Mn II , Fe III , Co II , Ni II , Cu II , Zn II , La III , Ru III , Hf IV , Zr IV and U VI complexes of 4-methylphenylamino acetoacetylacetone hydrazone have been synthesized and characterized by elementals analyses, i.r., u.v.-vis. spectra, magnetic moments, conductances, thermal analyses (d.t.a and t.g.a) and e.s.r measurements. The i.r. data show that, the ligand behaves as a neutral bidentate type (10), (13) and neutral tridentate type (4), (11), (12) and (21) monobasic bidentate type (7) or monobasic tridentate type (and (22) or dibasic tridentate type (5), (9) and (17) towards the metal ion. Molar conductances in DMF solution indicate that, the complexes are non-electrolytes. The e.s.r spectra of solid complexes (8) and (10) show axial type spectra with g k > g ? > 2:0023, a d (x 2 -y 2 ) ground state with significant covalent bond character. However, complex (12), shows an isotropic type, indicating a octahedral manganese(II) complex. Antibacterial and antifungal tests of the ligand and some of its metal complexes are also carried out and it has been observed that, the complexes are more potent bactericides and fungicides than the ligand.
Complexes of VO2+, Mn2+, Co2+, Ni2+, Cu2+, Zn2+, Ru3+ and UO22+ with (3‐(hydroxyimino)butan‐2‐ylidene)isonicotinohydrazide were synthesized and characterized using physical and spectral methods. Analytical data revealed that the complexes formed in 1:1 or 1:2 metal–ligand ratios. Spectral studies showed that the ligand bonded to the metal ion in neutral tridentate, monobasic tridentate or monobasic bidentate fashion through azomethine nitrogen atom, protonated/deprotonated imine oxime group and/or ketonic/enolic carbonyl group. From the electronic spectral data together with magnetic susceptibility values a square planar, tetrahedral or distorted octahedral structure can be proposed for all complexes. Electron spin resonance spectra for Cu2+ complexes (2–4) revealed axial symmetry with g|| > g⊥ > ge, indicating distorted octahedral or square planar structures and the unpaired electron exists in a
dx2−y2 orbital with marked covalent bond feature. The prepared complexes showed good to excellent biological activity, and the most active complexes against Aspergillus niger were 4 and 9 with zone of inhibition of 25 and 23 mm, respectively. Complexes 10 and 11 showed interesting activity against Escherichia coli with zone of inhibition of 44 and 32 mm, respectively.
Novel 13 mononuclear complexes derived from 3-(2-(2,4,6-trichlorophenyl) hydrazono) butan-2-one oxime with various molar ratio, geometry and different mode of interaction were prepared using transition metal Cd 2+ , Zn 2+ , Cu 2+ , Ni 2+ , Co 2+ , Fe 3+ , Mn 2+ , and VO 2+. The structure of these compounds was investigated physically, analytically, and spectrophotometrically. The ligation sites of the free 3-(2-(2,4,6-trichlorophenyl) hydrazono) butan-2-one oxime were designated via molecular modeling calculations. Furthermore, quantum chemical parameters for the ligand and its complexes were calculated. The analytical and spectral data revealed that the complexes (2-13) were formed with molar ratio of (1 M:1 L) or (1 M:2 L) in which hydrazone oxime adhered with the metal ion as a univalent or neutral bidentate chelator, via the imino nitrogen atom of hydrazone moiety and oximato nitrogen atom of deprotonated/protonated oxime moiety adopting different geometrical structures. The electron spin resonance (ESR) spectra of Cu 2+ complexes (7-8) and (10-11) were referred to axial symmetry with g jj > g ┴ > g e , which indicated that unpaired electron is localized in a d (x2 − y2) orbital with notable bonding covalency nature. The thermo analysis (thermogravimetry [TG]) confirmed that the complexes were decayed in one, two, three, or four steps starting with dehydration process, elimination of coordination water molecules, or removal of anions and completed with the whole decomposition of the complexes with the formation of metal oxide. The ligand did not exhibit antimicrobial activities, but its complexes showed variable activities.
A series of Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), La(III), Ru(III), Hf(IV), Zr(IV) and U(VI) complexes of phenylamino acetoacetylacetone hydrazone have been synthesized and characterized by elemental analyses, IR, UV-Vis, magnetic moments, conductances, thermal analyses (DTA and TGA) and ESR measurements. The IR data show that the ligand is neutral bidentate, monobasic bidentate, monobasic tridentate or dibasic tridentate towards the metal ion. Molar conductances in DMF indicate that the complexes are non-electrolytes. The ESR spectra of solid [(L)(HL)Cu 2 (NO 3 )(H 2 O)] Á 1/2H 2 O (10) and [(H 2 L)Cu(Cl) 2 (H 2 O) 2 ] (11) show axial spectra with g k 4g ? 42.0023 indicating d ðx 2 Ày 2 Þ ground state with significant covalent bond character. However, [(HL) 2 Mn 2 (Cl) 2 (H 2 O) 4 Á H 2 O (13) shows an isotropic spectrum, indicating manganese(II) to be octahedral. Antibacterial and antifungal tests of the ligand and some of its metal complexes revealed that the complexes are more potent bactericides and fungicides than the ligand.
In this work, new samples of PVA-TiO2/Cu nanocomposites were prepared via the casting method. The prepared samples were examined using different analytical methods. An XRD analysis showed the semi-crystalline nature of the PVA polymer, as well as showing a decrease in the degree of the crystallinity of the PVA structure as a result of the addition of the mixed nanoparticles. TEM images indicate the spherical shape of the Cu NPs, with a size ranging from 2 to 22 nm, and the rectangular shape of the TiO2 NPs, with a size ranging from 5 to 25 nm. It was evident via FTIR measurements that there were interactions between the functional groups of the PVA and the TiO2/Cu NPs. The optical properties of the PVA nanocomposites were improved with an increase in the content of the TiO2/Cu nanoparticles, as shown via a UV/Vis analysis. DSC curves showed an improvement in the thermal stability of the PVA-TiO2/Cu nanocomposites after the embedding of the TiO2/Cu nanoparticles. It was evident using impedance spectroscopy that the AC conductivity was improved by adding the TiO2 and Cu nanoparticles to the polymeric matrix. The maximum AC conductivity was found at 1.60 wt.% of TiO2/Cu nanoparticles in the PVA polymer, and this was 13.80 × 10−6 S/cm at room temperature. Relaxation occurred as a result of the charge carrier hopping between the localized state and the correlated barriers hopping model, describing the dominant mechanism, as presented in an electrical modulus analysis. These results indicate that the PVA-TiO2/Cu nanocomposite samples can be used in energy storage capacitor applications and in the alternative separator-rechargeable lithium-ion battery industry.
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