Prediction of grain size,thickness and absorbance of nanocrystalline tin oxide thin film by Taguchi robust design

Transparent conductive films of tin oxide were deposited on glass substrates under various deposition conditions. Taguchi analysis was used to model the dependence of the grain size, thickness and absorbance of nanocrystalline tin oxide on the process parameters namely pH value, concentration, time of deposition and bath temperature. The effect of the mentioned process parameters on the grain size, thickness and absorbance of deposited layer during the deposition of nanocrystalline was investigated using X-ray diffraction (XRD) technique, atomic force microscopy (AFM) and UV–Visible spectroscopy. Comparison between the model predictions and the experimental observations predicted a remarkable agreement between them. The predictions of the model and sensitivity analysis showed that among the effective process parameters, deposition time and concentration were the main parameters having significant effect on crystalline size. Bath temperature had the most significant effect on absorbance and deposition time had a dominant effect on thickness.     

Molecular structure and EPR spectra studies of saccharinate complexes with 4-acetylpyridine

The crystal structures of [Co(4-acpy)₂(H₂O)₄] (sac)₂ (1) and [Zn(4-acpy)₂(H₂O)₄] (sac)₂ (2) (4-acpy: 4-acetylpyridine, sac: saccharinate) complexes have been investigated by X-ray diffraction techniques. The magnetic environments of Cu²⁺ doped [Co(4-acpy)₂(H₂O)₄] (sac)₂ and [Zn(4-acpy)₂(H₂O)₄] (sac)₂ complexes have been identified by electron paramagnetic resonance (EPR) technique. Principal values of g and hyperfine tensors are determined and the ground state wave functions of Cu²⁺ ions are obtained using EPR parameters. The vibrational spectra were also discussed in relation with the other compounds containing saccharinate and 4-acetylpyridine complexes.     

Supramolecular Architecture in the 1:1 Co-Crystallization of 6,7-Dimethoxy-2-methyl-4-phenylisoquinolinium Cation with Perchlorate Anion

Abstract  X-ray crystallographic analysis of the title organic ion–pair complex, C₁₈H₁₈NO₂ ⁺ · ClO₄ ⁻, reveals that 6,7-dimethoxy-2-methyl-4-phenylisoquinolinium cation is co-crystallized with perchlorate counter-anions in 1:1 ratio. The complex crystallizes in space group P 2 ₁ /n, with a = 8.0226(7) ?, b = 12.2552(7) ?, c = 17.9734(16) ?, β = 93.908(7) °, Z = 4, D _x  = 1.431 g/cm³. Aromaticity of isoquinolinium fragment is considerably deformed by the existence of C–H···O type weak H-bonds, leading to chains of topology C ₃ ³(12)[R ₁²(4)] running along b-axis of the unit cell and pseudo-cyclic centrosymmetric R ₄⁴(24)[2R ₁²(4)] synthons. The weak H-bonds serve to stabilize both the extended structure and molecular geometry of the title complex, in particular the disordered perchlorate anion whose components adopt a distorted tetrahedron. Index Abstract  Molecular and the extended structure of 6,7-dimethoxy-2-methyl-4-phenylisoquinolinium perchlorate, C₁₈H₁₈NO₂ ⁺ · ClO₄ ⁻, were determined by single crystal X-ray diffraction study.     

An intramolecular substitution of hydroperoxy-endoperoxide to a bis-endoperoxide

[reaction: see text] A new and stereospecific synthesis for bis-endoperoxide has been developed starting from tetrahydronaphthalene. Photooxygenation of tetrahydronaphthalene resulted in the formation of hydroperoxy-endoperoxide. The bromination reaction of hydroperoxy-endoperoxide gave bis-endoperoxide, whose exact configuration has been determined by X-ray analysis. The lowest-energy conformer of bis-endoperoxide is the boat-chair form.     

Newly synthesized Cu(II) pyrazino[2,3‐f][1,10]phenanthroline complexes as potential anticancer candidates

New binary and ternary copper(II) complexes, [Cu(py‐phen)₂(NO₃)]NO₃ ( 1 ), [Cu₂(py‐phen)₂(gly)₂(NO₃)₂(H₂O)₂]?3H₂O ( 2 ) and [Cu₂(py‐phen)₂(tyr)₂(H₂O)₂](NO₃)₂?3H₂O ( 3 ) (py‐phen: pyrazino[2,3‐f][1,10]phenanthroline; gly: glycine; tyr: tyrosine), have been synthesized and characterized using CHN analysis, electrospray ionization mass spectrometry, Fourier transform infrared spectroscopy and single‐crystal X‐ray diffraction. Interaction of these complexes with calf thymus DNA has been investigated using absorption spectral titration, ethidium bromide and Hoechst 33258 displacement assay and thermal denaturation measurements. These complexes were found to be efficient cleaving agents and cleavage reactions were mediated by hydrolytic and oxidative pathways. The interaction between these complexes and bovine serum albumin (BSA) was investigated using electronic absorption and fluorescence spectroscopy. The experimental results show that the fluorescence quenching mechanism of these complexes and BSA is a static quenching process. Furthermore, in vitro cytotoxicities of these complexes against tumour cell lines (Caco‐2, MCF‐7 and A549) and healthy cell line (BEAS‐2B) showed that they exhibited anticancer activity with low IC₅₀ values. These complexes were markedly active against the cell lines and can be good drug candidates that are effective and safe for healthy tissue.     

Synthesis of eight-membered aminocyclitol analogues

The first syntheses of four stereoisomeric diaminocyclooctane diols, as well as a chlorocyclooctane aminodiol, are reported. In the first part, photooxygenation of cis,cis-1,3-cyclooctadiene gave a bicyclic endoperoxide, which was reduced with zinc followed by mesylation of the hydroxyl groups. Treatment with sodium azide afforded 1,4- and 1,2-cyclooctene diazides. Oxidation of the double bonds in the isomeric diazides with OsO₄, followed by hydrogenation of the azide groups, led to 3,8-diaminocyclooctane-1,2-diol and 3,4-diaminocyclooctane-1,2-diols. In the second part, cis-3,8-diazidocyclooctene was converted into the corresponding epoxide. Stereospecific hydrolysis of the epoxide ring with HCl_(g) in methanol, and hydrogenation of the azide groups gave 3,8-diamino-2-chloro-cyclooctan-1-ol. Bromination of the double bond in cyclooctene diacetate, followed by acetate deprotection, azidolysis of the bromides, and hydrogenation of the azide groups resulted in the formation of 2,3-diaminocyclooctane-1,4-diol.     

Synthesis,crystal structure,stability studies,DNA/albumin interactions,and antimicrobial activities of two Cu(II) complexes with amino acids and 5-nitro-1,10-phenanthroline

One-dimensional (1-D) coordination polymer and mononuclear copper(II) complexes, ([Cu(nphen)(asn)]ClO₄)_n (1) and [Cu(nphen)(gln)(H₂O)]ClO₄·H₂O (2) (nphen = 5-nitro-110-phenanthroline, asn = asparagine, gln = glutamine), have been synthesized and characterized by IR spectroscopy, ESI-MS, CHN analysis, and single-crystal X-ray diffraction. These binary and ternary complexes of copper(II) with nphen, asn, and gln have been investigated using potentiometric methods in 0.1 M KCl aqueous ionic media at 298.2 K. The protonation constants of the ligands and the stability constants of 1 and 2 have been calculated from the potentiometric data using the “BEST” software package. The potentiometric results have been analyzed using the “SPE” software package, and the distribution curves for the copper-containing species have been determined for the ternary systems. The CT-DNA-binding properties of these complexes have been investigated by thermal denaturation measurements and both absorption and emission spectroscopy. Further, the interaction of these complexes with bovine serum albumin (BSA) and human serum albumin (HSA) has been investigated using absorption and emission spectroscopy. The thermodynamic parameters, free energy change (ΔG), enthalpy change (ΔH), and entropy change (ΔS) were calculated by the van’t Hoff equation and discussed. The distances between the serum albumins and 1 and 2 have been obtained according to fluorescence resonance energy transfer (FRET). Conformational changes of serum albumins have been observed from synchronous fluorescence technique. The antimicrobial activity of the complexes has also been tested on some bacteria. The effect of different amino acids on the copper(II) complexes are discussed.     

Removal of thorium(IV) from aqueous solution by biosorption onto modified powdered waste sludge: experimental design approach

The biosorption of radioactive Th(IV) ions in the aqueous solutions onto the modified powdered waste sludge (MPWS) has been examined. In this context, the parameters affecting biosorption of Th(IV) from aqueous solutions has been examined by using MPWS biosorbent in Box Behnken statistical experimental design. The structure of MPWS biosorbent was characterized by using SEM and BET techniques. According to the experimental design results, MPWS and Th(IV) concentrations should be kept high to achieve the maximum efficiency in Th(IV) biosorption. On the other hand, MPWS, which is also used as a biosorbent, is an economical, effective and natural biosorbent.

     

Surface structure and photoluminescence properties of AZO thin films on polymer substrates

Al‐doped zinc oxide (AZO) thin films were deposited on indium tin oxide (ITO) coated polyethylene terephthalate (PET) substrates by radio frequency (RF) magnetron sputtering method at room temperature. The effects of film thickness on the surface structure and the photoluminescence properties of the films were investigated by atomic force microscopy (AFM), secondary ion mass spectroscopy (SIMS) and room temperature photoluminescence (PL). AFM analysis showed that the surface of all films was extremely flat and uniform at nanoscale. Root mean square (RMS) value of the surface roughness which scanned the surface area of 3 µm by 3 µm and grain size increased with increasing the film thickness. Thus, the surface morphology of the films became rough because of the coarse grains. The depth profile of AZO layers was analyzed by SIMS. It was found that the thickness of the AZO layer is almost same with the desired film thickness. The PL intensity of the dominant peak decreased and shifted slightly towards the shorter wavelengths with increasing the film thickness. According to the relationships between luminescence intensity and crystalline characteristics, it was observed that the intensity of the peak decreased by the increased surface area of the grains. Copyright © 2014 John Wiley & Sons, Ltd.     

Synthesis, experimental and theoretical characterization of palladium(II) and platinum(II) saccharinate complexes with 2-(2-pyridyl)benzimidazole

New palladium(II) and platinum(II) complexes of saccharinate (sac) with 2-(2-pyridyl)benzimidazole (pybim) have been synthesized and characterized by elemental analysis and spectroscopic techniques. From the experimental studies, these complexes were formulated as [Pd(pybim)(sac)2] (1), and [Pt(pybim)(sac)2]·4H2O (2). The ground-state geometries of both complexes were optimized using density functional theory (DFT) methods at the B3LYP level. A bidentate pybim ligand together with two N-coordinated sac ligands form the square-planar MN4 coordination geometry around the palladium(II) and platinum(II) ions. The calculated IR and UV-vis spectral data have been correlated to the experimental results. Thermal analysis data support the molecular structures of both complexes.