185 research outputs found
Di-μ2-acetato-1:2κ2 O:O′;2:3κ2 O:O′-bis(N,N′-dimethylformamide)-1κO,3κO-bis{μ2-2,2′-[propane-1,3-diylbis(iminomethylene)]diphenolato-1κ4 O,N,N′,O′:2κ2 O,O′;2κ2 O,O′:3κ4 O,N,N′,O′-1,3-dinickel(II)-2-cadmium(II)
The crystal structure of the title compound, [Ni2Cd(C17H16N2O2)2(C2H3O2)2(C3H7NO)2], contains discrete centrosymmetric hetero-trinuclear molecules in which Ni/Cd atom pairs are triply bridged via O atoms from the SALPD2− [N,N′-bis(salicylidene)-1,3-propanediaminate] and acetate ligands. The central CdII ion is in a distorted octahedral coordination environment formed by four O atoms from two SALPD2− ligands in the equatorial plane and two O atoms of two symmetry-related acetate ligands in the axial positions. The symmetry-related NiII ions are in slightly distorted octahedral environments, coordinated by two O and two N atoms from tetradendate SALPD2− ligands in the equatorial plane, while the axial positions are occupied by O atoms from a dimethylformamide and an acetate ligand. This results in the formation of three edge-shared octahedra in which the Ni⋯Cd distance is 3.1482 (15) Å. The crystal structure is stabilized by weak C—H⋯O hydrogen bonds
Synthesis, antimicrobial and thermal studies of nitropyridine-substituted double armed benzo-15-crown-5 ligands; alkali (Na+ and K+) and transition metal (Ag+) complexes; reduction of nitro compounds
Nitropyridine substituted double-armed benzo 15-crown-5 compounds (1–4) were synthesized by the reactions of 4′,5′-bis(bromomethyl)benzo-15-crown-5 with hydroxypyridine derivatives. Na+ and K+ complexes (1a–4a, 1b–4b) of crown ether compounds (1–4) were prepared with sodium picrate and potassium picrate, respectively. Transition metal complexes (1c–4c) of the synthesized ligands (1–4) were prepared from Ag+ cation. In addition, nitro compounds (1, 2 and 4) were reduced by using Pd/C and hydrazine hydrate and new amine compounds (5, 6 and 8) were obtained. The structures of new double-armed crown ether compounds (2–4), their metal complexes (1a–4a, 1b–4b, 2c–4c) and amine compounds (5, 6 and 8) were elucidated by FTIR, HRMS, 1H–NMR, 13C–NMR spectroscopic methods. The thermal behaviors of these nitro group containing ligands (1–4) were compared with the resulting silver complexes (1c–4c) and amine compounds (5, 6 and 8). All synthesized compounds were examined for antibacterial activity against pathogenic strains Listeria monocytogenes, Salmonella typhi H, Bacillus cereus, Staphylococcus aureus, Staphylococcus epidermidis, Micrococcus luteus, Escherichia coli, Klebsiella pneumonia, Proteus vulgaris, Serratia marcescens, Shigella dysenteria and antifungal activity against Candida albicans. Graphical abstract: [Figure not available: see fulltext.] © 2022, The Author(s), under exclusive licence to Springer Nature B.V
Dichlorido-1κCl,3κCl-bis{μ-2,2′-[propane-1,3-diylbis(iminomethylene)]diphenolato}-1:2κ6 O,N,N′,O′:O,O′;2:3κ6 O,O′:O,N,N′,O′-tricopper(II)
The title linear trinuclear copper(II) complex, [Cu3(C17H20N2O2)2Cl2], was obtained from N,N′-bis(2-hydroxybenzyl)-1,3-propanediamine and CuCl2. The overall charge of the three Cu2+ ions is balanced by four deprotonated phenol groups and two Cl− ligands. The complex is centrosymmetric with the central Cu2+ occupying a special position (). This Cu2+ ion is coordinated by the four phenolate O atoms in a square-planar fashion. The second Cu2+ occupies a general position in a square-pyramidal fashion. Two phenolate O atoms and two amine N form the basal plane, with Cl− ligands occupying the fifth coordination site
Thermal kinetic analysis, theoretical thermodynamic calculations and antimicrobial activity of three new energetic materials
WOS: 000425965400096Three new energetic agents were synthesized using 3,5-dinitro-4-chlorobenzonitrile, sodium azide and hydrazine, which were 2,6-dinitro-4-cyano-azidobenzene (I), N-2,6-dinitro-cyanophenyl-hydrazine (II) and bis-N,N'(2,6-dinitro-4-cyanophenyl)hydrazine (III). These energetic substances were first characterized by elemental analysis, IR, mass, H-1 NMR and C-13 NMR spectroscopic methods. The energetic substances were studied by thermogravimetry, and it was understood that the mechanism of the thermal decomposition reactions consists of two successive exothermic thermal reactions. In the first thermal reaction, the energetic material was converted to furoxane compounds, and then, these furoxane compounds were decomposed by the second thermal reaction. Activation energies and Arrhenius pre-exponential factors of thermal responses were determined by using isothermal (Coats-Redfern) and nonisothermal/isoconvertional (Kissinger-Akahira-Sunose, Ozawa-Flynn-Wall) methods with thermogravimetry and differential scanning calorimetry (DSC) data. With these calculated values, other thermodynamic parameters reaction enthalpy, entropy changes and free energy were calculated. Formation enthalpies of the elements of the energetic substances were theoretically calculated using the CBS-4M algorithm in the Gaussian 09 program for the synthesized energetic substances. In the thermal decomposition reactions, the products were estimated with the aid of literature data and the enthalpies of explosion reactions were theoretically calculated according to the Hess Law. Besides, the exothermic energies in the first and second thermal reactions of the energetic substances were measured by DSC. The results measured by DSC were compared with the calculated theoretical results and were found to be very close to each other. In the study, antimicrobial activity was estimated to be high because energetic molecules are strained molecules, and it is possible this tension can affect the medium. According to this thought, antimicrobial activity was determined by using five different bacteria and a fungus. Antimicrobial activity values were determined by "agar dilution" method, and results were found as minimum inhibition concentration. Among the three energetic substances, 2,6-dinitro-4-cyano-azidobenzene was found to have the most active compound.Scientific Research Fund of the University of Ankara [16H0430004]; Scientific Research Fund of the Ahi Evran University [FEF.A4.17.001]This work was supported by the Scientific Research Fund of the University of Ankara (project no. 16H0430004) and Scientific Research Fund of the Ahi Evran University (grant no: FEF.A4.17.001)
Poly[(μ-benzene-1,2,4,5-tetracarboxylato)tetrasilver(I)]
In the centrosymmetric title compound, [Ag4(C10H2O8)]n, the benzene ring has irregular bond lengths but remains planar (r.m.s. deviation 0.0002 Å). The Ag—O bond lengths are in the range 2.153 (3)–2.615 (4) Å. The carboxylate groups are oriented at dihedral angles of 26.4 (5) and 74.9 (4)° to the benzene ring. The coordination behaviour of each carboxylate O atom is different: in one carboxylate, the O atoms are coordinated to a single and two Ag atoms; in the other carboxylate, the O atoms are coordinated to two and three Ag atoms. Non-classical intermolecular C—H⋯O hydrogen bonding is present in the crystal structure. The title compound forms a three-dimensional polymeric network due to the coordination of the Ag atoms
Bis{μ-2-[(2-oxidobenzylidene)aminomethyl]phenolato-κ3 O,N,O′}bis[(pyridine-κN)zinc(II)]
In the title centrosymmetric zinc(II) complex, [Zn2(C4H13NO2)2(C6H5N)2], each ZnII atom is coordinated by two 2-[(2-oxidobenzylidene)aminomethyl]phenolate (L) ligands and one pyridine (py) molecule in a distorted trigonal-bipyramidal geometry. Each L ligand behaves as a tridentate ligand and provides a phenolate oxygen bridge which links the two ZnII atoms. The ZnL(py) units are linked by π–π interactions between adjacent pyridine molecules, with a centroid–centroid distance of 3.724 Å, resulting in a two-dimensional structure
Investigation of energetic materials prepared by reactions of diamines with picryl chloride
Five compounds containing picryl group(s) were synthesized from reactions of hydrazine, 1,2-diaminoethane, 1,3-diaminopropane, 1,4-diaminobutane and 1,7-diaminoheptane with picryl chloride under hydrothermal conditions in methanol. Hydrazine reaction yielded N-2,4,6-trinitrophenylhydrazine which has a single picryl group, whereas the other reactants formed symmetric products with both amine groups connected to picryl groups. These compounds are N,N′-di-2,4,6-trinitrophenyl-1,2-diaminoethane, bis-N,N′-di-2,4,6-trinitrophenyl-1,3-diaminopropane, bis-N,N′-di-2,4,6-trinitrophenyl-1,4-diaminobutane and bis-N,N′-di-2,4,6-trinitrophenyl-1,7-diaminoheptane. Molecular structures of two of these compounds, N-2,4,6-trinitrophenylhydrazine and bis-N,N′-di-2,4,6-trinitrophenyl-1,3-diaminopropane, were revealed by XRD methods. All compounds were investigated by TG and DSC methods. The thermal behaviour of N-2,4,6-trinitrophenylhydrazine was explosive, undergoing a strong explosion in a very short temperature interval, 180–185 °C. In cases of the other compounds, it was found out that the carbon chain between two picryl groups reduced the explosion enthalpy. In addition, the theoretical formation enthalpy of N-2,4,6-trinitrophenylhydrazine was calculated by running CBS-4 M energy calculations under Gaussian 09 software package. From the calculated value, reaction enthalpy values for the possible explosion pathways were investigated in accordance with the experiment. The path with reaction enthalpy closest to the experimental value was proposed as the explosion mechanism
Liquid-Liquid Extraction Based Simple Trans-Resveratrol Analysis In Wine Samples
Abstract: 3,5,4-trans-trihydroxystilbene (trans-resveratrol) is quite soluble in CH2Cl2 and CHCl3. Wine samples are shaken in and rinsed with CHCl3 to obtain fine extracts of trans-resveratrol. The obtained CHCl3 solutions were directly injected to HPLC system for analysis. Determinations were made in 60% MeCN: 40% EtOH, and by trans-resveratrol standard addition. The resolution is calculated to be about 1.0 in the chromatogram. In 9 wine samples produced in Turkey, resveratrol concentrations were detected in between 1.46 and 6.53 ppm. By consecutive extractions, extraction ratio of resveratrol was determined and by increasing the amount of the samples, accuracy of the method was tested. It was found that the recovery is about 100.42 %.
Key words: Resveratrol determination, wine, HPLC, liquid-liquid extraction.
Şarap Örneklerinde Sıvı-Sıvı Ekstraksiyonu İle Trans-Resveratrol Analizi
Özet: 3,5,4-trans-trihidroksistilben (trans-resveratrol)'in CH2Cl2 ve CHCl3 içindeki çözünürlüğü oldukça fazladır. Trans-resveratrolü tam ekstrakte etmek için, şarap örnekleri CHCl3 içinde çalkalandı. Elde edilen CHCl3 çözeltisi HPLC sistemine direk olarak enjekte edildi. Analiz, %60 MeCN: %40 EtOH içinde ve trans-resveratrol standart eklenmesiyle gerçekleştirildi. Kromatogramdaki rezolüsyon yaklaşık 1.0 olarak hesaplandı. Türkiye de üretilmiş olan 9 şarap örneğinde resveratrol konsantrasyonu 1.46-6.53 ppm olarak bulundu. Resveratrolün ekstraksiyon oranı, ardışık ekstraksiyon ile tespit edildi ve örnek miktarı arttırılarak, metodun doğruluğu test edildi. Geri kazanım % 100.42 olarak bulundu.
Anahtar kelimeler: Resveratrol tayini, şarap, HPLC, sıvı-sıvı ekstraksiyonu
Synthesis, crystal structure, chromatographic seperation, and thermogravimetric investigation of a ONNO type asymmetric Schiff base and its trinuclear complexes
Inal, Emine Kubra/0000-0001-8334-2791;WOS: 0003404554000071,3-Propanediamine was put to react with 2-hydroxybenzaldehyde and 2-hydroxyacetophenone sequentially in aprotic medium. The crystalline product was examined by high performance liquid chromatography. The composition was 66% asymmetric Schiff base N(2-hydroxybenzylidene)-N'(2-hydroxyacetophenone)-1,3-propanediamine (SALLACH(2)) and 33% bis-N,N'(2-hydroxyacetophenylidene)-1,3-propanediamine (LACH2). As the crystals were uniform and of appropriate size, the molecular model of the material was revealed by X-ray diffraction. It was seen that two molecules of SALLACH(2) and one molecule of LACH(2) formed the mixed crystals. The substance was separated to its components and the asymmetric Schiff base was purified with a silica column. The substance was characterized with elemental analysis, FT-IR, MS, (HNMR)-H-1, and C-13 NMR. In addition, six tri-nuclear complex with the nuclear structure of Ni-II-Ni-II-Ni-II, Ni-II-Cu-II-Ni-II, Ni-II-Mn-II-Ni-II were prepared from this Schiff base and stoichiometry was determined by elemental analysis, FT-IR and thermogravimetry. Finally, the molecular structures of two complexes were brought to light by XRD which highlights the asymmetry of the ligand more clearly.University of Ankara Scientific Research FundAnkara University [12B4240003]; Ahi Evran University Scientific Research FundAhi Evran University [4001.12.014]Financial support of this work by the University of Ankara Scientific Research Fund (contract no. 12B4240003) and Ahi Evran University Scientific Research Fund (contract no. 4001.12.014) are gratefully acknowledged. We are indebted to and thank Prof. Dr. Wolfgang Donner for providing laboratory facilities at TU Darmstadt
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