New vic-dioxime transition metal complexes

New vic-dioxime ligands and their Cu^II, Co^III, Ni^II and VO^IV complexes have been prepared and characterized by elemental analyses, i.r. and u.v. spectra, magnetic moments and molar conductance data. The Co^III complexes are diamagnetic. The ¹H- and ¹³C-n.m.r. and g.c./m.s. spectra of the vic-dioxime ligands and their Co^III complexes were recorded. The compounds are all non-electrolytes.     

Antimicrobial activity studies of mononuclear and binuclear mixed-ligand copper(II) complexes derived from Schiff base ligands and 1,10-phenanthroline

Mixed-ligand complexes of copper(II) with 1,10-phenanthroline and various Schiff bases have been prepared and characterized by elemental analysis, electronic and i.r. spectra, magnetic moment and molar conductance data. The Schiff base behave as bidentate ligands, and the mixed-ligand copper(II) complexes of the ligands HL1, HL2 and HL4 are binuclear. The conductivity data for all the complexes are consistent with those expected for an electrolyte. Antimicrobial activities of some of the ligands and complexes have been tested against Bacillus megaterium and Candida tropicalis. 1H and 13C n.m.r. spectra have been recorded in order to solve the solution structure of the ligands. Thermal properties of all complexes have been studied by the d.t.a. and t.g.a. techniques.     

Characteristics of traps in TlInS2 single crystals

Characteristics of charge traps in TlInS₂ single crystals are investigated by the use of thermally stimulated current (TSC) technique. The TSC spectra of the sample from 80 K to 300 K are recorded at a constant heating rate. The spectra reveal that there are several trapping levels associated with the complex structure of overlapping peaks. The experimental results indicate that the traps in TlInS₂ associated with the spectra in the measuring range of temperature obey the monomolecular (first order) kinetics. Thus, the spectra are resolved into first order shaped peaks by the use of computerized best fit procedure. The trapping parameters; such as the energy depth, temperature dependent frequency factor and capture cross section, together with concentrations of the corresponding six discrete levels are computed. These centers all having low capture cross sections with strong temperature dependence are found to be at the energies of 0.11 eV, 0.22 eV, 0.25 eV, 0.26 eV, 0.29 eV and 0.30 eV with high concentrations of 6.6 × 10¹⁶, 2.0 × 10¹⁷, 3.3 × 10¹⁷, 9.6 × 10¹⁶, 2.3 × 10¹⁷ and 4.0 × 10¹⁷ cm^?3, respectively.     

Amino alcohol based chiral solvating agents: synthesis and applications in the NMR enantiodiscrimination of carboxylic acids

Four optically active amino alcohols were synthesized via the ring opening of (R)-N-(2,3-epoxypropyl)phthalimide with (R)-2-phenyl glycinol, (1R,2S)-cis-1-amino-2-indanol, (R)-2-amino-1-butanol and (S)-phenyl ethylamine in 73-93% yields. The enantioselective recognition of these receptors towards the enantiomers of racemic carboxylic acids was studied by ¹H NMR spectroscopy. The molar ratio and the association constants of the chiral compounds with each of the enantiomers of the guests were determined by using Job plots and a non-linear least-squares fitting method, respectively. Large non-equivalent chemical shifts (up to 30.0 Hz) can be achieved in the presence of chiral amino alcohols 2 and 5. Amongst the chiral receptors used, compound 5 was found to be the best chiral shift reagent, and was effective in the determination of the enantiomeric excess of chiral carboxylic acids.     

Transition metal complexes of bidentate Schiff base ligands

New Schiff base ligands derived from vanillin (HL¹), 4-dimethylaminobenzaldehyde (HL²) and 3,5-di-t-butyl-4-hydroxybenzaldehyde (HL³) with N-(pyridyl)-3-methoxy-4-hydroxy-5-aminobenzylamine (2) and their copper(II), cobalt(II), nickel(II), oxovanadium(IV) and zinc(II) transition metal complexes have been synthesized and characterized by elemental analyses, electronic and i.r. spectra, molar conductance data and by 1H and ¹³C n.m.r. spectra. The results indicate that the ligands coordinate through azomethine nitrogen and phenolic oxygen to the metal ions. In like manner, it was found that the pyridine and amine nitrogen atoms are not coordinated to the metal ions. The ¹H and ¹³C n.m.r. spectral data confirmed the suggested structure for the Schiff base ligands, and the mass spectra results confirmed the proposed structure of the ligands. The antimicrobial activity properties of the ligands and their metal complexes have been studied.     

Synthesis of new chiral calix[4]azacrowns for enantiomeric recognition of carboxylic acids

Two novel chiral calix[4]azacrown ethers 4 and 5 bearing a furfuryl group on the nitrogen atom were developed by the reaction of dibromo- or ditosyl derivatives of p-tert-butylcalix[4]arenes 2 and 3 with a chiral diol, 1. The enantioselective recognition of these receptors towards the enantiomers of racemic carboxylic acids has been studied by ¹H NMR spectroscopy. The molar ratio and the association constants of the chiral compounds 4 and 5 with each of the enantiomers of guest molecules were determined by using Job plots and a nonlinear least-squares fitting method, respectively. The Job plots indicate that both of the hosts form 1:1 instantaneous complexes with (R)- or (S)-mandelic acid and (l)- or (d)-dibenzoyltartaric acid. The receptors exhibited different chiral recognition abilities towards the enantiomers of racemic guests.     

Mechanical, thermal, and fire retardant properties of poly(ethylene terephthalate) fiber containing zinc phosphinate and organo-modified clay

The effect of zinc bisdiethylphosphinate (ZnPi) and organoclay on mechanical, thermal, and flame retardant properties of poly(ethylene terephthalate) (PET) fiber was investigated. ZnPi was preferred due to its fusible character at spinning temperature and organoclay was used for synergistic interaction. The mechanical, thermal, and flame retardant properties of fibers were examined by tensile testing, thermogravimetric analysis (TG), and micro combustion calorimeter (MCC). The tensile strength of the PET fiber reduced with the addition of both ZnPi and organoclay. The TG results showed that the inclusion of ZnPi increased the char residue. The MCC results showed that the addition of organoclay increased the barrier effect of formed char which depends on char amount, thickness, and integrity and reduces the maximum heat evolved during the test. This result was also important in terms of showing that the organoclay was effective in thermally thin samples.     

Inequality constrained ridge regression estimator

We carry out the idea of inequality constrained least squares (ICLS) estimation of Liew (1976) to the inequality constrained ridge regression (ICRR) estimation. We propose ICRR estimator by reducing the primal–dual relation to the fundamental problem of Dantzig and Cottle, 1967, Cottle and Dantzig, 1974 with Lemke (1962) algorithm. Furthermore, we conduct a Monte Carlo experiment.     

Calix[4]arene-triazine conjugate intermediate: optical properties and gas sensing responses against aromatic hydrocarbons in Langmuir–Blodgett films

Research on Chemical Intermediates - The detection of organic vapors by chemically based sensors was achieved with macromolecules having convenient molecular cavities. Addressed herein, a...     

A novel triazine‒bearing calix[4]arene: Design,synthesis and gas sensing affinity for volatile organic compounds

A novel triazine-calix[4]arene conjugate was designed and synthesized with the aim to study gas sensing against volatile organic compounds (VOCs) such as dichloromethane, chloroform and carbon tetrachloride. This novel compound was fully characterized by spectroscopic techniques such as FTIR, ¹H and ¹³C NMR along with HRMS and BET analysis. The triazine based calix[4]arene organic materials were fabricated onto quartz glasses and quartz crystal substrates to form a thin film chemical sensor element by using Langmuir-Blodgett (LB) technique. Quartz Crystal Microbalance, UV–Visible Spectroscopy, Atomic Force Microscopy and Scanning Electron Microscopy techniques were employed to characterize all these LB thin film layers. Fick's Equations were used for analyzing the swelling process of LB thin film sensor and diffusion coefficient values of organic vapours for swelling were obtained. The initial experiments have revealed that new triazine appended calix[4]arene derivative exhibited an effective chemical gas sensor characteristic with a large response to dichloromethane vapour.