methylphenyl) propan-1-ol and (c = 58%, E = 27 ± 1) for R-(+)-2-(3- methoxy-4-methylphenyl) propan-1-ol resolution processes were developed via lipase-catalyzed reaction. We found lipase Aspergillus oryzae (AOL) and Porcine pancreas (PPL) are selective to transesterification and hydrolysis in organic and aqueous phase. Modified demethylated substrate is appropriate for enantioselective hydrolysis reaction without any additives. Enantiopure chiral alcohol was crystallized from ethyl acetate/ n-hexane co-solvent system. Gram scale resolved chiral intermediate will facilitate the synthesis of the unnatural S-(+)-xanthorrhizol, the corresponding isomer of the natural one.

New transition metal complexes of 2,4-dihydroxybenzaldehyde benzoylhydrazone Schiff base (H2dhbh): Synthesis, spectroscopic characterization, DNA binding/cleavage and antioxidant activity

Science.gov (United States)

Aboafia, Seyada A.; Elsayed, Shadia A.; El-Sayed, Ahmed K. A.; El-Hendawy, Ahmed M.

2018-04-01

New complexes [VO2(Hdhbh)] (1), [VO(phen)(dhbh)].1.5H2O (2), [Zn(Hdhbh)2] (3), [MoO2(dhbh)(D)] (D = H2O (4) or MeOH (5)), [Ru(PPh3)(dhbh)Cl(H2O)] (6), and [Pd(Hdhbh)Cl]·H2O (7) (H2dhbh = Schiff base derived from 2,4-dihydroxybenzaldehyde and benzoylhydrazone) have been isolated and characterized by IR, 1H NMR, Mass, UV-Visible and ESR spectroscopy. They were also investigated by cyclic voltammetry, thermal and magnetic measurements and the structure of complex cis-[MoO2(dhbh)(H2O)] (4) was solved by X-ray crystallography. Analytical data showed that H2dhbh behaves as monobasic/or dibasic tridentate ligand via phenolate O, azomethine N and amide O/or deprotonated amide O atoms. Antioxidant activity of the complexes has been evaluated against DPPH (2,2-diphenyl-1-picrylhydrazyl) radical and it has been found that oxovandium (IV) complex (2) displays the highest radical scavenging potency comparable to ascorbic acid as a standard antioxidant. The DNA binding properties of the ligand and its complexes have been investigated by electronic spectroscopy together with DNA cleavage by gel electrophoresis whose results showed also that vanadium (IV) complex (2) has a significant oxidative cleavage among other complexes.

Synthesis and Comparison of In Vitro Leishmanicidal Activity of 5-(Nitroheteroaryl-1, 3, 4-Thiadiazols Containing Cyclic Amine of Piperidin-4-ol at C-2 with Acyclic Amine Analogues against Iranian Strain of Leishmania major (MRHO/IR/75/ER

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Azar Tahghighi

2017-04-01

Full Text Available Background: Cutaneous Leishmaniasis (CL is endemic in many tropical and subtropical regions of the world. Due to the prolonged duration of therapy, adverse effect and resistance to current drugs in the treatment of CL, the dis­covery of novel, efficient, and safe leishmanicidal drugs is required. The aims of the present study was to synthesis of new compounds based on the active compounds of 5-(5-nitrofuran-2-yl- and 5-(5-nitrothiophen-2-yl-1,3,4-thia­diazole bearing the linear amino alcohol of 3-aminopropan-1-ol in the C-2 position of thiadiazole ring and evaluation of their activity against the promastigote and amastigote forms of Leishmania major.Methods: Reaction between the solution of 5-(5-nitro heteroaryl-2-chloro-1, 3, 4-thiadiazole and piperidin-4-ol in absolute ethanol was performed and the resulting products were evaluated against promastigotes form of L. major with MTT assay and amastigote form of L. major in murine peritoneal macrophages. In addition, the toxicity of these compounds was assessed against mouse peritoneal macrophages with MTT assay.Results: New synthetic compounds 5a-b showed moderate in vitro antileishmanial activity against L. major pro­mastigotes with IC50 values of 68.9 and 27 µM, respectively. These compounds have also demonstrated a good antiamastigote activity in terms of amastigote number per macrophage, the percentage of macrophage infectivity and infectivity index.Conclusion: Novel cyclic compounds 5a-b were synthesized and exhibited less antipromastigote and antiamastigote activity compared to linear analogues.

Complexation of Cm(III) and Eu(III) with 2,6-bis(5-(2,2-dimethylpropyl)-1H-pyrazol-3-yl)pyridine and 2-bromohexanoic acid studied by time-resolved laser fluorescence spectroscopy

International Nuclear Information System (INIS)

Bremer, A.; Panak, P.J.; Heidelberg Univ.; Geist, A.

2013-01-01

The complexation of Cm(III) and Eu(III) with 2,6-bis(5-(2,2-dimethylpropyl)-1H-pyrazol-3-yl)pyridine (C5-BPP) and 2-bromohexanoic acid as lipophilic anion has been investigated by time-resolved laser fluorescence spectroscopy. Upon increasing ligand concentration three different Cm(III)-C5-BPP species with emission bands at 604.1 nm, 607.9 nm and 611.4 nm, respectively, are found and attributed to complexes with one, two and three C5-BPP molecules in the inner coordination sphere. Comparison with results of TRLFS experiments without 2-bromohexanoic acid shows that the C5-BPP ligand is able to completely displace the lipophilic anion from the inner coordination sphere, forming [Cm(C5-BPP) 3 ] 3+ complexes. This complex is also found in the organic phase of an extraction experiment performed with Cm(III), demonstrating that the lipophilic anion required for the extraction is not directly coordinated to the metal ion in the species formed during extraction. In case of Eu(III) the number of different species formed cannot be determined accurately. Nevertheless, the formation of the complex [EU(C5-BPP) 3 ] 3+ in the presence of 2-bromohexanoic acid is confirmed. (orig.)

Crystal structure, DNA binding, cleavage, antioxidant and antibacterial studies of Cu(II), Ni(II) and Co(III) complexes with 2-((furan-2-yl)methylimino)methyl)-6-ethoxyphenol Schiff base

Science.gov (United States)

Venkateswarlu, Kadtala; Kumar, Marri Pradeep; Rambabu, Aveli; Vamsikrishna, Narendrula; Daravath, Sreenu; Rangan, Krishnan; Shivaraj

2018-05-01

Three novel binary metal complexes; 1 [Cu(L)2], 2 [Ni(L)2] and 3 [Co(L)3] where, L (2-(((furan-2-yl) methylimino)methyl)-6-ethoxyphenol, C14H15NO3), were synthesized and characterized by various spectral techniques. Based on spectral studies square planar geometry is assigned for Cu(II) and Ni(II) complexes, whereas Co(III) owned octahedral geometry. Ligand, [Cu(L)2] and [Ni(L)2] are crystallized and found to be monoclinic crystal systems. CT-DNA absorption binding studies revealed that the complexes show good binding propensity (Kb = 5.02 × 103 M-1, 2.77 × 103 M-1, 1.63 × 104 M-1 for 1, 2 and 3 respectively). The role of these complexes in the oxidative and photolytic cleavage of supercoiled pBR322 DNA was studied and found that the complexes cleave the pBR322 DNA effectively. The catalytic ability of 1, 2 and 3 follows the order: 3 > 1 >2. Antioxidant studies of the new complexes revealed that they exhibit significant antioxidant activity against DPPH radical. The Schiff base and its metal complexes have been screened for antibacterial studies by Minimum Inhibitory Concentration method. It is observed that all metal complexes showed more activity than free ligand.

A new rhodamine-based fluorescent probe for the discrimination of Fe"3"+ from Fe"2"+

International Nuclear Information System (INIS)

You, Qi Hua; Huang, Hua Bin; Zhuang, Zhi Xia; Wang, Xiao Ru; Chan, Wing Hong

2016-01-01

A new rhodamine-based fluorescent probe for the discrimination of Fe"3"+ from Fe"2"+ has been designed and investigated. The probe shows an immediate visual color change in response to Fe"3"+ and Cu"2"+, while only Fe"3"+ triggers the fluorescent change of the probe. The existence of large amount of other metal ions shows negligible interference in the detection of Fe"3"+. The association constant K_a_s_s of 4.64 × 10"8 M"-"2 (R"2 = 0.994) and 5.38 × 10"8 M"-"2 (R"2 = 0.991) of the complex was derived from UV/Vis and fluorescence titration assuming 1:2 stoichiometry of probe–Fe"3"+ complex, respectively

Synthesis, characterisation and antibacterial activity of [(p-cym)RuX(L)](+/2+) (X = Cl, H2O; L = bpmo, bpms) complexes.

Science.gov (United States)

Tripathy, Suman Kumar; Taviti, Ashoka Chary; Dehury, Niranjan; Sahoo, Anupam; Pal, Satyanaryan; Beuria, Tushar Kant; Patra, Srikanta

2015-03-21

Mononuclear half-sandwiched complexes [(p-cym)RuCl(bpmo)](ClO4) {[1](ClO4)} and [(p-cym)RuCl(bpms)](PF6) {[2](PF6)} have been prepared by reacting heteroscorpionate ligands bpmo = 2-methoxyphenyl-bis(3,5-dimethylpyrazol-1-yl)methane and bpms = 2-methylthiophenyl-bis(3,5-dimethylpyrazol-1-yl)methane, respectively, with a dimeric precursor complex [(p-cym)RuCl(μ-Cl)]2 (p-cym = 1-isopropyl-4-methylbenzene) in methanol. The corresponding aqua derivatives [(p-cym)Ru(H2O)(bpmo)](ClO4)2 {[3](ClO4)2} and [(p-cym)Ru(H2O)(bpms)](PF6)2 {[4](PF6)2} are obtained from {[1](ClO4)} and {[2](PF6)}, respectively, via Cl(-)/H2O exchange process in the presence of appropriate equivalents of AgClO4/AgNO3 + KPF6 in a methanol-water mixture. The molecular structures of the complexes {[1]Cl, [3](ClO4)2 and [4](PF6)(NO3)} are authenticated by their single crystal X-ray structures. The complexes show the expected piano-stool geometry with p-cym in the η(6) binding mode. The aqua complexes [3](ClO4)2 and [4](PF6)2 show significantly good antibacterial activity towards E. coli (gram negative) and B. subtilis (gram positive) strains, while chloro derivatives ({[1](ClO4)} and {[2](PF6)} are found to be virtually inactive. The order of antibacterial activity of the complexes according to their MIC values is [1](ClO4) (both 1000 μg mL(-1)) < [2](PF6) (580 μg mL(-1) and 750 μg mL(-1)) < [3](ClO4)2 (both 100 μg mL(-1)) < [4](PF6)2 (30 μg mL(-1) and 60 μg mL(-1)) for E. coli and B. subtilis strains, respectively. Further, the aqua complexes [3](ClO4)2 and [4](PF6)2 show clear zones of inhibition against kanamycin, ampicillin and chloramphenicol resistant E. coli strains. The detailed mechanistic aspects of the aforesaid active aqua complexes [3](ClO4)2 and [4](PF6)2 have been explored, and it reveals that both the complexes inhibit the number of nucleoids per cell in vivo and bind to DNA in vitro. The results indeed demonstrate that both [3](ClO4)2 and [4](PF6)2 facilitate the inhibition of

Dynamics of Pseudomonas aeruginosa azurin and its Cys3Ser mutant at single crystal gold surfaces investigated by cyclic voltammetry and atomic force microscopy

DEFF Research Database (Denmark)

Friis, Esben P.; Andersen, Jens Enevold Thaulov; Madsen, Lars Lithen

1997-01-01

Cyclic voltammetry of Pseudomonas aeruginosa azurin on polycrystalline gold is reversible (E0=360mV vs she;50mM ammonium acetate) but the voltammetric signals decay with time constants of about 3x10-3 s-1. No signal is observed for monocrystalline Au(111). Cys3Ser azurin is electrochemically inac...... into the solution, recovering the free Au(111) surface. The cyclic voltammetry and AFM data are consistent with time dependent adsorption of the azurins on gold via the disulphide bridge (wild-type) or free thiol group (Cys3Ser mutant).......Cyclic voltammetry of Pseudomonas aeruginosa azurin on polycrystalline gold is reversible (E0=360mV vs she;50mM ammonium acetate) but the voltammetric signals decay with time constants of about 3x10-3 s-1. No signal is observed for monocrystalline Au(111). Cys3Ser azurin is electrochemically...... inactive on either type of gold electrode but shows a reversible although decaying peak (362mV, 50mM ammonium acetate; decay time constant ~ 2x10-3 s-1) on edge-plane pyrolytic graphite.Ex situ and in situ atomic force microscopy (AFM) of the azurins on Au(111) show initially arrays of protein structures...

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.

Synthesis, characterization, in-vitro antimicrobial properties, molecular docking and DFT studies of 3-{(E-[(4,6-dimethylpyrimidin-2-ylimino]methyl} naphthalen-2-ol and Heteroleptic Mn(II, Co(II, Ni(II and Zn(II complexes

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Chioma Festus

2018-03-01

Full Text Available Heteroleptic divalent metal complexes [M(L (bipy(Y]•nH2O (where M = Mn, Co, Ni, and Zn; L = Schiff base; bipy = 2,2’-bipyridine; Y = OAc and n = 0, 1 have been synthesized from pyrimidine Schiff base ligand 3-{(E-[(4,6-dimethylpyrimidin-2-ylimino]methyl} naphthalen-2-ol, 2,2’-bipyridine and metal(II acetate salts. The Schiff base and its complexes were characterized by analytical (CHN elemental analyses, solubility, melting point, conductivity measurements, spectral (IR, UV-vis, 1H and 13C-NMR and MS and magnetometry. The elemental analyses, Uv-vis spectra and room temperature magnetic moment data provide evidence of six coordinated octahedral geometry for the complexes. The metal complexes’ low molar conductivity values in dimethylsulphoxide suggested that they were non-ionic in nature. The compounds displayed moderate to good antimicrobial and antifungal activities against S. aureus, P. aeruginosa, E. coli, B. cereus, P. mirabilis, K. oxytoca, A. niger, A. flevus and R. Stolonifer. The compounds also exhibited good antioxidant potentials with ferrous ion chelation and, 1-diphenyl-2-picryl-hydrazyl (DPPH radical scavenging assays. Molecular docking studies showed a good interaction with drug targets used. The structural and electronic properties of complexes were further confirmed by density functional theory calculations.

Electrochemistry of TiF{sub 4} in 1-butyl-2,3-dimethylimidazolium tetrafluoroborate

Energy Technology Data Exchange (ETDEWEB)

Andriyko, Yuriy, E-mail: yuriy.andriyko@cest.a [Centre of Electrochemical Surface Technology (CEST), Viktor Kaplan-Strasse 2, A-2700 Wiener Neustadt (Austria); Andriiko, Alexander [National Technical University of Ukraine ' Kyiv Polytechnic Institute' , Prospect Peremogy 37, 03057 Kyiv (Ukraine); Babushkina, Olga B. [Centre of Electrochemical Surface Technology (CEST), Viktor Kaplan-Strasse 2, A-2700 Wiener Neustadt (Austria); Nauer, Gerhard E. [Centre of Electrochemical Surface Technology (CEST), Viktor Kaplan-Strasse 2, A-2700 Wiener Neustadt (Austria); Vienna University, Faculty of Chemistry, Waehringer Strasse 42, A-1090 Wien (Austria)

2010-01-01

Electrochemical behaviour of Ti(IV) species in the ionic liquid (IL) 1-butyl-2,3-dimethylimidazolium tetrafluoroborate (BMMImBF{sub 4}) was studied by means of chronopotentiometry (CP) and cyclic voltammetry (CV) in melts with different concentrations of TiF{sub 4} (2-35 mol%) within a temperature range of 65-180 deg. C. The electrochemical reduction of Ti(IV) was suggested to proceed via the sequence of one-electron steps with the formation of poorly soluble low valence intermediates (LVI). LVIs undergo further solid-state electrochemical reduction to Ti metal. Thin Ti coatings on a Pt substrate were thus obtained and characterized by ESEM method. FTIR spectroscopy was used for identification of the electrochemical active species of Ti(IV). The reaction 2BF{sub 4}{sup -} + TiF{sub 4} reversible TiF{sub 6}{sup 2-} + 2BF{sub 3}arrow up takes place in the concentrated solutions of TiF{sub 4} at elevated temperatures.

Fluorescence spectra and collisional energy transfer of YO (A2PIsub(1/2, 3/2)) molecules in flames

International Nuclear Information System (INIS)

Wijchers, T.

1981-01-01

The aim of this investigation was (a) to determine, from fluorescence spectra in the visible, the normalized, radiatively induced extra populations of vibronic levels of a diatomic metal compound; (b) to calculate therefrom the normalized collisional transition probabilities between vibrational levels in an excited electronic state. Yttrium monoixde (YO) was chosen as the metal compound and A 2 PIsub(1/2,3/2) as the state(s) to be investigated. (Auth.)

Platinum(0-1,3-divinyl-1,1,3,3-tetramethyldisiloxane Complex as a Pt Source for Pt/SnO2 Catalyst

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Agnieszka Martyla

2014-01-01

Full Text Available This paper presents new preparation method of Pt/SnO2, an important catalytic system. Besides of its application as a heterogenic industrial catalyst, it is also used as a catalyst in electrochemical processes, especially in fuel cells. Platinum is commonly used as an anode catalyst in low temperature fuel cells, fuelled with alcohols of low molecular weight such as methanol. Platinum(0-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex was used as a precursor of metallic phase. The aim of the research was to obtain a highly active in electrochemical system Pt/SnO2 catalyst with low metal load. Considering small size of Pt crystallites, it should result in high activity of Pt/SnO2 system. The presented method of SnO2 synthesis allows for obtaining support consisting of nanoparticles. The effect of the thermal treatment on activity of Pt/SnO2 gel was demonstrated. The system properties were investigated using TEM, FTIR (ATR, and XRD techniques to describe its thermal structural evolution. The results showed two electrocatalytical activity peaks for drying at a temperature of 430 K and above 650 K.

Synthesis, solvatochromaticity and bioactivities of some transition metal complexes with 2-(R-benzylideneamino)-pyridin-3-ol Schiff base derivatives

Science.gov (United States)

Ahmed, I. S.; Kassem, M. A.

2010-10-01

New four Schiff bases are prepared by condensation of 2-amino-pyridin-3-ol with 3, 4-dihydroxy-benzaldehyde (I), 2-hydroxybenzaldehyde (II), 5-bromo-2-hydroxybenzaldehyde (III), and 4-dimethylaminobenzaldehyde (IV). The structures of these compounds are characterized based on elemental analyses (C. H. N), IR and 1H NMR. Also, the electronic absorption spectra are recorded in organic solvents of different polarity. The solvents are selected to be covered a wide range of parameters (refractive index, dielectric constant and hydrogen bonding capacity). The UV-vis absorption spectra of Schiff base compounds are investigated in aqueous buffer solutions of varying pH and utilized for the determination of ionization constant, p Ka and activation free energy, Δ G* of the ionization process. The biological activity against bacterial species and fungi as microorganisms representing different microbial categories such as (two Gram-negative bacteria, Eschericha coli and Agrobacterium sp.),three Gram-positive bacteria ( Staphylococcus aureus, Bacillus subtlus and Bacillus megatherium), yeast ( Candida albicans), and fungi ( Aspergillus niger) were studied.

BF3·Et2O-promoted cleavage of the Csp-Csp2 bond of 2-propynolphenols/anilines: route to C2-alkenylated benzoxazoles and benzimidazoles.

Science.gov (United States)

Song, Xian-Rong; Qiu, Yi-Feng; Song, Bo; Hao, Xin-Hua; Han, Ya-Ping; Gao, Pin; Liu, Xue-Yuan; Liang, Yong-Min

2015-02-20

A novel BF3·Et2O-promoted tandem reaction of easily prepared 2-propynolphenols/anilines and trimethylsilyl azide is developed to give C2-alkenylated benzoxazoles and benzimidazoles in moderate to good yields. Most reactions could be accomplished in 30 min at room temperature. This tandem process involves a Csp-Csp2 bond cleavage and a C-N bond formation. Moreover, both tertiary and secondary propargylic alcohols with diverse functional groups were tolerated under the mild conditions.

Synthesis of Novel Antibacterial Agents: 1-(2', 4'-Dihydroxy-5'-chlorophenyl-3-arylpropane-1, 3-Diones

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J. I. Sheikh

2009-01-01

Full Text Available 1-(2', 4'-Dihydroxy-5'-chlorophenyl-3-arylpropane-1, 3-diones(3a-h have been synthesized by a simple and convenient method employing Baker-Venkatraman transformation on 2-aroyloxy-4-hydroxy-5-chloroacetophenones (2a-h with NaOH in dimethylsuphoxide regardless of pyridine. The structures of the synthesized compounds have been assigned on the basis of elemental and spectral analyses (IR, 1HNMR, 13C NMR, Mass. The synthesized compounds were evaluated for the antibacterial efficacy against gram negative and gram positive bacteria.

An analysis method for flavan-3-ols using high performance liquid chromatography coupled with a fluorescence detector

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Liuqing Wang

2017-07-01

Full Text Available Procyanidins belong to a family of flavan-3-ols, which consist of monomers, (+-catechin and (−-epicatechin, and their oligomers and polymers, and are distributed in many plant-derived foods. Procyanidins are reported to have many beneficial physiological activities, such as antihypertensive and anticancer effects. However, the bioavailability of procyanidins is not well understood owing to a lack of convenient and high-sensitive analysis methods. The aim of this study was to develop an improved method for determining procyanidin content in both food materials and biological samples. High performance liquid chromatography (HPLC coupled with a fluorescence detector was used in this study. The limits of detection (LODs of (+-catechin, (−-epicatechin, procyanidin B2, procyanidin C1, and cinnamtannin A2 were 3.0×10−3 ng, 4.0×10−3 ng, 14.0×10−3 ng, 18.5×10−3 ng, and 23.0×10−3 ng, respectively; the limits of quantification (LOQs were 10.0×10−3 ng, 29.0×10−3 ng, 28.5×10−3 ng, 54.1×10−3 ng, and 115.0×10−3 ng, respectively. The LOD and LOQ values indicated that the sensitivity of the fluorescence detector method was around 1000 times higher than that of conventional HPLC coupled with a UV-detector. We applied the developed method to measure procyanidins in black soybean seed coat extract (BE prepared from soybeans grown under three different fertilization conditions, namely, conventional farming, basal manure application, and intertillage. The amount of flavan-3-ols in these BEs decreased in the order intertillage > basal manure application > conventional farming. Commercially available BE was orally administered to mice at a dose of 250 mg/kg body weight, and we measured the blood flavan-3-ol content. Data from plasma analysis indicated that up to the tetramer oligomerization, procyanidins were detectable and flavan-3-ols mainly existed in conjugated forms in the plasma. In conclusion, we developed a highly

1-[2-(2-Methoxyphenylaminoethylamino]-3-(naphthalene-1- yloxypropan-2-ol May Be a Promising Anticancer Drug

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Tomoyuki Nishizaki

2014-12-01

Full Text Available We have originally synthesized the naftopidil analogue 1-[2-(2-methoxyphenylaminoethylamino]-3-(naphthalene-1-yloxypropan-2-ol (HUHS 1015 as a new anticancer drug. HUHS1015 induces cell death in a wide variety of human cancer cell lines originated from malignant pleural mesothelioma, lung cancer, hepatoma, gastric cancer, colorectal cancer, bladder cancer, prostate cancer, and renal cancer. HUHS1015-induced cell death includes necrosis (necroptosis and apoptosis, and the underlying mechanism differs depending upon cancer cell types. HUHS1015 effectively suppresses tumor growth in mice inoculated with NCI-H2052, MKN45, or CW2 cells, with a potential similar to or higher than that of currently used anticancer drugs. Here we show how HUHS1015 might offer brilliant hope for cancer therapy.

DNA-binding, catalytic oxidation, C—C coupling reactions and antibacterial activities of binuclear Ru(II thiosemicarbazone complexes: Synthesis and spectral characterization

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Arumugam Manimaran

2012-07-01

Full Text Available New hexa-coordinated binuclear Ru(II thiosemicarbazone complexes of the type {[(B(EPh3(COClRu]2L} (where, E = P or As; B = PPh3 or AsPh3 or pyridine; L = mononucleating NS donor of N-substituted thiosemicarbazones have been synthesized and characterized by elemental analysis, FT-IR, UV–vis and 31P{1H} NMR cyclic voltammetric studies. The DNA-binding studies of Ru(II complexes with calf thymus DNA (CT-DNA were investigated by UV–vis, viscosity measurements, gel-electrophoresis and fluorescence spectroscopy. The new complexes have been used as catalysts in C—C coupling reaction and in the oxidation of alcohols to their corresponding carbonyl compounds by using NMO as co-oxidant and molecular oxygen (O2 atmosphere at ambient temperature. Further, the new binucleating thiosemicarbazone ligands and their Ru(II complexes were also screened for their antibacterial activity against Klebsiella pneumoniae, Shigella sp., Micrococcus luteus, Escherichia coli and Salmonella typhi. From this study, it was found out that the activity of the complexes almost reaches the effectiveness of the conventional bacteriocide.

Synthesis and antibacterial activity of bis-[2-hydroxy-3-(1,7,8,9,10-pentamethyl-3,5-dioxo-4-aza-tricyclo[5.2.1.0(2,6)]dec-8-en-4-yloxy)-propyl]-dimethyl-ammonium chloride.

Science.gov (United States)

Struga, Marta; Kossakowski, Jerzy; Stefańska, Joanna; Zimniak, Andrzej; Koziol, Anna E

2008-06-01

A new quaternary ammonium compound, bis-[2-hydroxy-3-(1,7,8,9,10-pentamethyl-3,5-dioxo-4-aza-tricyclo[5.2.1.0(2,6)]dec-8-en-4-yloxy)-propyl]-dimethyl-ammonium chloride (4), was synthesized. The compound was investigated for antibacterial activity, including Gram-positive cocci and Gram-negative rods, and antifungal activity. Compound 4 showed significant inhibition against Staphylococcus aureus. Research was carried out over 4 standard strains and 40 hospital strains. Elementary analysis and/or MS, (1)H NMR and (13)C NMR spectra confirmed the identity of the products. The molecular structure of 3 was determined by an X-ray analysis.

Heteroleptic complexes of Zn(II) based on 1-(5-bromo-2-hydroxybenzylidene)-4-phenylthiosemicarbazide: Synthesis, structural characterization, theoretical studies and antibacterial activity

Science.gov (United States)

Azarkish, Mohammad; Akbari, Alireza; Sedaghat, Tahereh; Simpson, Jim

2017-04-01

Four new ternary complexes, [ZnL (2,2‧-bipy)] (1), Zn2L2(4,4‧-bipy)] (2), [ZnL(Imd)]·H2O (3) and [ZnL3(MeImd)] (4), have been synthesized from the reaction of Zn(II) acetate with 1-(5-bromo-2-hydroxybenzylidene)-4-phenylthiosemicarbazide (H2L) in the presence of a heterocyclic base, 2,2‧-bipyridine, 4,4‧-bipyridine, imidazole or 2-methylimidazole, as an auxiliary ligand. The complexes have been investigated by elemental analysis and FT-IR, UV-Vis and 1HNMR spectroscopy. These data show that the thiosemicarbazone acts as a tridentate dianionic ligand and coordinates via the thiol group, imine nitrogen, and phenolic oxygen. The coordination sphere was completed by the nitrogen atom(s) of the secondary ligand. The structure of 1 was also confirmed by X-ray crystallography and shown to be a five coordinate complex with coordination geometry between the square-pyramidal and trigonal-bipyramidal. Density functional theory (DFT) calculations including geometry optimization, vibrational frequencies and electronic absorptions have been performed for 1 with the B3LYP functional at the TZP(6-311G*) basis set using the Gaussian 03 or ADF 2009 packages. The optimization calculation showed that the crystallographically determined geometry parameters can be reproduced with that basis set. Experimental IR frequencies and calculated vibration frequencies also support each other. The in vitro antibacterial activities of the ligand and complexes have been evaluated against Gram-positive (B. subtilis and S. aureus) and Gram-negative (P. aeruginosa) bacteria and compared with the standard antibacterial drugs. The results reveal that all of the complexes show much better activity in comparison to the individual thiosemoicarbazone ligand (H2L), against all bacterial strains used, with complex 3 showing the most promising results.

Complexation of trichlorosalicylic acids by alkaline and first row transition metals as a switch for their antibacterial activity

KAUST Repository

Kumar, Vijay; Chawla, Mohit; Cavallo, Luigi; Basit Wani, Abdul; Manhas, Anu; Kaur, Sukhmanpreet; Poater, Albert; Chadar, Hemlata; NirajUpadhyay

2017-01-01

3,5,6-trichlorosalicylic acid (TCSA) does not show a good antibacterial activity. In contrast, here metal complexes with TCSA have shown better antibacterial activity for selected bacterial strains with a good degree of selectivity. Amongst

Synthesis and Electroluminescent Properties of Bis(3H-1,2,3-triazolo-[4,5-b]pyridine-3-olzinc Zn(TAP2

Directory of Open Access Journals (Sweden)

Trinh Dac Hoanh

2012-01-01

Full Text Available A new light-emissive material, bis(3H-1,2,3-triazolo-[4,5-b]pyridine-3-olzinc (Zn(TAP2, has been synthesized and characterized by FT-NMR, FT-IR, UV-Vis, and elemental analysis. The photoluminescence (PL of Zn(TAP2 was measured from the DMF solution at 460 nm. The HOMO (6.5 eV and LUMO (2.8 eV energy levels of Zn(TAP2 were estimated from the measurement of cyclic voltammetry. The devices with structures of ITO/NPB/Zn(TAP2/LiF/Al and ITO/NPB/Zn(TAP2/Alq3/LiF/Al were constructed to investigate their electroluminescent (EL performance. Zn (TAP2 is supposed to be a good emitting material in the EL device.

Field induced 4f5d [Re(salen)]2O3[Dy(hfac)3(H2O)]2 single molecule magnet.

Science.gov (United States)

Pointillart, Fabrice; Bernot, K; Sessoli, R; Gatteschi, D

2010-05-03

The reaction between the mononuclear [ReO(salen)(OMe)] (salen(2-) = N,N'-ethan-1,2-diylbis(salicylidenamine) dianion) and Dy(hfac)(3).2H(2)O (hfac(-) = 1,1,1,5,5,5-hexafluoroacetylacetonate anion) complexes lead to the formation of a compound with the formula {[Re(salen)](2)O(3)[Dy(hfac)(3)(H(2)O)](2)}(CHCl(3))(2)(CH(2)Cl(2))(2) noted (Dy(2)Re(2)). This compound has been characterized by single crystal and powder X-ray diffraction and has been found isostructural to the Y(III) derivative (Y(2)Re(2)) that we previously reported. The cyclic voltammetry demonstrates the redox activity of the system. The characterization of both static and dynamic magnetic properties is reported. Static magnetic data has been analyzed after the cancellation of the crystal field contribution by two different methods. Weak ferromagnetic exchange interactions between the Dy(III) ions are highlighted. The compound Dy(2)Re(2) displays slow relaxation of the magnetization when an external magnetic field is applied. Alternating current susceptibility shows a thermally activated behavior with pre-exponential factors of 7.13 (+/-0.10) x 10(-6) and 5.76 (+/-0.27) x 10(-7) s, and energy barriers of 4.19 (+/-0.02) and 8.52 (+/-0.55) K respectively for low and high temperature regimes.

A simple and highly selective ‘turn-on’ type fluorescence chemodosimeter for Hg2+ based on 1-(2-phenyl-2H-[1,2,3]triazole-4-carbonyl)thiosemicarbazide

International Nuclear Information System (INIS)

Lin, Hui; Shi, Wei; Tian, Yong; Ma, Fudong; Xu, Linxian; Ma, Junchi; Hui, Yonghai; Xie, Zhengfeng

2015-01-01

1-(2-phenyl-2H-[1,2,3]triazole-4-carbonyl)-4- (4-methylphenyl)thiosemicarbazide (M1) has been synthesized and investigated as a fluorescence chemodosimeter for Hg 2+ in dimethylsulfoxide. Highly selective ‘turn-on’ fluorescence alterations of M1 were observed upon the addition of Hg 2+ . Detection limit of Hg 2+ by M1 reaches ~3.7×10 −8 mol/L (evaluated by 3σ criteria).The coexistent metal ions rendered no obvious interference toward the optical response of M1 for Hg 2+ .The mechanism of M1 for the recognition of Hg 2+ has been investigated by FT-IR, 1 H NMR and MS analyses. - Highlights: • A type of thiosemicarbazide-derivatived compound (M1) was synthesized. • The fluorescence of M1 displayed highly selective ‘turn-on’ type fluorescence alteration with the presence of Hg 2+ . • Detection limit of ~3.7×10 −8 M for Hg 2+ can be obtained by this probing system. • Hg 2+ -induced intramolecular desulfurization and cyclization process of thiosemicarbazide moieties is the plausible probing mechanism

New coordination polymers from 1D chain, 2D layer to 3D framework constructed from 1,2-phenylenediacetic acid and 1,3-bis(4-pyridyl)propane flexible ligands

Science.gov (United States)

Xin, Ling-Yun; Liu, Guang-Zhen; Wang, Li-Ya

2011-06-01

The hydrothermal reactions of Cd, Zn, or Cu(II) acetate salts with H 2PHDA and BPP flexible ligands afford three new coordination polymers, including [Cd(PHDA)(BPP)(H 2O)] n(1), [Zn(PHDA)(BPP)] n(2), and [Cu 2(PHDA) 2(BPP)] n(3) (H 2PHDA=1,2-phenylenediacetic acid, BPP=1,3-bis(4-pyridyl)propane). The single-crystal X-ray diffractions reveal that all three complexes feature various metal carboxylate subunits extended further by the BPP ligands to form a diverse range of structures, displaying a remarked structural sensitivity to metal(II) cation. Complex 1 containing PHDA-bridged binuclear cadmium generates 1D double-stranded chain, complex 2 results in 2D→2D interpenetrated (4,4) grids, and complex 3 displays a 3D self-penetrated framework with 4 86 68 rob topology. In addition, fluorescent analyses show that both 1 and 2 exhibit intense blue-violet photoluminescence in the solid state.

Formation, stability and structural characterization of ternary MgUO{sub 2}(CO{sub 3}){sub 3}{sup 2-} and Mg{sub 2}UO{sub 2}(CO{sub 3}){sub 3}(aq) complexes

Energy Technology Data Exchange (ETDEWEB)

Lee, Jun-Yeop; Yun, Jong-Il [KAIST, Daejeon (Korea, Republic of). Dept. of Nuclear and Quantum Engineering; Vespa, Marika; Gaona, Xavier; Dardenne, Kathy; Rothe, Joerg; Rabung, Thomas; Altmaier, Marcus [Karlsruhe Institute of Technology, Karlsruhe (Germany). Inst. for Nuclear Waste Disposal

2017-06-01

The formation of ternary Mg-UO{sub 2}-CO{sub 3} complexes under weakly alkaline pH conditions was investigated by time-resolved laser fluorescence spectroscopy (TRLFS) and extended X-ray absorption fine structure (EXAFS) and compared to Ca-UO{sub 2}-CO{sub 3} complexes. The presence of two different Mg-UO{sub 2}-C{sub 3} complexes was identified by means of two distinct fluorescence lifetimes of 17±2 ns and 51±2 ns derived from the multi-exponential decay of the fluorescence signal. Slope analysis in terms of fluorescence intensity coupled with fluorescence intensity factor as a function of log [Mg(II)] was conducted for the identification of the Mg-UO{sub 2}-CO{sub 3} complexes forming. For the first time, the formation of both MgUO{sub 2}(CO{sub 3}){sub 3}{sup 2-} and Mg{sub 2}UO{sub 2}(CO{sub 3}){sub 3}(aq) species was confirmed and the corresponding equilibrium constants were determined as log β {sub 113}=25.8±0.3 and β {sub 213}=27.1±0.6, respectively. Complementarily, fundamental structural information for both Ca-UO{sub 2}-CO{sub 3} and Mg-UO{sub 2}-CO{sub 3} complexes was gained by extended EXAFS revealing very similar structures between these two species, except for the clearly shorter U-Mg distance (3.83 Aa) compared with U-Ca distance (4.15 Aa). These results confirmed the inner-sphere character of the Ca/Mg-UO{sub 2}-CO{sub 3} complexes. The formation constants determined for MgUO{sub 2}(CO{sub 3}){sub 3}{sup 2-} and Mg{sub 2}UO{sub 2}(CO{sub 3}){sub 3}(aq) species indicate that ternary Mg-UO{sub 2}-CO{sub 3} complexes contribute to the relevant uranium species in carbonate saturated solutions under neutral to weakly alkaline pH conditions in the presence of Mg(II) ions, which will induce notable influences on the U(VI) chemical species under seawater conditions.

Fragrance material review on 1-(3,3-dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one.

Science.gov (United States)

Scognamiglio, J; Letizia, C S; Api, A M

2013-12-01

A toxicologic and dermatologic review of 1-(3,3-dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one when used as a fragrance ingredient is presented. 1-(3,3-Dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-(3,3-dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one were evaluated then summarized and includes physical properties, skin irritation, mucous membrane (eye) irritation, and skin sensitization data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones When Used as Fragrance Ingredients (submitted for publication) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

Electrodeposition of Fe{sub 2}O{sub 3} nanoparticles and its supercapacitive properties

Energy Technology Data Exchange (ETDEWEB)

Kadam, S. L., E-mail: snehal.kadam54@gmail.com; Padwal, P. M., E-mail: pal-soni279@yahoo.com; Mane, S. M., E-mail: manesagar99@gmail.com; Kulkarni, S. B., E-mail: sbk-physics@yahoo.com [Department of Physics, The Institute of Science, Madam Cama Road, Mumbai-400032 (India)

2016-04-13

Fe{sub 2}O{sub 3} metal oxide nanoparticles are synthesized by electrodeposition method on stainless steel substrate. The crystal structure and surface morphological studies of the obtained metal oxide thin film are carried out by using X-ray diffraction (XRD) technique and Scanning Electron Microscopy (SEM) respectively. The electrochemical properties of Fe{sub 2}O{sub 3} thin film like Cyclic Voltammetry (CV), Galvonostatic Charge-Discharge (GCD) and Electrochemical Impedance Spectroscopy (EIS) are studied in a bath of 0.5 M Na{sub 2}SO{sub 4} as electrolyte. The observed specific capacitance shows improved values 135 Fg{sup −1} at 5 mVs{sup −1} scan rate. The electrochemical stability of Fe{sub 2}O{sub 3} electrode is investigated using cyclic voltammetry for 1000 cycles at a scan rate 50 mVs{sup −1}. The Fe{sub 2}O{sub 3} electrode exhibits superior cycling stability with only 4-5% capacitance loss after one thousand cycles. The values of specific power and specific energy of Fe{sub 2}O{sub 3} electrode obtained from Galvonostatic charge discharge studies are 2250 W.kg{sup −1} and 63.15 Wh.kg{sup −1} respectively at current density 1 A/g. From all the electrochemical properties of Fe{sub 2}O{sub 3} electrode, it indicates that it will be promising electrode material for supercapacitor application.

Dioxouranium(VI) complexes with benzimidazole and benzoxazole derivatives

International Nuclear Information System (INIS)

Mansingh, P.S.; Dash, K.C.

1995-01-01

UO 2 LηX 2 [X = NO 3 ,NCS and 0.5 SO 4 and when n = 2, L = 2-(2-hydroxyphyenyl) benzimidazole (HPBI) or 2-(2-aminophenyl) benzimidazole(APBI) and for n=1, L = 2-(2-pyridyl) benzoxazole (PBO)] were synthesized and characterized by several physico chemical techniques including molar conductance data, IR, 1 H and 13 C NMR and thermogravimetric analysis. (author). 5 refs

Synthesis and fluorescence of new 3-biphenylpyrrolo[1,2-c]pyrimidines

Directory of Open Access Journals (Sweden)

Marian-Laurentiu Tatu

2017-07-01

Full Text Available New pyrrolo[1,2-c]pyrimidines derivates having a biphenyl moiety at position 3 have been synthesized by 1,3-dipolar cycloaddition of their corresponding N-ylides with activated alkynes. FTIR, 1H and 13C NMR spectroscopy and elemental analysis have been used to characterize the structures of the new nine pyrrolo[1,2-c]pyrimidine derivates. Absorption and fluorescence spectra have been recorded. The appropriate solvent for the photoluminescence properties of the studied compounds has been found to be chloroform:acetonitrile mixture (1:1. The main spectral features such as molar extinction coefficients (ε, Stokes shifts, quantum yields using quinine sulphate as standard, fluorescence quenching in the presence of benzoquinone and Stern-Volmer constants have been calculated. The substituent effects on intensity of absorption, maximum absorbance wavelengths and fluorescence parameters have been discussed. The highest quantum yield value was found for ethyl 3-(4-biphenylyl-7-(3,4-dimethoxybenzoylpyrrolo[1,2-c]pyrimidine-5-carboxylate (0.55. The obtained results suggest that the studied compounds are promising candidates for future study in order to evaluate their use in practical applications in fluorescent chemical sensors.

trans-Methylpyridine cyclen versus cross-bridged trans-methylpyridine cyclen. Synthesis, acid-base and metal complexation studies (metal = Co2+, Cu2+, and Zn2+).

Science.gov (United States)

Bernier, Nicolas; Costa, Judite; Delgado, Rita; Félix, Vítor; Royal, Guy; Tripier, Raphaël

2011-05-07

The synthesis of the cross-bridged cyclen CRpy(2) {4,10-bis((pyridin-2-yl)methyl)-1,4,7,10-tetraazabicyclo[5.5.2]tetradecane}, a constrained analogue of the previously described trans-methylpyridine cyclen Cpy(2) is reported. The additional ethylene bridge confers to CRpy(2) proton-sponge type behaviour which was explored by NMR and potentiometric studies. Transition metal complexes have been synthesized (by complexation of both ligands with Co(2+), Cu(2+) and Zn(2+)) and characterized in solution and in the solid state. The single crystal X-ray structures of [CoCpy(2)](2+), [CuCpy(2)](2+) and [ZnCpy(2)](2+) complexes were determined. Stability constants of the complexes, including those of the cross-bridged derivative, were determined using potentiometric titration data and the kinetic inertness of the [CuCRpy(2)](2+) complex in an acidic medium (half-life values) was evaluated by spectrophotometry. The pre-organized structure of the cross-bridged ligand imposes an additional strain for the complexation leading to complexes with smaller thermodynamic stability in comparison with the related non-bridged ligand. The electrochemical study involving cyclic voltammetry underlines the importance of the ethylene cross-bridge on the redox properties of the transition metal complexes.

Biosynthesis of cyclic 2,3-diphosphoglycerate. Isolation and characterization of 2-phosphoglycerate kinase and cyclic 2,3-diphosphoglycerate synthetase from Methanothermus fervidus.

Science.gov (United States)

Lehmacher, A; Vogt, A B; Hensel, R

1990-10-15

Starting from 2-phosphoglycerate the biosynthesis of cDPG comprises two steps: (i) the phosphorylation of 2-phosphoglycerate to 2,3-diphosphoglycerate and (ii) the intramolecular cyclization to cyclic 2,3-diphosphoglycerate. The involved enzymes, 2-phosphoglycerate kinase and cyclic 2,3-diphosphoglycerate synthetase, were purified form Methanothermus fervidus. Their molecular and catalytic properties were characterized.

Quantitative roughness characterization and 3D reconstruction of electrode surface using cyclic voltammetry and SEM image

Energy Technology Data Exchange (ETDEWEB)

Dhillon, Shweta; Kant, Rama, E-mail: rkant@chemistry.du.ac.in

2013-10-01

Area measurements from cyclic voltammetry (CV) and image from scanning electron microscopy (SEM) are used to characterize electrode statistical morphology, 3D surface reconstruction and its electroactivity. SEM images of single phased materials correspond to two-dimensional (2D) projections of 3D structures, leading to an incomplete characterization. Lack of third dimension information in SEM image is circumvented using equivalence between denoised SEM image and CV area measurements. This CV-SEM method can be used to estimate power spectral density (PSD), width, gradient, finite fractal nature of roughness and local morphology of the electrode. We show that the surface morphological statistical property like distribution function of gradient can be related to local electro-activity. Electrode surface gradient micrographs generated here can provide map of electro-activity sites. Finally, the densely and uniformly packed small gradient over the Pt-surface is the determining criterion for high intrinsic electrode activity.

Quantitative roughness characterization and 3D reconstruction of electrode surface using cyclic voltammetry and SEM image

International Nuclear Information System (INIS)

Dhillon, Shweta; Kant, Rama

2013-01-01

Area measurements from cyclic voltammetry (CV) and image from scanning electron microscopy (SEM) are used to characterize electrode statistical morphology, 3D surface reconstruction and its electroactivity. SEM images of single phased materials correspond to two-dimensional (2D) projections of 3D structures, leading to an incomplete characterization. Lack of third dimension information in SEM image is circumvented using equivalence between denoised SEM image and CV area measurements. This CV-SEM method can be used to estimate power spectral density (PSD), width, gradient, finite fractal nature of roughness and local morphology of the electrode. We show that the surface morphological statistical property like distribution function of gradient can be related to local electro-activity. Electrode surface gradient micrographs generated here can provide map of electro-activity sites. Finally, the densely and uniformly packed small gradient over the Pt-surface is the determining criterion for high intrinsic electrode activity.

Fluorescence tuning of 2-(1H-Benzimidazol-2-yl)phenol-ESIPT process

International Nuclear Information System (INIS)

Prakash, S.M.; Jayamoorthy, K.; Srinivasan, N.; Dhanalekshmi, K.I.

2016-01-01

Catalytic synthesis of potential chemosensor 2-(1H-Benzimidazol-2-yl)phenol (HBYP) has been prepared by three components cyclization reaction. It can behaves as a selective fluorescent sensor for the detection of Fe 3+ metal ion. HBYP has been characterized by 1 H NMR, 13 C NMR, mass spectral studies and elemental analysis. Single crystal XRD analysis has been carried out to confirm the structure of HBYP and it shows the imidazole ring is essentially planar and monoclinic crystal. Addition and increasing concentration of Fe 3+ ions into HBYP results dramatic fluorescence quenching. Other cations, including Ca 2+ , Co 2+ , Ni 2+ , Cd 2+ , Pb 2+ , Zn 2+ and Mg 2+ had little influence in the fluorescence intensity. Surprisingly reversible fluorescence enhancement has been observed with the addition of H 3 PO 4 due to the deactivation of iron complex.

S-Alkylated/aralkylated 2-(1H-indol-3-yl-methyl)-1,3,4- oxadiazole-5 ...

African Journals Online (AJOL)

Purpose: To evaluate the antibacterial, enzyme-inhibitory and hemolytic activities of Salkylated/aralkylated 2-(1H-indol-3-ylmethyl)-1,3,4-oxadiazole-5-thiol derivatives. Methods: Antibacterial activities of the compounds were evaluated using broth dilution method in 96 well plates. Enzyme inhibitory activities assays were ...

1,3-dialkyl- and 1,3-diaryl-3,4,5,6-tetrahydropyrimidin-2-ylidene rhodium(i) and palladium(II) complexes: synthesis, structure, and reactivity.

Science.gov (United States)

Mayr, Monika; Wurst, Klaus; Ongania, Karl-Hans; Buchmeiser, Michael R

2004-03-05

The synthesis of novel 1,3-diaryl- and 1,3-dialkylpyrimidin-2-ylidene-based N-heterocyclic carbenes (NHCs) and their rhodium(i) and palladium(II) complexes is described. The rhodium compounds bromo(cod)[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene]rhodium (7), bromo(cod)(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)rhodium (8) (cod=eta(4)-1,5-cyclooctadiene, mesityl=2,4,6-trimethylphenyl), chloro(cod)(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)rhodium (9), and chloro(cod)[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene]rhodium (10) were prepared by reaction of [[Rh(cod)Cl](2)] with lithium tert-butoxide followed by addition of 1,3-dimesityl-3,4,5,6-tetrahydropyrimidinium bromide (3), 1,3-dimesityl-3,4,5,6-tetrahydropyrimidinium tetrafluoroborate (4), 1,3-di-2-propyl-3,4,5,6-tetrahydropyrimidinium bromide (6), and 1,3-di-2-propyl-3,4,5,6-tetrahydropyrimidinium tetrafluoroborate, respectively. Complex 7 crystallizes in the monoclinic space group P2(1)/n, and 8 in the monoclinic space group P2(1). Complexes 9 and 10 were used for the synthesis of the corresponding dicarbonyl complexes dicarbonylchloro(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)rhodium (11), and dicarbonylchloro[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene]rhodium (12). The wavenumbers nu(CO I)/nu(CO II) for 11 and 12 were used as a quantitative measure for the basicity of the NHC ligand. The values of 2062/1976 and 2063/1982 cm(-1), respectively, indicate that the new NHCs are among the most basic cyclic ligands reported so far. Compounds 3 and 6 were additionally converted to the corresponding cationic silver(i) bis-NHC complexes [Ag(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)(2)]AgBr(2) (13) and [Ag[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene](2)]AgBr(2) (14), which were subsequently used in transmetalation reactions for the synthesis of the corresponding palladium(II) complexes Pd(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2

Synthesis, Spectroscopic Characterization and Biological Activities of Transition Metal Complexes Derived from a Tridentate Schiff Base

Directory of Open Access Journals (Sweden)

J. Senthil Kumaran

2013-01-01

Full Text Available A new series of Cu (II, Ni (II, Co (II and Zn (II complexes have been synthesized from the Schiff base derived from 4-hydroxy-3-methoxybenzylidine-4-aminoantipyrine and 2-aminophenol. The structural features have been determined from their elemental analysis, magnetic susceptibility, molar conductance, Mass, IR, UV-Vis, 1H-NMR, 13C-NMR and ESR spectral studies. The redox behavior of the copper complex has been studied by cyclic voltammetry. The data confirm that the complexes have composition of ML2 type. The electronic absorption spectral data of the complexes propose an octahedral geometry around the central metal ion. All the metal complexes with DNA structure were guided by the presence of inter-molecular C–H⋯O and C–H⋯N hydrogen bonds. The biological activity of the synthesized compounds were tested against the bacterial species such as Bacillus subtilis, Staphylococcus aureus, Proteus vulgaris and fungal species such as Candida albicans by the well-diffusion method.

A new rhodamine-based fluorescent probe for the discrimination of Fe{sup 3+} from Fe{sup 2+}

Energy Technology Data Exchange (ETDEWEB)

You, Qi Hua; Huang, Hua Bin; Zhuang, Zhi Xia; Wang, Xiao Ru [Dept. of Science and Technology for Inspection, Xiamen Huaxia University, Xiamen (China); Chan, Wing Hong [Dept. of of Chemistry, Hong Kong Bap tist University, Hong Kong (China)

2016-11-15

A new rhodamine-based fluorescent probe for the discrimination of Fe{sup 3+} from Fe{sup 2+} has been designed and investigated. The probe shows an immediate visual color change in response to Fe{sup 3+} and Cu{sup 2+}, while only Fe{sup 3+} triggers the fluorescent change of the probe. The existence of large amount of other metal ions shows negligible interference in the detection of Fe{sup 3+}. The association constant K{sub ass} of 4.64 × 10{sup 8} M{sup -2} (R{sup 2} = 0.994) and 5.38 × 10{sup 8} M{sup -2} (R{sup 2} = 0.991) of the complex was derived from UV/Vis and fluorescence titration assuming 1:2 stoichiometry of probe–Fe{sup 3+} complex, respectively.

Benzoxazole derivatives suppress lipopolysaccharide-induced mast cell activation.

Science.gov (United States)

Cho, Kyung-Ah; Park, Minhwa; Kim, Yu-Hee; Choo, Hea-Young Park; Lee, Kyung Ho

2018-05-01

Mast cells are central regulators of allergic inflammation that function by releasing various proallergic inflammatory mediators, including histamine, eicosanoids and proinflammatory cytokines. Occasionally, bacterial infections may initiate or worsen allergic inflammation. A number of studies have indicated that activation of lipoxygenase in mast cells positive regulates allergic inflammatory responses by generating leukotrienes and proinflammatory cytokines. In the present study, the effects of benzoxazole derivatives on the lipopolysaccharide (LPS)‑induced expression of proinflammatory cytokines, production of histamine and surface expression of co‑stimulatory molecules on bone marrow-derived mast cells (BMMCs) were studied. The benzoxazole derivatives significantly reduced the expression of interleukin (IL)‑1β, IL‑6, IL‑13, tumor necrosis factor‑α, perilipin (PLIN) 2, and PLIN3 in BMMCs treated with LPS. Furthermore, histamine production was suppressed in BMMCs treated with LPS, or treated with phorbol-12-myristate-13-acetate/ionomycin. Benzoxazole derivatives marginally affected the surface expression of cluster of differentiation (CD)80 and CD86 on BMMCs in the presence of LPS, although LPS alone did not increase the expression of those proteins. Therefore, benzoxazole derivatives inhibited the secretion of proinflammatory cytokines in mast cells and may be potential candidate anti‑allergic agents to suppress mast cell activation.

Steady state oxygen reduction and cyclic voltammetry

DEFF Research Database (Denmark)

Rossmeisl, Jan; Karlberg, Gustav; Jaramillo, Thomas

2008-01-01

The catalytic activity of Pt and Pt3Ni for the oxygen reduction reaction is investigated by applying a Sabatier model based on density functional calculations. We investigate the role of adsorbed OH on the activity, by comparing cyclic voltammetry obtained from theory with previously published ex...

Fragrance material review on 4-phenyl-3-buten-2-ol.

Science.gov (United States)

Scognamiglio, J; Letizia, C S; Api, A M

2012-09-01

A toxicologic and dermatologic review of 4-phenyl-3-buten-2-ol when used as a fragrance ingredient is presented. 4-Phenyl-3-buten-2-ol is a member of the fragrance structural group Aryl Alkyl Alcohols and is a secondary alcohol. The AAAs are a structurally diverse class of fragrance ingredients that includes primary, secondary, and tertiary alkyl alcohols covalently bonded to an aryl (Ar) group, which may be either a substituted or unsubstituted benzene ring. The common structural element for the AAA fragrance ingredients is an alcohol group -C-(R1)(R2)OH and generically the AAA fragrances can be represented as an Ar-C-(R1)(R2)OH or Ar-Alkyl-C-(R1)(R2)OH group. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 4-phenyl-3-buten-2-ol were evaluated then summarized and includes physical properties, and genotoxicity data. A safety assessment of the entire Aryl Alkyl Alcohols will be published simultaneously with this document; please refer to Belsito et al. (2012) for an overall assessment of the safe use of this material and all Aryl Alkyl Alcohols in fragrances. Copyright © 2011 Elsevier Ltd. All rights reserved.

Fragrance material review on 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one.

Science.gov (United States)

Scognamiglio, J; Letizia, C S; Api, A M

2013-12-01

A toxicologic and dermatologic review of 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one when used as a fragrance ingredient is presented. 3-Methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one were evaluated then summarized and includes physical properties, acute toxicity, skin irritation, mucous membrane (eye) irritation, sensitization, phototoxicity, photoallergy, and genotoxicity data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones when used as fragrance ingredients. Submitted for publication) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis, crystal structure, fluorescent and antioxidation properties of cerium(III) and europium(III) complexes with bis(3-methoxysalicylidene)-3-oxapentane-1,5-diamine

Energy Technology Data Exchange (ETDEWEB)

Tang, Xia; Shi, Xinkui; Xu, Yuling; Shen, Kesheng; Mao, Shanshan; Wu, Huilu [School of Chemical and Biological Engineering, Lanzhou Jiaotong University, Gansu (China)

2017-03-02

Two aliphatic ether Schiff base lanthanide complexes (Ln = Eu, Ce) with bis(3-methoxysalicylidene)-3-oxapentane-1,5-diamine (Bod), were synthesized and characterized by physicochemical and spectroscopic methods. [Eu(Bod)(NO{sub 3}){sub 3}] (1) is a discrete mononuclear species and [Ce(Bod)(NO{sub 3}){sub 3}DMF]{sub ∞} (2) exhibits an inorganic coordination polymer. In the two complexes, the metal ions both are ten-coordinated and the geometric structure around the Ln{sup III} atom can be described as distorted hexadecahedron. Under excitation at room temperature, the red shift in the fluorescence band of the ligand in the complexes compared with that of the free ligand can be attributed to coordination of the rare earth ions to the ligand. Moreover, the antioxidant activities of the two complexes were investigated. The results demonstrated that the complexes have better scavenging activity than both the ligand and the usual antioxidants on the hydroxyl and superoxide radicals. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Crystal structure of dichlorido{2-methyl-2-[(pyridin-2-ylmethylamino]propan-1-ol-κ3N,N′,O}copper(II from synchrotron data

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Jong Won Shin

2016-10-01

Full Text Available The title compound, [CuCl2(C10H16N2O], has been synthesized and characterized by synchrotron single-crystal X-ray diffraction and FT–IR spectroscopy. The 2-methyl-2-[(pyridin-2-ylmethylamino]propan-1-ol (mpmapOH ligand, including pyridine, amine and hydroxy groups, was synthesized by the reaction of 2-amino-2-methylpropan-1-ol with pyridine-2-carbaldehyde and was characterized by NMR spectroscopy. In its CuII complex, the metal ion has a distorted square-pyramidal coordination geometry with two N and one O atom of the mpmapOH ligand and one chloride anion in the equatorial plane, and the second chloride in an axial position. The bond lengths involving the CuII ion range from 1.9881 (10 to 2.0409 (9 for the Cu—N and Cu—O bonds, and from 2.2448 (5 to 2.5014 (6 Å for the equatorial and axial Cu—Cl bonds, respectively. Intermolecular hydrogen bonds (N—H...Cl and O—H...Cl and face-to-face π–π interactions stabilize the molecular structure and give rise to a two-dimensional supramolecular structure extending parallel to (101.

Syntheses, structures, and physicochemical properties of diruthenium compounds of tetrachlorocatecholate with metal-metal bonded Ru(3+)(mu-OR)(2)Ru(3+) and Ru(3.5+)(mu-OR)(2)Ru(3.5+) cores (R = CH(3) and C(2)H(5)).

Science.gov (United States)

Miyasaka, H; Chang, H C; Mochizuki, K; Kitagawa, S

2001-07-02

) A for 4 and 5, respectively). These structural features and magnetic and ESR data revealed the electronic configurations of sigma(2)pi(2)delta(2)delta(2)pi(2) and sigma(2)pi(2)delta(2)delta(2)pi(1) for Ru(3+)(mu-OR)(2)Ru(3+) and Ru(3.5+)(mu-OR)(2)Ru(3.5+), respectively, in which the former is diamagnetic and the latter is paramagnetic with S = (1)/(2) ground state. Compound 5 forms a one-dimensional chain with alternating arrangement of a Ru(3.5+)(mu-OMe)(2)Ru(3.5+) unit and a free benzo-15-crown-5-ether molecule by intermolecular hydrogen bonds (O(H(2)O).O(crown-ether) = 2.91-3.04 A). The cyclic voltammetry in DMF affords characteristic metal-origin voltammograms; two reversible and two quasi-reversible redox waves were observed. The feature of cyclic voltammograms for the Ru(3+)(mu-OR)(2)Ru(3+) species (2, 3, and 6) and the Ru(3.5+)(mu-OR)(2)Ru(3.5+) species (4 and 7) are similar to each other, indicating that both species are electrochemically stable. The isolation of the pyrazine-trans-coordinated species, [Ph(4)P][Ru(Cl(4)Cat)(2)(L)(2)] (L = pyrazine (8), 2,5-dimethylpyrazine (9)), revealed the selective isolation of 6 from pyrazine-containing solution. UV-vis spectral variation by ethanolysis for 9 demonstrated the selective conversion from the pyrazine-trans-coordinated species to the Ru(3+)(mu-OEt)(2)Ru(3+) species without an oxidation to the Ru(3.5+)(mu-OEt)(2)Ru(3.5+) species. This result suggests the presence of equilibrium between [Ru(Cl(4)Cat)(2)(L)(2)](-) and Ru(3+)(mu-OEt)(2)Ru(3+) species in the synthetic condition for 6.

(μ-3-Acetyl-5-carboxylato-4-methylpyrazolido-1:2κ4N2,O3:N1,O5-μ-chlorido-tetrapyridine-1κ2N,2κ2N-chlorido-1κCl-dicopper(II propan-2-ol solvate

Directory of Open Access Journals (Sweden)

Sergey Malinkin

2009-10-01

Full Text Available The title compound, [Cu2(C7H6N2O3Cl2(C5H5N4]·C3H8O, is a binuclear pyrazolate complex, in which the two CuII atoms have different coordination numbers and are connected by a bridging Cl atom. One CuII atom has a distorted square-pyramidal coordination environment formed by two pyridine N atoms, one bridging Cl atom and an N,O-chelating pyrazolate ligand. The other CuII atom adopts an octahedral geometry defined by two pyridine N atoms at the axial positions, two Cl atoms and the coordinated pyrazolate ligand in the equatorial plane. An O—H...O hydrogen bond connects the complex molecules and propan-2-ol solvent molecules into pairs. These pairs form columns along the a axis.

Complexation of trichlorosalicylic acids by alkaline and first row transition metals as a switch for their antibacterial activity

KAUST Repository

Kumar, Vijay

2017-09-14

3,5,6-trichlorosalicylic acid (TCSA) does not show a good antibacterial activity. In contrast, here metal complexes with TCSA have shown better antibacterial activity for selected bacterial strains with a good degree of selectivity. Amongst the eight synthesized essential metal complexes complexed with TCSA, Mn(II)-TCSA and Ni(II)-TCSA have been found to be more effective with MIC range 20-50 µg/L as compared to control (chloramphenicol). The activity of an individual complex against different microbes was not found to be identical, indicating the usage of an individual metal chelate against a targeted bacterial strain. Further, the protein (BSA) binding constant of TCSA and its metal complexes were determined and ordered as Ca(II)-TCSA > Cu(II)-TCSA > Mg(II)-TCSA >> Mn(II)-TCSA >> Zn(II)-TCSA >>> Ni(II)-TCSA >>> Co(II)-TCSA > Fe(II)-TCSA > TCSA. The present study has confirmed enhanced antibacterial activities and binding constants for metal chelates of TCSA as compared to free TCSA, which seems directly related with the antioxidant activities of these complexes. Further, bearing the ambiguity related to the structural characterization of the metal complexed with TCSA ligands, DFT calculations have been used as the tool to unravel the right environment around the metals, studying basically the relative stability of square planar and octahedral metal complexes with TCSA.

Characteristics of curcumin using cyclic voltammetry, UV–vis, fluorescence and thermogravimetric analysis

International Nuclear Information System (INIS)

Masek, Anna; Chrzescijanska, Ewa; Zaborski, Marian

2013-01-01

Highlights: • Electrooxidation of curcumin was investigated with cyclic voltammetry. • The curcumin is irreversibly oxidized at the platinum electrode in anhydrous media. • Absorbance, fluorescence and thermogravimetric analysis of curcumin was studied. • The HOMO and Mapped Electron Densities were calculated using HyperChem. • Oxidation mechanism for curcumin proposed. -- Abstract: Curcumin, the yellow, primary bioactive component of turmeric, has recently received attention from chemists due its wide range of potential biological applications as an antioxidant, anti-inflammatory, and anti-carcinogenic agent. The electrochemical behaviour of curcumin at a platinum electrode has been studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The oxidation of curcumin is an irreversible process that proceeds in two steps in 0.1 M (C 4 H 9 ) 4 NClO 4 in acetonitrile. The process of oxidation and its kinetics have been investigated. The rate constant, electron transfer coefficient and diffusion coefficients for the electrochemical oxidation of curcumin were determined. A mechanism for the oxidation of curcumin is proposed. The data obtained are consistent with the current literature and suggest that voltammetric studies on mechanically transferred solids may be a convenient method for elucidating the electrochemical oxidation mechanisms of compounds in anhydrous media. Theoretical calculations regarding the optimization of curcumin, electronic properties like highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) were calculated using with HyperChem software by AM1 semi-empirical method. The properties of curcumin in a homogeneous environment were investigated using spectroscopic techniques and thermogravimetric analysis

Synthesis and Antibacterial Activities of Novel 2,5-Diphenylindolo[2,3-e] Pyrazolo[1',5':3",4"]pyrimido[2",1"-c] [1,2,4]triazines

Directory of Open Access Journals (Sweden)

Mohamed G. Marei

2011-12-01

Full Text Available The formation of (E-3-{2-(2,5-diphenylpyrazolo[1,5-c]pyrimidin-7-ylhydrazono}indolin-2-ones 3 has been achieved by condensation of equimolar amounts of 7-hydrazino-2,5-diphenylpyrazolo[1,5-c]pyrimidine (1 and isatin (or isatin derivatives 2 at room temperature. The (E-products could be isomerized into corresponding the (Z-3 isomers. Reactions of the latter fused heterocyclic hydrazones towards different electro-philic reagents yielded the corresponding 3-substituted derivatives 4–7. Dehydrative cyclisation of the hydrazones 3 using phosphorus oxychloride afforded the 2,5-diphenyl- indolo[2,3-e]pyrazolo[1',5':3",4"]pyrimido[2",1"-c][1,2,4] triazines 13. The polyfused heterocyclic ring system 13 underwent electrophilic substitution reactions at position 4 rather than at position 3. The 3-bromo isomer of 17 was prepared by a sequence of reactions starting from 2,5-diphenylpyrazolo[1,5-c]pyrimidine-7(6H-thione (11. The orientation of the electrophilic attack was supported by spectroscopic and chemical evidence. Some of the synthesized compounds were found to possess slight to moderate activity against the microorganisms Bacillus subtilis, Micrococcus luteus, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa.

Enhancement of electrochemical performance of LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 by surface modification with MnO_2

International Nuclear Information System (INIS)

Guo, Xin; Cong, Li-Na; Zhao, Qin; Tai, Ling-Hua; Wu, Xing-Long; Zhang, Jing-Ping; Wang, Rong-Shun; Xie, Hai-Ming; Sun, Li-Qun

2015-01-01

LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 is successfully coated with MnO_2 by a chemical deposition method. The X-ray diffraction (XRD), scanning electron microscope (SEM) and high resolution transmission electron microscope (HRTEM) results demonstrate that MnO_2 forms a thin layer on the surface of LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 without destroying the crystal structure of the core material. Compared with pristine LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2, the MnO_2-coated sample shows enhanced electrochemical performance especially the rate capability. Even at a current density of 750 mA g"−"1, the discharge capacity of MnO_2-coated LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 is 155.15 mAh g"−"1, while that of the pristine electrode is only 132.84 mAh g"−"1 in the range of 2.5–4.5 V. The cyclic voltammetry (CV) and X-ray photoelectron spectroscopy (XPS) curves show that the MnO_2 coating layer reacts with Li"+ during cycling, which is responsible for the higher discharge capacity of MnO_2-coated LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2. Electrochemical impedance spectroscopy (EIS) results confirmed that the MnO_2 coating layer plays an important role in reducing the charge transfer resistance on the electrolyte–electrode interfaces. - Highlights: • MnO_2 coated LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 cathode material is synthesized for the first time. • MnO_2 offers available sites for insertion of extracted lithium. • The preserved surface and crystal structures results in the improved kinetics.

Heterospin systems constructed from [Cu2Ln]3+ and [Ni(mnt)2]1-,2- Tectons: First 3p-3d-4f complexes (mnt = maleonitriledithiolato).

Science.gov (United States)

Madalan, Augustin M; Avarvari, Narcis; Fourmigué, Marc; Clérac, Rodolphe; Chibotaru, Liviu F; Clima, Sergiu; Andruh, Marius

2008-02-04

New heterospin complexes have been obtained by combining the binuclear complexes [{Cu(H(2)O)L(1)}Ln(O(2)NO)(3)] or [{CuL(2)}Ln(O(2)NO)(3)] (L(1) = N,N'-propylene-di(3-methoxysalicylideneiminato); L(2) = N,N'-ethylene-di(3-methoxysalicylideneiminato); Ln = Gd(3+), Sm(3+), Tb(3+)), with the mononuclear [CuL(1)(2)] and the nickel dithiolene complexes [Ni(mnt)(2)](q)- (q = 1, 2; mnt = maleonitriledithiolate), as follows: (1)infinity[{CuL(1)}(2)Ln(O(2)NO){Ni(mnt)(2)}].Solv.CH(3)CN (Ln = Gd(3+), Solv = CH(3)OH (1), Ln = Sm(3+), Solv = CH(3)CN (2)) and [{(CH(3)OH)CuL(2)}(2)Sm(O(2)NO)][Ni(mnt)(2)] (3) with [Ni(mnt)2]2-, [{(CH(3)CN)CuL(1)}(2)Ln(H(2)O)][Ni(mnt)(2)]3.2CH(3)CN (Ln = Gd(3+) (4), Sm(3+) (5), Tb(3+) (6)), and [{(CH(3)OH)CuL(2)}{CuL(2)}Gd(O(2)NO){Ni(mnt)(2)}][Ni(mnt)(2)].CH(2)Cl(2) (7) with [Ni(mnt))(2]*-. Trinuclear, almost linear, [CuLnCu] motifs are found in all the compounds. In the isostructural 1 and 2, two trans cyano groups from a [Ni(mnt)2]2- unit bridge two trimetallic nodes through axial coordination to the Cu centers, thus leading to the establishment of infinite chains. 3 is an ionic compound, containing discrete [{(CH(3)OH)CuL(2)}(2)Sm(O(2)NO)](2+) cations and [Ni(mnt)(2)](2-) anions. Within the series 4-6, layers of discrete [CuLnCu](3+) motifs alternate with stacks of interacting [Ni(mnt)(2)](*-) radical anions, for which two overlap modes, providing two different types of stacks, can be disclosed. The strength of the intermolecular interactions between the open-shell species is estimated through extended Hückel calculations. In compound 7, [Ni(mnt)(2)](*-) radical anions coordinate group one of the Cu centers of a trinuclear [Cu(2)Gd] motif through a CN, while discrete [Ni(mnt)(2)](*-) units are also present, overlapping in between, but also with the coordinated ones. Furthermore, the [Cu(2)Gd] moieties dimerize each other upon linkage by two nitrato groups, both acting as chelate toward the gadolinium ion from one unit and monodentate toward a

Crystal structures and catalytic performance of three new methoxy substituted salen type nickel(II) Schiff base complexes derived from meso-1,2-diphenyl-1,2-ethylenediamine

Science.gov (United States)

Ghaffari, Abolfazl; Behzad, Mahdi; Pooyan, Mahsa; Amiri Rudbari, Hadi; Bruno, Giuseppe

2014-04-01

Three new nickel(II) complexes of a series of methoxy substituted salen type Schiff base ligands were synthesized and characterized by IR, UV-Vis and 1H NMR spectroscopy and elemental analysis. The ligands were synthesized from the condensation of meso-1,2-diphenyl-1,2-ethylenediamine with n-methoxysalicylaldehyde (n = 3, 4 and 5). Crystal structures of these complexes were determined. Electrochemical behavior of the complexes was studied by means of cyclic voltammetry in DMSO solutions. Catalytic performance of the complexes was studied in the epoxidation of cyclooctene using tert-butylhydroperoxide (TBHP) as oxidant under various conditions to find the optimum operating parameters. Low catalytic activity with moderate epoxide selectivity was observed in in-solvent conditions but in the solvent-free conditions, enhanced catalytic activity with high epoxide selectivity was achieved.

2-(2-Oxo-1,4-dihydro-2H-quinazolin-3-yl)- and 2-(2,2-dioxo-1,4-dihydro-2H-2lambda6-benzo[1,2,6]thiadiazin-3-yl)-N-hydroxy-acetamides as potent and selective peptide deformylase inhibitors.

Science.gov (United States)

Apfel, C; Banner, D W; Bur, D; Dietz, M; Hubschwerlen, C; Locher, H; Marlin, F; Masciadri, R; Pirson, W; Stalder, H

2001-06-07

Potent, selective, and structurally new inhibitors of the Fe(II) enzyme Escherichia coli peptide deformylase (PDF) were obtained by rational optimization of the weakly binding screening hit (5-chloro-2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-acetic acid hydrazide (1). Three-dimensional structural information, gathered from Ni-PDF complexed with 1, suggested the preparation of two series of related hydroxamic acid analogues, 2-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-N-hydroxy-acetamides (A) and 2-(2,2-dioxo-1,4-dihydro-2H-2lambda(6)-benzo[1,2,6]thiadiazin-3-yl)-N-hydroxy-acetamides (B), among which potent PDF inhibitors (37, 42, and 48) were identified. Moreover, two selected compounds, one from each series, 36 and 41, showed good selectivity for PDF over several endoproteases including matrix metalloproteases. However, these compounds showed only weak antibacterial activity.

Highly efficient water-mediated approach to access benzazoles: metal catalyst and base-free synthesis of 2-substituted benzimidazoles, benzoxazoles, and benzothiazoles.

Science.gov (United States)

Bala, Manju; Verma, Praveen Kumar; Sharma, Deepika; Kumar, Neeraj; Singh, Bikram

2015-05-01

An efficient water-catalyzed method has been developed for the synthesis of 2-substituted benzimidazoles, benzoxazoles, and benzothiazoles in one step. The present method excludes the usage of toxic metal catalysts and bases to produce benzazoles in good to excellent yields. An efficient and versatile water-mediated method has been established for the synthesis of various 2-arylbenzazoles. The present protocol excludes the usage of any catalyst and additive provided excellent selectivities and yields with high functional group tolerance for the synthesis of 2-arylated benzimidazoles, benzoxazoles, and benzothiazoles. Benzazolones were also synthesized using similar reaction protocol.

Ternary complexes of Zn(II) and Cu(II) with 1-((2-hydroxynaphthalen-1-yl)methylene)-4-phenylthiosemicarbazide in the presence of heterocyclic bases as auxiliary ligands: Synthesis, spectroscopic and structural characterization and antibacterial activity

Science.gov (United States)

Azarkish, Mohammad; Akbari, Alireza; Sedaghat, Tahereh; Simpson, Jim

2018-03-01

The new ternary complexes, ZnLL‧ [L = 1-((2-hydroxynaphthalen-1-yl)methylene)-4-phenylthiosemicarbazide and L‧ = imidazole (1), 2, 2‧-bipyridine (2) and 2-methyimidazole (3)], Zn2L2L‧ [L‧ = 4, 4‧-bipy (4)] and CuLL‧ [L‧ = 2, 2‧-bipy (5)] have been synthesized by the reaction of a metal(II) acetate salt with the thiosemicarbazone and in presence of heterocyclic bases as auxiliary ligands. The synthesized compounds were investigated by elemental analysis and IR, 1H NMR, and 13C NMR spectroscopy and complex 5 was structurally characterized by X-ray crystallography. The results indicate the thiosemicarbazone doubly deprotonated and coordinates to metal through the thiolate sulfur, imine nitrogen and phenolic oxygen atoms. The nitrogen atom(s) of the auxiliary ligand complete the coordination sphere. Complex 4 is binuclear with 4, 4‧-bipy acting as a bridging ligand. The structure of 5 is a distorted square pyramid with one of the bipyridine nitrogen atoms in the apical position. This compound creates an inversion dimer in solid state by intermolecular hydrogen bonds of Nsbnd H⋯S type. The in vitro antibacterial activity of the synthesized compounds were evaluated against Gram-positive (B. subtilis and S. aureus) and Gram-negative (P. aeruginosa) bacteria and is compared to that of standard antibacterial drugs. All complexes exhibit good inhibitory effects and are significantly more effective than the parent ligand.

Crystal structures of nitrato-(2-[2-(1-pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) aquacopper and chloro-(2-[2-phenyl(pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) copper

Energy Technology Data Exchange (ETDEWEB)

Chumakov, Yu. M. [Academy of Sciences of Moldova, Institute of Applied Physics (Moldova, Republic of); Paholnitcaia, A. Yu. [State University of Moldova (Moldova, Republic of); Petrenko, P. A. [Academy of Sciences of Moldova, Institute of Applied Physics (Moldova, Republic of); Tsapkov, V. I., E-mail: vtsapkov@gmail.com [State University of Moldova (Moldova, Republic of); Poirier, D. [Centre Hospitalier Universitaire de Quebec (Canada); Gulea, A. P. [State University of Moldova (Moldova, Republic of)

2015-01-15

Two crystal modifications of nitrato-(2-[2-(1-pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) aquacopper (I and II) and two modifications of chloro-(2-[2-phenyl(pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) copper (III and IV) have been synthesized and studied by X-ray diffraction. In structures I and II, the copper atoms coordinate a monodeprotonated molecule of the organic ligand, nitrate ions, and a water molecule. In crystals of I, the complexes are monomeric, whereas complexes II are linked via nitrate ions to form polymeric chains. In both structures the coordination polyhedron of the copper atom can be described as a distorted tetragonal bipyramid—(4 + 1 + 1) in I and (4 + 2) in II. These coordination polyherdra have different compositions. In structures III and IV, the metal atoms coordinate a monodeprotonated (2-[2-phenyl(pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazole molecule and chloride ions. In III the complex-forming ion has square-planar coordination geometry, whereas structure IV consists of centrosymmetric dimers with two bridging chlorine atoms. It was found that nitrato-(2-[2-(1-pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) aquacopper possesses antitumor activity.

Solution equilibrium of metal ions-binary complexes with 3-(2-ethylamino-1-hydroxyethyl] phenol (Effortil

Directory of Open Access Journals (Sweden)

Mohamed Magdy Khalil

2016-11-01

Full Text Available Formation of binary complexes of Al(III, Cr(III, Fe(III, Th(IV, UO2(II, Ce(III, La(III, and Gd(III with 3-(2-ethylamino-1-hydroxyethyl] phenol (Effortil were studied potentiometrically at 37.0 °C and I = 0.16 mol dm−3 NaNO3 in aqueous solution. The acid–base properties of Effortil were investigated and discussed. The order of stability of the complexes was investigated and is discussed in terms of the metal ion. The experimental pH titration data were analyzed in order to evaluate the formation constants of various intermediate species formed. The concentration distribution of various species formed in solution was evaluated.

Thermodynamics of complexation of lanthanides with 2,6-bis(5,6-diethyl-1,2,4-triazin-3-yl) pyridine

Energy Technology Data Exchange (ETDEWEB)

Rawat, N.; Bhattacharyya, A.; Tomar, B.S. [Bhabha Atomic Research Centre, Trombay, Mumbai (India). Radiochemistry Div.; Ghosh, S.K.; Gadly, T. [Bhabha Atomic Research Centre, Trombay, Mumbai (India). Bioorganic Div.

2011-07-01

Solvent extraction studies on separation of trivalent actinides from lanthanides using 2,6-bis(5,6-dialkyl-1,2,4-triazin-3-yl) pyridines have shown promising results with respect to separation factor and efficiency in acidic medium. In order to understand their complexation behavior, the stability constant (log {beta}) of trivalent lanthanides (La, Nd, Eu, Tb, Ho, Tm, Lu) with 2,6-bis(5,6-diethyl-1,2,4-triazin-3-yl)pyridine (ethyl-BTP) have been determined in methanol medium (ionic strength 0.01 M) using spectrophotometric titrations. The stoichiometry of the complexes is found to vary with the ionic size of lanthanide ion. The variation in log {beta} across the lanthanide series is attributed to variation in solvation characteristics of the metal ion. Comparison of log {beta} for Ln(III)-ethyl-BTP complexes with other alkyl derivatives showed increase in the stability with increasing length of the alkyl group due to hydrophobic interaction. In the case of Eu(III), the speciation was also corroborated by time resolved fluorescence spectroscopy. The thermodynamic parameters ({delta} G, {delta} H, {delta} S) for complexation of Eu(III) with ethyl-BTP, were determined by microcalorimetry, which revealed strong metal ion-ligand interaction with the reactions driven mainly by enthalpy. (orig.)

A treatise on benzimidazole based Schiff base metal(II) complexes accentuating their biological efficacy: Spectroscopic evaluation of DNA interactions, DNA cleavage and antimicrobial screening

Energy Technology Data Exchange (ETDEWEB)

Kumaravel, Ganesan; Raman, Natarajan, E-mail: ramchem1964@gmail.com

2017-01-01

Two novel imidazole derived Schiff bases, (Z)-1-(1H-benzo[d]imidazol-2-yl)-N-benzylidenemethanamine (L{sup 1}) and 1-(1H-benzo[d]imidazol-2-yl)-N-(4-nitrobenzylidene) methanamine, and a series of their transition metal complexes of the types [M(L{sup 1}){sub 2}]Cl{sub 2} and [M(L{sup 2}){sub 2}]Cl{sub 2} where, M = Cu(II), Ni(II), Co(II) and Zn(II) have been designed and synthesized. These compounds were characterized by various spectral and physicochemical data. UV–Vis, magnetic susceptibility and molar conductivity data indicate that all the complexes adopt square planar geometry. The EPR spectral data of the Cu(II) complexes have provided supportive evidence to the conclusion derived on the basis of electronic absorption and magnetic moment values. Moreover, the interaction of complexes with DNA via intercalation has been explored by absorption, fluorescence spectroscopy, cyclic voltammetry, viscosity and circular dichroism. Agarose gel electrophoresis technique reveals that the complexes are good metallonucleases. All the compounds have relatively high antibacterial and antifungal potencies. Among the metal complexes, Cu(II) complexes exhibit higher efficacy against all the pathogens. - Highlights: • Synthesis of new and efficient benzimidazole based DNA targeting complexes • Synthesis of efficient metallointercalators • Excellent DNA exploiting ability of Cu(II) complexes • Efficient antimicrobial agents against various pathogens.

Mononuclear zinc(II) complexes of 2-((2-(piperazin-1-yl)ethylimino)methyl)-4-substituted phenols: Synthesis, structural characterization, DNA binding and cheminuclease activities

Science.gov (United States)

Ravichandran, J.; Gurumoorthy, P.; Karthick, C.; Kalilur Rahiman, A.

2014-03-01

Four new zinc(II) complexes [Zn(HL1-4)Cl2] (1-4), where HL1-4 = 2-((2-(piperazin-1-yl)ethylimino)methyl)-4-substituted phenols, have been isolated and fully characterized using various spectro-analytical techniques. The X-ray crystal structure of complex 4 shows the distorted trigonal-bipyramidal coordination geometry around zinc(II) ion. The crystal packing is stabilized by intermolecular NH⋯O hydrogen bonding interaction. The complexes display no d-d electronic band in the visible region due to d10 electronic configuration of zinc(II) ion. The electrochemical properties of the synthesized ligands and their complexes exhibit similar voltammogram at reduction potential due to electrochemically innocent Zn(II) ion, which evidenced that the electron transfer is due to the nature of the ligand. Binding interaction of complexes with calf thymus DNA was studied by UV-Vis absorption titration, viscometric titration and cyclic voltammetry. All complexes bind with CT DNA by intercalation, giving the binding affinity in the order of 2 > 1 ≫ 3 > 4. The prominent cheminuclease activity of complexes on plasmid DNA (pBR322 DNA) was observed in the absence and presence of H2O2. Oxidative pathway reveals that the underlying mechanism involves hydroxyl radical.

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).

Cloning, Sequencing, and Expression of the Gene Encoding Cyclic 2,3-Diphosphoglycerate Synthetase, the Key Enzyme of Cyclic 2,3-Diphosphoglycerate Metabolism in Methanothermus fervidus

OpenAIRE

Matussek, Karl; Moritz, Patrick; Brunner, Nina; Eckerskorn, Christoph; Hensel, Reinhard

1998-01-01

Cyclic 2,3-diphosphoglycerate synthetase (cDPGS) catalyzes the synthesis of cyclic 2,3-diphosphoglycerate (cDPG) by formation of an intramolecular phosphoanhydride bond in 2,3-diphosphoglycerate. cDPG is known to be accumulated to high intracellular concentrations (>300 mM) as a putative thermoadapter in some hyperthermophilic methanogens. For the first time, we have purified active cDPGS from a methanogen, the hyperthermophilic archaeon Methanothermus fervidus, sequenced the coding gene, and...

Preparation, thermodynamic property and antimicrobial activity of some rare-earth (III) complexes with 3-bromo-5-iodobenzoic acid and 1,10-phenanthroline

Energy Technology Data Exchange (ETDEWEB)

Liu, Jing-Yu [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Ren, Ning [Department of Chemistry, Handan College, Handan 056005 (China); Zhang, Jian-Jun, E-mail: jjzhang6@126.com [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Zhang, Cun-Ying [No.1 High School of Shijiazhuang, Shijiazhuang 050011 (China)

2013-10-20

Graphical abstract: Four new rare-earth complexes of general formula [Ln(3-Br-5-IBA){sub 3}phen]{sub 2} [Ln = Er (1), Tb (2), Dy (3) and Ho (4); 3-Br-5-IBA = 3-bromo-5-iodobenzoate; phen = 1,10-phenanthroline] were synthesized and characterized by elemental analysis, IR, UV and TG/DSC-FTIR technology. Heat capacities of the four complexes were measured by differential scanning calorimetry (DSC). The antimicrobial activity against Escherichia coli, Staphylococcus aureus and Candida albicans were tested using disc diffusion method. - Highlights: • Four new complexes [Ln(3-Br-5-IBA){sub 3}phen]{sub 2} were synthesized and characterized. • The non-isothermal kinetics of the first stage for the complexes was studied. • The heat capacities of the complexes were measured by differential scanning calorimeter. • The antimicrobial activities for these complexes were tested. • The fluorescence properties of the complexes 2 and 3 were studied. - Abstract: Four new rare-earth complexes of general formula [Ln(3-Br-5-IBA){sub 3}phen]{sub 2} (Ln(III) = Er (1), Tb (2), Dy (3) and Ho (4); 3-Br-5-IBA = 3-bromo-5-iodobenzoate; phen = 1,10-phenanthroline) were synthesized by solution-precipitation method, and investigated using elemental analysis, infrared spectra, ultraviolet spectra and TG/DSC-FTIR technology. The non-isothermal kinetics of the first stage for the complexes was studied by using non-linear integral isoconversional method and double equal-double steps method. The heat capacities of the complexes were measured between 263.15 and 485.55 K by means of differential scanning calorimeter, and the values of the experimental heat capacities were fitted to a polynomial equation with the least-squares method. And the thermodynamic functions [H{sub T} − H{sub 298.15}], [S{sub T} − S{sub 298.15}] and [G{sub T} − G{sub 298.15}] were also derived based on the fitted polynomials and thermodynamic relationships with temperature interval of 10 K. Moreover, the

Enzymatic degradation of cyclic 2,3-diphosphoglycerate to 2,3-diphosphoglycerate in Methanobacterium thermoautotrophicum

International Nuclear Information System (INIS)

Krishna Sastry, M.V.; Robertson, D.E.; Moynihan, J.A.; Roberts, M.F.

1992-01-01

2,3-Diphosphoglycerate (2,3-DPG) has been found to be the product of the enzymatic degradation of cyclic 2,3-diphosphoglycerate (cDPG) in the archaebacterium Methanobacterium thermoautotrophicum ΔH. Although 2,3-DPG has not previously been detected as a major soluble component of M. thermoautotrophicum, large pools accumulated at an incubation temperature of 50C. Under these conditions, cellular activity was significantly decreased; a return of the culture to the optimum growth temperature restored the 2,3-DPG pool back to original low levels and caused steady-state cDPG levels to increase again. While 13 CO 2 -pulse/ 12 CO 2 -chase experiments at 50C showed that the cDPG turned over, the appearance of 2,3-DPG at NMR-visible concentrations required at least 10 h. Production of 2,3-DPG in vivo was prevented by exposure of the cells to O 2 . the enzyme responsible for this hydrolysis of cDPG was purified by affinity chromatography and appears to be a 33-kDa protein. Activity was detected in the presence of oxygen and was enhanced by a solution of 1 M KCl, 25 mM MgCl 2 , and dithiothreitol. Both K m and V max have been determined at 37C; kinetics also indicate that in vitro the product, 2,3-DPG, is an inhibitor of cDPG hydrolysis. These findings are discussed in view of a proposed role for cDPG in methanogens

Crystal structure of 1,3-bis[(E-4-methoxybenzylideneamino]propan-2-ol

Directory of Open Access Journals (Sweden)

Augusto Rivera

2016-12-01

Full Text Available The title Schiff base, C19H22N2O3, was synthesized via the condensation reaction of 1,3-diaminopropan-2-ol with 4-methoxybenzaldehyde using water as solvent. The molecule exists in an E,E conformation with respect to the C=N imine bonds and the dihedral angle between the aromatic rings is 37.25 (15°. In the crystal, O—H...N hydrogen bonds link the molecules into infinite C(5 chains propagating along the a-axis direction. The packing of these chains is consolidated by C—H...O interactions and C—H...π short contacts, forming a three-dimensional network.

Zn-Doped LiNi1/3Co1/3Mn1/3O2 Composite as Cathode Material for Lithium Ion Battery: Preparation, Characterization, and Electrochemical Properties

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Han Du

2015-01-01

Full Text Available Zn-doped LiNi1/3Co1/3Mn1/3O2 composite, Li(Ni1/3Co1/3Mn1/31–xZnxO2 (x = 0.02; 0.05; 0.08, is synthesized by the sol-gel method. The crystal structure, morphology, and electrochemical performance are investigated via X-ray diffraction (XRD, scanning electron microscope (SEM, cyclic voltammetry (CV, and constant current charge/discharge experiment. The result reveals that Zn-doping cathode material can reach the initial charge/discharge capacity of 188.8/162.9 mAh·g−1 for Li(Ni1/3Co1/3Mn1/30.98Zn0.02O2 and 179.0/154.1 mAh·g−1 for Li(Ni1/3Co1/3Mn1/30.95Zn0.05O2 with the high voltage of 4.4 V at 0.1 C. Furthermore, the capacity retention of Li(Ni1/3Co1/3Mn1/30.98Zn0.02O2 is 95.1% at 0.5 C after 50 cycles at room temperature. The improved electrochemical properties of Zn-doped LiNi1/3Co1/3Mn1/3O2 are attributed to reduced electrode polarization, enhanced capacity reversibility, and excellent cyclic performance.

Preparation and Luminescent Properties of the antibacterial materials of the La3+ Doped Sm3+-Hydroxyapatite

Science.gov (United States)

Lv, Yuguang; Shi, Qi; Jin, Yuling; Ren, Hengxin; Qin, Yushan; Wang, Bo; Song, Shanshan

2018-03-01

In this paper, the La3+-doped Sm3+ hydroxyapatite (La/Sm/HAP) complexes were prepared by a precipitation method. The sample was defined by IR spectra, fluorescence spectra and X ray diffraction analysis et al. The structure of complexes were discussed. The emission wavelength of heat treatment of Sm3+ do not change, but will affect the intensity of the peak Sm3+ luminescence properties and the occupy hydroxyapatite in the lattice Ca( II )and Ca( I ) loci with Sm3+ doped concentration and the proportion of the sintering temperature change and change: The nano hydroxyapatite complex of the La3+ doped samarium obtain the good fluorescence intensity, by La3+ doping content of Sm3+ were hydroxyapatite 6% (La3+, Sm3+ mole ratio) device. The complex of La3+ doped samarium HAP have Stable chemical property, fluorescence property and excellent biological activity. The ligand HAP absorbs energy or captures an electron-hole pair and then transfers it to the lanthanide ions. The catalytic activity influence of the La3+-doped Sm3+hydroxyapatite was discussed, the La/Sm/HAP had excellent antibacterial property, which used as potential biological antibacterial material.

Comparison the Antibacterial Activity of Vitamin D2 and D3

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Intesar N. Khelkal

2017-03-01

Full Text Available An attempt has been made to determine the antimicrobial activity of vitamin D; D3 & D2 against clinical bacterial isolates as well as perform a comparative analytical study between the effects of both forms of vitamin. The ability of vitamin D (both D2 ergocalciferol& D3 cholecalciferol  to  inhibit bacterial growth of some clinical isolates have been tested . Forty - three pathogenic bacterial isolates (Gr+ ,Gr- have been identified  from fifty - five specimen  was collected from  different sources ; 24 urine, 17 sputum , 9 blood , 5 skin at Al-Kindey hospital for a period of two months . Antibiotic sensitivity was carried out towards 12 different antibiotic discs. The most resistant isolates have been chosen to be tested in the study. Two bacterial suspensions of the selected isolates have been prepared; the first was adjusted to McFarland standard No. 0.5 (1 ×10 8 CFU /mL; the second = 1×1010 CFU /mL. Three concentrations of both vitamins have been prepared; 50,000, 70,000 and 90,000 IU/mL as well as the control ( solvent only . Antibacterial activity has been examined by using agar diffusion (pore plating method to determine the most effective concentration among the three concentrations of the two forms of vitamin D. Results were suggesting the important role of vitamin D specially D3 as antibacterial agent .The third concentration (90,000 IU/mL was causing the largest inhibition zone with all tested isolates even with the high turbidity culture (1010CFU/mL ,followed by the second one (70,000 IU/mL, the lower inhibitor concentration was (50,000 IU/mL. Significant differences have been appeared among the measurements of the diameters of inhibition zones towards three vitamin concentrations when compared one to another and to control.

Base-Free Selective Oxidation of Glycerol over LDH Hosted Transition Metal Complexes Using 3% H2O2 as Oxidant

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Xiaoli Wang

2016-07-01

Full Text Available A series of transition metal sulphonato-Schiff base complexes were intercalated into Mg–Al layered-double hydroxides (LDHs. The obtained catalysts were characterized by FTIR, XRD, N2 sorption, SEM and elemental analysis, and then were used in the selective oxidation of glycerol (GLY using 3% H2O2 as an oxidant. It was found that their catalytic performances were closely related to the loading of active complexes, the Schiff base ligands and the metal centers of the catalysts, as well as the reaction conditions. The optimal conversion of GLY was 85.0%, while the selectivity of 1,3-dihydroxyacetone (DHA was 56.5%. Moreover, the catalysts could be reused at least 10 times.

Synthesis, Spectroscopic Characterization, and Biological Activities of Metal Complexes of 4-((4-Chlorophenyldiazenyl-2-((p-tolyliminomethylphenol

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C. Anitha

2013-01-01

Full Text Available Azo Schiff base complexes of VO(II, Mn(II, Co(II, Ni(II, Cu(II, and Zn(II have been synthesized from 4-((4-chlorophenyldiazenyl-2-((p-tolyliminomethylphenol (CDTMP. The nature of bonding and the structural features of the complexes have been deduced from elemental analysis, molar conductance, magnetic susceptibility measurements, IR, UV-Vis, 1H-NMR, EPR, mass, SEM, and fluorescence spectral studies. Spectroscopic and other analytical studies reveal square-planar geometry for copper, square-pyramidal geometry for oxovanadium, and octahedral geometry for other complexes. The EPR spectra of copper(II complex in DMSO at 300 K and 77 K were recorded, and its salient features are reported. Antimicrobial studies against several microorganisms indicate that the complexes are more potent bactericides and fungicides than the ligand. The electrochemical behavior of the copper(II complex was studied by cyclic voltammetry. All the synthesized compounds can serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic conversion efficiency of the synthesized azo Schiff base was found to be higher than that of urea and KDP (potassium dihydrogen phosphate. SEM image of copper(II complex implies the crystalline state and surface morphology of the complex.

Antibacterial and Herbicidal Activity of Ring-Substituted 3-Hydroxynaphthalene-2-carboxanilides

Czech Academy of Sciences Publication Activity Database

Kos, J.; Zadražilová, I.; Pesko, M.; Keltosova, S.; Tengler, J.; Goněc, T.; Bobál, P.; Kauerová, T.; Oravec, Michal; Kolař, P.; Čížek, A.; Králová, K.; Jampílek, J.

2013-01-01

Roč. 18, č. 7 (2013), s. 7977-7997 ISSN 1420-3049 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0073 Institutional support: RVO:67179843 Keywords : hydroxynaphthalene-2-carboxanilides * lipophilicity * photosynthetic electron transport inhibition * spinach chloroplasts * in vitro antibacterial activity * in vitro antimycobacterial activity * in vitro cytotoxicity * structure-activity relationships Subject RIV: EH - Ecology, Behaviour Impact factor: 2.095, year: 2013

Unexpected Formation of Naphtyl 1,3-Diaminopropane-2-ol Derivative through Azetidinium Ion Intermediate

International Nuclear Information System (INIS)

Han, Minsoo; Hahn, Hohgyu

2012-01-01

The cause of depression is commonly associated with a deficiency of monoamine neurotransmitters such as serotonin, norepinephrine and dopamine in the brain. Inhibition of monoamine reuptake has been an effective pharmacological treatment of various CNS disorders.1 As a part of our continuing efforts to develop novel antidepressants for multiple therapeutic utilities, we designed diaminopropan-2-ol 1 through structure analysis and molecular modification and of currently marketed reuptake transporter based antidepressants. 3-amino-1,2-diol derivatives 7 were converted to the corresponding diaminopropan-2-ol derivatives 9 by the reaction with MsCl in the presence of triethylamine followed by the treatment of either amine or thiol. We proposed azetdinium ion 11 or azetidinium ylide 12 as an intermediate in the reaction, and prepared 7 analogues by similar manner

Unexpected Formation of Naphtyl 1,3-Diaminopropane-2-ol Derivative through Azetidinium Ion Intermediate

Energy Technology Data Exchange (ETDEWEB)

Han, Minsoo; Hahn, Hohgyu [Korea Institute of Science and Technology, Seoul (Korea, Republic of)

2012-11-15

The cause of depression is commonly associated with a deficiency of monoamine neurotransmitters such as serotonin, norepinephrine and dopamine in the brain. Inhibition of monoamine reuptake has been an effective pharmacological treatment of various CNS disorders.1 As a part of our continuing efforts to develop novel antidepressants for multiple therapeutic utilities, we designed diaminopropan-2-ol 1 through structure analysis and molecular modification and of currently marketed reuptake transporter based antidepressants. 3-amino-1,2-diol derivatives 7 were converted to the corresponding diaminopropan-2-ol derivatives 9 by the reaction with MsCl in the presence of triethylamine followed by the treatment of either amine or thiol. We proposed azetdinium ion 11 or azetidinium ylide 12 as an intermediate in the reaction, and prepared 7 analogues by similar manner.

Influence of anode material on the electrochemical oxidation of 2-naphthol Part 1. Cyclic voltammetry and potential step experiments

International Nuclear Information System (INIS)

Panizza, M.; Cerisola, G.

2003-01-01

The anodic oxidation of 2-naphthol has been studied by cyclic voltammetry and chronoamperometry, using a range of electrode materials such as Ti-Ru-Sn ternary oxide, lead dioxide and boron-doped diamond (BDD) anodes. The results show that polymeric films, which cause electrode fouling, are formed during oxidation in the potential region of supporting electrolyte stability. IR spectroscopy verified the formation of this organic film. While the Ti-Ru-Sn ternary oxide surface cannot be reactivated, PbO 2 and BDD can be restored to their initial activity by simple anodic treatment in the potential region of electrolyte decomposition. In fact, during the polarization in this region, complex oxidation reactions leading to the complete incineration of polymeric materials can take place on these electrodes due to electrogenerated hydroxyl radicals. Moreover, it was found that BDD deactivation was less pronounced and its reactivation was faster than that of the other electrodes

SYNTHESIS, CHARACTERIZATION AND ANTI-BACTERIAL ACTIVITY OF CERTAIN 2,3,4,5-TETRAHYDROPYRIDAZINONE ANALOGUES

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Gaurav ALANG

2011-04-01

Full Text Available In the present study, six new derivatives of PYridazinone were synthesized and evaluate their anti-bacterial activity. The experimental work involves the synthesis of benzoyl propionic acid (a, then 6-phenyl-2,3,4,5-tetrahydro pyridazin-3-one (b which was then condensed with various, aldehydes to form respective derivatives, AH the synthesized compounds were identified by IR, 1HNMR and antimicrobial activity was performed on the compounds synthesized against Staphylococcus aureus (MTCC 737, Staphylococcus epidermidis (MTCC 3615, Pseudomonas aeruginosa (MTCC 424 and Escherichia coli (MTCC 1687

Thermochemical Properties of the Complexes RE(HSal)3·2H2O (RE=La, Ce, Pr, Nd, Sm)

Institute of Scientific and Technical Information of China (English)

无

2006-01-01

Five solid rare earth salicylate complexes were synthesized by low hydrated lathanide chloride and salicylic acid. The complexes in this experiment were identified as the general formula RE(Hsal)3·2H2O(RE=La, Ce, Pr, Nd, Sm) by elemental analysis and EDTA volumetric analysis. IR spectra of the complexes show that carboxyl of salicylic acid coordinates to RE3+ ions. Electrochemical behaviors of the complexes on the glass-carbon electrode were researched with cyclic voltammetry (CV). It is indicated that the electrochemical process of the complexes is a one-electron redox process and the electrochemical reversibility of complexes is less than that of the lanthanide chlorides. The constant-volume combustion energies of complexes, ΔcU, were determined with a precise rotating-bomb calorimeter at 298.15 K. Their standard molar enthalpies of combustion, ΔcHθm, and standard molar enthalpies of formation, ΔfHθm, were calculated.

SPR imaging combined with cyclic voltammetry for the detection of neural activity

Directory of Open Access Journals (Sweden)

Hui Li

2014-03-01

Full Text Available Surface plasmon resonance (SPR detects changes in refractive index at a metal-dielectric interface. In this study, SPR imaging (SPRi combined with cyclic voltammetry (CV was applied to detect neural activity in isolated bullfrog sciatic nerves. The neural activities induced by chemical and electrical stimulation led to an SPR response, and the activities were recorded in real time. The activities of different parts of the sciatic nerve were recorded and compared. The results demonstrated that SPR imaging combined with CV is a powerful tool for the investigation of neural activity.

Enzymatic degradation of cyclic 2,3-diphosphoglycerate to 2,3-diphosphoglycerate in Methanobacterium thermoautotrophicum.

Science.gov (United States)

Sastry, M V; Robertson, D E; Moynihan, J A; Roberts, M F

1992-03-24

2,3-Diphosphoglycerate (2,3-DPG) has been found to be the product of the enzymatic degradation of cyclic 2,3-diphosphoglycerate (cDPG) in the archaebacterium Methanobacterium thermoautotrophicum delta H. Although 2,3-DPG has not previously been detected as a major soluble component of M. thermoautotrophicum, large pools accumulated at an incubation temperature of 50 degrees C (below the optimum growth temperature of 62 degrees C). Under these conditions, cellular activity was significantly decreased; a return of the culture to the optimum growth temperature restored the 2,3-DPG pool back to original low levels and caused steady-state cDPG levels to increase again. While 13CO2-pulse/12CO2-chase experiments at 50 degrees C showed that the cDPG turned over, the appearance of 2,3-DPG at NMR-visible concentrations required at least 10 h. Production of 2,3-DPG in vivo was prevented by exposure of the cells to O2. The enzyme responsible for this hydrolysis of cDPG was purified by affinity chromatography and appears to be a 33-kDa protein. Activity was detected in the presence of oxygen and was enhanced by a solution of 1 M KCl, 25 mM MgCl2, and dithiothreitol. Both Km and Vmax have been determined at 37 degrees C; kinetics also indicate that in vitro the product, 2,3-DPG, is an inhibitor of cDPG hydrolysis. These findings are discussed in view of a proposed role for cDPG in methanogens.

Synthesis and structural characterization of ternary Cu (II) complexes of glycine with 2,2'-bipyridine and 2,2'-dipyridylamine. The DNA-binding studies and biological activity.

Science.gov (United States)

Mohamed, Mervat S; Shoukry, Azza A; Ali, Ayat G

2012-02-01

In this study two new complexes [Cu(bpy)(Gly)Cl]·2H(2)O (1) and [Cu(dpa)(Gly)Cl]·2H(2)O (2) (bpy=2,2'-bipyridine; dpa=2,2'-dipyridylamine, Gly=glycine) have been synthesized and characterized by elemental analysis, IR, TGA, UV-vis and magnetic susceptibility measurements. The binding properties of the complexes with CT-DNA were investigated by electronic absorption spectra. The intrinsic binding constants (K(b)) calculated from UV-vis absorption studies were 1.84 × 10(3) M(-1) and 3.1 × 10(3) M(-1) for complexes 1 and 2 respectively. Thermal denaturation has been systematically studied by spectrophotometric method and the calculated ΔT(m) was nearly 5 °C for each complex. All the results suggest that the interaction modes between the complexes and CT-DNA were electrostatic and/or groove binding. The redox behavior of the two complexes was investigated by cyclic voltammetry. Both complexes, in presence and absence of CT-DNA show a quasi-reversible wave corresponding to Cu(II)/Cu(I) redox couple. The change in E(1/2), ΔE and I(pc)/I(pa) ascertain the interaction of complexes 1 and 2 with CT-DNA. Further insight into the binding of complexes with CT-DNA has been made by gel electrophoresis, where the binding of complexes is confirmed through decreasing the mobility and intensity of DNA bands. In addition, the antitumor activity of the complexes was tested on two cancer cell lines; the breast cancer (MCF7) and the human hepatocellular carcinoma (HEPG2), as well as one normal cell line; the human normal melanocytes (HFB4). The results showed that complex 1 was more potent antitumor agent than complex 2. The in-vitro antimicrobial activity of the two complexes was carried out using the disc diffusion method against different species of pathogenic bacteria and fungi. The activity data showed that complex 2 was more active in inhibiting the growth of the tested organisms. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis, reactions and biological activity of 3-arylidene-5-(4-methylphenyl-2(3H-furanones

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ASIF HUSAIN

2009-02-01

Full Text Available 3-Arylidene-5-(4-methylphenyl-2(3H-furanones 2a–m were prepared from 3-(4-methyl-benzoylpropanoic acid 1 and several aromatic aldehydes. Some of the selected furanones were reacted with ammonia gas and benzylamine to give corresponding 3-arylidene-1,3-dihydro-5-(4-methylphenyl-2H-pyrrol-2-ones 3a–h and 3-arylidene-1-benzyl-1,3-dihydro-5-(4-methylphenyl-2H-pyrrol-2-ones 4a–f, respectively, which were characterized on the basis of IR, 1H-NMR, mass spectral data and elemental analysis results. These compounds were tested for their anti-inflammatory and antibacterial activities. The compounds, which showed significant anti-inflammatory activity, were further screened for their analgesic and ulcerogenic activities. Three new compounds (2e, 2h and 4d, out of twenty-seven showed very good anti-inflammatory activity in the carrageenan induced rat paw edema test, with significant analgesic activity in the acetic acid induced writhing test together with negligible ulcerogenic action. The antibacterial activity is expressed as the corresponding MIC values.

Synthesis and in vitro antibacterial activity of N-methylnitrone and nitrovinyl derivatives of some N-substituted 2-chloroindol-3-carboxaldehydes

Energy Technology Data Exchange (ETDEWEB)

Gatti, R.; Cavrini, V.; Roveri, P.; Bianucci, F.; Legnani, P.

1981-02-01

N-methylnitrones and nitrovinyl derivatives from 1-substituted-2-chloroindol-3-carboxaldehydes were synthesized and evaluated for their in vitro antibacterial activity. Some nitrovinyl derivatives displayed good in vitro activity against Gram-positive bacteria; the compound (II e), 1-(o-chlorobenzyl)-2-chloro-3-(2-nitroethenyl)indole, was more active than nitrofurantoin against Staphylococcus aureus and Streptococcus pyogenes. Some structure-activity relationships are discussed.

Antimicrobial activity study of a μ3-oxo bridged [Fe3O(PhCO2)6(MeOH)3](NO3)(MeOH)2] cluster

Science.gov (United States)

Pathak, Sayantan; Jana, Barun; Mandal, Manab; Mandal, Vivekananda; Ghorai, Tanmay K.

2017-11-01

Synthesis, characterization and antimicrobial activity of a tri-nuclear μ3-Oxobridged Fe(III) cluster [Fe3O(PhCO2)6(MeOH)3](NO3)(MeOH)2(1) is reported. Cluster 1 is synthesized in a single pot reaction among Fe(NO3)3·9H2O, C6H5COOH, NaN3 (1:4:1) in MeOH. Single crystal X-ray diffraction studies of the isolated crystals show that it is μ3-Oxo bridged trimeric assembly of three Fe atoms via bridging benzoate anions. Furthermore, BVS calculations show that all three Fe atoms in complex 1 are in +3 oxidation state and are surrounded by benzoate anions and methanol in octahedral environment. The oxidation state of iron is also confirmed from the cyclic voltamogram. FT-IR spectroscopy and CHN analysis of the isolated crystals further supports the functional group attached to the periphery of the complex. The nanomolecular size of complex 1 is 1.29 nm. The antimicrobial efficiency studies of the complex 1 show significant inhibition of the growth of the organisms, viz. B. cereus MTCC 1272, S. epidermidis MTCC 3086 and S. typhimurium MTCC 98 and produced 23 ± 1.93 mm, 16 ± 1.77 mm and 12 ± 2.42 mm inhibition zones respectively. However, it shows zero inhibition to the strain of E. coli MTCC 723.

Influence of anode material on the electrochemical oxidation of 2-naphthol Part 1. Cyclic voltammetry and potential step experiments

Energy Technology Data Exchange (ETDEWEB)

Panizza, M.; Cerisola, G

2003-10-15

The anodic oxidation of 2-naphthol has been studied by cyclic voltammetry and chronoamperometry, using a range of electrode materials such as Ti-Ru-Sn ternary oxide, lead dioxide and boron-doped diamond (BDD) anodes. The results show that polymeric films, which cause electrode fouling, are formed during oxidation in the potential region of supporting electrolyte stability. IR spectroscopy verified the formation of this organic film. While the Ti-Ru-Sn ternary oxide surface cannot be reactivated, PbO{sub 2} and BDD can be restored to their initial activity by simple anodic treatment in the potential region of electrolyte decomposition. In fact, during the polarization in this region, complex oxidation reactions leading to the complete incineration of polymeric materials can take place on these electrodes due to electrogenerated hydroxyl radicals. Moreover, it was found that BDD deactivation was less pronounced and its reactivation was faster than that of the other electrodes.

Synthesis, structural studies and antimicrobial activity of N'-((2Z, 3E)-3-(hydroxyimino)butan-2-ylidene)-2-phenylacetohydrazide and its Co(II), Ni(II) complexes

Science.gov (United States)

Karadeniz, Şeyma; Ataol, Cigdem Yuksektepe; Şahin, Onur; İdil, Önder; Bati, Hümeyra

2018-06-01

A new aroylhydrazoneoxime, N'-((2Z, 3E)-3-(hydroxyimino)butan-2-ylidene)-2-phenylacetohydrazide ligand (LH2) and its Ni(II) and Co(II) complexes, have been synthesized and characterized by elemental and thermal analyses, IR and UV-vis spectroscopy, magnetic moment and X-ray diffraction. The antimicrobial activities of these compounds were tested by using minimal inhibitory concentration method (MIC). The ligand-containing aroylhydrazone and oxime groups and its Ni complex crystallize in the triclinic system and P 1 - space group, while its Co complex crystallizes in the monoclinic system and the C 2/c space group. X-ray results show that the ligand in the keto form is transformed into enolic form when it forms coordination. From elemental analysis data, the stoichiometry of Co(II) complex was found to be 1:2 (metal/ligand), but 1:1 for Ni(II). IR spectra indicate that the ligand acts as monoanionic NNO- tridentate and coordination takes place form through the oxime nitrogen, imine nitrogen, and enolate oxygen atoms.

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 and fluorescence study of sodium-2-(4'-dimethyl-aminocinnamicacyl)-3,3-(1',3'-alkylenedithio) acrylate

International Nuclear Information System (INIS)

Si Zhenjun; Shao Yun; Li Chunxia; Liu Qun

2007-01-01

We synthesized two new compounds: Sodium 2-(4'-dimethyl-aminocinnamicacyl)-3,3-(1',3'- ethyl- enedithio) acrylate (STAA-1) and Sodium 2-(4'-dimethyl-aminocinnamicacyl)-3, 3-(1',3'-propylenedithio) acrylate (STAA-2). The maximum absorption of these compounds ranges from 460 to 520 nm with different molecular structures in different solvents. Meanwhile, the emission peak of these compounds arranges from yellow (510 nm) to red (605 nm). The emission spectra show red shift according to the strength of the hydrogen bonding property of the solvent. But the absorption spectra do not show clearly relationship with the strength of the hydrogen bonding property of the solvent. The Stoke shift of the compounds ranges from 42 to 102 nm. It changes in the following order, EtOH>H 2 O>DMF, and STAA-1>STAA-2 in the same solvent. The fluorescent quantum yield of STAA-1 was measured to be 7.12% with quinine sulphate as the standard compound in ethanol. Furthermore, the relationship of the fluorescence of STAA-1 with pH (ranges form 4 to 14) in water (c=∼10 -4 ) was studied to make sure that these compounds could be used as proton sensors

Results of sampling and analysis of groundwater from multi-packered boreholes OL-KR1, OL-KR3, OL-KR5, OL-KR9, OL-KR11 and OL-KR12 at Olkiluoto, Eurajoki, in 2004

Energy Technology Data Exchange (ETDEWEB)

Hirvonen, H. [Teollisuuden Voima Oyj, Eurajoki (Finland); Hatanpaeae, E. [lnsinoeoeritoimisto Paavo Ristola Oy, Hollola (Finland)

2005-12-15

Nine groundwater samples were collected at Olkiluoto from deep multi-packered boreholes OL-KR1, OL-KR3, OL-KR5, OL-KR9, OL-KR11 and OL-KR12 between spring 2004 and the beginning of 2005. The aim of the ground water sampling was to get information for the basis of the monitoring program (OMO) during ONKALO construction. Sampling sections were mainly chosen so that the results of the chemical analyses from earlier studies could be used for comparison. This study presents the sampling methods and the results of the laboratory analyses of groundwater samples from the deep multi-packered boreholes OL-KR1 (151.2-156.8 m, 311.2-336.8 m and 524.4-528.4 m), OL-KR3 (242.6-253.2 m), OL-KR5 (277.2-284.6 m and 457.2-476.2 m), OL-KR9 (468.2-482.2 m), OL-KR11 (597.5-628.1 m) and OLKR12 (363-368 m). The analytical results of the groundwater samplings are compared to earlier analytical results. According to Davis and De Wiest's (1967) classification, the collected groundwater samples represent either the borehole water type Na-Cl (OL-KR1/T/151.2-156.8 m, OLK-R1/ T/311.2-336.8 m, OL-KR3/T/242.6-253.2 m, OL-KR5/T/277.2-284.6 m, OL-KR11/ T/597.5-628.1 m and OL-KR12/T/363-368 m) or Na-Ca-Cl (OL-KR1/T/524.4- 528.4 m, OL-KR5/T/457.2-476.2 m and OL-KR9/T/468.2-482.2 m). The groundwater samples from OL-KR1/T/151.2-156.8 m, OL-KR3/T/242.6- 253.2 m, OL-KR3/T/242.6-253.2 m, OL-KR5/T/277.2-284.2 m, OL-KR11/T/597.5-628.1 m and OL-KR12/T/363-368 m were brackish (1000 mg/L < TDS < 10000 mg/L) according to Davis's (1964) TDS classification. Other samples (OL-KR1/T/524.4-528.4 m, OL-KR5/ T/457.2-476.2 m and OL-KR9/T/468.2-482.2 m), were saline (TDS> 10000 mg/L). Comparison of analytical results of the samples to earlier results shows that some changes were seen between samplings done at the different times. Only the groundwater sampled from OL-KR1/T/311.2-336.8 m had significant changes in its chemical composition during the reference period, but also in OL-KR1/T/524.4-528.4 m, OL-KR5/ T

Cyclic voltammetry modeling of proton transport effects on redox charge storage in conductive materials: application to a TiO2 mesoporous film.

Science.gov (United States)

Kim, Y S; Balland, V; Limoges, B; Costentin, C

2017-07-21

Cyclic voltammetry is a particularly useful tool for characterizing charge accumulation in conductive materials. A simple model is presented to evaluate proton transport effects on charge storage in conductive materials associated with a redox process coupled with proton insertion in the bulk material from an aqueous buffered solution, a situation frequently encountered in metal oxide materials. The interplay between proton transport inside and outside the materials is described using a formulation of the problem through introduction of dimensionless variables that allows defining the minimum number of parameters governing the cyclic voltammetry response with consideration of a simple description of the system geometry. This approach is illustrated by analysis of proton insertion in a mesoporous TiO 2 film.

Acridine-based fluorescence chemosensors for selective sensing of Fe3+ and Ni2+ ions

Science.gov (United States)

Wang, Chaoyu; Fu, Jiaxin; Yao, Kun; Xue, Kun; Xu, Kuoxi; Pang, Xiaobin

2018-06-01

Two novel acridine-based fluorescence chemosensors (L1 and L2) were prepared and their metal ions sensing properties were investigated. L1 (L2) exhibited an excellent selective fluorescence response toward Fe3+ (Ni2+) and the stoichiometry ratio of L1-Fe3+ and L2-Ni2+ were 1:1. The detection limits of L1 and L2 were calculated by the fluorescence titration to be 4.13 μM and 1.52 μM, respectively, which were below the maximum permissive level of Fe3+ and Ni2+ ions in drinking water set by the EPA. The possible mechanism of the fluorescence detection of Fe3+ and Ni2+ had been proposed according to the analysis of Job's plot, IR spectra and ESI-MS. The determination of Fe3+ and Ni2+ ions in living cells had been applied successfully.

Synthesis, characterization and biological activity of some transition metals with Schiff base derived from 2-thiophene carboxaldehyde and aminobenzoic acid

Science.gov (United States)

Mohamed, Gehad G.; Omar, M. M.; Hindy, Ahmed M. M.

2005-12-01

Metal complexes of Schiff base derived from 2-thiophene carboxaldehyde and 2-aminobenzoic acid (HL) are reported and characterized based on elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance and thermal analysis (TGA). The ligand dissociation as well as the metal-ligand stability constants were calculated pH metrically at 25 °C and ionic strength μ = 0.1 (1 M NaCl). The complexes are found to have the formulae [M(HL) 2](X) n· yH 2O (where M = Fe(III) (X = Cl, n = 3, y = 3), Co(II) (X = Cl, n = 2, y = 1.5), Ni(II) (X = Cl, n = 2, y = 1) and UO 2(II) (X = NO 3, n = 2, y = 0)) and [M(L) 2] (where M = Cu(II) (X = Cl) and Zn(II) (X = AcO)). The molar conductance data reveal that Fe(III) and Co(II), Ni(II) and UO 2(II) chelates are ionic in nature and are of the type 3:1 and 2:1 electrolytes, respectively, while Cu(II) and Zn(II) complexes are non-electrolytes. IR spectra show that HL is coordinated to the metal ions in a terdentate manner with ONS donor sites of the carboxylate O, azomethine N and thiophene S. From the magnetic and solid reflectance spectra, it is found that the geometrical structure 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*, Δ H*, Δ S* and Δ G* 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 Schiff base ligand against one or more bacterial species.

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)

Versatility of {l_brace}M(30-crown-10){r_brace} (M = K{sup +}, Ba{sup 2+}) as a guest in UO{sub 2}{sup 2+} complexes of 3.1.3.1 - and 3.3.3 homo-oxa-calixarenes

Energy Technology Data Exchange (ETDEWEB)

Masci, B. [Univ Roma La Sapienza, Dipartimento Chim, I-00185 Rome, (Italy); Thuery, P. [CEA Saclay, DSM/DRECAM/SCM, CNRS-URA 331, F-91191 Gif Sur Yvette, (France)

2007-07-01

The reaction between p-R-[3.1.3.1]- or [3.3.3] homo-oxa-calixarenes and uranyl salts in the presence of 30-crown-10 and the alkali or alkaline-earth metal cations K{sup +} or Ba{sup 2+} gives various supramolecular assemblages characterized by 'complex-within-complex' architectures. These can be of the simple nesting or sandwich types, as in [{l_brace}Ba(30-crown-10){r_brace}{l_brace}UO{sub 2}(L{sup 1}){r_brace}]. 2H{sub 2}O.3CHCl{sub 3} (L{sup 1}H{sub 4} p-tert-butyl[3.1.3.1] homo-oxa-calixarene) and [{l_brace}Ba(30-crown-10){r_brace}{l_brace}UO{sub 2}(L{sup 4}){r_brace}{sub 2}].2CHCl{sub 3} (L{sup 4}H{sub 3} p-bromo[3.3.3]homo-oxa-calixarene), respectively, with the cation held in the cavity of the homo-oxa-calixarene complexes in cone conformation by weak interactions, but more original structures arise when uranyl-cation bonds are present. In [{l_brace}Ba(30-crown-10){r_brace}{l_brace}UO{sub 2}(L{sup 2}){r_brace}] (L{sup 2}H{sub 4} p-phenyl[3.1.3.1] homo-oxa-calixarene), the barium ion included in the crown ether is bound to the uranyl oxo group located out of the calixarene cavity, resulting in the formation of a neutral species which self-organizes to form a columnar assembly by auto-inclusion. In [{l_brace}K(30-crown-10){r_brace}{l_brace}UO{sub 2}K(L{sup 1})(H{sub 2}O){sub 3}{r_brace}]{sub 2}.6H{sub 2}O, the nesting-type subunit dimerizes around two oxo-bound potassium ions. Finally, the use of the coordinating solvent dimethylsulfoxide leads to the neutral complex [UO{sub 2}Ba(L{sup 3})(dmso){sub 2}(MeOH)]{sub 2} (L{sup 3}H{sub 4} = p-methyl[3.1.3.1] homo-oxa-calixarene), in which the crown ether is absent and two oxo-, phenoxo- and ether-bound barium atoms ensure the dimerization of the uranyl complex. (authors)

Organometallic Trinuclear Niobium Cluster Complex in Aqueous Solution: Synthesis and Characterization of Niobium Complexes Containing Nb-3(mu-eta(2):eta(2) (perpendicular to)-NCCH3)(mu(2)-O)(3)(6+) Cluster Core

DEFF Research Database (Denmark)

Joensen, H.A.N.; Hansson, G. K.; Kozlova, S.G.

2010-01-01

) and a broad peak at 565 nm (epsilon similar to 335 M-1 cm(-1)) in the UV-visible region. It is electron paramagnetic resonance (EPR)-active (g = 1.98), but no hyperfine interaction with the Nb-93 nuclear spin (I = 9/2) was observed. The cyclic voltammogram of [Nb-3(mu-eta(2):eta(2)-NCCH3)O-3(H2O)(9)](6+) in 4...

Tunable regioselectivity in 1,3-butadiene polymerization by using 2,6-bis(dimethyl-2-oxazolin-2-yl)pyridine incorporated transition metal (Cr, Fe and Co) catalysts

KAUST Repository

Gong, Dirong; Liu, Wen; Pan, Weijing; Chen, Tao; Jia, Xiaoyu; Huang, Kuo-Wei; Zhang, Xuequan

2015-01-01

Tridentate complexes Cr(III)Cl3L, [L = 2,6-bis(dimethyl-2-oxazolin-2-yl) pyridine], Fe(III)Cl3L, Fe(II)Cl2L and Co(II)Cl2L have been prepared and fully characterized. The solid structures of Cr(III)Cl3L, Fe(III)Cl3L and Co(II)Cl2L have been revealed by single crystal X-ray diffraction, and the Cr(III)Cl3L and Fe(III)Cl3L complexes both exhibit a distorted octahedral geometry, while the Co(II)Cl2L complex has a trigonal bipyramidal conformation. Four complexes have been examined in regioselective polymerization of butadiene in combination with MAO in toluene at room temperature. The trans-1,4, cis-1,4 enchainment of resultant polybutadiene are controlled by the metal center. Activated by MAO, complex Cr(III)Cl3L produces high level of trans-1,4 selectivity (trans-1,4 up to 93.3%) with moderate polymer yield, complexes Fe(III)Cl3L and Fe(II)Cl2L both show equal cis-1,4 and trans-1,4 with minor 1,2 selectivity (<10%), and Co(II)Cl2L catalyst displays predominated cis-1,4 selectivity, which can be shifted to 1,2 selectivity by adding PPh3 as an additive. Thus, tuning of the cis-1,4, trans-1,4 and 1,2 selectivity in full range via central metal and additive chosen by these 2,6-bis(dimethyl-2-oxazolin-2-yl) pyridine supported catalysts has been achieved. © 2015 Elsevier B.V. All rights reserved.

Tunable regioselectivity in 1,3-butadiene polymerization by using 2,6-bis(dimethyl-2-oxazolin-2-yl)pyridine incorporated transition metal (Cr, Fe and Co) catalysts

KAUST Repository

Gong, Dirong

2015-05-21

Tridentate complexes Cr(III)Cl3L, [L = 2,6-bis(dimethyl-2-oxazolin-2-yl) pyridine], Fe(III)Cl3L, Fe(II)Cl2L and Co(II)Cl2L have been prepared and fully characterized. The solid structures of Cr(III)Cl3L, Fe(III)Cl3L and Co(II)Cl2L have been revealed by single crystal X-ray diffraction, and the Cr(III)Cl3L and Fe(III)Cl3L complexes both exhibit a distorted octahedral geometry, while the Co(II)Cl2L complex has a trigonal bipyramidal conformation. Four complexes have been examined in regioselective polymerization of butadiene in combination with MAO in toluene at room temperature. The trans-1,4, cis-1,4 enchainment of resultant polybutadiene are controlled by the metal center. Activated by MAO, complex Cr(III)Cl3L produces high level of trans-1,4 selectivity (trans-1,4 up to 93.3%) with moderate polymer yield, complexes Fe(III)Cl3L and Fe(II)Cl2L both show equal cis-1,4 and trans-1,4 with minor 1,2 selectivity (<10%), and Co(II)Cl2L catalyst displays predominated cis-1,4 selectivity, which can be shifted to 1,2 selectivity by adding PPh3 as an additive. Thus, tuning of the cis-1,4, trans-1,4 and 1,2 selectivity in full range via central metal and additive chosen by these 2,6-bis(dimethyl-2-oxazolin-2-yl) pyridine supported catalysts has been achieved. © 2015 Elsevier B.V. All rights reserved.

Ion radical rupture of the carbon-carbon bond in oxidation of 1,3,1',3'-tetramethyl-2,3,2',3'- tetrahydro-2,2'-diperimidinyl

International Nuclear Information System (INIS)

Sabanov, V.Kh.; Kibizova, A.Yu.; Klimov, E.S.; Berberova, N.T.; Okhlobystin, O.Yu.

1987-01-01

Electrochemical and chemical oxidation of 1,3,1',3'-tetramethyl-2,3,2',3'-tetrahydro-2,2'-dipyriminyl takes place with rupture of the C-C bond in the initially formed cation radical. In the oxidation of the compound with aluminum chloride in nitrobenzene, ESR revealed a cation radical with an unresolved hyperfine structure. Oxidation of the dihydrodimer with nitrosonium perchlorate in nitrobenzene or nitromethane resulted in the same spectra. Cyclic volt-ampere diagrams are included

Oxovanadium(IV), cerium(III), thorium(IV) and dioxouranium(VI) complexes of 1-ethyl-4-hydroxy-3-(nitroacetyl)quinolin-2(1H)-one: Synthesis, spectral, thermal, fluorescence, DFT calculations, antimicrobial and antitumor studies

Science.gov (United States)

El-Shafiy, H. F.; Shebl, Magdy

2018-03-01

A new series of mononuclear oxovanadium(IV), cerium(III), thorium(IV) and dioxouranium(VI) complexes of a quinolinone ligand; 1-ethyl-4-hydroxy-3-(nitroacetyl)quinolin-2(1H)-one (H2L) have been synthesized. The metal complexes were characterized by different techniques such as elemental and thermal analyses, IR, 1H NMR, electronic, ESR, mass spectra and powder XRD, TEM in addition to magnetic susceptibility and conductivity measurements. The quinolinone ligand acts as a dibasic bidentate ligand forming mononuclear complexes, which can be formulated as: [(L)VO(H2O)2]·0.5H2O, [(L)M(NO3)x(H2O)y]·nH2O; M = Ce or Th, x = 1 or 2, y = 3 or 4 and n = 2 or 7 and [(L)UO2(H2O)x(MeOH)y]·nH2O; x = 2 or 3, y = 0 or 1 and n = 0.5 or 2.5. The photoluminescent properties of the prepared complexes were studied. The ligand and its thorium(IV) complex are characterized by an intense green emission. Kinetic parameters (Ea, A, ΔH, ΔS and ΔG) of the thermal decomposition stages have been evaluated using Coats-Redfern equations. The geometry of the ligand and its oxovanadium(IV) complex has been optimized using density functional theory (DFT). Total energy, energy of HOMO and LUMO, dipole moment and structure activity relationship were performed and confirmed practical antimicrobial and antitumor results. The antimicrobial activity of the ligand and its metal complexes was conducted against the microorganisms S. aureus, K. pnemonia, E. coli, P. vulgaris and C. albicans and the MIC values were determined. The antitumor activity of the ligand and its metal complexes was investigated against human Hepatocelluar carcinoma and human breast cancer cell lines.

Off-on fluorescent sensor based on the bis(2,4,7,8,9-pentamethyldipyrrolylmethene-3-yl)methane for detection of Cd{sup 2+} and Hg{sup 2+} cations

Energy Technology Data Exchange (ETDEWEB)

Bumagina, Natalia A., E-mail: nad@isc-ras.ru [G.A. Krestov Institute of Solution Chemistry of Russian Academy of Sciences (ISC RAS), 1 Akademicheskaya St., 153045 Ivanovo (Russian Federation); Antina, Elena V., E-mail: eva@isc-ras.ru [G.A. Krestov Institute of Solution Chemistry of Russian Academy of Sciences (ISC RAS), 1 Akademicheskaya St., 153045 Ivanovo (Russian Federation); Sozonov, Dmitry I., E-mail: super_dk@mail.ru [Ivanovo State University of Chemistry and Technology (ISUCT), 7 Sheremetevskij Prosp., 153000 Ivanovo (Russian Federation)

2017-03-15

The off-on fluorescent chemosensor based on the bis(2,4,7,8,9-pentamethyldipyrrolylmethene-3-yl)methane for detection of Cd{sup 2+} and Hg{sup 2+} ions was obtained and its metal ion sensing properties were investigated. The bis(dipyrrin) exhibited remarkably fluorescence enhancement (150- and 40-fold) to Cd{sup 2+} and Hg{sup 2+} ions, respectively, with significant color change on the background of other metal ions in propanol-1/cyclohexane (1:30) binary mixture. Consequently, it can be used as a “naked eye” indicator with an obvious color change from yellow-orange to orange-green color upon the addition of Cd{sup 2+} and Hg{sup 2+}. The fluorescent response mechanism of bis(dipyrrin) to Cd{sup 2+} and Hg{sup 2+} was based on the fluorescence enhancement effect upon complexation (CHEF) due to formation of a metal–ligand (2:2) complex [M{sub 2}L{sub 2}]. The detection limit of Cd{sup 2+} and Hg{sup 2+} ions was 2 × 10{sup –9} and 1.7 × 10{sup –8} M ions, respectively.

Absorption and fluorescence spectroscopy of 3-hydroxy-3-phenyl-1-o-carboxyphenyltriazene and its copper (II), nickel (II) and zinc (II) complexes: a novel fluorescence sensor

International Nuclear Information System (INIS)

Ressalan, S.; Iyer, C.S.P.

2005-01-01

Absorption and fluorescence spectroscopic properties of 3-hydroxy-3-phenyl-1-o-carboxyphenyltriazene (HT) are studied. The mechanism of photo-induced electron transfer (PET) followed by energy transfer process of the ligand and the Cu (II), Ni (II) and Zn (II) metal complexes have been investigated. The excited state photo induced intramolecular hydrogen transfer from N-OH to triazene 1-nitrogen atom is explained. The effect of pH, solvent and concentration on the absorption and fluorescence of the ligand is studied and it has been found that the absorption and fluorescence of HT is highly pH, solvent and concentration dependent. Participation of the N-OH proton of HT in the solvent assisted O to N-proton transfer has also been proposed. The fluorescence band shift and changes in intensity is modulated by protonation and complexation with metal ions. This fluorophore can thus be used as a pH dependent and M (n+1)+ /M n+ redox on/off switchable molecular sensor

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.

Effect of metal salts on antibacterial activity of zingiber officinale roscoe extract

International Nuclear Information System (INIS)

Sohail, T.; Yaqeen, Z.; Imran, H.; Rehman, Z.; Fatima, N.

2013-01-01

The antibacterial activity of ethanol extract of Zingiber Officinale Roscoe (ginger) and its combination with different salts like CuSO/sub 4/, ZnSO/sub 4/ and MnCl/sub 2/ was investigated. Both Gram positive and Gram negative bacteria were tested by agar diffusion method. The results showed that ethanol extract of Zingiber Officinale gave the maximum zone of inhibition at 50 mg/ml concentrations against Escherichia coli among Gram negative bacteria and against Staphylococcus aureus in Gram positive bacteria. However antibacterial activity of the ginger and metal salts combination was greater than activity of ethanol extract. These investigations indicate that though ethanol extract has antibacterial activity against Gram positive and Gram negative bacteria, ginger and metal salts complex has more inhibitory effect on microorganisms. Antibacterial activity was also compared with standard drug ampicillin. The minimum inhibitory concentration (MIC) of ginger extract and metal salts complexes against all test organisms ranged from 0.3125 to 2.5 mg/ml. (author)

An Efficient Synthesis of 3,4-Dihydro-3-substituted-2H-naphtho[2,1-e][1,3]oxazine Derivatives Catalyzed by Zirconyl(IV) Chloride and Evaluation of its Biological Activities

Energy Technology Data Exchange (ETDEWEB)

Kategaonkar, Amol H.; Sonar, Swapnil S.; Pokalwar, Rajkumar U.; Shingate, Bapurao B.; Shingare, Murlidhar S. [Babasaheb Ambedkar Marathwada University, Maharashtra (India); Kategaonkar, Atul H. [Maharashtra Institute of Pharmacy, Maharashtra (India)

2010-06-15

An efficient and novel one-pot synthesis of new 3,4-dihydro-3-substituted-2H-naphtho[2,1-e][1,3]oxazine derivatives from 1-naphthol, various anilines and formalin at room temperature grinding is presented. The six-membered N,O-heterocyclic skeleton was constructed via zirconyl(IV) chloride promoted Mannich type reaction. In vitro antimicrobial activities of synthesized compounds have been investigated against Gram-positive Bacillus subtilis, Gram negative Escherichia coli and two fungi Candida albicans and Aspergillus niger in comparison with standard drugs. The results of preliminary bioassay indicate that some of title compounds possess significant antibacterial and antifungal activity.

A Facile Solvent Free Microwave Induced Synthesis and Antibacterial Activity of Some 3-(2’-Hydroxyphenyl-5-(Substituted Aryl-2-Pyrazoline-N1-Caboxaldehydes

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Birbal Bajia

2007-01-01

Full Text Available A novel one pot formylation of 3-(2’-hydroxyphenyl-5-(substituted 2-pyrazolines has been carried out using microwave irradiation with formic acid. solvent free reaction afforded title compounds in 80-90% yield with high purity.synthesized compounds were tested for their antibacterial activity using standard drug.

Evaluation of DNA binding, DNA cleavage, protein binding, radical scavenging and in vitro cytotoxic activities of ruthenium(II) complexes containing 2,4-dihydroxy benzylidene ligands

Energy Technology Data Exchange (ETDEWEB)

Mohanraj, Maruthachalam; Ayyannan, Ganesan; Raja, Gunasekaran; Jayabalakrishnan, Chinnasamy, E-mail: drcjbstar@gmail.com

2016-12-01

The new ruthenium(II) complexes with hydrazone ligands, 4-Methyl-benzoic acid (2,4-dihydroxy-benzylidene)-hydrazide (HL{sup 1}), 4-Methoxy-benzoic acid (2,4-dihydroxy-benzylidene)-hydrazide (HL{sup 2}), 4-Bromo-benzoic acid (2,4-dihydroxy-benzylidene)-hydrazide (HL{sup 3}), were synthesized and characterized by various spectro analytical techniques. The molecular structures of the ligands were confirmed by single crystal X-ray diffraction technique. The DNA binding studies of the ligands and complexes were examined by absorption, fluorescence, viscosity and cyclic voltammetry methods. The results indicated that the ligands and complexes could interact with calf thymus DNA (CT-DNA) through intercalation. The DNA cleavage activity of the complexes was evaluated by gel electrophoresis assay, which revealed that the complexes are good DNA cleaving agents. The binding interaction of the ligands and complexes with bovine serum albumin (BSA) was investigated using fluorescence spectroscopic method. Antioxidant studies showed that the complexes have a strong radical scavenging properties. Further, the cytotoxic effect of the complexes examined on cancerous cell lines showed that the complexes exhibit significant anticancer activity. - Highlights: • Synthesis of ruthenium(II) hydrazone complexes • Molecular structure of the ligands was elucidated by single crystal X-ray diffraction method. • The ligands and complexes interact with CT-DNA via intercalation. • The complexes possess significant antioxidant activity against DPPH, OH and NO radicals. • The complex 6 shows higher IC{sub 50} value than the other complexes against cancer cells.

Cobalt(II), nickel(II), copper(II), and zinc(II) complexes with [3(5)]adamanzane, 1,5,9,13-tetraazabicyclo[7.7.3]nonadecane and [(2.3)(2).2(1)]adamanzane, 1,5,9,12-tetraazabicyclo[7.5.2]hexadecane

DEFF Research Database (Denmark)

Broge, Louise; Pretzmann, Ulla; Jensen, Nicolai

2001-01-01

) and of three cobalt(II), four nickel(II), one copper(II), and two zinc(II) complexes with [3(5)]adamanzane. For nine of these compounds (2-8, 10b, and 12) the single-crystal X-ray structures were determined. The coordination geometry around the metal ion is square pyramidal in [Cu([(2.3)(2).2(1)]adz)Br]ClO4 (2......) and trigonal bipyramidal in the isostructural structures [Cu([3(5)]adz)Br]Br (3), [Ni-([3(5)]adz)Cl]Cl (5), [Ni([3(5)]adz)Br]Br (6), and [Co([3(5)]adz)Cl]Cl (8). In [Ni([3(5)]adz)(NO3)]NO3 (4) and [Ni([3(5)]-adz)(ClO4)]ClO4 (7) the coordination geometry around nickel(II) is a distorted octahedron...... with the inorganic ligands at cis positions. The coordination polyhedron around the metal ion in [Co([3(5)]adz)][ZnCl4] (10b) and [Zn([3(5)]adz)][ZnCl4] (12) is a slightly distorted tetrahedron. Anation equilibrium constants were determined spectrophotometrically for complexes 2-6 at 25 and 40 degreesC and fall...

Ternary composite of TiO2 nanotubes/Ti plates modified by g-C3N4 and SnO2 with enhanced photocatalytic activity for enhancing antibacterial and photocatalytic activity.

Science.gov (United States)

Faraji, Masoud; Mohaghegh, Neda; Abedini, Amir

2018-01-01

A series of g-C 3 N 4 -SnO 2 /TiO 2 nanotubes/Ti plates were fabricated via simple dipping of TiO 2 nanotubes/Ti in a solution containing SnCl 2 and g-C 3 N 4 nanosheets and finally annealing of the plates. Synthesized plates were characterized by various techniques. The SEM analysis revealed that the g-C 3 N 4 -SnO 2 nanosheets with high physical stability have been successfully deposited onto the surface of TiO 2 nanotubes/Ti plate. Photocatalytic activity was investigated using two probe chemical reactions: oxidative decomposition of acetic acid and oxidation of 2-propanol under irradiation. Antibacterial activities for Escherichia coli (E. coli) bacteria were also investigated in dark and under UV/Vis illuminations. Detailed characterization and results of photocatalytic and antibacterial activity tests revealed that semiconductor coupling significantly affected the photocatalyst properties synthesized and hence their photocatalytic and antibacterial activities. Modification of TiO 2 nanotubes/Ti plates with g-C 3 N 4 -SnO 2 deposits resulted in enhanced photocatalytic activities in both chemical and microbial systems. The g-C 3 N 4 -SnO 2 /TiO 2 nanotubes/Ti plate exhibited the highest photocatalytic and antibacterial activity, probably due to the heterojunction between g-C 3 N 4 -SnO 2 and TiO 2 nanotubes/Ti in the ternary composite plate and thus lower electron/hole recombination rate. Based on the obtained results, a photocatalytic and an antibacterial mechanism for the degradation of E. coli bacteria and chemical pollutants over g-C 3 N 4 -SnO 2 /TiO 2 nanotubes/Ti plate were proposed and discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

Arp2/3 complex activity in filopodia of spreading cells

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Mendes Paula M

2008-12-01

Full Text Available Abstract Background Cells use filopodia to explore their environment and to form new adhesion contacts for motility and spreading. The Arp2/3 complex has been implicated in lamellipodial actin assembly as a major nucleator of new actin filaments in branched networks. The interplay between filopodial and lamellipodial protrusions is an area of much interest as it is thought to be a key determinant of how cells make motility choices. Results We find that Arp2/3 complex localises to dynamic puncta in filopodia as well as lamellipodia of spreading cells. Arp2/3 complex spots do not appear to depend on local adhesion or on microtubules for their localisation but their inclusion in filopodia or lamellipodia depends on the activity of the small GTPase Rac1. Arp2/3 complex spots in filopodia are capable of incorporating monomeric actin, suggesting the presence of available filament barbed ends for polymerisation. Arp2/3 complex in filopodia co-localises with lamellipodial proteins such as capping protein and cortactin. The dynamics of Arp2/3 complex puncta suggests that they are moving bi-directionally along the length of filopodia and that they may be regions of lamellipodial activity within the filopodia. Conclusion We suggest that filopodia of spreading cells have regions of lamellipodial activity and that this activity affects the morphology and movement of filopodia. Our work has implications for how we understand the interplay between lamellipodia and filopodia and for how actin networks are generated spatially in cells.

Synthesis and characterization of n-alkylamino derivatives of vitamin K3: Molecular structure of 2-propylamino-3-methyl-1,4-naphthoquinone and antibacterial activities

Science.gov (United States)

Chadar, Dattatray; Camilles, Maria; Patil, Rishikesh; Khan, Ayesha; Weyhermüller, Thomas; Salunke-Gawali, Sunita

2015-04-01

We would like to introduce eight analogues of n-alkylamino derivatives of vitamin K3 (2-methyl-1,4-naphthoquinone) viz, 2-(n-alkylamino)-3-methyl-1,4-naphthoquinone (where n-alkyl is methyl; LM-1, ethyl; LM-2, propyl; LM-3, butyl; LM-4, pentyl; LM-5, hexyl; LM-6, heptyl; LM-7, octyl; LM-8). All the above analogues have been successfully synthesized from vitamin K3 and characterized using different analytical techniques. Furthermore, in order to understand the mechanistic aspects of formation of LM-1 to LM-8 compounds, we could propose the mechanism. The FT-IR analysis of LM-1 to LM-8 indicate the presence of characteristic band of Nsbnd H group ∼3287-3364 cm-1, the variation was attributed to extensive intramolecular hydrogen bonding interaction. The molecular structure of LM-3 compound has been confirmed by single crystal X-ray diffraction analysis. LM-3 compound crystallises in triclinic space group P1. There were four independent molecules in asymmetric unit cell and their molecular interactions observed via Nsbnd H⋯O, Csbnd H⋯O and π-π stacking of quinonoid rings. Pharmacological potential of all compounds has been evaluated in terms of their antibacterial activities against Pseudomonas aeruginosa and Staphylococcus aureus. All the compounds were active against both the strains while LM-2 was found to be more effective with a minimum inhibition concentration of 0.3125 μg/mL and 0.156 μg/mL respectively.

Dihydroxo-bridged dimeric Cu(II) system containing sandwiched non-coordinating phenylacetate anion: Crystal structure, spectroscopic, anti-bacterial, anti-fungal and DNA-binding studies of [(phen)(H2O)Cu(OH)2Cu(H2O)(phen)]2L.6H2O: (HL = phenylacetic acid; phen = 1,10-phenanthroline)

Science.gov (United States)

Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Shah, Naseer Ali

2017-09-01

This paper reports the synthesis, X-ray crystal structure, DNA-binding, antibacterial and antifungal studies of a rare dihydroxo-bridged dinuclear copper(II) complex including 1,10-phenanthroline (Phen) ligands and phenylacetate (L) anions, [Cu2(Phen)2(OH)2(H2O)2].2L.6H2O. Structural data revealed distorted square-pyramidal geometry for each copper(II) atom with the basal plane formed by the two nitrogen atoms of the phenantroline ligand and the oxygen atoms of two bridging hydroxyl groups. The apical positions are filled by the oxygen atom from a water molecule. This forms a centrosymmetric cationic dimer where the uncoordinated phenylacetate ligands serve to balance the electrical charge. The dimers interact by means of hydrogen bonds aided by the coordinated as well as uncoordinated water molecules and phenyl-acetate moieties in the crystal lattice. The binding ability of the complex with salmon sperm DNA was determined using cyclic voltammetry and absorption spectroscopy yielding binding constants 2.426 × 104 M-1 and 1.399 × 104 M-1, respectively. The complex was screened against two Gram-positive (Micrococcus luteus and Bacillus subtilis) and one Gram-negative (Escherichia coli) bacterial strains exhibiting significant activity against all the three strains. The complex exhibited significant, moderate and no activity against fungal strains Mucor piriformis, Helminthosporium solani and Aspergillus Niger, respectively. These preliminary tests indicate the competence of the complex towards the development of a potent biological drug.

Synthesis of Fe3O4@SiO2@OSi(CH2)3NHRN(CH2PPh2)2PdCl2 type nanocomposite complexes: Highly efficient and magnetically-recoverable catalysts in vitamin K3 synthesis.

Science.gov (United States)

Uruş, Serhan

2016-12-15

The synthesis of aminomethylphosphine-metal complexes have opened a new perspective to the catalytic applications of organic compounds. Magnetic Fe3O4 nano-core was synthesized using the closed quartz tube with Teflon cover and microwaved 200°C for 1h with power controlled instrument set to max. 600W. Novel nano-composite supported; Fe3O4@SiO2(CH2)3NHArN(CH2PPh2)2 and Fe3O4@SiO2(CH2)3N(CH2PPh2)2 type bis(diphenylphosphinomethyl)amino ligands and their Pd(II) complexes have been synthesized and characterized with FT-IR, SEM, EDX, TEM, UV-Visible, XRD and TG/DTA techniques. All the complexes were used as heterogeneous catalysts in the oxidation of 2-methyl naphthalene (2MN) to 2-methyl-1, 4-naphthoquinone (vitamin K3, menadione, 2MNQ) in the presence of hydrogen peroxide and acetic acid. Selectivity reached about 55-60% with a conversion of 90-96% using the nano-magnetite supported aminomethylphosphine-Pd(II) complexes. The complexes were very active in three times in the catalytic recycling experiments in five catalytic cycles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Raman and Fluorescence Spectroscopy of CeO2, Er2O3, Nd2O3, Tm2O3, Yb2O3, La2O3, and Tb4O7

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Jianlan Cui

2015-01-01

Full Text Available To better understand and ascertain the mechanisms of flotation reagent interaction with rare earth (RE minerals, it is necessary to determine the physical and chemical properties of the constituent components. Seven rare earth oxides (CeO2, Er2O3, Nd2O3, Tm2O3, Yb2O3, La2O3, and Tb4O7 that cover the rare earth elements (REEs from light to heavy REEs have been investigated using Raman spectroscopy. Multiple laser sources (wavelengths of 325 nm, 442 nm, 514 nm, and 632.8 nm for the Raman shift ranges from 100 cm−1 to 5000 cm−1 of these excitations were used for each individual rare earth oxide. Raman shifts and fluorescence emission have been identified. Theoretical energy levels for Er, Nd, and Yb were used for the interpretation of fluorescence emission. The experimental results showed good agreement with the theoretical calculation for Er2O3 and Nd2O3. Additional fluorescence emission was observed with Yb2O3 that did not fit the reported energy level diagram. Tb4O7 was observed undergoing laser induced changes during examination.

Novel 2D or 3D alkaline-earth metal sulfonate-phosphonates based on [O 3S-C 2H 4-PO 3H] 2- ligand

Science.gov (United States)

Du, Zi-Yi; Wen, He-Rui; Xie, Yong-Rong

2008-11-01

Three novel alkaline-earth metal sulfonate-phosphonates based on [O 3S-C 2H 4-PO 3H] 2- ligand, namely, [Ca(O 3SC 2H 4PO 3H)(H 2O) 2] ( 1), [Sr(O 3SC 2H 4PO 3H)] ( 2) and [Ba 2(O 3SC 2H 4PO 3H) 2] ( 3), have been synthesized by hydrothermal reactions. They represent the first structurally characterized alkaline-earth metal complexes of phosphonic acid attached with a sulfonate group. The structure of compound 1 features a 2D layer based on 1D chains of [Ca 2(PO 3) 2] bridged by -CH 2-CH 2-SO 3- groups. Compounds 2 and 3 show pillar-layer architecture based on two different inorganic layers linked by -CH 2-CH 2- groups. The inorganic layer in compound 2 features a 1D chain of edge-sharing SrO 8 polyhedra whereas that in compound 3 features an edge-sharing Ba 2O 14 di-polyhedral unit which is further corner-shared with four neighboring ones. The [O 3S-C 2H 4-PO 3H] 2- ligand shows diverse coordination modes in the three alkaline-earth metal sulfonate-phosphonates.

New Fluorescence Probes for Biomolecules

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Katarzyna Jurek

2015-07-01

Full Text Available Steady state fluorescence measurements have been used for the investigation of interaction between the bovine serum albumin (BSA and fluorescence probes: 3-hydroxy-2,4- bis[(3-methyl-1,3-benzoxazol-2(3H-ylidenemethyl]cyclobut-2-en-1-one (SQ6, 3-hydroxy- 2,4-bis[(3-methyl-1,3-benzothiazol-2(3H-ylidenemethyl]cyclobut-2-en-1-one (SQ7 and 3-hydroxy-2,4-bis[(1,3,3-trimethyl-1,3-dihydro-2H-indol-2-ylidenemethyl]cyclobut-2-en-1-one (SQ8. The binding constant between bovine serum albumin and squarine dyes has been determined by using both the Benesi-Hildebrand and Stern-Volmer equations. The negative value of free energy change indicates the existence of a spontaneous complexation process of BSA with squarine dyes.

Fluorescent property of 3-hydroxymethyl imidazo[1,2-a]pyridine and pyrimidine derivatives

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Velázquez-Olvera Stephania

2012-08-01

Full Text Available Abstract Background Imidazo[1,2-a]pyridines and pyrimidines are important organic fluorophores which have been investigated as biomarkers and photochemical sensors. The effect on the luminescent property by substituents in the heterocycle and phenyl rings, have been studied as well. In this investigation, series of 3-hydroxymethyl imidazo[1,2-a]pyridines and pyrimidines were synthesized and evaluated in relation to fluorescence emission, based upon the hypothesis that the hydroxymethyl group may act as an enhancer of fluorescence intensity. Results Compounds of both series emitted light in organic solvents dilutions as well as in acidic and alkaline media. Quantitative fluorescence spectroscopy determined that both fused heterocycles fluoresced more intensely than the parent unsubstituted imidazo[1,2-a]azine fluorophore. In particular, 3-hydroxymethyl imidazo[1,2-a]pyridines fluoresced more intensely than 3-hydroxymethyl imidazo[1,2-a]pyrimidines, the latter emitting blue light at longer wavelengths, whereas the former emitted purple light. Conclusion It was concluded that in most cases the hydroxymethyl moiety did act as an enhancer of the fluorescence intensity, however, a comparison made with the fluorescence emitted by 2-aryl imidazo[1,2-a]azines revealed that in some cases the hydroxymethyl substituent decreased the fluorescence intensity.

Kinetics of degradation of ascorbic acid by cyclic voltammetry method

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Grudić Veselinka V.

2015-01-01

Full Text Available Cyclic voltammetry was used to examine the kinetics of degradation of ascorbic acid (AA at different temperatures. It has been shown that the reduction of the concentration of AA in all temperatures follow the kinetics of the first order reaction. The rate constant of the oxidation reaction increases with temperature as follows: 5x10-5; 2x10-4; 1x10-3 and 3x10-3 min-1 at temperatures of 25°C, 35°C, 65°C and 90°C, respectively. The temperature dependence of the rate constant follows Arrhenius equation, and the value of activation energy of the reaction degradation is 48.2 kJ mol-1 . The effect of storage time at a temperature of 90 °C on AA content in fresh juice of green peppers was investigated. It was shown that AA oxidation reaction in the juice is also the first order reaction, while the lower rate constant in relation to the pure AA (5x10-3 min-1 indicates the influence of other substances present in peppers.

The preparation and role of Li_2ZrO_3 surface coating LiNi_0_._5Co_0_._2Mn_0_._3O_2 as cathode for lithium-ion batteries

International Nuclear Information System (INIS)

Xu, Yue; Liu, Yang; Lu, Zhongpei; Wang, Haiying; Sun, Deqin; Yang, Gang

2016-01-01

Graphical abstract: LiNi_0_._5Co_0_._2Mn_0_._3O_2 is coated by Li_2ZrO_3 layer with the thickness about 20 nm. Li_2ZrO_3 coating effectively improves cycling performance and rate capability. LZO-LMO delivers 194 mAh g"−"1 at 0.2 C and presents improved cyclic performance at 55 °C. - Highlights: • LiNi_0_._5Co_0_._2Mn_0_._3O_2 is coated by Li_2ZrO_3 layer with the thickness about 20 nm. • Li_2ZrO_3 coating effectively improves cycling performance and rate capability. • LZO-LMO delivers 194 mAh g"−"1 at 0.2 C and presents improved cyclic performance at 55 °C. • Li_2ZrO_3 coating suppresses cation dissolution and enhances the structural stability. - Abstract: Li_2ZrO_3-coated LiNi_0_._5Co_0_._2Mn_0_._3O_2 (LZO-LMO) is successful synthesized by using a wet chemical method. Li_2ZrO_3 coating formed a uniform layer on LiNi_0_._5Co_0_._2Mn_0_._3O_2 particles (LMO) without changing the crystal structure. Cyclic voltammetry (CV) and charge–discharge tests show that the Li_2ZrO_3-modified layer can improve the cyclic and rate performance. In the cut-off voltage of 2.7–4.6 V, LZO-LMO maintains 86% of the initial capacity at the 50th cycle, which is much higher than LMO with the retention of 66% of the initial capacity. The coating layer of LZO plays the positive role in conductivity of lithium diffusion and improves rate performance of LMO. At 10 C rates, LZO-LMO delivers the initial capacity of 95 mAh g"−"1 which is much higher than 40 mAh g"−"1 delivered by LMO. At the environmental temperature of 55 °C, LZO-LMO delivers the initial capacity of 194 mAh g"−"1 at 0.2 C rate and presents an improved cyclic performance in comparison with LMO. The elemental analysis of electrodes carried out after 50 charge/discharge cycles shows minor Ni content deviation in LMO, but LZO-LMO still remains the stoichiometric ratio, because the Li_2ZrO_3 coating efficiently hinders the metal dissolution during charge/discharge.

(μ-3-Acetyl-5-carboxyl­ato-4-methyl­pyrazolido-1:2κ4 N 2,O 3:N 1,O 5)-μ-chlorido-tetra­pyridine-1κ2 N,2κ2 N-chlorido-1κCl-dicopper(II) propan-2-ol solvate

Science.gov (United States)

Malinkin, Sergey; Penkova, Larisa; Pavlenko, Vadim A.; Haukka, Matti; Fritsky, Igor O.

2009-01-01

The title compound, [Cu2(C7H6N2O3)Cl2(C5H5N)4]·C3H8O, is a binuclear pyrazolate complex, in which the two CuII atoms have different coordination numbers and are connected by a bridging Cl atom. One CuII atom has a distorted square-pyramidal coordination environment formed by two pyridine N atoms, one bridging Cl atom and an N,O-chelating pyrazolate ligand. The other CuII atom adopts an octa­hedral geometry defined by two pyridine N atoms at the axial positions, two Cl atoms and the coordinated pyrazolate ligand in the equatorial plane. An O—H⋯O hydrogen bond connects the complex mol­ecules and propan-2-ol solvent mol­ecules into pairs. These pairs form columns along the a axis. PMID:21577764

Metal Complexes of New Bioactive Pyrazolone Phenylhydrazones; Crystal Structure of 4-Acetyl-3-methyl-1-phenyl-2-pyrazoline-5-one phenylhydrazone Ampp-Ph

Directory of Open Access Journals (Sweden)

Omoruyi G. Idemudia

2016-05-01

Full Text Available The condensation reaction of phenylhydrazine and dinitrophenylhydrazine with 4-acetyl and 4-benzoyl pyrazolone precipitated air-stable acetyldinitrophenylhydrazone Ampp-Dh, benzoylphenylhydrazone Bmpp-Ph and benzoyldinitrophenylhydrazone Bmpp-Dh in their keto imine form; a study inspired by the burning interest for the development of new bioactive materials with novel properties that may become alternative therapeutic agents. Elemental analysis, FTIR, 1H, and 13C NMR, and mass spectroscopy have been used to justify their proposed chemical structures, which were in agreement with the single crystal structure of Bmpp-Dh earlier reported according to X-ray crystallography. The single crystal structure of 4-acetyl-3-methyl-1-phenyl--pyrazoline-5-one phenylhydrazone Ampp-Ph, which crystallizes in a triclinic crystal system with a P-1 (No. 2 space group is presented. Octahedral Mn(II, Ni(II, Co(II, and Cu(II complexes of these respective ligands with two molecules each of the bidentate Schiff base, coordinating to the metal ion through the azomethine nitrogen C=N and the keto oxygen C=O, which were afforded by the reaction of aqueous solutions of the corresponding metal salts with the ligands are also reported. Their identity and proposed structures were according to elemental analysis, FTIR spectroscopy, UV-VIS spectrophotometry (electronic spectra and Bohr magnetic moments, as well as thermogravimetric analysis (TGA results. A look at the antibacterial and antioxidant activities of synthesized compounds using the methods of the disc diffusion against some selected bacterial isolates and 1,1-diphenyl-2-picryl-hydrazil (DPPH respectively, showed biological activities in relation to employed standard medicinal drugs.

Synthesis, Antibacterial and Antitubercular Activities of Some 5H-Thiazolo[3,2-a]pyrimidin-5-ones and Sulfonic Acid Derivatives

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Dong Cai

2015-09-01

Full Text Available A series of 5H-thiazolo[3,2-a]pyrimidin-5-ones were synthesized by the cyclization reactions of S-alkylated derivatives in concentrated H2SO4. Upon treatment of S-alkylated derivatives at different temperatures, intramolecular cyclization to 7-(substituted phenylamino-5H-thiazolo[3,2-a]pyrimidin-5-ones or sulfonation of cyclized products to sulfonic acid derivatives occurred. The structures of the target compounds were confirmed by IR, 1H-NMR, 13C-NMR and HRMS studies. The compounds were evaluated for their preliminary in vitro antibacterial activity against some Gram-positive and Gram-negative bacteria and screened for antitubercular activity against Mycobacterium tuberculosis by the broth dilution assay method. Some compounds showed good antibacterial and antitubercular activities.

Ag-decorated Fe_3O_4@SiO_2 core-shell nanospheres: Seed-mediated growth preparation and their antibacterial activity during the consecutive recycling

International Nuclear Information System (INIS)

Li, Miaomiao; Wu, Wenjie; Qiao, Ru; Tan, Linxiang; Li, Zhengquan; Zhang, Yong

2016-01-01

We demonstrated a seed-mediated growth approach to synthesize Ag nanoparticles-decorated Fe_3O_4@SiO_2 core-shell nanospheres without use of surface functionalization. The particle size and decoration density of the immobilized Ag nanoparticles on SiO_2 surface were tunable by adjusting the added AgNO_3 concentration and the alternating repetition times in seed-mediated growth procedure. The as-prepared Ag-decorated Fe_3O_4@SiO_2 nanospheres exhibited excellent antibacterial activities against Escherichia coli, Bacillus subtilis and Candida albicans, in which the minimum inhibitory concentration were 12.5 μg mL"−"1, 50 μg mL"−"1 and 50 μg mL"−"1, respectively. It is speculated that their antibacterial activity is attributed to both the interaction of released Ag ions with the functional groups of vital enzymes and proteins and the strong oxidation of reactive oxygen species generated under the action of photoinduced electrons in Ag nanoparticles. Besides studying their antibacterial mechanism, we also investigated the variation of antibacterial activity of these heterostructured nanospheres during the consecutive magnetic separation and recycling. It shows that the magnetic antibacterial agent could be reused and its activity remained stable even after nine cycles, which enable it to be promisingly applied in biomedical areas. - Highlights: • Ag-decorated Fe_3O_4@SiO_2 were synthesized via a seed-mediated growth method. • The core-shell heterostructures exhibited excellent antibacterial activity. • The activity was attributed to the effect of released Ag"+ with ROS oxidation. • The antibacterial agent was reused during magnetic separation and recycling.

Structural features of AgCaCdMg2(PO4)3 and AgCd2Mg2(PO4)3, two new compounds with the alluaudite-type structure, and their catalytic activity in butan-2-ol conversion

International Nuclear Information System (INIS)

Kacimi, Mohammed; Ziyad, Mahfoud; Hatert, Frederic

2005-01-01

AgCaCdMg 2 (PO 4 ) 3 and AgCd 2 Mg 2 (PO 4 ) 3 , two new compounds with the alluaudite-type structure, were synthesized by a solid state reaction in air at 750 deg. C. The X-ray powder diffraction pattern of AgCaCdMg 2 (PO 4 ) 3 indicates the presence of small amounts of (Ca, Mg) 3 (PO 4 ) 2 with the whitlockite structure, as impurity, whereas AgCd 2 Mg 2 (PO 4 ) 3 is constituted by pure alluaudite. The Rietveld refinements of the X-ray powder diffraction patterns indicate an ordered cationic distribution for AgCd 2 Mg 2 (PO 4 ) 3 , with Ag on A(2)', Cd on A(1) and M(1), and Mg on M(2), whereas a disordered distribution of Cd and Ca between the A(1) and M(1) sites is observed for AgCaCdMg 2 (PO 4 ) 3 . The catalytic properties of these compounds has been measured in reaction of butan-2-ol dehydrogenation. In the absence of oxygen, both samples exhibit poor dehydrogenation activity. All samples displayed no dehydration activity. Introduction of oxygen into the feed changed totally the catalytic behavior of the catalysts. The production of methyl ethyl ketone increases with time on stream and the reaction temperature. AgCaCdMg 2 (PO 4 ) 3 is more efficient than AgCd 2 Mg 2 (PO 4 ) 3

Preparation of YBa2Cu3O7-δ powders by the thermal decomposition of a heteronuclear complex, CuY1/3Ba2/3(dhbaen)(NO3)1/3(H2O)3

International Nuclear Information System (INIS)

Hasegawa, E.; Aono, H.; Sadaoka, Y.; Traversa, E.

1999-01-01

YBa 2 Cu 3 O 7-δ powders were prepared by the thermal decomposition of a heteronuclear complex, CuY 1/3 Ba 2/3 (dhbaen)(NO 3 ) 1/3 (H 2 O) 3 . The products of the complex thermal decomposition were analyzed by TG-DTA, XRD, SEM-Auger and XPS. The decomposition of the CuY 1/3 Ba 2/3 -complex was obtained at about 500 C and the product was a mixture of oxides and carbonates. The formation of YBa 2 Cu 3 O 7-δ proceeded at 800 C, with a gradual decomposition of the carbonates. A homogeneous distribution of each element, Y, Ba, and Cu, was observed for the decomposed CuY 1/3 Ba 2/3 -complex by SEM-Auger analysis. The binding energy values of Ba3d 5/2 and O1s photolines from Ba and O in the superconductive lattice did not shift during the sputtering period. Furthermore, the formation of Ba rich regions on the surface was depressed by using the complex as a starting material for homogeneous 123-oxide, YBa 2 Cu 3 O 7-δ . (orig.)

Cyclic [G(2',5')pA(3',5')p] is the metazoan second messenger produced by DNA-activated cyclic GMP-AMP synthase.

Science.gov (United States)

Gao, Pu; Ascano, Manuel; Wu, Yang; Barchet, Winfried; Gaffney, Barbara L; Zillinger, Thomas; Serganov, Artem A; Liu, Yizhou; Jones, Roger A; Hartmann, Gunther; Tuschl, Thomas; Patel, Dinshaw J

2013-05-23

Recent studies identified cyclic GMP-AMP (cGAMP) as a metazoan second messenger triggering an interferon response. cGAMP is generated from GTP and ATP by cytoplasmic dsDNA sensor cGAMP synthase (cGAS). We combined structural, chemical, biochemical, and cellular assays to demonstrate that this second messenger contains G(2',5')pA and A(3',5')pG phosphodiester linkages, designated c[G(2',5')pA(3',5')p]. We show that, upon dsDNA binding, cGAS is activated through conformational transitions, resulting in formation of a catalytically competent and accessible nucleotide-binding pocket for generation of c[G(2',5')pA(3',5')p]. We demonstrate that cyclization occurs in a stepwise manner through initial generation of 5'-pppG(2',5')pA prior to cyclization to c[G(2',5')pA(3',5')p], with the latter positioned precisely in the catalytic pocket. Mutants of cGAS dsDNA-binding or catalytic pocket residues exhibit reduced or abrogated activity. Our studies have identified c[G(2',5')pA(3',5')p] as a founding member of a family of metazoan 2',5'-containing cyclic heterodinucleotide second messengers distinct from bacterial 3',5' cyclic dinucleotides. Copyright © 2013 Elsevier Inc. All rights reserved.

Electronic Properties and Photovoltaic Performances of a Series of Oligothiophene Copolymers Incorporating Both Thieno[3,2-b]thiophene and 2,1,3-Benzothiadiazole Moieties.

Science.gov (United States)

Biniek, Laure; Chochos, Christos L; Hadziioannou, Georges; Leclerc, Nicolas; Lévêque, Patrick; Heiser, Thomas

2010-04-06

A series of donor-acceptor alternated conjugated copolymers, composed of thiophene, bithiophene, thieno[3,2-b]thiophene, and 2,1,3-benzothiadiazole units and differing from each other by the nature and the number of 3-alkylthiophene in the backbone, have been synthesized by Stille cross-coupling polymerization. The material's optical and electrochemical properties, in solution and in thin films, have been investigated using UV-Visible absorption and cyclic voltammetry. Bulk heterojunction solar cells using blends of the newly synthesized copolymers, as electron donor, and C60-PCBM or C70-PCBM, as electron transporting material, have been elaborated. A maximum power conversion efficiency of 1.8% is achieved with a 1:4 PPBzT(2) -C12:C70-PCBM weight ratio. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Utility of Lithium in Rare-Earth Metal Reduction Reactions to Form Nontraditional Ln2+ Complexes and Unusual [Li(2.2.2-cryptand)]1+ Cations.

Science.gov (United States)

Huh, Daniel N; Darago, Lucy E; Ziller, Joseph W; Evans, William J

2018-02-19

The utility of lithium compared to other alkali metals in generating Ln 2+ rare-earth metal complexes via reduction of Ln 3+ precursors in reactions abbreviated as LnA 3 /M (Ln = rare-earth metal; A = anionic ligand; M = alkali metal) is described. Lithium reduction of Cp' 3 Ln (Cp' = C 5 H 4 SiMe 3 ; Ln = Y, Tb, Dy, Ho) under Ar in the presence of 2.2.2-cryptand (crypt) forms new examples of crystallographically characterizable Ln 2+ complexes of these metals, [Li(crypt)][Cp' 3 Ln]. In each complex, lithium is found in an N 2 O 4 donor atom coordination geometry that is unusual for the cryptand ligand. Magnetic susceptibility data on these new examples of nontraditional divalent lanthanide complexes are consistent with 4f n 5d 1 electronic configurations. The Dy and Ho complexes have exceptionally high single-ion magnetic moments, 11.35 and 11.67 μ B , respectively. Lithium reduction of Cp' 3 Y under N 2 at -35 °C forms the Y 2+ complex (Cp' 3 Y) 1- , which reduces dinitrogen upon warming to room temperature to generate the (N 2 ) 2- complex [Cp' 2 Y(THF)] 2 (μ-η 2 :η 2 -N 2 ). These results provide insight on the factors that lead to reduced dinitrogen complexes and/or stable divalent lanthanide complexes as a function of the specific reducing agent and conditions.

Synthesis and antibacterial activity of some new 3-hydroxy-2-naphthoic acid hydrazide derivatives for dyeing polyester fabrics

Directory of Open Access Journals (Sweden)

Abd El-Galil M. Khalil

2016-03-01

Full Text Available Dibenzobarallene was used as a key intermediate for the synthesis of 2-(3-hydroxy-2-naphthoyl-3,4,4a,5,10,10a-hexahydro-1H-5,10-benzenobenzo[g]phthalazine-1,4-dione (2. The previous compound was coupled with the appropriate diazonium chloride to give the corresponding 4-arylazo-2-naphthol derivatives 3a–l. Also, nitration, nitrosation and bromination of compound 2 afforded the corresponding nitro, nitroso and bromo derivatives 4–6, respectively. The synthesized compounds were established and evaluated as antibacterial agents. The results showed clearly that compounds 2, 3a, 3c, 3d, 3g, 3i, 4, 5 and 6 exhibited interesting high activities compared with reference drugs. Also, these compounds were applied to polyester as disperse dyes in which their color measurement and fastness properties were evaluated.

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.

Variation sweep rate cyclic voltammetry on the capacitance electrode activated carbon/PVDF with polymer electrolyte

Science.gov (United States)

Rohmawati, L.; Setyarsih, W.; Nurjannah, T.

2018-03-01

Sweep rate of the process voltammetry cyclic characterization is very influential towards the electrode capacitance value, especially on activated carbon electrodes/PVDF. A simple method of this research by use a mixing for electrode activated carbon/10 wt. % PVDF and the separator is made of a polymer electrolyte (PVA/H3PO4) by a sol gel method. The prototype supercapacitor is made in the form of a sandwich with a separator placed between two electrodes. Electrodes and separators are arranged in layers at a pressure of 1500 psi, then heated at 50°C for 10 minutes. Next done cyclic voltammetry in a potential range of -1 V to 1 V with a sweep rate of 5 mV/s, 10 mV/s, 20 mV/s, 25 mV/s and 50 mV/s. This results of curves voltammogram is reversible, the most wide curve on the sweep rate of 5 mV/s and most narrow curve on a sweep rate of 50 mV/s. Supercapacitor capacitance values obtained by 86 F/g, 43 F/g, 21 F/g, 16 F/g, and 8 F/g.

Oxidative dehydrogenation of the 2-aminomethylpyridine (EDTA) ruthenium (III) complex

International Nuclear Information System (INIS)

Toma, H.E.; Tsurumaki, M.

1990-01-01

The oxidative dehydrogenation of the 2-aminomethylpyridine (ampy) ligand coordinated to the (EDTA)RU(III) complex was investigated based on cyclic voltammetry, spectoelectrochemistry and stopped-flow kinetic measurements in aqueous solution. The reaction mechanism is consistent with the deprotonation of the ampy ligand (pk a =7.48), followed by a reversible one-electron transfer step. The intermediate species generated at this step undergoes a metal-induced electron transfer process, with k=227 s -1 , converting into the corresponding 2-iminomethylpyridine complex. (author) [pt

Electroreduction of CO2 Catalyzed by a Heterogenized Zn–Porphyrin Complex with a Redox-Innocent Metal Center

Science.gov (United States)

2017-01-01

Transition-metal-based molecular complexes are a class of catalyst materials for electrochemical CO2 reduction to CO that can be rationally designed to deliver high catalytic performance. One common mechanistic feature of these electrocatalysts developed thus far is an electrogenerated reduced metal center associated with catalytic CO2 reduction. Here we report a heterogenized zinc–porphyrin complex (zinc(II) 5,10,15,20-tetramesitylporphyrin) as an electrocatalyst that delivers a turnover frequency as high as 14.4 site–1 s–1 and a Faradaic efficiency as high as 95% for CO2 electroreduction to CO at −1.7 V vs the standard hydrogen electrode in an organic/water mixed electrolyte. While the Zn center is critical to the observed catalysis, in situ and operando X-ray absorption spectroscopic studies reveal that it is redox-innocent throughout the potential range. Cyclic voltammetry indicates that the porphyrin ligand may act as a redox mediator. Chemical reduction of the zinc–porphyrin complex further confirms that the reduction is ligand-based and the reduced species can react with CO2. This represents the first example of a transition-metal complex for CO2 electroreduction catalysis with its metal center being redox-innocent under working conditions. PMID:28852698

Synthesis, spectroscopic and thermal characterization of sulpiride complexes of iron, manganese, copper, cobalt, nickel, and zinc salts. Antibacterial and antifungal activity

Science.gov (United States)

Mohamed, Gehad G.; Soliman, Madiha H.

2010-08-01

Sulpiride (SPR; L) is a substituted benzamide antipsychotic which is reported to be a selective antagonist of central dopamine receptors and claimed to have mood-elevating properties. The ligation behaviour of SPR drug is studied in order to give an idea about its potentiality towards some transition metals in vitro systems. Metal complexes of SPR have been synthesized by reaction with different metal chlorides. The metal complexes of SPR with the formula [MCl 2(L) 2(H 2O) 2]· nH 2O [M = Mn(II), Co(II), Ni(II), Cu(II) and Zn(II); n = 0-2] and [FeCl 2(HL)(H 2O) 3]Cl·H 2O have been synthesized and characterized using elemental analysis (CHN), electronic (infrared, solid reflectance and 1H NMR spectra) and thermal analyses (TG and DTA). The molar conductance data reveal that the bivalent metal chelates are non-electrolytes while Fe(III) complex is 1:1 electrolyte. IR spectra show that SPR is coordinated to the metal ions in a neutral monodentate manner with the amide O. From the magnetic and solid reflectance spectra, octahedral geometry is suggested. The thermal decomposition processes of these complexes were discussed. The correlation coefficient, the activation energies, E*, the pre-exponential factor, A, and the entropies, Δ S*, enthalpies, Δ H*, Gibbs free energies, Δ G*, of the thermal decomposition reactions have been derived from thermogravimetric (TG) and differential thermogravimetric (DTG) curves. The synthesized ligand and its metal complexes were also screened for their antibacterial and antifungal activity against bacterial species ( Escherichia coli and Staphylococcus aureus) and fungi ( Aspergillus flavus and Candida albicans). The activity data show that the metal complexes are found to have antibacterial and antifungal activity than the parent drug and less than the standard.

Synthesis, characterization and crystal structure of [Cu2(LH2]•(ClO42. Influence of the weak Cu•••O(perchlorate interaction on the structure of Cu2N2O2 metallocycle

Directory of Open Access Journals (Sweden)

Mirković Marija

2014-01-01

Full Text Available The diimine-dioxime ligand, 4,9-diaza-3,10-diethyl-3,9-dodecadiene-2,11-dione bisoxime (LH2, containing a N4 donor set was prepared by Schiff base condensation of 2-hydroxyimino-3-pentanone and 1,4-diaminobutane in two ways: in protic and in aprotic solvent. Higher yield of (LH2 imine was obtained when the synthesis was carried out using protic solvent (C2H5OH instead of aprotic benzene (78% and 30%, respectively. Cu(II metal complex of diimine-dioxime was synthesized in CH3OH from metal salt and LH2 in mole ratio 1:1. The isolated complex was characterized by the elemental analysis, IR spectroscopy and cyclic voltammetry. The structure of [Cu2(LH2]•(ClO42 was determined by the single-crystal X-ray diffraction analysis. Comparison with the structurally related diimine-dioxime Cu(II complexes revealed the influence of the weak Cu•••O(perchlorate interaction on the geometry of the metallocycle. [Projekat Ministarstva nauke Republike Srbije, br. 45015, br. 172013, br. 172065 i br. 172014

Highly Productive Synthesis, Characterization, and Fluorescence and Heavy Metal Ion Adsorption Properties of Poly(2,5-dimercapto-1,3,4-thiadiazole Nanosheets

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Chao Li

2017-12-01

Full Text Available Poly(2,5-dimercapto-1,3,4-thiadiazole (PBT nanosheets were synthesized by chemical oxidative synthesis under mild conditions. The media, oxidant species, monomer concentrations, oxidant/monomer molar ratio, and temperature were optimized to achieve higher yields and better performance. The molecular structure, morphology, and properties of the nanosheets were analyzed by Fourier transform infrared (FT-IR, ultraviolet-visible (UV-Vis, and fluorescence spectroscopies, wide-angle X-ray diffraction (WAXD, matrix-assisted laser desorption/ionization/time-of-flight (MALDI-TOF mass spectrometry, X-ray photoelectron spectroscopy (XPS, scanning electronic microscopy (SEM, transmission electron microscopy (TEM, and simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC. It was found that the polymerization of 2,5-dimercapto-1,3,4-thiadiazole occurs via dehydrogenation coupling between two mercapto groups to form the –S–S– bond. PBTs show the highest polymerization yield of up to 98.47% and form uniform nanosheets with a thickness of 89~367 nm. poly(2,5-dimercapto-1,3,4-thiadiazole polymers (PBTs exhibit good chemical resistance, high thermostability, interesting blue-light emitting fluorescence, and wonderful heavy metal ion adsorption properties. Particularly, the PBT nanosheets having a unique synergic combination of three kinds of active –S–, –SH, and =N– groups with a moderate specific area of 15.85 m2 g−1 exhibit an ultra-rapid initial adsorption rate of 10,653 mg g−1 h−1 and an ultrahigh adsorption capacity of up to 680.01 mg g−1 for mercury ion, becoming ultrafast chelate nanosorbents with a high adsorption capacity. With these impressive properties, PBT nanosheets are very promising materials in the fields of water treatment, sensors, and electrodes.

Modeling the butterfly: the voltammetry of ((sqrt(3)xsqrt(3))R30 and p(2x2) overlayers of (111) electrodes

NARCIS (Netherlands)

Koper, M.T.M.; Lukkien, J.J.

2000-01-01

The voltammetry of the formation of (v3×v3)R30° and p(2×2) overlayers on (111) electrodes is modeled by analytical and Monte Carlo techniques. Both ordered structures are formed by second-order order–disorder phase transitions that lead to sharply-peaked ‘butterfly’ features in the voltammogram. The

Excess Molar Volume and Apparent Molar Volume of Binary Mixtures of 2—Methyl—3—buten—2—ol with 1—Alcohol at 298.15K

Institute of Scientific and Technical Information of China (English)

LIUDixia; LIHaoran; 等

2002-01-01

Excess molar volumes (VmE) of binary mixtures of 2-methyl-3-buten-2-ol[CH3C(OH)(CH3)CHCH2] with four 1-alcohols:methanol,ethanol,1-propanol and 1-butanol at 298.15K and atmospheric pressure are derived from density measurements with a vibrating-tube densimeter.All the excess volumes are negative in the systems over the entire composition range. The results are correlated with the Redlich-Kister equation.The effects of chain length of 1-alcohols on VmE are discussed.The apparent molar volumes of 2-methyl-3-buten-2-ol and 1-alcohols are calculated respectively.

Antibacterial and Herbicidal Activity of Ring-Substituted 2-Hydroxynaphthalene-1-carboxanilides

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Katarina Kralova

2013-08-01

Full Text Available In this study, a series of twenty-two ring-substituted 2-hydroxynaphthalene-1‑carboxanilides were prepared and characterized. Primary in vitro screening of the synthesized compounds was performed against Staphylococcus aureus, three methicillin-resistant S. aureus strains, Mycobacterium marinum, M. kasasii, M. smegmatis. and M. avium paratuberculosis. The compounds were also tested for their activity related to inhibition of photosynthetic electron transport (PET in spinach (Spinacia oleracea L. chloroplasts. 2-Hydroxy-N-phenylnaphthalene-1-carboxanilide and 2-hydroxy-N-(3-trifluoromethylphenylnaphthalene-1-carboxamide (IC50 = 29 µmol/L were the most active PET inhibitors. Some of tested compounds showed the antibacterial and antimycobacterial activity against the tested strains comparable or higher than the standards ampicillin or isoniazid. Thus, for example, 2-hydroxy-N-(3-nitrophenylnaphthalene-1-carboxamide showed MIC = 26.0 µmol/L against methicillin-resistant S. aureus and MIC = 51.9 µmol/L against M. marinum, or 2-hydroxy-N-phenylnaphthalene-1-carboxamide demonstrated MIC = 15.2 µmol/L against M. kansasii. The structure-activity relationships for all compounds are discussed.

Synthesis of New Chiral Amines with a Cyclic 1,2-Diacetal Skeleton Derived from (2R, 3R-(+-Tartaric Acid

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Ana Maria Faísca Phillips

2006-03-01

Full Text Available The syntheses of new chiral cyclic 1,2-diacetals from (2R, 3R-( -tartaric acidare described. C2-symmetrical diamines were prepared via direct amidation of the tartrate orfrom the corresponding bismesylate via reaction with sodium azide. For C1-symmetricalcompounds, the Appel reaction was used to form the key intermediate, amonochlorocarbinol, from the diol. Some of the new chiral compounds, produced in good tohigh yields, may be potentially useful as asymmetric organocatalysts or as nitrogen andsulfur chelating ligands for asymmetric metal catalyzed reactions. Thus, a bis-N-methyl-methanamine derivative, used in substoichiometric amounts, was found to catalyze theenantioselective addition of cyclohexanone to (E-β-nitrostyrene with highdiastereoselectivity (syn / anti = 92:8, albeit giving moderate optical purity (syn: 30 %.

New glyme-cyclic imide lithium salt complexes as thermally stable electrolytes for lithium batteries

Science.gov (United States)

Tamura, Takashi; Hachida, Takeshi; Yoshida, Kazuki; Tachikawa, Naoki; Dokko, Kaoru; Watanabe, Masayoshi

New glyme-Li salt complexes were prepared by mixing equimolar amounts of a novel cyclic imide lithium salt LiN(C 2F 4S 2O 4) (LiCTFSI) and a glyme (triglyme (G3) or tetraglyme (G4)). The glyme-Li salt complexes, [Li(G3)][CTFSI] and [Li(G4)][CTFSI], are solid and liquid, respectively, at room temperature. The thermal stability of [Li(G4)][CTFSI] is much higher than that of pure G4, and the vapor pressure of [Li(G4)][CTFSI] is negligible at temperatures lower than 100 °C. Although the viscosity of [Li(G4)][CTFSI] is high (132.0 mPa s at 30 °C), because of its high molar concentration (ca. 3 mol dm -3), its ionic conductivity at 30 °C is relatively high, i.e., 0.8 mS cm -1, which is slightly lower than that of a conventional organic electrolyte solution (1 mol dm -3 LiTFSI dissolved in propylene carbonate). The self-diffusion coefficients of a Li + cation, a CTFSI - anion, and a glyme molecule were measured by the pulsed gradient spin-echo NMR method (PGSE-NMR). The ionicity (dissociativity) of [Li(G4)][CTFSI] at 30 °C is ca. 0.5, as estimated from the PGSE-NMR diffusivity measurements and the ionic conductivity measurements. Results of linear sweep voltammetry revealed that [Li(G4)][CTFSI] is electrochemically stable in an electrode potential range of 0-4.5 V vs. Li/Li +. The reversible deposition-stripping behavior of lithium was observed by cyclic voltammetry. The [LiCoO 2|[Li(G4)][CTFSI]|Li metal] cell showed a stable charge-discharge cycling behavior during 50 cycles, indicating that the [Li(G4)][CTFSI] complex is applicable to a 4 V class lithium secondary battery.

2-([1,2,4]triazolo[1,5-c]quinazolin-2-yl-alkyl-(alkaryl-, aryl--amines and their derivatives. (3Н-quinazolin-4-ylidenhydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-ylalkyl-(alkaryl-, aryl-carboxylic acids: features of synthesis, modification and ant

Directory of Open Access Journals (Sweden)

Yu. V. Martynenko

2016-08-01

the synthesized compounds have never been active against St. aureus, E. aerogenes, P. aeruginosa, E. coli, K. pneumoniaе (growth inhibition zone 6 mm. However, compounds 2.1, 2.2 are found among the (3H-quinazoline-4-ylidenehydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl-alkyl-(aralkyl-, aryl-carboxylic acids (2.1–2.9 and inhibit the growth of E. faecalis zone 7 mm. Conducted cyclocondensation of 2.1–2.9 compounds does not lead to increase of antibacterial activity of corresponding [1,2,4]triazolo[1,5-c]quinazoline-2-yl-alkyl-(alkaryl-, aryl--isoindol-1,3(2H-diones (3.1–3.9 against E. faecalis. Thus, the antibacterial effect against E. faecalis is characteristic only for compounds 3.2, 3.3 and 3.4 (growth inhibition zone 7 mm and is slightly lower than the corresponding activity of ampicillin.

Activation and thermostabilization effects of cyclic 2, 3-diphosphoglycerate on enzymes from the hyperthermophilic Methanopyrus kandleri.

Science.gov (United States)

Shima, S; Hérault, D A; Berkessel, A; Thauer, R K

1998-11-01

Enzymes involved in methane formation from carbon dioxide and dihydrogen in Methanopyrus kandleri require high concentrations (> 1 M) of lyotropic salts such as K2HPO4/KH2PO4 or (NH4)2SO4 for activity and for thermostability. The requirement correlates with high intracellular concentrations of cyclic 2,3-diphosphoglycerate (cDPG; approximately 1 M) in this hyperthermophilic organism. We report here on the effects of potassium cDPG on the activity and thermostability of the two methanogenic enzymes cyclohydrolase and formyltransferase and show that at cDPG concentrations prevailing in the cells the investigated enzymes are highly active and completely thermostable. At molar concentrations also the potassium salts of phosphate and of 2,3-bisphosphoglycerate, the biosynthetic precursor of cDPG, were found to confer activity and thermostability to the enzymes. Thermodynamic arguments are discussed as to why cDPG, rather than these salts, is present in high concentrations in the cells of Mp. kandleri.

Molecular structure and vibrational spectrum of the complex [ErL(H2O)(NO3)3] (L 1,4,10,13-tetraoxi-7,16-diaza(diphenylphosphinylmethyl) cyclooctadecane

International Nuclear Information System (INIS)

Minacheva, L.Kh.; Ivanova, I.S.; Kireeva, I.K.; Sakharova, V.G.; Tsivadze, A.Yu.; Sergienko, V.S.; Baulin, V.E.

2000-01-01

Synthesis of podandocoronand on the basis of diazo-18-crown-6 (DA18K6) 1,4,10,13-tetraoxi-7,16-diazo (diphenylphosphynylmethyl)cyclooctadecane (L) and erbium nitrate complex with L of the [ErL(H 2 O)(NO 3 ) 3 ] (I) composition is described. The IR-spectra of the free ligand L and complex I are studied and interpreted.The crystals are monoclinic: a = 10.432(2), b = 19.909(4), c = 21.361(4), β = 100.39(3) Deg, V = 4364(2) A 3 , sp. gr. P2 1 /n, Z = 4, ρ = 1.617 g/cm 3 . The structure I is formed of discrete molecular complexes. The Er atom coordination number is equal to 9. Three nitrate groups are bidentate-cyclic coordinated; two of them are in trans-position to each other; the H 2 O molecule is trans-position to the third NO 3 -group. The ligand L is coordinated by metal through two oxygen phosphoryl atoms. Thus, the Er atom coordination polyhedron may be described as octahedron, if each NO 3 -group occupies one coordination position. The Er-O(L) and Er-O(NO 3 ) overage distances are equal to 2.25 and 2.43 A correspondingly. Er-O(H 2 O) - 2.29 A. The H 2 O coordinated molecule forms intermolecular hydrogen atom and two oxygen atoms of the DA18K6 macrocycle [ru

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.

Electrochemical behavior and assembly of tetranuclear Dawson-derived sandwich compound [Cd4(H2O)2(As2W15O56)2]16- on 4-aminobenzoic acid modified glassy carbon electrode

International Nuclear Information System (INIS)

Bi Lihua; Shen Yan; Jiang Junguang; Wang Erkang; Dong Shaojun

2005-01-01

The transition metal-substituted heteropolyoxoanion, Cd 4 (H 2 O) 2 (As 2 W 15 O 56 ) 2 12- (As 4 W 30 Cd 4 ), is one of the trivacant Dawson derivatives. Its redox electrochemistry has been studied in acid buffer solutions using cyclic voltammetry. It exhibited three steps of four-electron redox waves attributed to redox processes of the tungsten-oxo framework. Through layer-by-layer assembly, the compound was first successfully immobilized on a 4-aminobenzoic acid modified glassy carbon electrode surface by alternate deposition with a quaternized poly(4-vinylpyridine) partially complexed with [Os(bpy) 2 Cl] 2+/+ (denoted as QPVP-Os). Thus, prepared multilayer films have been characterized by cyclic voltammetry (CV), X-ray photoelectron spectroscopy (XPS) and UV-vis spectroscopy (UV-vis). The electrocatalytic activities of the multilayer films containing As 4 W 30 Cd 4 have been investigated on the reduction of three substrates of important analytical interests, NO 2 - , BrO 3 - and IO 3 - . And with the increase of the number of As 4 W 30 Cd 4 layers, the catalytic current towards the reduction of BrO 3 - was enhanced and the catalytic potential shifted positively

Solution Synthesis, Structure, and CO2 Reduction Reactivity of a Scandium(II) Complex, {Sc[N(SiMe3 )2 ]3 }.

Science.gov (United States)

Woen, David H; Chen, Guo P; Ziller, Joseph W; Boyle, Timothy J; Furche, Filipp; Evans, William J

2017-02-13

The first crystallographically characterizable complex of Sc 2+ , [Sc(NR 2 ) 3 ] - (R=SiMe 3 ), has been obtained by LnA 3 /M reactions (Ln=rare earth metal; A=anionic ligand; M=alkali metal) involving reduction of Sc(NR 2 ) 3 with K in the presence of 2.2.2-cryptand (crypt) and 18-crown-6 (18-c-6) and with Cs in the presence of crypt. Dark maroon [K(crypt)] + , [K(18-c-6)] + , and [Cs(crypt)] + salts of the [Sc(NR 2 ) 3 ] - anion are formed, respectively. The formation of this oxidation state of Sc is also indicated by the eight-line EPR spectra arising from the I=7/2 45 Sc nucleus. The Sc(NR 2 ) 3 reduction differs from Ln(NR 2 ) 3 reactions (Ln=Y and lanthanides) in that it occurs under N 2 without formation of isolable reduced dinitrogen species. [K(18-c-6)][Sc(NR 2 ) 3 ] reacts with CO 2 to produce an oxalate complex, {K 2 (18-c-6) 3 }{[(R 2 N) 3 Sc] 2 (μ-C 2 O 4 -κ 1 O:κ 1 O'')}, and a CO 2 - radical anion complex, [(R 2 N) 3 Sc(μ-OCO-κ 1 O:κ 1 O')K(18-c-6)] n . © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigations on the synthesis and pharmacological properties of 4-alkoxy-2-[2-hydroxy-3-(4-aryl-1-piperazinyl)propyl]-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones.

Science.gov (United States)

Sladowska, Helena; Filipek, Barbara; Szkatuła, Dominika; Sabiniarz, Aleksandra; Kardasz, Małgorzata; Potoczek, Joanna; Sieklucka-Dziuba, Maria; Rajtar, Grazyna; Kleinrok, Zdzisław; Lis, Tadeusz

2002-11-01

Synthesis of 2-[2-hydroxy-3-(4-aryl-1-piperazinyl)propyl] derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones (8-12) is described. The chlorides used in the above synthesis can exist in two isomeric forms: chain (18-20) and cyclic (19a, 20a). The compounds 8-12 exhibited potent analgesic activity which was superior than that of acetylsalicylic acid in two different tests. Most of the investigated imides suppressed significantly spontaneous locomotor activity in mice.

Metabolism of the insecticidally active GABAA receptor antagonist 4-sec-[3,4-3H2]butyl-1-(4-cyanophenyl)-2,6,7-trioxabicyclo[2.2.2]octane

International Nuclear Information System (INIS)

Deng, Yanli; Palmer, C.J.; Toia, R.F.; Casida, J.E.

1990-01-01

4-sec-[3,4- 3 H 2 ]Butyl-1-(4-cyanophenyl)-2,6,7-trioxabicyclo[2.2.2]octane (referred to as [ 3 H]COB) was examined as an example of a new class of insecticidally active compounds that block the γ-aminobutyric acid gated chloride channel. Metabolites were identified by thin-layer cochromatography with standards from synthesis and by consideration of their hydrolytic and oxidative degradation products formed in situ on two-dimensional silica gel chromatoplates. Metabolism of [ 3 H]COB by mouse liver and housefly abdomen microsomes is dependent on fortification with NADPH. The O-methylene and sec-butyl sites are sensitive to oxidation. Each carbon of the sec-butyl group is individually functionalized with strong preference for the methylene site in the mouse but not the housefly microsomal system. O-Methylene hydroxylation initiates spontaneous cage opening to form an aldehyde that undergoes metabolic reduction, ultimately yielding the same cyanobenzoate ester of 2,2-bis-(hydroxymethyl)-3-methylpentan-1-ol formed by direct hydrolysis. Houseflies injected with [ 3 H]COB form many if not all of the same metabolites, with major products being the aforementioned cyanobenzoate, the orthoester oxidized at the sec-butyl methylene site, and polar conjugates

Synthesis and electrochemical characterization of bimetallic ruthenium complexes with the bridging h2(s,s-1,3-butadiyne-1,4-diyl ligand

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Stein Edison

2000-01-01

Full Text Available The bis(rutheniumalkyne complex [cis-{RuCl (bpy2(mu-CºC-}]2 (1 was obtained by treatment of 1 equiv of either 1,4-bis(trimethylsilyl-1,3-butadiyne or bis(trimetylsilylacetylene with 2 equiv of cis-[RuCl2(bpy2].2H2O, NaF and NaBF4 salts in methanol/CH2Cl2 mixture (10/1 in 52% and 35% yields, respectively. ¹H, 13C{H} NMR and principally electrochemical analyses confirmed that the same product was obtained from the two reactions. Cyclic voltammetric analyses of (1 from 0 to 1.20 V displays two one-electron quasi-reversible oxidation peaks attributed to the Ru(II/Ru(III couple. The redox processes are separated by 520 mV, indicating a significant electronic communication between the two metallic centers.

Highly selective rhodamine-based fluorescence turn-on chemosensor for Al3+ ion

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Manjunath, Rangasamy; Kannan, Palaninathan

2018-05-01

A new rhodamine-based colorimetric and fluorescent turn-on chemosensor (L) has been designed and synthesized for selective and sensitive detection of Al3+ ion. The sensing behavior toward metal ion was investigated by UV/Vis and fluorescence spectroscopy. Upon addition of Al3+ ion to solution of L provided a visual color change as well as significantly fluorescent enhancement, while other metal ions including Na+, Mg2+, K+, Mn2+, Fe3+, Ni2+, Cu2+, Zn2+, Pb2+, Cd2+ and Hg2+ ions fails to generate a distinct color and spectral changes, the distinct color change and rapid switch-on fluorescence also provide naked eye detection for Al3+ ion. The mechanism involved equilibrium between non-fluorescent spirocyclic form and highly fluorescent ring open form process was utilized and 1:2 stoichiometry for L-Al3+ complex formed with an association constant of 1.42 × 103 M-1. Moreover, chemosensor L was applied for living cell imaging and confirmed that can be used as a fluorescent probe for monitoring Al3+ ion in living cells.

Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

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Alatraktchi, Fatima AlZahra’a; Breum Andersen, Sandra; Krogh Johansen, Helle; Molin, Søren; Svendsen, Winnie E.

2016-01-01

Pyocyanin is a virulence factor uniquely produced by the pathogen Pseudomonas aeruginosa. The fast and selective detection of pyocyanin in clinical samples can reveal important information about the presence of this microorganism in patients. Electrochemical sensing of the redox-active pyocyanin is a route to directly quantify pyocyanin in real time and in situ in hospitals and clinics. The selective quantification of pyocyanin is, however, limited by other redox-active compounds existing in human fluids and by other metabolites produced by pathogenic bacteria. Here we present a direct selective method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between −1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58–0.82 V that is unaffected by other redox-active interferents. The linear quantification of pyocyanin has an R2 value of 0.991 across the clinically relevant concentration range of 2–100 µM. The proposed method was tested on human saliva showing a standard deviation of 2.5% ± 1% (n = 5) from the known added pyocyanin concentration to the samples. This inexpensive procedure is suggested for clinical use in monitoring the presence and state of P. aeruginosa infection in patients. PMID:27007376

Synthesis of new chiral amines with a cyclic 1,2-diacetal skeleton derived from (2R, 3R)-(+)-tartaric acid.

Science.gov (United States)

Barros, M Teresa; Phillips, Ana Maria Faísca

2006-03-17

The syntheses of new chiral cyclic 1,2-diacetals from (2R, 3R)-( )-tartaric acid are described. C(2)-symmetrical diamines were prepared via direct amidation of the tartrate or from the corresponding bismesylate via reaction with sodium azide. For C1-symmetrical compounds, the Appel reaction was used to form the key intermediate, a monochlorocarbinol, from the diol. Some of the new chiral compounds, produced in good to high yields, may be potentially useful as asymmetric organocatalysts or as nitrogen and sulfur chelating ligands for asymmetric metal catalyzed reactions. Thus, a bis-N-methyl-methanamine derivative, used in substoichiometric amounts, was found to catalyze the enantioselective addition of cyclohexanone to (E)-beta-nitrostyrene with high diastereoselectivity (syn / anti = 92:8), albeit giving moderate optical purity (syn: 30 %).

A novel photo-active Cd:1,4-benzene dicarboxylate metal organic framework templated using [Ru(ii)(2,2'-bipyridine)3]2+: synthesis and photophysics of RWLC-5.

Science.gov (United States)

Larsen, Randy W; Mayers, Jacob M; Wojtas, Lukasz

2017-09-26

The development of photoactive porous materials is of significant importance for applications ranging from sustainable energy to pharmaceutical development and catalysis. A particularly attractive class of photo-active materials is the metal-organic framework (MOF)-based platform in which the photo-active elements are components of the framework itself or photo-active guests encapsulated within the MOF cavities. It has now been demonstrated that the photo-active [Ru(2,2'-bipyridine) 3 ] 2+ (RuBpy) complex can template the formation of MOFs with varying three dimensional structures. Here we report the synthesis and structural and photo-physical characterization of a new RuBpy-templated MOF composed of Cd 2+ ions with 1,4-benzenedicarboxylate ligands (RWLC-5) that contains crystallographically resolved RuBpy complexes. The new material displays a biphasic emission decay (130 ns and 1180 ns, T = 20 °C) and a bathochromically shifted emission maximum, relative to RuBpy in solution (603 nm for RuBpy in ethanol vs. 630 nm for RWLC-5). The emission lifetimes also do not display temperature-dependent decays which are characteristic of RuBpy type complexes as well as other RuBpy templated MOFs. The lack of temperature dependence is consistent with the complete deactivation of the 3 LF state of the encapsulated RuBpy complex due to a constrained environment. The fast phase decay is attributed to a water molecule hydrogen bonded to a bipyridine ligand associated with ∼38% of the encapsulated RuBpy complexes resulting in the nonradiative deactivation of the 3 MLCT state.

Mixed ligand complexes of Cu(II)/Zn(II) ions containing (m-)/(p-) carboxylato phenyl azo pentane 2,4-dione and 2,2'-bipyridine/1,10 phenanthroline: Synthesis, characterization, DNA binding, nuclease and topoisomerase I inhibitory activity.

Science.gov (United States)

Hasan, Md Amin; Kumari, Niraj; Singh, Kanhaiya; Singh, Kiran; Mishra, Lallan

2016-01-05

Metal complexes of type [Cu(L1H)2(bpy)] (1), [Zn(L1H)2(bpy)] (2), [Cu(L2H)2(bpy)] (3) and [Cu(L2H)2(Phen)] (4) (L1H2=3-[N'-(1-acetyl-2-oxo-propylidene)-hydrazino]-benzoic acid, L2H2=4-[N'-(1-acetyl-2-oxo-propylidene)-hydrazino]-benzoic acid, bpy=2,2'-bipyridine, Phen=1,10 phenanthroline) are synthesized and characterized using spectroscopic techniques (FT-IR, (1)H NMR, (13)C NMR, electronic absorption and emission) and elemental analysis data. The assembly of the complexes involving intramolecular H-bonding is displayed using corresponding crystal structure. Binding of the complexes separately with Calf Thymus DNA is monitored using UV-vis spectral titrations. The displacement of ethidium bromide (EB) bound to DNA by the complexes, in phosphate buffer solution (pH∼7.2) is monitored using fluorescence spectral titrations. Nuclease activity of the complexes follow the order 4>3>1>2. The gel electrophoretic mobility assay measurement in presence of minor groove binder 4',6-diamidino-2-phenylindole (DAPI), suggests that complexes preferably bind with the minor groove of DNA. Topoisomerase I inhibitory activity of the complexes 3 and 4 inhibit topoisomerase I activity with IC50 values of 112 and 87μM respectively. Copyright © 2015 Elsevier B.V. All rights reserved.