Structural studies of six and four coordinate zinc(II), nickel(II) and dioxovanadium(V) complexes with thiosemicarbazones

Three Zn(II) complexes of di-2-pyridyl ketone thiosemicarbazone, an octahedral Ni(II) complex of 2-acetylpyridine hexamethyleneiminyl-3-thiosemicarbazone, and a V(V) complex of 2-acetylpyridine morpholyl-3-thiosemicarbazone were prepared and characterized. Crystal structure of Ni(II) and V(V) complexes are reported. The ligand in the nickel complex is found to coordinate in the thione form with a pseudo octahedral geometry and the vanadium(V) complex has trigonal bipyramidal geometry.     

Catalytic determination of silver by means of the 1,2-diaminoethane—peroxodisulphate reaction

A kinetic method for the determination of 5.0 × 10^-3–8.0 × 10^-6 M silver ion is based on the catalysis by silver of the reaction between 1,2-diaminoethane and peroxodisulphate, and titration of the residual oxidant. Copper and manganese interfere at 10:1 mole ratios; zinc and iron are tolerated.     

4-Salicylideneamino-3-methyl-1,2,4-triazole-5-thione as a sensor for aniline recognition

Tridentate triazole based Schiff base 4-salicylideneamino-3-methyl-1,2,4-triazole-5-thione has been found to selectively detect toxic aromatic amines such as aniline and benzene-1,4-diamine by simple titration techniques like UV-visible, fluorescence spectral studies (PL) and 1H NMR titrations. The Schiff base receptor utilizes, thione sulfur, NH-thione and the phenolic hydroxyl group to form hydrogen bonded adduct of aniline and benzene-1,4-diamine with high binding affinity, followed by a slow removal of the corresponding hydrogens thus providing a promising candidate and an unique receptor for toxic aromatic amines.     

Multiple beams surface plasmon interference generation: A theoretical analysis

In this paper, multiple beams surface plasmon (SP) interference generation based on prism coupling technique is theoretically analyzed and presented. The proposed multiple beams SP interference configuration is investigated for nanolithography application for two-dimensional feature fabrication. The configuration is then numerically and experimentally analyzed by employing aluminum metal at 364-nm illumination wavelengths to realize high resolution and high aspect ratio two-dimensional periodic nanoscale dot array patterns on the recording medium.     

Desvenlafaxine succinate monohydrate

The title compound {systematic name: [2‐(1‐hydroxycyclohexyl)‐2‐(4‐hydroxyphenyl)ethyl]dimethylammonium 3‐carboxypropanoate monohydrate}, C₁₆H₂₆NO₂⁺·C₄H₅O₄⁻·H₂O, is a succinate salt of O‐desmethylvenlafaxine (desvenlafaxine). The present structure is one of four reported polymorphs of this salt, which is a new antidepressant drug. The carboxyl group of the succinate anion adopts a rare anti conformation and is engaged in a very short O—H...O⁻ hydrogen‐bond contact. Both cations and anions are involved separately in the formation of distinct O—H...O hydrogen‐bonded networks. Desvenlafaxine cations and water molecules self‐assemble to generate a honeycomb layer, while the succinate anions form a linear tape structure. These hydrogen‐bonded networks are interlinked via N—H...O and O—H...O hydrogen bonds. The hydrogen‐bonding network is so strong that desolvation and melting occur together at approximately 402 K. Thus, the crystal structure may be used to understand the thermal stability and solubility of the compound at the molecular level.     

Selection of pH-related parameters in ion-exchange chromatography using pH-gradient operations

This work demonstrates that the type of ion-exchanger (anion or cation), the mode of operation (bind-and-elute or flow-through), and the operational pH of ion-exchange chromatography (IEX) can be selected in a fast and rational way by analytical pH-gradient IEX operations, thereby eliminating the need for pH scouting or high-throughput screening. The developed approach was applied for the selection of an IEX process for the capture of a monoclonal antibody (MAb) from hybridoma cell culture supernatant (CCS). It was found within a day that MAb can optimally be captured by bind-and-elute mode cation-exchange chromatography (CEX) at pH 4.5 or anion-exchange chromatography (AEX) at pH 7.2 without lowering the salt concentration in the CCS. The performance of both CEX and AEX was predicted to be equal for this particular MAb capture.     

Differentiating the gum resins of two closely related Indian Gardenia species, G. gummifera and G. lucida, and establishing the source of dikamali gum resin using high-performance thin-layer chromatography and ultra-performance liquid chromatography-UV/MS

Dikamali is a gum resin obtained from the leaf buds of Gardenia lucida or G. gummifera. There is controversy regarding the botanical source of this gum resin with some stating it to be from G. lucida while others claim it to be from G. gummifera. Analytical methods including UPLC and HPTLC were developed for the qualitative analysis of Gardenia species and various commercial samples. The separation using a UPLC method was achieved within 12.0 min by using C18 column material, a water/acetonitrile mobile phase, both containing formic acid, a gradient system, and a temperature of 40 degrees C. Extensive studies of dikamali collected from various parts of India in comparison with the gum resins collected from G. lucida and G. gummifera clearly indicated that the botanical source of commercially available dikamali is G. lucida, not G. gummifera. The marker compounds isolated from a market sample of dikamali were present only in the gum resin of G. lucida and the compounds isolated from G. gummifera were not present in any of the dikamali samples, confirming the botanical source of dikamali. This work is of utmost importance, given the ambiguity regarding the botanical source of the gum resin dikamali. LC/MS coupled with electrospray ionization is described for the identification and confirmation of nine compounds from various samples of the gum resin. An HPTLC method was also developed for the fast chemical fingerprint analysis of Gardenia samples.     

Alkali promoted rare earth metal phosphates for vapour phase O-alkylation of α- and β-naphthols with methanol

The vapor-phase catalytic O-alkylation of - and -naphthols with methanol has been investigated over lanthanum, cerium, samarium, and antimony phosphate catalysts promoted with cesium hydroxide. Among various catalysts investigated, the Cs-SmPO₄ combination catalyst provided better catalytic activity and selectivity. The CsOH promoter suppressed formation of C-alkylated side products and enhanced the O-alkylation selectivity. Characterization of these catalysts by X-ray diffraction and FT-infrared techniques revealed that the cesium promoter has no influence on the bulk structure of the catalysts. Temperature programmed desorption of anhydrous ammonia over promoted and unpromoted catalysts revealed that the cesium promoter decreases total surface acidity of the catalysts.     

Highly efficient Pd‐PEPPSI‐IPr catalyst for N‐(4‐pyridazinyl)‐bridged bicyclic sulfonamides via Suzuki–Miyaura coupling reaction

A protocol for the Suzuki–Miyaura coupling of novel 2‐(6‐chloropyridazin‐3‐yl)‐5‐(aryl/heteroarylsulfonyl)‐2,5‐diazabicyclo[2.2.1]heptanes and heteroarylboronic acids to afford variety of coupled products was realized. Pd‐PEPPSI‐IPr catalyst was found to be a powerful and reusable catalyst under relatively mild reaction conditions.     

Modeling the coupling of reaction kinetics and hydrodynamics in a collapsing cavity

We introduce a model of cavitation based on the multiphase Lattice Boltzmann method (LBM) that allows for coupling between the hydrodynamics of a collapsing cavity and supported solute chemical species. We demonstrate that this model can also be coupled to deterministic or stochastic chemical reactions. In a two-species model of chemical reactions (with a major and a minor species), the major difference observed between the deterministic and stochastic reactions takes the form of random fluctuations in concentration of the minor species. We demonstrate that advection associated with the hydrodynamics of a collapsing cavity leads to highly inhomogeneous concentration of solutes. In turn these inhomogeneities in concentration may lead to significant increase in concentration-dependent reaction rates and can result in a local enhancement in the production of minor species.