Hydrothermal synthesis, crystal structures, and properties of Co and Ni supramolecular complexes with 2,4,6-trimethyl benzoate and 4,4′-bipyridyl

Two new coordination complexes, viz. [Co(tmb)₂(4,4′-bpy)₂(H₂O)₂](Htmb)₂ (1) and {[Ni(tmb)₂(μ-4,4′-bpy)₂(H₂O)₂](4,4′-bpy)}_n (2), have been hydrothermally synthesized by reaction of the corresponding metal acetate with 2,4,6-trimethylbenzoic acid (Htmb) and 4,4′-bipyridyl (4,4′-bpy). X-ray single-crystal diffraction suggests that complex 1 represents a discrete mononuclear species in which the central metal ion is coordinated by the terminal carboxylate moiety and the 4,4′-bipyridyl ligand. The crystal structure of complex 2 reveals a 1D chain coordination polymer in which the Ni(II) ions are connected by the bridging 4,4′-bipyridyl ligands. In both cases, the coordination arrays are further extended via hydrogen bonding interactions to generate 3D supramolecular networks. Complexes 1 and 2 have also been characterized by spectroscopic (IR and UV/Vis), thermal (TGA) and magnetic susceptibility measurements. In addition, both complexes exhibit antimicrobial activity.     

A lab-on-a-chip for rapid blood separation and quantification of hematocrit and serum analytes

In this work, a new lab-on-a-chip for rapid analysis of low volume blood samples was designed, fabricated and demonstrated for integration of serum separation, hematocrit evaluation, and protein quantitation. Blood separation was achieved using microchannel flow-based separation. A novel method for evaluating hematocrit from microfluidic flow-separated blood samples was developed using gray scale analysis of a point-and-shoot digital photograph of separated blood in a micochannel. Protein quantitation was subsequently performed in a high surface area-to-volume ratio microfluidic chemiluminescent immunoassay using cell depleted serum produced by microfluidic flow-based separation of whole blood samples. All three steps were achieved in a single microchannel with separation of blood samples and hematocrit evaluation in less than 1 min, and protein quantitation in 5 min.     

Faster oxygen atom transfer catalysis with a tungsten dioxo complex than with its molybdenum analog

The synthesis and characterization of a series of molybdenum ([MoO(2)Cl(L(n))]; L(1) (1), L(2) (3)) and tungsten ([WO(2)Cl(L(n))]; L(1) (2), L(2) (4)) dioxo complexes (L(1) = 1-methyl-4-(2-hydroxybenzyl)-1,4-diazepane and L(2) = 1-methyl-4-(2-hydroxy-3,5-di-tert-butylbenzyl)-1,4-diazepane) of tridentate aminomonophenolate ligands HL(1) and HL(2) are reported. The ligands were obtained by reductive amination of 1-methyl-1,4-diazepane with the corresponding aldehyde. Complexes 3 and 4 were obtained by the reaction of [MO(2)Cl(2)(dme)(n)] (M = Mo, n = 0; W, n = 1) with the corresponding ligand in presence of a base, whereas for the preparation of 1 and 2 the ligands were deprotonated by KH prior to the addition to the metal. They were characterized by NMR and IR spectroscopy, by cyclic voltammetry, mass spectrometry, elemental analysis and by single-crystal X-ray diffraction analysis. Solid-state structures of the molybdenum and tungsten cis-dioxo complexes reveal hexa-coordinate metal centers surrounded by two oxo groups, a chloride ligand and by the tridentate monophenolate ligand which coordinates meridionally through its [ONN] donor set. In the series of compounds 1-4, complexes 3 and 4 have been used as catalysts for the oxygen atom transfer reaction between dimethyl sulfoxide (DMSO) and trimethyl phosphine (PMe(3)). Surprisingly, faster oxygen atom transfer (OAT) reactivity has been observed for the tungsten complex [WO(2)Cl(L(2))] (4) in comparison to its molybdenum analog [MoO(2)Cl(L(2))] (3) at room temperature. The kinetic results are discussed and compared in terms of their reactivity.     

Influence of alkali metal sodium doping on the properties of potassium hydrogen phthalate (KHP) crystals

The effect of doping sodium on the growth process and properties of potassium hydrogen phthalate (KHP) single crystals by slow evaporation solution growth technique has been investigated. Incorporation of sodium into the crystalline matrix even in the presence of low dopant concentration in aqueous growth medium is well confirmed by energy dispersive X-ray spectroscopy and quantified by atomic absorption spectroscopy and inductively coupled plasma emission spectrometer (ICP) techniques. The FT-IR spectral analysis confirms the slight distortion of the structure of the crystals as a result of doping. The TG-DTA studies reveal the purity of the material and no decomposition is observed up to the melting point. Low Na-doping (10 mol%) slightly increases the second harmonic generation efficiency, whereas heavy doping {[KHP]:[Na] = 1:1} results in significant enhancement. It has also been found that the doping results in morphological changes.     

Growth of <201> 8-hydroxyquinoline organic crystal by Czochralski method and its characterizations

In this study, 8-Hydroxyquinoline (8HQ) single crystal has been successfully grown by Czochralski method. The unit cell parameters of 8HQ single crystal were confirmed by single crystal X-ray diffraction analysis. The crystalline perfection of grown crystal has been analyzed by high-resolution X-ray diffractometry. Fourier transform infrared spectral studies have been performed to identify the functional groups. The UV?CVis-NIR studies show that the grown 8HQ crystal??s cutoff wavelength is around 390?nm. The thermal property of the grown crystal was studied by thermogravimetric and differential thermal analysis. The laser damage threshold value of the grown crystal was measured at multiple-shot mode using Nd:YAG laser. The dielectric measurements were carried out to determine the dielectric behavior for the crystal. The SHG efficiency of 8HQ is 0.8 times that of KDP.     

Effect of bismuth on liquid-phase epitaxy (LPE) grown GaAs layer using Ga–As–Bi melt

GaAs epitaxial layers of high structural quality have been realised from Ga–As–Bi melt using liquid-phase epitaxy (LPE). LPE grown GaAs epitaxial layer using bismuth solvent on GaAs substrate has been found to be of good structural perfection as compared to layers using gallium solvent. The temperature-dependent PL spectra of GaAs layer, grown from Ga+Bi mixed solvent has shown that the use of bismuth does not change the band energy. ECV depth profile of heavily zinc-doped epitaxial layer shows uniform doping in the GaAs layer grown using gallium solvent as compared to the layer grown using bismuth solvent.     

Sub-boundaries on (002) cleavages of Li2CO3 single crystals

Linear arrays of dislocations (straight, terminating and curved) are observed on etching with 2% citric acid (002) cleavages of lithium carbonate (Li₂CO₃) single crystals, grown by zone melting technique. As the dislocations are non-uniformly spaced and disappear on successive etching, they may not be revealing low-angle grain boundary, nor slip traces as they are terminating and curved meaning crystallographically non-oriented. On the observation of experiments on successive etching and etching of matched pairs, it is concluded that the arrays of etch pits reveal dislocation walls (dislocation density 1.1 × 10⁶ — 1.5 × 10⁷ pits cm⁻²) probably created due to the localized thermal stresses released as a result of high temperature annealing of the crystal during growth. The implications are discussed.     

Crystallization of an organic intercalation compound: cholic acid

Crystals of cholic acid have been grown in silica and tetramethoxy silane gels. Crystals grew with different morphology and Leisegang rings were also seen in some cases. Crystals were analyzed by X-ray, IR and microhardness studies. The grown crystals were found to be monohydrate and the hardness of the crystals were found to decrease with increase of load.     

Fourier‐transform infrared and Raman spectra,vibrational assignment and density functional theory calculations of 1,4,5‐triazanaphthalene

The Fourier‐transform infrared (FT‐IR) (4000–50 cm⁻¹) and Raman spectra (3500–100 cm⁻¹) of 1,4,5‐triazanaphthalene in polycrystalline state were measured. Comparison between the spectra by two techniques, a series of density functional theory (DFT) calculations and the spectral behaviour upon deuteration were used for the assignment of the vibrational spectra of the title compound. The calculated vibrational wavenumbers by the B3LYP density functionals are generally consistent with the observed spectra. Copyright © 2009 John Wiley & Sons, Ltd.