Preparation, characterization and thermolysis of metal nitrate complexes with 4,4’-bipyridine

Two bis(bipyridine) polymeric metal nitrate complexes with 4,4’-bipyridine of simple formula like [M(bipy)₂](NO₃)2⋅xH₂O (where M=Co, Ni and Cu; x=4, 2 and 0, respectively) have been prepared and characterized. Their thermal decomposition has been undertaken using simultaneous TG-DTG-DTA and DSC in nitrogen atmosphere and non-isothermal TG in air atmosphere. Isothermal TG has been performed at decomposition temperature range of the complexes to evaluate the kinetics of decomposition by applying model-fitting as well as isoconversional method. Possible mechanistic pathways have also been proposed for the thermolysis. Ignition delay measurements have been carried out to investigate the response of these complexes under the condition of rapid heating.     

Carbocyclic galanthamin analogs: 4a,5,9,10,11,12‐hexahydro‐6H‐benzo[b]cyclohepta[cd]benzofurans

The synthesis of a novel unnatural carbocyclic analog of the acetylcholine esterase inhibitor galanthamine with a K₃[Fe(CN)₆] promoted oxidative tandem cyclization as the key step is reported.     

Determination of the magnetic symmetry of hexagonal manganites by second harmonic generation

Optical second harmonic spectroscopy is introduced as a powerful supplement for the determination of complex magnetic structures. Experimental efforts are simplified and new degrees of freedom are opened. Thereby, some principal or technical restrictions of neutron or magnetic x-ray diffraction experiments are overcome. High spatial resolution leads to additional information about magnetically ordered matter. As an example, the noncollinear magnetic structure of the hexagonal manganites RMnO3 ( R = Sc, Y, Ho, Er, Tm, Yb, Lu) is analyzed. The results show that some earlier conclusions on their magnetic symmetry and properties should be revised.     

Dielectric recovery of copper chromium vacuum interrupter contactsafter short-circuit interruption

The recovery of a vacuum interrupter gap after short-circuit interruption was measured by application of an overshooting transient recovery voltage (TRV) several tens of microseconds after current zero. Copper chromium contact materials were employed varying in composition (25 and 50% chromium content), gas content, and production method. The gap failure was either pure dielectric or it was dominated by a significant postarc current. Therefore, postarc current phenomena were experimentally investigated focused on the relationship among the postarc current, the power frequency current amplitude, and the gap length. It was found that two postarc current maxima exist: the first strongly dependent on the power frequency current, and the second on the field strength. A correlation among postarc current facilitated failures, the ultimately dielectric recovery, and the erosion rate of the material was found. Strong indication is given that all of these effects are dominated by the metal vapor pressure rise given by the constricted rotating arc. A significant influence of the material properties can be drawn from these experiments, allowing a good estimation of the capability for short-circuit current interruption, thus providing a useful tool for material development     

Antimicrobial and cytotoxic activities of leaves, twigs and stem bark of Scutia buxifolia Reissek

The antimicrobial and cytotoxic activities of the dichloromethane, ethyl acetate and butanolic fractions from the leaves, twigs and stem bark of Scutia buxifolia were evaluated using the broth microdilution method and the brine shrimp lethality method, respectively. Phytochemical analysis was performed by thin layer chromatography (TLC) and high-performance liquid chromatography (HPLC). The antimicrobial results demonstrated that the strongest effect occurred with the butanol fraction from the twigs and the ethyl acetate fraction from the stem bark against Saccharomyces cerevisiae (minimal inhibitory concentration; MIC?=?62.5?μg?mL(-1)), whereas the ethyl acetate and butanolic fractions from the twigs and stem bark were effective against Pseudomonas aeruginosa and Staphylococcus aureus, with MIC values ranging from 125 to 500?μg?mL(-1). LD(50) values varied from 50.00?±?0.22 to 82.23?±?0.34?μg?mL(-1). Quercetin, quercitrin, isoquercitrin and rutin were identified by HPLC and may be partially responsible for the antimicrobial activities observed. This study reports for the first time the antimicrobial and cytotoxic activities of S. buxifolia leaves, twigs and stem bark.     

Catechol imine ligands: from helicates to supramolecular tetrahedra

Di- and tricatechol imines are easily accessible by condensation of appropriate amines with 2,3-dihydroxybenzaldehyde. Dicatechol imines can be used for the alkali metal template-directed self-assembly of dinuclear triple-stranded helicates or meso-helicates with high diastereoselectivity. Tricatechol imines lead in self-assembly processes to metallosupramolecular 4 [ratio] 4 tetrahedra with a huge internal cavity, which is able to encapsulate guest species. Hereby the special features of the imine unit can be used to control the outcome of the self-assembly process.     

Isolation and chromatographic analysis of bioactive triterpenoids from the bark extract of Cariniana domestica (Mart) Miers

The Lecythidaceae family is composed of 25 genera and 400 species that occur in the form of trees with a pantropical distribution. The genera Cariniana belongs to the family Lecythidaceae, and there are few reports considering these species. In this work, fractionation of the dichloromethane fraction obtained from the aqueous extract of the stem bark of Cariniana domestica (Mart) Miers, popularly known as Jequitibá-roxo, led to the isolation of two mixtures of triterpenoids: lupeol and β-amyrin and β-sitosterol and stigmasterol. The structures of the isolated compounds were elucidated by spectroscopic (NMR) and chromatographic (GC-MS) techniques as well as literature data comparisons. β-Sitosterol, stigmasterol, lupeol and β-amyrin were quantified in dichloromethane fraction by high-performance liquid chromatography (HPLC/DAD). The dichloromethane fraction was also investigated for antioxidant and antifungal activities. The isolated compounds and their biological activities are reported for the first time for the species C. domestica.     

Effect of Ti doping on Ta2O5 stacks with Ru and Al gates

The Ti-doped Ta₂O₅ thin films (<10 nm) obtained by rf sputtering are studied with respect to their composition, dielectric and electrical properties. The incorporation of Ti is performed by two methods - a surface doping, where a thin Ti layer is deposited on the top of Ta₂O₅ and a bulk doping where the Ti layer is sandwiched between two layers of Ta₂O₅. The effect of the process parameters (the method and level of doping) on the elemental distribution in-depth of the films is investigated by the time of flight secondary ion mass spectroscopy (ToF-SIMS). The Ti and Ta₂O₅ are intermixed throughout the whole thickness but the layers are very inhomogeneous. Two sub-layers exist in all the samples — a near interfacial region which is a mixture of Ta-, Ti-, Si-oxides as well as TaSiO, and an upper Ti-doped Ta₂O₅ sub-layer. For both methods of doping, Ti tends to pile-up at the Si interface. The electrical characterisation is performed on capacitors with Al- and Ru-gate electrodes. The two types of MIS structures exhibit distinctly different electrical behavior: the Ru gate provides higher dielectric permittivity while the stacks with Al electrode are better in terms of leakage currents. The specific metal-dielectric reactions and metal-induced electrically active defects for each metal electrode/high-k dielectric stack define its particular electrical behavior. It is demonstrated that the Ti doping of Ta₂O₅ is a way of remarkable improvement of leakage characteristics (the current reduction with more than four orders of magnitude as compared with undoped Ta₂O₅) of Ru-gated capacitors which originates from Ti induced suppression of the oxygen vacancy related defects.     

Dicatechol-diimines: easily accessible ligands for the self-assembly of dinuclear triple-stranded helicates

Dicatechol ligands 3b-g-H4 are simply prepared by imine formation of 2,3-dihydroxybenzaldehyde 2 with a series of different diamines 1b-g . An X-ray structural analysis was obtained for the butyl-bridged compound 3e-H4, showing an intramolecular proton transfer and the formation of a chinoidic "keto-amine" structure. The dicatechol derivatives 3b-g-H4 form dinuclear triple-stranded helicates M4[(3)3Ti2] with titanium(IV) ions in the presence of alkali-metal carbonate. For the phenyl- and the trans-1,4-cyclohexyl-bridged complexes, K4[(3b)3Ti2] and Na4[(3f)3Ti2], X-ray structures were obtained.