scholarly journals Synthesis, Characterization and Thermogravimetric Study of Some Metal Complexes of Selenazone Ligand Nanoparticles Analogue of Dithizone

2021 ◽  
Vol 21 (5) ◽  
pp. 1231
Author(s):  
Zuhair Ali Abdulnabi ◽  
Faris Abdulridhah Jassim Al-doghachi ◽  
Hassan Thamir Abdulsahib

A new method for preparing 1,5-diphenylselenocarbazone (selenazone) nanoparticles and their complexes with Pb2+, Cd2+, Co2+, and Ni2+ has been performed using hot methanol solvent. The ligand and its complexes were characterized using FT-IR, UV-Vis, 1H-NMR, 13C-NMR, X-ray powder diffraction (XRD), EI-mass spectrometry, scanning electron microscopy (SEM), HG and flame-atomic absorption spectrophotometer, thermal analysis (TG/DTA), and molar conductance measurements. The molar conductance measurements in all complexes were recorded low values in DMSO, indicating that all the metal complexes were non-electrolytes except the nickel complex that possessed an electrolytic nature. Kinetic and thermodynamic parameters of complexes (A, E, ∆H, ∆S, and ∆G) have been computed using three kinetic models of Coast-Redfern, Broido, and Horowitz-Metzger, that illustrated the decomposition reactions in all steps were nonspontaneous. Thermogravimetric analyses (TG/DTA) were consistent with the atomic spectroscopy data proving that the geometry shape of all the complexes was octahedral.

2021 ◽  
Vol 16 (1) ◽  
pp. 111-119
Author(s):  
Iman Abdullah ◽  
Riri Andriyanti ◽  
Dita Arifa Nurani ◽  
Yuni Krisyuningsih Krisnandi

Carbon dioxide is a highly potential renewable C1 source for synthesis of fine chemicals. Utilization of CO2 in carboxylation reactions requires catalysts, such as: nickel complex for CO2 activation. However, the use of homogeneous catalysts in the reaction is still less efficient due to the difficulty of separating the product and catalyst from reaction mixture. Therefore, it is necessary to heterogenize the nickel complex in a solid support such as mesoporous carbon. In this report, mesoporous carbon (MC) prepared from phloroglucinol and formaldehyde through soft template method was used as a solid support for Ni-phenanthroline complex (Ni-phen). The catalyst was characterized by Fourier Transform Infra Red (FT-IR), X-Ray Diffraction (XRD), Scanning Electron Microscope - Energy Dispersive X-Ray (SEM-EDX), and Surface Area Analyzer (SAA). The result of SAA characterization showed that the pore diameter of MC was 6.7 nm and Ni-phen/MC was 5.1 nm which indicates that the materials have meso-size pores. Ni-phen/MC material was then used as a heterogeneous catalyst in the carboxylation reaction of phenylacetylene under an ambient CO2 pressure. The reactions were carried out in several variations of conditions such as temperature, time and catalyst types. Based on the results of the reaction, the best conditions were obtained at 25 °C for 8 h of reaction time using Ni-phen/MC catalyst.  Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0). 


2019 ◽  
Vol 41 (5) ◽  
pp. 770-770
Author(s):  
Ali apan Ali apan ◽  
Erdal Canpolat Erdal Canpolat ◽  
Henar Sleman and Niyazi Bulut Henar Sleman and Niyazi Bulut

In this work, new Schiff baz ligand was synthesized by reaction of p-iminoacetophenone oxime with 3,5-dichlorosalicylaldehyde. Metal complexes of Co+2, Ni+2, Cu+2 and Zn+2 acetate metal salts were synthesized with this ligand. The ligand and complexes are characterized in experimental by their elemental analyses, X-ray, 1H-NMR, 13C-NMR, UV-Vis, FT-IR, magnetic susceptibility and thermogravimetric analyses (TGA) and also have been investigated by using quantum mechanical methods. The transition metals are coordinated to the schiff base through the azomethine nitrogen and the carboxyl oxygen atom. Obtained metal complexes were studied the magnetic properties and their geometries were determined. Co+2, Ni+2 and Zn+2 complexes have been found tetrahedral geometry and Cu+2 complex has been found four coordinated geometry.


2020 ◽  
Vol 2020 ◽  
pp. 1-8 ◽  
Author(s):  
F. K. Ommenya ◽  
E. A. Nyawade ◽  
D. M. Andala ◽  
J. Kinyua

A new series of Mn (II), Co (II), Ni (II), Cu (II), and Zn (II) complexes of the Schiff base ligand, 4-chloro-2-{(E)-[(4-fluorophenyl)imino]methyl}phenol (C13H9ClFNO), was synthesized in a methanolic medium. The Schiff base was derived from the condensation reaction of 5-chlorosalicylaldehyde and 4-fluoroaniline at room temperature. Elemental analysis, FT-IR, UV-Vis, and NMR spectral data, molar conductance measurements, and melting points were used to characterize the Schiff base and the metal complexes. From the elemental analysis data, the metal complexes formed had the general formulae [M(L)2(H2O)2], where L = Schiff base ligand (C13H9ClFNO) and M = Mn, Co, Ni, Cu, and Zn. On the basis of FT-IR, electronic spectra, and NMR data, “O” and “N” donor atoms of the Schiff base ligand participated in coordination with the metal (II) ions, and thus, a six coordinated octahedral geometry for all these complexes was proposed. Molar conductance studies on the complexes indicated they were nonelectrolytic in nature. The Schiff base ligand and its metal (II) complexes were tested in vitro to evaluate their bactericidal activity against Gram-negative bacteria (Escherichia coli and Pseudomonas aeruginosa) and Gram-positive bacteria (Bacillus subtilis and Staphylococcus typhi) using the disc diffusion method. The antibacterial evaluation results revealed that the metal (II) complexes exhibited higher antibacterial activity than the free Schiff base ligand.


1976 ◽  
Vol 31 (2) ◽  
pp. 203-207 ◽  
Author(s):  
Walter Siebert ◽  
Roland Full ◽  
Carl Krueger ◽  
Yi-Hung Tsay

2,5-Dimethyl-3,4-diethyl-1,2,5-thiadiborolene (1) and Ni(CO)4 yield yellow 1 • Ni(CO)2, which is converted to the corresponding bis( 1,2,5-thiadiborolene)-nickel(0), the first thermostable thioborane nickel complex. Spectroscopic data indicate a pentahapto sandwich compound with the electron-donating groups in approximately tetrahedral arrangement. This is confirmed by X-ray structural analysis. The title compound crystallizes in the space group p21/c with α = 19.594(2), b = 11.8593(4), c = 9.3736(3) Å, β = 102.848(6)° and four molecules per unit cell.


2017 ◽  
Vol 751 ◽  
pp. 461-466 ◽  
Author(s):  
Jaturon Kumchompoo ◽  
Wasinee Wongwai ◽  
Ratchadaporn Puntharod

In this research, sodium silicate (Na2SiO3) was prepared by rice husk ash reacted with 10 M sodium hydroxide. The mixtures were heated by microwave at 400, 600, and 800 watt for 5 and 10 minutes. The formation of sodium silicate was characterized by Fourier transform infrared spectrophotometer. The vibrations of (Na)O–Si–O(Na) and O–Si–O were observed at 595 and 1023-986 cm-1, respectively, except at 800 watt disappeared those vibrations. The results of flame atomic absorption spectrophotometer provided the mole ratio of sodium and silicon was 2:1 as heating the product at 600 watt for 5 and 10 minutes. The phase of sodium silicate was characterized by X-ray diffraction. Sodium silicate could be used as catalyst as in biodiesel production from palm oil. The percentage of yield was 81 by volume.


2012 ◽  
Vol 9 (3) ◽  
pp. 1113-1121 ◽  
Author(s):  
A. P. Mishra ◽  
A. Tiwari ◽  
S. K. Gupta ◽  
Rajendra Jain

Some new Schiff base metal complexes of Co(II), Ni(II) and Cu(II) derived from 3-chloro-4-fluoroaniline (HL1) and 4-fluoroaniline (HL2) with 2-thiophenecarboxaldehyde have been synthesized and characterized by elemental analysis, FT-IR, FAB-mass, molar conductance, electronic spectra, ESR and magnetic susceptibility. The complexes exhibit coordination number 4 or 6. The complexes are colored and stable in air. Analytical data revealed that all the complexes exhibited 1:2 (metal: ligand) ratio. FAB-mass data show degradation pattern of the complexes. The Schiff base and metal complexes show a good activity against the bacteria;B. subtilis,E. coliandS. aureusand fungiA. niger,A. flavusandC. albicans. The antimicrobial results also indicate that the metal complexes are better antimicrobial agents as compared to the Schiff bases.


2016 ◽  
Vol 20 (06) ◽  
pp. 677-688 ◽  
Author(s):  
Ahmad Shaabani ◽  
Zeinab Hezarkhani

Functionalized wool with cobalt(II), copper(II), and iron(II) tetrasulfophthalocyanine (CoTSPc@wool, CuTSPc@wool, and FeTSPc@wool) have been synthesized and their structures characterized by flame atomic absorption spectroscopy (FAAS), FT-IR, UV-vis, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and the energy dispersive spectroscopy (EDS) analysis. The catalytic activity of the synthesized catalysts was investigated for the aerobic oxidation of alkyl arenes and alcohols to their corresponding carbonyl compounds in the absence of any co-promoter and additional oxidizing reagent. We found the best catalyst for the mentioned reactions is the CoTSPc@wool from the solvent, conversion, temperature, and reaction time point of views. The synthesized catalysts can be readily recycled and reused for several runs without significant loss of efficiency.


2015 ◽  
Vol 2015 ◽  
pp. 1-12 ◽  
Author(s):  
Narendra Kumar Chaudhary ◽  
Parashuram Mishra

Two new metal complexes of general formula M(Haαft)2[M =NiIIandCuII] of asymmetrical Schiff base ligand (HL = Haαft) derived from amoxicillin andα-formylthiophene have been prepared and characterized by various physicochemical and spectral techniques. Molar conductance measurement indicates nonelectrolytic nature of the metal complexes. FT-IR spectral study reveals the ligation of metal ions at two different nitrogen [NN] donor sites of Haαft. FT-IR and electronic absorption spectral evidences suggest distorted tetrahedral and square planar geometry forCuIIandNiIIcomplexes, respectively. The structure optimization by molecular mechanics (MM) force field calculation through ArgusLab 4.0.1 version software also supports the concerned geometry of the complexes. The cell dimensions as suggested by XRPD study,a(6.753 Å),b(13.904 Å),c(20.122 Å),α(142.76°),β(106.580°), andγ(72.4343°) forCuIIanda(24.2547 Å),b(6.6371 Å),c(5.5047 Å) (α=β=γ= 90°) forNiIIcomplexes, are in good agreement with their triclinic and orthorhombic crystal systems. Particle size calculation by Scherrer’s formula indicates nanocrystalline nature of the complexes. The antibacterial sensitivity study suggests promising activities of Haαft (Ligand) and M(Haαft)2complexes against four clinical pathogenic bacteria, namely,E. coli,P. vulgaris,P. aeruginosa, andS. aureus, though being less active than the standard drug amikacin.


2008 ◽  
Vol 5 (s1) ◽  
pp. S997-S1007
Author(s):  
E. Yildiz ◽  
N. Bozok

A ligand which has reactive dye character and its transition metal complexes such as Cu(II), Co(II), Cr(III), Ni(II) containing vinylsulfone and fluorine groups were synthesized. The diazotation reaction has been studied at 0-5°C carefully. Completion of the reaction was monitored by the TLC method. FT-IR, UV,1H-NMR, TGA and microanalysis methods were used for determination of the synthesized compounds. We assumed that copper complex indicated dimeric structure based on magnetic susceptibility result. All the synthesized compounds which have dye character were applied on cotton, polyamide and nylon fibers. Their dyeing and fastness properties were investigated according to international standards. These properties gave good results for all synthesized dyes except light fastnesses of chromium and nickel complex dyes.


2017 ◽  
Vol 72 (6) ◽  
pp. 415-420 ◽  
Author(s):  
Xiu-Yan Dong ◽  
Quan-Peng Kang ◽  
Bo-Xian Jin ◽  
Wen-Kui Dong

AbstractA new dinuclear Ni(II) complex, [{Ni(L)(C5H5N)}2], has been synthesized with 4-chloro-4′,6′-dibromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol (H2L), and characterized by elemental analyses, FT-IR, UV/Vis, molar conductance and X-ray crystallographic analysis. Each Ni(II) atom is located at a N2O2 coordination site of a completely deprotonated (L)2− unit. Two μ-phenoxo oxygen atoms from two [Ni(L)] units and two pyridine nitrogen atoms coordinate with two Ni(II) atoms. The two hexa-coordinated Ni(II) atoms have slightly distorted octahedral geometries. The μ-phenoxo bridges play important roles in assembling Ni2+ and (L)2− units. This 2:2 (Ni2+:(L)2−) structure is different from that of other Salamo-type Ni(II) complexes reported earlier.


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