MIXED-LIGAND HETEROMETALLIC COMPLEXES OF Ge(IV)-M2+ (Mn, Fe, Co, Ni, Zn) WITH 1,3-DIAMINO-2-HYDROXYPROPANE N,N,N',N'-TETRAACETIC ACID

There have been developed a novel synthetic method that allowed to obtain raw of mixed-ligand heterometallic binuclear complexes of Ge(IV)-M2+ (Mn, Fe, Co, Ni, Zn) with 1,3-diamino‑2-hydroxypropane N, N, N’, N’-tetraacetic acid (H5hpdta). Compounds have been characterized by the set of methods: elemental analysis, thermogravimetry, IR‑spectroscopy, spectrum of diffuse reflection, magnetic suspensibility. According to the elemental analysis, the molar ratio Ge: M: H5hpdta: bipy= 1:1:1:1 in the obtained compounds 1‑5 corresponds to the formula [(H2O)(OH)Ge(m-hpdta)M(bipy)]·nН2О (M=Mn n=3 (1), Fe n=2 (2), Co n=4 (3), Ni n=4 (4), Zn n=3 (5). Complexes have yellow (1), red (2), orange (3), violet (4) and pink (5) colors and are stable on air. Compounds 1‑5 exist in the form of crystal hydrates, that contain certain amount of water molecules, that are eliminated into the gas phase while heating in the wide range of temperatures (t=80‑250 °C), which is accompanied with the low-temperature endothermic effect. This indicates the presence of a system of stable hydrogen bonds in their crystal structure. Analysis of the IR‑spectra 1‑5 revealed that form and coordination of ligands is similar. Deprotonation of all carboxylic groups in the ligands (H5hpdta) and their bonding to germanium and d-metal is confirmed with the absence in the IR‑spectra 1‑5 absorption bands characteristic for the free СООН H5hpdta (1716 сm‑1) and nas(СОО-) і ns(СОО-) bands. Disappearance of the ν(С-OН)-1210 сm‑1 and appearance of the ν(С-O)alk., νas(Ge-O-M), νs(Ge-O- M) absorption band indicates that OH‑group of H5hpdta is deprotonated and performs bridging function. 2,2`-bipyridine bidentatly coordinates to the d-metal, binds to the O, N‑atoms of hpdta5- ligand and reaches coordination number 6. The last ligand plays the bringing role between Ge-dmetal, shows itself as ditopic, octadentate in total. According to the magnetic moments of 3, 4 and their diffuse reflection spectra, polyhedrons of Co (II), Ni (II) are octahedrons, which are realized due to the bidentate coordination of bipyridine and four bonds with nitrogen and oxygen of hpdta5-. Structure of heterometallic binuclear complexes 1‑5 is similar. Ligand hpdta5- shows itself as octadentate ditopic, all carboxylate groups monodentatly coordinate to metals, oxygen atom of the deprotonated OH‑group performs the bridging function.

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Solution and solid state studies of mixed ligand binuclear complexes containing one binucleating ligand

Canadian Journal of Chemistry ◽

10.1139/v93-161 ◽

1993 ◽

Vol 71 (8) ◽

pp. 1253-1258 ◽

Cited By ~ 5

Author(s):

Pushpa Patel ◽

P.K. Bhattacharya

Keyword(s):

Solid State ◽

Elemental Analysis ◽

Mixed Ligand ◽

Binuclear Complexes ◽

Computer Programme ◽

Magnetic Studies ◽

Dinucleating Ligands ◽

Coordination Sites ◽

Stability Order ◽

The Stability

Stability constants of homobinuclear binary Cu(II) complexes of the dinucleating ligands, having equivalent coordination sites, 5,5′-methylene-bis-salicylaldehyde (H2A1), 5,5′-methylene-bis-(3-bromosalicylaldehyde) (H2A2), and 5,5′-methylene-bis-(3-nitrosalicylaldehyde) (H2A3), and mixed ligand Cu(II) complexes with one of the above ligands and bipyridyl (L1) or 1,10-phenanthroline (L2) as second ligand, have been determined potentiometrically in water:dioxane medium (50:50 and 30:70,v/v using a computer programme. The values of [Formula: see text] and [Formula: see text] have been compared within the series of complexes having different H2A and L. Probable explanations for the stability order have been extended. The complexes (Cu2AL2)(ClO4)2 have been isolated and characterized by elemental analysis, electronic and ESR spectral, and magnetic studies.

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Mixed Ligand Complexes ofN-Methyl-N-phenyl Dithiocarbamate: Synthesis, Characterisation, Antifungal Activity, and Solvent Extraction Studies of the Ligand

Bioinorganic Chemistry and Applications ◽

10.1155/2015/913424 ◽

2015 ◽

Vol 2015 ◽

pp. 1-10 ◽

Cited By ~ 13

Author(s):

Anthony C. Ekennia ◽

Damian C. Onwudiwe ◽

Cyril Ume ◽

Eno E. Ebenso

Keyword(s):

Antifungal Activity ◽

Elemental Analysis ◽

Magnetic Moment ◽

Uv Spectroscopy ◽

Cobalt Complex ◽

Pathogenic Fungi ◽

Mixed Ligand ◽

Bidentate Coordination ◽

Nickel Ions ◽

Monodentate Coordination

A series of mixed ligand dithiocarbamate complexes with a general formula [ML2(py)2], where M = Mn(II), Co(II), Ni(II), and Cu(II), py = pyridine, and L =N-methyl-N-phenyl dithiocarbamate have been prepared and characterised by elemental analysis, FTIR and Uv spectroscopy, magnetic moment, and thermogravimetric and conductance analysis. The infrared spectra showed that symmetrical bidentate coordination occurred with the dithiocarbamate moiety through the sulfur atoms, while neutral monodentate coordination occurred through the nitrogen atom for the pyridine molecule in the complexes. The electronic spectra, elemental analysis, and magnetic moment results proved that the complexes adopted octahedral geometry. The conductance measurement showed that the complexes are nonelectrolytes proving their nonionic nature. The compounds were screened for three human pathogenic fungi:Aspergillus flavus, Aspergillus niger, andCandida albicans. The cobalt complex showed the best antifungal activity among the test compounds. Liquid-liquid extractive abilities of the ligand towards copper and nickel ions in different solvent media were investigated. The ligand showed a strong binding affinity towards the metals ions with an extractive efficiency of about 99%.

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Synthesis and Physico-Chemical Studies of Heterometallic Nitrilotriacetates of Chromium(III) with Some 3d Metals

Chemistry Journal of Moldova ◽

10.19261/cjm.2006.01(1).05 ◽

2006 ◽

Vol 1 (1) ◽

pp. 84-87

Author(s):

Victor Ciornea ◽

Aurelian Gulea

Keyword(s):

Chemical Composition ◽

Ir Spectra ◽

Elemental Analysis ◽

Nitrilotriacetic Acid ◽

Heterometallic Complexes ◽

Chemical Bonds ◽

3D Metals ◽

Thermogravimetric Study ◽

Physico Chemical ◽

Chemical Studies

Heterometallic complexes of chromium (III) with some 3d metals have been synthesized based on nitrilotriacetic acid (H3nta), like M(bpy)2Cr2(OH)2(nta)2·nH2O, where M = Mn2+, Co2+, Ni2+ and Zn2+; bpy = α,α′- bipyridine; n = 8 or 9. Their chemical composition has been determined from the results of the elemental analysis and thermogravimetric study. The coordination modes of the nta3 ̄ ligand and the type of chemical bonds have been proposed basing on IR spectra.

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Isocyanate und verwandte Verbindungen des trimeren Phosphornitriddifluorids / Isocyanates and Related Compounds of Trimeric Phosphor-difluoronitride

Zeitschrift für Naturforschung B ◽

10.1515/znb-1971-0708 ◽

1971 ◽

Vol 26 (7) ◽

pp. 679-683 ◽

Cited By ~ 5

Author(s):

Herbert W. Roesky ◽

Enno Janssen

Keyword(s):

Ir Spectra ◽

Elemental Analysis ◽

Mass Spectra ◽

H Nmr ◽

Carbonic Acids ◽

Related Compounds

P3N3F5NCO was prepared by reaction of P3N3F5NSO with (COCl) 2. Substituted amides were obtained from the reaction of P3N3F5NSO with carbonic acids e. g. P3N3F5NHCOCH3, P3N3F5NHCOC2H5, and P3N3F5NHCOC3H7. If these substances were treated with PCl5 the following compounds P3N3F5N = CClCH3, P3N3F5N = CClCH5, and P3N3F5TN = CClC3H7 were formed. They reacted with nucleophiles to give P3N3F5N = CNH2CH3, P3N3F5N = TN (CH3) 2C2H5, and P3N3F5N = CN (CH3) 2CH7. The properties of these compounds are described. They were characterized by elemental analysis and IR-spectra. 19F-, 1H-NMR, and mass spectra are reported.

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Mixed-ligand copper(ii)-phenolate complexes: structure and studies on DNA/protein binding profiles, DNA cleavage, molecular docking and cytotoxicity

RSC Advances ◽

10.1039/c5ra20607c ◽

2016 ◽

Vol 6 (3) ◽

pp. 1810-1825 ◽

Cited By ~ 39

Author(s):

Sellamuthu Kathiresan ◽

Subramanian Mugesh ◽

Maruthamuthu Murugan ◽

Feroze Ahamed ◽

Jamespandi Annaraj

Keyword(s):

Mass Spectrometry ◽

Molecular Docking ◽

Electrospray Ionization ◽

Elemental Analysis ◽

Dna Cleavage ◽

Mixed Ligand ◽

Ionization Mass ◽

Electrochemical Studies ◽

Mixed Ligands ◽

Ft Ir

Copper(ii) complexes with simple and mixed ligands, [Cu(L)(ClO4)] and [Cu(L)(diimine)]ClO4 were synthesized and characterized by elemental analysis, UV-vis, FT-IR, electrospray ionization-mass spectrometry (ESI-MS) and electrochemical studies.

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Peroxidase: a multifunctional enzyme in grapevines

Functional Plant Biology ◽

10.1071/fp02096 ◽

2003 ◽

Vol 30 (6) ◽

pp. 577 ◽

Cited By ~ 44

Author(s):

Alfonso Ros Barceló ◽

Federico Pomar ◽

Matías López-Serrano ◽

Maria Angeles Pedreño

Keyword(s):

Cell Wall ◽

Metabolic Regulation ◽

Trichoderma Viride ◽

Visible Spectrum ◽

H2o2 Production ◽

Class Iii ◽

Absorption Bands ◽

Peroxidase Isoenzyme ◽

Wide Range ◽

Uv C

Peroxidases are heme-containing enzymes that catalyse the one-electron oxidation of several substrates at the expense of H2O2. They are probably encoded by a large multigene family in grapevines, and therefore show a high degree of polymorphism. Grapevine peroxidases are glycoproteins of high thermal stability, whose molecular weight usually ranges from 35 to 45 kDa. Their visible spectrum shows absorption bands characteristic of high-spin class III peroxidases. Grapevine peroxidases are capable of accepting a wide range of natural compounds as substrates, such as the cell wall protein extensin, plant growth regulators such as IAA, and phenolics such as benzoic acids, stilbenes, flavonols, cinnamyl alcohols and anthocyanins. They are located in cell walls and vacuoles. These locations are in accordance with their key role in determining the final cell wall architecture, especially regarding lignin deposition and extensin insolubilization, and the turnover of vacuolar phenolic metabolites, a task that also forms part of the molecular program of disease resistance. Although peroxidase is a constitutive enzyme in grapevines, its levels are strongly modulated during plant cell development and in response to both biotic and abiotic environmental factors. To gain an insight into the metabolic regulation of peroxidase, several authors have studied how grapevine peroxidase and H2O2 levels change in response to a changing environment. Nevertheless, the results obtained are not always easy to interpret. Despite such difficulties, the response of the peroxidase–H2O2 system to both UV-C radiation and Trichoderma viride elicitors is worthy of study. Both UV-C and T. viride elicitors induce specific changes in peroxidase isoenzyme / H2O2 levels, which result in specific changes in grapevine physiology and metabolism. In the case of T. viride-elicited grapevine cells, they show a particular mechanism for H2O2 production, in which NADPH oxidase-like activities are apparently not involved. However, they offer a unique system whereby the metabolic regulation of peroxidase by H2O2, with all its cross-talks and downstream signals, may be elegantly dissected.

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SYNTHESIS AND PROPERTIES OF OLIGODIURETANEDIOLS BASED ON A MIXTURE OF (2,4–2,6) TOLUILENDIISOCYANATE

Polymer journal ◽

10.15407/polymerj.43.03.198 ◽

2021 ◽

Vol 43 (3) ◽

pp. 198-203

Author(s):

S.M. KUZMENKO ◽

◽

E.O. SPORYAGIN ◽

O.M. KUZMENKO ◽

A.YA. PUZENKO ◽

...

Keyword(s):

Molecular Weight ◽

Ir Spectra ◽

Azeotropic Distillation ◽

Synthesis Temperature ◽

Side Reactions ◽

Absorption Bands ◽

Formation Reaction ◽

Viscous Liquids ◽

Urethane Formation ◽

Product Control

The paper describes the synthesis, the reaction of a mixture of isomers (2,4–2,6) of toluilendiisocyanate with a double molar excess of aliphatic individual or oligomeric diols, a number of previously unknown oligodiuretanediols and their physicochemical constants. It is shown that with an increase in the synthesis temperature from 50 to 70 °C, the reaction time to complete depletion in the mixture of free NCO-groups decreases from 8–9 hours to 3–4 hours. The reaction temperature of 70–2 °С should be considered optimal, because at higher temperatures side reactions of free NCO-groups with already formed urethane ones are possible. Because the presence of even a small amount of moisture in the diols can provoke side effects during the urethane formation reaction, all of the above diols were dried from the adsorbed moisture by azeotropic distillation with toluene before use in the reaction. Since the final products are even at the synthesis temperature (68–70 °C) viscous liquids, and there are difficulties with the homogenization of the reaction mass during synthesis, and when unloading the finished product from the reaction plant, in all cases, the synthesis was performed in solution cyclohexanone by 50 % by weight of the final product. Control of the reaction was performed by changing the % wt. free NCO-groups in time. The reaction was considered complete if the measured % wt. free NCO-groups in the reaction mixture for at least one hour twice showed zero. The isolated oligodiuretanediols range from solid at room temperature to very viscous products, which significantly depends on the molecular weight of the diol used in the reaction (ie the concentration of urethane groups formed). They are homogeneous, transparent compounds that are readily soluble in esters, ethers, aromatic and halide-containing, aprotic solvents, ketones, poorly or completely insoluble in aliphatic saturated hydrocarbons. The structure of the synthesized oligomeric products is confirmed by functional analysis, IR–spectra. In the IR-spectra of each of the synthesized oligodiuretanediols there are no absorption bands in the region of 2270 cm-1, which confirms the complete completion of the reaction of urethane formation according to the scheme. At the same time, the absorption bands in the region of 3450 cm-1, 1720 cm-1, 1540 cm-1 are fixed, which are characteristic of the presence of urethane groups in the structure of the target products. As the chain length of the diol component –R– increases in the target product (which synchronously leads to an increase in molecular weight), the intensity of these absorption bands decreases, which is associated with a decrease in the concentration of formed urethane groups in the structure of oligodiuretanediols. The refractive index also decreases synchronously. Synthesized series of oligodiuretanediols can be used for synthesis on its basis of other classes of oligomers with the simultaneous presence in the structure of urethane groups. The ability of such compounds to be soluble in solvents of different nature has been studied, which provides information for the directions of their further use (varnishes, enamels, primers).

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New Perfluorophtalate Complexes of Platinum(II) With Chemotherapeutic Potential

Metal-Based Drugs ◽

10.1155/mbd.1996.117 ◽

1996 ◽

Vol 3 (3) ◽

pp. 117-122

Author(s):

M. B. de Oliveira ◽

J. Miller ◽

R. E. Banks ◽

L. R. Kelland ◽

C. A. McAuliffe ◽

...

Keyword(s):

Ir Spectra ◽

Ovarian Carcinoma ◽

Elemental Analysis ◽

Nmr Spectra ◽

Carcinoma Cell ◽

Acquired Resistance ◽

Cross Resistance ◽

Carcinoma Cell Lines ◽

Human Ovarian Carcinoma ◽

Anti Hiv

Two new platinum(II) complexes have been synthesized and their anti-tumour and anti-HIV activities have been evaluated.The new complexes are: (i) cis-tetrafluorophthalate-ammine-morpholine-platinum(II) or MMF3 and (ii) cis-tetrafluorophthalate- ammine-piperidine-platinum(II) or MPF4. They were characterized by elemental analysis, IR spectra and H1 and C13 NMR spectra.They were tested against five human ovarian carcinoma cell lines, viz., CH1, CH1cisR, A2780, A2780cisR and SKOV-3. They were less active than cis-platin and showed cross-resistance with cis-platin in the CH1cisR and A2780cisR acquired resistance lines.They were also tested for possible anti-HIV activity using the HIV-I IIIB virus and C8166 cells, but they were inactive compared with AZT.

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A III B VI PHOTOVOLTAIC RECEPTORS FOR EXPERIMENTAL DETERMINATION OF CARBON COMPOUNDS IN ATMOSPHERE

Journal of Engineering Studies and Research ◽

10.29081/jesr.v19i3.111 ◽

2016 ◽

Vol 19 (3) ◽

Author(s):

IULIANA CARAMAN ◽

IGOR EVTODIEV ◽

OXANA RACOVEŢ ◽

MARIUS STAMATE

Keyword(s):

Electric Fields ◽

Full Range ◽

Absorption Bands ◽

Gaseous State ◽

Wide Range ◽

Carbon Compounds ◽

Strong Electric Fields ◽

Qualitative Measurements ◽

Semiconductor Type

This paper examines the prospects of using semiconductor layered A III B VI type - photovoltaic cells and the photoresistors as receptors for quantitative and qualitative measurements of carbon oxides. Carbon compounds in gaseous state form absorption bands of electromagnetic radiation in a wide range of spectrum (200 ÷ 100 000) cm-1. The light absorbed or emitted in these bands at the excitations with ionizing radiation (X, γ) or strong electric fields contain direct information about the concentration of these molecules. The frequencies that correspond to maxima of these bands are characteristic parameters of absorbing molecules. Fundamental absorption bands of CO, CO 2 and NC have the edge of band at the border of ultraviolet-vacuum, while the emission bands d cover their full range of wave numbers from 45000 cm-1 to 10000 cm-1. Two types of radiation receptors from lamellar semiconductor type AIIIBVI photosensitive in this spectral range are studied.

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IDENTIFICATION OF COFFEE BEANS USING FTIR-SPECTROSCOPY AND MULTIVARIATE ANALYSIS

Известия вузов. Пищевая технология ◽

10.26297/0579-3009.2021.5-6.17 ◽

2021 ◽

Author(s):

Д.А. МЕТЛЕНКИН ◽

Ю.Т. ПЛАТОВ ◽

Р.А. ПЛАТОВА ◽

А.Е. РУБЦОВ ◽

А.М. МИХАЙЛОВА

Keyword(s):

Multivariate Analysis ◽

Discriminant Analysis ◽

Ir Spectra ◽

Ftir Spectroscopy ◽

Spectral Data ◽

Calibration Model ◽

Absorption Bands ◽

Coffee Beans ◽

The Matrix ◽

Decaffeinated Coffee

Для идентификации кофе используют методы газовой и жидкостной хроматографии, которые дают точную и подробную информацию о его химическом составе, однако трудоемки, сложны по пробоподготовке и непригодны для оперативного мониторинга качества. Цель настоящего исследования – разработка и апробация метода идентификации кофе по ботаническому виду, географическому месту произрастания и обжарке с применением Фурье-ИК-спектроскопии и многомерного анализа. В качестве объектов исследования были образцы кофе в зернах, различающиеся по ботаническому виду (арабика/робуста), географическому месту произрастания (Азия/Америка/Африка) и обжарке (жареный/нежареный). Для разработки моделей идентификации кофе в зернах была сформирована база спектральных данных и применены методы многомерного анализа – метод главных компонент (МГК) и дискриминантный анализ (ДА). ИК-спектры образцов кофе регистрировали с помощью Фурье-ИК-спектрометра Bruker ALPHA с алмазным модулем НПВО в диапазоне 4000–400 см–1 при разрешающей способности спектрометра 2 см–1. Спектральные данные были экспортированы из встроенного программного обеспечения OPUS 7.3.5.0 в Excel. При анализе матрицы спектральных данных выявлены наиболее интенсивные полосы поглощения ИК-спектра, приписываемые наличию функциональных групп воды, липидов, полисахаридов, кофеина и хлорогеновой кислоты в кофе. При сравнении ИК-спектров образцов кофеина, декофеинизированного кофе и кофе в зернах выявлены полосы поглощения спектра, которые можно использовать для построения калибровочной модели содержания кофеина в составе кофе в зернах. По спектральным данным МГК построена многомерная модель градации образцов кофе в зависимости от ботанического вида и наличия обжарки. По матрице факторных нагрузок выявлены полосы поглощения спектра, объясняющие различия образцов по ботаническому виду и обжарке и вносящие наибольший вклад в разделение образцов кофе на группы. Методом ДА по 19 переменным – коэффициентам поглощения на волновых числах спектра разработана система классификационных функций градации образцов кофе по географическому месту произрастания. Доказано, что сочетание Фурье-ИК-спектроскопии с методами многомерного анализа можно использовать как быстрый и неразрушающий инструмент для идентификации кофе в зернах. Gas and liquid chromatography methods are used to identify coffee. They provide accurate and detailed information about its chemical composition; however they are time-consuming, complex in sample preparation and unsuitable for operational quality monitoring. The purpose of this study is to develop and test a method for identifying coffee by botanical species, geographical place of growth and roasting using FTIR-spectroscopy and multivariate analysis. Samples of coffee beans were selected as objects of research, differing in botanical type (Arabica/Robusta), geographical place of growth (Asia/America/Africa) and roasting (roasted/not roasted). To develop models for the identification of grain coffee, a spectral database was formed and the methods of multivariate analysis were applied: principal components analysis (PCA), discriminant analysis. The IR-spectra of coffee samples were recorded using a Bruker ALPHA FTIR-spectrometer with a diamond module in the range of 4000–400 cm–1 with a resolution of the spectrometer of 2 cm–1. Spectral data were exported from the OPUS 7.3.5.0 embedded software to Excel. During analysis the matrix of spectral data, the most intense absorption bands of the IR-spectrum were revealed, attributed to the presence of functional groups of water, lipids, polysaccharides, caffeine and chlorogenic acid in grain coffee. By comparison the IR spectra of the samples: caffeine, decaffeinated coffee and grain coffee, absorption bands of the spectrum were revealed, which can be used to build a calibration model of the caffeine content in the composition of coffee beans. Using PCA based on the spectral data, a multivariate model of the gradation of coffee by botanical type and depending on the roast was build. According to the matrix of factor loadings, absorption bands of the spectrum were revealed, explaining the differences between the samples in botanical type and roasting and making the greatest contribution to the division of coffee samples into groups. By the method of discriminant analysis using 19 variables – absorption coefficients at the wave numbers of the spectrum – a system of classification functions for the gradation of grain coffee samples according to the geographical place of growth has been developed. It is proved that the combination of FTIR-spectroscopy with multivariate analysis methods can be used as a fast and non-destructive tool for identifying coffee beans.

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