Crystal Structures of [Bu2Sn(O2PPh2)2], [Ph2Sn(O2PPh2)2], and [PhClSn(O2PPh2)OMe]2. Raman Spectra of [Ph2Sn(O2PPh2)2] and [PhClSn(O2PPh2)OMe]2

[(n‐Bu)₂Sn(O₂PPh₂)₂] ( 1 ), and [Ph₂Sn(O₂PPh₂)₂] ( 2 ) have been synthesized by the reactions of R₂SnCl₂ (R=n‐Bu, Ph) with HO₂PPh₂ in Methanol. From the reaction of Ph₂SnCl₂ with diphenylphosphinic acid a third product [PhClSn(O₂PPh₂)OMe]₂ ( 3 ) could be isolated. X‐ray diffraction studies show 1 to crystallize in the monoclinic space group P2₁/c with a = 1303.7(1) pm, b = 2286.9(2) pm, c = 1063.1(1) pm, β = 94.383(6)°, and Z = 4. 2 crystallizes triclinic in the space group , the cell parameters being a = 1293.2(2) pm, b = 1478.5(4) pm, c = 1507.2(3) pm, α = 98.86(3)°, β = 109.63(2)°, γ = 114.88(2)°, and Z = 2. Both compounds form arrays of eight‐membered rings (SnOPO)₂ linked at the tin atoms to form chains of infinite length. The dimer 3 consists of a like ring, in which the tin atoms are bridged by methoxo groups. It crystallizes triclinic in space group with a = 946.4(1) pm, b = 963.7(1) pm, c = 1174.2(1) pm, α = 82.495(6)°, β = 66.451(6)°, γ = 74.922(6)°, and Z = 1 for the dimer. The Raman spectra of 2 and 3 are given and discussed.     

Utilization of 4-chloro-7-nitro-2,1,3-benzoxadiazole (NBD-Cl) for kinetic spectrophotometric assay of befunolol hydrochloride in its pharmaceutical formulation

A simple, accurate, precise, and sensitive kinetic spectrophotometric method for determination of befunolol hydrochloride is described. The method is based on the formation of a colored product with 4-chloro-7-nitro-2,1,3-benzoxadiazole (NBD-Cl) in methanol at 70 degrees C for 45 min. The red-colored product was measured at 523 nm. The optimization of various experimental conditions is described; Beer's law was obeyed in the range 15.25 x 10(-6) to 122.04 x 10(-6) M. The results obtained showed good recoveries (100.1 +/- 0.80%). Application of the proposed method to a pharmaceutical formulation was successfully achieved. The determination of befunolol hydrochloride by fixed time, fixed concentration, and rate constant methods was feasible with the calibration equation obtained. However, the fixed time method proved to be more applicable.     

Anti-Alzheimer and Anti-COX-2 Activities of the Newly Synthesized 2,3′-Bipyridine Derivatives (II)

3-Amino-4-aryl-6-pyridin-3-ylthieno[2,3-b]pyridine-2-carbohydrazides 3a,b were used as the starting materials in the present study. Our targets here were represented by the synthesis of several 3-amino-N′-4-arylmethylenes 5a,b, N-formamides 8a,b, ethyl imidoformate 10b, N,N-dimethyl-N′-imidoformamides 12a,b, N-acetyl-N-acetamides 14a,b, 1,3,4-oxadiazole-2-thiol 16a,b, pyrazolothienopyridines 20a,b, 2-[(3,5-dimethyl-1H-pyrazol-1-yl)carbonyl]-4-aryl-6-pyridin-3-ylthieno[2,3-b]pyridin-3-amines 22a,b, 2-carbonyl-5-methyl-2,4-dihydro-3H-pyrazol-3-ones 24a,b, and 2-carbonyl-pyrazolidine-3,5-diones 26a,b. The newly synthesized heterocyclic compounds were tested as anti-Alzheimer and anti-COX-2 agents, and their structures were elucidated by considering the data of IR, ¹H NMR, mass spectra, and elemental analyses.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Synthesis,Spectroscopic Studies and Crystal Structures of [Et2Sn(O2AsMe2)2] and [Ph2Sn(O2AsMe2)(μ‐OMe)]2

[Et₂Sn(O₂AsMe₂)₂] ( 1 ) and [Ph₂Sn(O₂AsMe₂)(μ‐OMe)]₂ ( 2 ) were synthesized by treatment of Et₂SnO and Ph₂SnS with HO₂AsMe₂ in Methanol, respectively. The compounds were characterized by elemental analyses, vibrational spectroscopy and mass spectrometry. According to X‐ray diffraction measurements compound 1 crystallizes monoclinic in space group P2₁/n with cell parameters a = 804.89(3), b = 987.11(5), c = 966.42(4) pm, β = 113.354(3)°. The unit cell parameters of 2 , which crystallizes in the same space group, are a = 974.4(1), b = 1463.3(1), c = 1228.9(1) pm, β = 111.324(3)°. The (SnOAsO)₄ rings of 1 are linked and form a two‐dimensional network with the SnEt groups pointing into the holes of the next layer. Compound 2 occurs as a dimer with internal Sn(OMe)₂Sn bridges in the (SnOAsO)₂ rings. The vibrational and mass spectra are given and discussed.     

Comparison of Electropolishing of Aluminum in a Deep Eutectic Medium and Acidic Electrolyte

Research advances in electropolishing, with respect to the field of metalworking, have afforded significant improvements in the surface roughness and conductivity properties of aluminum polished surfaces in ways that machine polishing and simple chemical polishing cannot. The effects of a deep eutectic medium as an acid-free electrolyte were tested to determine the potential energy thresholds during electropolishing treatments based upon temperature, experiment duration, current, and voltage. Using voltammetry and chronoamperometry tests during electropolishing to supplement representative recordings via atomic force microscopy (AFM), surface morphology comparisons were performed regarding the electropolishing efficiency of phosphoric acid and acid-free ionic liquid treatments for aluminum. This eco-friendly solution produced polished surfaces superior to those surfaces treated with industry standard acid electrochemistry treatments of 1 M phosphoric acid. The roughness average of the as-received sample became 6.11 times smoother, improving from 159 nm to 26 nm when electropolished with the deep eutectic solvent. This result was accompanied by a mass loss of 0.039 g and a 7.2 µm change in step height along the edge of the electropolishing interface, whereas the acid treatment resulted in a slight improvement in surface roughness, becoming 1.63 times smoother with an average post-electropolishing roughness of 97.7 nm, yielding a mass loss of 0.0458 g and a step height of 8.1 µm.     

Surface layer-by-layer chemical deposition reaction for thin film formation of nano-sized metal 8-hydroxyquinolate complexes

The feasibility of a novel and simple layer-by-layer chemical deposition method for the preparation of nano-sized metal 8-hydroxyquinolate complexes has been investigated and reported. Uniform nanocrystalline films have been synthesized via dipping a substrate alternately in metal ion solution followed by ligand solution. The stoichiometry of the as-grown anhydrous Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) complex crystals were confirmed from the metal analysis and molar stoichiometric ratio of metal ion to 8-hydroxyquinoline. This was characterized as 1:2 for the Co(II), Ni(II), Cu(II) and Zn(II)–quinolate complexes. The Fe(III)–quinolate thin film was found to exhibit a 1:3 ratio. Electron impact-mass spectra (EI-MS) of all the synthesized thin film metal quinolate complexes were recorded and the results refer to the existence of the molecular ion peak at the corresponding m/z values. Confirmation of such stoichiometric 1:2 and 1:3 ratios were also evident from the (EI-MS) study. The deposited thin films were also subjected to analysis by a scanning electron microscope (SEM) and a particle size ?50 nm was detected. FT-IR and UV–Vis spectroscopy were further used to confirm the structure of the metal 8-hydroxyquinolate complexes. Thermal gravimetric analysis (TGA) was also used to follow up the possible thermal decomposition steps and to calculate the thermodynamic parameters of the nano-sized metal complexes.     

über Verbindungen des Thoriums mit Stickstoff und Wasserstoff

Preparation and Vibrational Spectra of N-Trimethylsilyl-Tris(trimethylsiloxy)-Vanadium (V) imine, (Me₃SiO)₃V?N? SiMe₃ The preparation of the title compound from VOCl₃ and hexamethyl-disilazane is described. The vibrational spectra of the compound suggest a vanadium-nitrogen triple bond and a near linear vanadium–nitrogen–silicon arrangement.     

Analytical model for dust generated by air-cushion vehicles

The air-cushion vehicle (ACV) is widely used over unconsolidated soils and rugged terrain. This off-the-road vehicle can have mobility problems as well as cause environmental problems. Most of these problems cannot be fully controlled but measures can be taken to minimize their effect. Two of the mobility problems are dust generation and ground surface erosion. This research is a continuation of previous attempts at understanding the mechanics of dust generation and the evaluation of parameters representing soil resistance to disturbance under the air cushion pressure. Specifically this research provides a comprehensive analytical approach by which the characteristics of ACV dust raising, residence time and sedimentation rates are evaluated. Stoke's Law is used in this analysis with concomitant practical assumptions. Field utilization of these models is developed, and predetermination of dust size distribution above ground level, as well as possible particulate dispersions during the dust raising stage are reported. With this information the dust distribution and amount of dust in the atmosphere can be predicted at any time and at any elevation above the ground. Relationships between the quasi-theoretical analyses and the experimental results were considered and found to be in good agreement.     

Solubility and thermodynamic studies of sparingly soluble tellurite salts

Journal of Thermal Analysis and Calorimetry - In the past few years, tellurium has attracted much attention as it is widely used in a large number of important industrial applications. Despite its...