Green synthesis of zinc oxide particles with apple-derived compounds and their application as catalysts in the transesterification of methyl benzoates
ZnO nanoparticles (ZnONPs) were successfully synthesized using bravo-de-esmolfe apple extract in aqueous medium at room temperature. ZnO microparticles, prepared with a pure apple phytochemical, quercetin (ZnOq), or without phytochemicals (ZnO) were studied for comparative purposes. The re-use of apple waste for highly efficient catalyst production, based on green synthetic routes, can be added to the concept of a circular economy. The synthesized ZnO particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and N2 adsorption/desorption Brunauer-Emmett-Teller (BET) theory.
The XRD patterns indicated the formation of a hexagonal wurtzite phase with high purity and SEM and TEM analyses revealed the morphology of the particles. The apple extract produced spherical ZnONPs composed of round lamina-like structures, similar to the micro sized lamina-like shape of ZnOq and dissimilar to the flower-like shape of ZnO. The green synthesized ZnO nanoparticles (ZnONPs) led to a high product yield of ca. 96% within 24 h of reaction time in the transesterification reaction of different carboxylic esters.
Study on the substitution effects of zinc benzoate terpyridine complexes on photoluminescence, antiproliferative potential and DNA binding properties
Six zinc(II) complexes, [Zn(OCOPh)2LR] (R = 1, 2, 3, 4, 5, 6) were synthesized by the reaction of zinc benzoate and six para-substituted 4-phenyl-terpyridine complexes and their structures were confirmed by elemental analysis, FT-IR, 1H NMR and X-ray single crystal diffraction analysis. Their photoluminescent properties in solid and in solutions of DMSO were studied. Three human cancer cell lines were used for antiproliferative potential: human lung cancer cell line (A549), human esophageal cancer cell line (Eca-109) and human breast cancer cell line (MCF-7). The results have shown that these zinc complexes have good inhibitory effects on cancer cells, which are better than that of the commonly used clinical drug cisplatin.
The ability of the complexes to binding to CT-DNA was studied by UV spectroscopy and fluorescence titration, while the interaction between the complexes and CT-DNA, AT6, GC6 short-chain DNA sequences and G-quadruplex were analyzed by circular dichroism (CD). It is found that these complexes can bind to DNA, and the binding mode is mainly intercalator. The docking of the complexes with the DNA fragment was simulated using molecular docking software. All the results clearly display that the substituents at these ligands of the complexes have the substitution effects on the properties of photoluminescence, antiproliferative potential and DNA binding study.
Crystal structure of tri-aqua-(4-cyano-benzoato-κ(2) O,O’)(nicotinamide-κN (1))zinc 4-cyano-benzoate.
The asymmetric unit of the title salt, [Zn(C8H4NO2)(C6H6N2O)(H2O)3](C8H4NO2), contains one complex cation and one 4-cyano-benzoate (CNB) counter-anion. The Zn(II) atom in the cation is coordinated by one 4-cyano-benzoate ligand, one nicotinamide (NA) ligand and three water mol-ecules, the CNB anion thereby coordinating in a bidentate O,O’-mode through the carboxyl-ate group. The latter, together with one water O atom and the N atom of the NA ligand, form a distorted square-planar arrangement, while the considerably distorted octa-hedral coordination sphere of the Zn(II) atom is completed by the two O atoms of additional water mol-ecules in the axial positions. The dihedral angles between the planar carboxyl-ate groups and the adjacent benzene rings in the two anions are 10.25 (10) and 5.89 (14)°. Inter-molecular O-H⋯O hydrogen bonds link two of the coordinating water mol-ecules to two free CNB anions. In the crystal, further hydrogen-bonding inter-actions are present, namely N-H⋯O, O-H⋯O and C-H⋯O hydrogen bonds that link the mol-ecular components, enclosing R 2 (2)(12), R 3 (3)(8) and R 3 (3)(9) ring motifs and forming layers parallel to (001). π-π contacts between benzene rings [centroid-to-centroid distances = 3.791 (1) and 3.882 (1) Å] may further stabilize the crystal structure.
trans-Tetra-aqua-bis-(isonicotinamide-κN (1))zinc bis-(3-hy-droxy-benzoate) tetra-hydrate.
The asymmetric unit of the title compound, [Zn(C6H6N2O)2(H2O)4](C7H5O3)2·4H2O, contains half of the complex cation with the Zn(II) ion located on an inversion center, a 3-hy-droxy-benzoate counter-anion and two uncoordinating water mol-ecules. Four water O atoms in the equatorial plane around the Zn(II) ion [Zn-O = 2.089 (2) and 2.128 (2) Å] form a slightly distorted square-planar arrangement and the distorted octa-hedral geometry is completed by the two N atoms [Zn-N = 2.117 (2) Å] from two isonicotinamide ligands.
In the anion, the carboxyl-ate group is twisted from the attached benzene ring at 9.0 (2)°. In the crystal, a three-dimensional hydrogen-bonding network, formed by classical O-H⋯O and N-H⋯O and weak C-H⋯O hydrogen bonds, consolidates the crystal packing, which exhibits π-π stacking between the benzene and pyridine rings, with centroid-centroid distances of 3.458 (2) and 3.609 (2) Å. One of the two H atoms of each uncoordinating water mol-ecule is disordered over two orientations with an occupancy ratio of 0.60:0.40.
Crystal structure, spectral, thermal and dielectric studies of a new zinc benzoate single crystal.
Single crystals of zinc benzoate with a novel structure were grown in gel media. Sodium metasilicate of gel density 1.04 g/cc at pH 6 was employed to yield transparent single crystals. The crystal structure of the compound was ascertained by single crystal X-ray diffractometry. It was noted that the crystal belongs to monoclinic system with space group P2(1)/c with unit cell parameters a=10.669(1)Å, b=12.995(5)Å, c=19.119(3)Å, and β=94.926(3)°. The crystal was seen to possess a linear polymeric structure along b-axis; with no presence of coordinated or lattice water. CHN analysis established the stoichiometric composition of the crystal.
The existence of functional groups present in the single crystal system was confirmed by FT-IR studies. The thermal characteristic of the sample was analysed by TGA-DTA techniques, and the sample was found to be thermally stable up to 280°C. The kinetic and thermodynamic parameters were also determined. UV-Vis spectroscopy corroborated the transparency of the crystal and revealed the optical band gap to be 4 eV. Dielectric studies showed decrease in the dielectric constant of the sample with increase in frequency.
Investigation of the zinc(II)-benzoate-2-pyridinealdoxime reaction system.
The employment of pyridine-2-carbaldehyde oxime (paoH) in zinc(II) benzoate chemistry, in the absence or presence of azide ions, is described. The syntheses, crystal structures and spectroscopic characterization are reported for the complexes [Zn(O(2)CPh)(2)(paoH)(2)] (1), [Zn(12)(OH)(4)(O(2)CPh)(16)(pao)(4)] (2) and [Zn(4)(OH)(2)(pao)(4)(N(3))(2)] (3). The Zn(II) centre in octahedral 1 is coordinated by two monodentate PhCO(2)(-) groups and two N,N’-chelating paoH ligands.
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The metallic skeleton of 2 describes a tetrahedron encapsulated in a distorted cube. The {Zn(12)(μ-OH)(4)(μ(3)-ΟR)(4)}(16+) core of the cluster can be conveniently described as consisting of a central {Zn(4)(μ(3)-ΟR)(4)}(4+) cubane subunit (RO(-) = pao(-)) linked to four {Zn(2)(μ-OH)}(3+) subunits via the OH(-) group of each of the latter, which becomes μ(3). The molecule of 3 has an inverse 12-metallacrown-4 topology. Two triply bridging hydroxido groups are accommodated into the metallacrown ring. Each pao(-) ligand adopts the η(1) : η(1) : η(1) : μ coordination mode, chelating one Zn(II) atom and bridging a Zn(II)(2) pair. Complexes 1 and 2 display photoluminescence with maxima at ∼355 nm and ∼375 nm, upon maximum excitation at 314 nm; the origin of the photoluminescence is discussed.
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