New palladium(II) complexes with pyrazole ligands Part II. Synthesis, spectral and thermal studies, and antitumor evaluation

This study describes the synthesis, IR, (1)H, and (13)C{(1)H} NMR spectroscopic as well the thermal characterization of the new palladium(II) pyrazolyl complexes [PdCl(2)(HmPz)(2)] 1, [PdBr(2)(HmPz)(2)] 2, [PdI(2)(HmPz)(2)] 3, [Pd(SCN)(2)(HmPz)(2)] 4 {HmPz = 4-methylpyrazole}. The residues of the thermal decomposition were identified as Pd(0) by X-ray powder diffraction. From the initial decomposition temperatures, the thermal stability of the complexes can be ordered in the sequence: 1 > 2 > 4 a parts per thousand 3. The cytotoxic activities of the complexes and the ligand were investigated against two murine cancer cell lines: mammary adenocarcinoma (LM3) and lung adenocarcinoma (LP07) and compared to cisplatin under the same experimental conditions.

Mono- and dinuclear palladium(II) compounds containing N,S donor ligands - Synthesis, characterization and thermal behavior

Synthesis, spectroscopic characterization and thermal analysis of the compounds [Pd-2(dmba)(2)(mu-NCO)(mu-2-qnS)] (1), [Pd-2(dmba)(2)(mu-NCO)(mu-8-qnS)] (2), [Pd(2-qnS)(2)] (3) and [Pd(8-qn(S))2] (4) (dmba=N,N-dimethylbenzylamine; 2-qnS=2-quinolinethiolate; 8-qnS=8-quinolinethiolate) are described. The thermal decomposition of these compounds occurs in four consecutive steps and the final decomposition products were identified as Pd(0) by X-ray powder diffraction. The thermal stability order of the complexes is 4 > 3 > 1 > 2.

Microstructural and electrochemical study of La0.5Li0.5TiO3

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Monoclinic-tetragonal phase transition in Pb(Zr1-xTix)O-3 studied by infrared spectroscopy

The discovery of a new monoclinic phase in the PbZr1-xTixO3 (PZT) system in the vicinity of the morphotropic phase boundary (MPB), previously considered as a region where the rhombohedral and tetragonal phases of PZT coexist, was recently reported. Investigations of this new phase were reported using different techniques such as high-resolution synchrotron x-ray powder diffraction and Raman spectroscopy. The main objective has been to define a new phase diagram of PZT. In this context, infrared spectroscopic studies were performed in the vicinity of the MPB and studies were initially centred on a PZT sample with x = 0.49 mol% Ti content. Results suggested that the monoclinic --> tetragonal phase transition occurs at 237 K, confirming the use of IR as a useful technique to investigate this phase transition.

Infrared studies of the monoclinic-tetragonal phase transition in Pb(Zr, Ti)O-3 ceramics

Recently, the observation of a new monoclinic phase in the PbZr1-xTixO3 (PZT) system in the vicinity of the morphotropic phase boundary was reported. Investigations of this new phase were reported using different techniques such as high-resolution synchrotron x-ray powder diffraction and Raman spectroscopy. In this work, the monoclinic --> tetragonal phase transition in PbZr0.50Ti0.50O3 ceramics was studied using infrared spectroscopy between 1000 and 400 cm(-1). The four possible nu(1)-stretching modes (Ti-O and Zr-O stretch) in the BO6 octahedron in the ABO(3) structure of PZT in this region were monitored as a function of temperature. The lower-frequency mode nu(1)-(Zr-O) remains practically unaltered, while both intermediate nu(1)-(Ti-O) modes decrease linearly as temperature increases from 89 to 263 K. In contrast, the higher-frequency nu(1)-(Ti-O) and nu(1)-(Zr-O) modes present anomalous behaviour around 178 K. The singularity observed at this mode was associated with the monoclinic --> tetragonal phase transition in PbZr0.50Ti0.50O3 ceramics.

Hydrothermal Microwave: A New Route to Obtain Photoluminescent Crystalline BaTiO3 Nanoparticles

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural and dielectric properties of relaxor Sr0.5Ba0.5Bi2Nb2O9 ceramic

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Desenvolvimento de sistema magnético polimérico contendo antimicrobianos para tratamento de infecções por Helicobacter pylori

Helicobacter pylori is the main cause of gastritis, gastroduodenal ulcer disease and gastric cancer. The most recommended treatment for eradication of this bacteria often leads to side effects and patient poor compliance, which induce treatment failure. Magnetic drug targeting is a very efficient method that overcomes these drawbacks through association of the drug with a magnetic compound. Such approach may allow such systems to be placed slowed down to a specific target area by an external magnetic field. This work reports a study of the synthesis and characterization of polymeric magnetic particles loaded with the currently used antimicrobial agents for the treatment of Helicobacter pylori infections, aiming the production of magnetic drug delivery system by oral route. Optical microscopy, scanning electron microscopy, transmission electron microscopy, x-ray powder diffraction, nitrogen adsorption/desorption isotherms and vibrating sample magnetometry revealed that the magnetite particles, produced by the co-precipitation method, consisted of a large number of aggregated nanometer-size crystallites (about 6 nm), creating superparamagnetic micrometer with high magnetic susceptibility particles with an average diameter of 6.8 ± 0.2 μm. Also, the polymeric magnetic particles produced by spray drying had a core-shell structure based on magnetite microparticles, amoxicillin and clarithromycin and coated with Eudragit® S100. The system presented an average diameter of 14.2 ± 0.2 μm. The amount of magnetite present in the system may be tailored by suitably controlling the suspension used to feed the spray dryer. In the present work it was 2.9% (w/w). The magnetic system produced may prove to be very promising for eradication of Helicobacter pylori infections

Structural and dielectric characterization of praseodymium-modified lead titanate ceramics synthesized by the OPM route

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Crystal structure of isotibolone: a major degradation product of tibolone

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Synchrotron structural characterization of electrochemically synthesized hexacyanoferrates containing K(+): A revisited analysis of electrochemical redox

The presumably soluble KFe(+3)[Fe(2+)(CN)(6)] structure of electrochemically synthesized hexacyanoferrate materials (Prussian Blue) containing K(+) ions was determined for the first time in this study. Prior to drawing conclusions from a structural analysis, the main goal was to make a precise analysis of the inferred soluble structure, that is, KFe(+3) [Fe(2+)(CN)(6)], which is frequently referred to in the literature as the final stable electrochemically synthesized structure. Indeed, a successful X-ray powder diffraction experiment using X-ray synchrotron radiation was made of a powder placed in a 0.5 mm diameter borosilicate glass capillary, which was obtained by removing sixty 90 nm thin films from the substrates on which they were prepared. However, the conclusions were highly unexpected, because the structure showed that the [Fe(CN)61 group was absent from similar to 25% of the structure, invalidating the previously presumed soluble KFe(+3)[Fe(2+)(CN)(6)] structure. This information led to the conclusion that the real structure of Prussian Blue electrochemically synthesized after the stabilization process is Fe(4)[Fe(CN)(6)](3)center dot mH(2)O containing a certain fraction of inserted K(+) ions. In fact, based on an electrogravimetric analysis (Gimenez-Romero et al., J. Phys. Chem. B 2006, 110, 2715 and 19352) complemented by the Fourier maps. it is possible to affirm that the K(+) was part of the water crystalline substructure. Therefore, the interplay mechanism was reexamined considering more precisely the role played by the water crystalline substructure and the K+ alkali metal ion. As a final conclusion, it is proposed that the most precise way to represent the structure of electrochemically synthesized and stabilized hexacyanoferrate materials is Fe(4)(3+) Fe(2+)(CN)(6)](3)center dot[K(h)(+)center dot OH(h)(-)center dot mH(2)O]. The importance of this result is that the widespread use of the terms soluble and insoluble in the electrochemical literature could be reconsidered. Indeed, only one type of structure is insoluble, and that is Fe(4)[Fe(CN)(6)](3)center dot mH(2)O hence, the use of the terms soluble and insoluble is inappropriate from a structural point of view. The result of the presence of the [Fe(CN)61 vacancy a, roup is that the water Substructure cannot be ignored in the ionic interplay mechanism which controls the intercalation and redox process, as was previously confirmed by electrogravimetric analyses (Gimenez-Romero et al., J. Phys. Chem. B 2006, 110, 2715 Garcia-Jareno et al., Electrochim. Acta 1998, 44, 395: Kulesza, Inorg. Chem. 1990, 29, 2395).

Using thermal and spectroscopic data to investigate the thermal behavior of epinephrine

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Thermal and spectroscopic investigation on N,N-dimethylbenzylamine based cyclopalladated compounds containing isonicotinamide

Synthesis, spectroscopic characterization and thermal analysis of the [Pd(dmba)(Cl)(iso)] (1), [Pd(dmba)(NCO)(iso)] (2), [Pd(dmba)(N(3))(iso)] (3) and [Pd(dmba)(Br)(iso)] (4) (dmba = N,N'-dimethylbenzylamine; iso = isonicotinamide) compounds are described in this work. The complexes were investigated by infrared spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition were identified as Pd(o) by X-ray powder diffraction. The thermal stability order of the complexes varied as [Pd(dmba)(Cl)(iso)] (1) > [Pd(dmba)(Br)(iso)] (4) > [Pd(dmba)(NCO)(iso)] (2) > [Pd(dmba)(N(3))(iso)] (3).

Synthesis, characterization, and thermal behavior of palladium(II) coordination compounds containing isonicotinamide

Palladium(II) coordination compounds of general formula trans-[PdX(2)(isn)(2)], X = Cl(-) (1), N(3) (-) (2), SCN(-) (3), NCO(-) (4), isn = isonicotinamide; were synthesized and characterized in solid state by elemental analysis, infrared spectroscopy, and simultaneous TG-DTA. TG experiments reveal that the compounds 1-4 undergo thermal decomposition in three or four stages, yielding Pd(0) as final residue, according to calculus and identification by X-ray powder diffraction.

Synthesis, spectral and thermal studies on dicarboxylate-bridged palladium(II) coordination polymers. Part I

This work describes the synthesis, IR and (13)C CPMAS NMR spectroscopic as well the thermal characterization of the new dicarboxylate complexes [Pd(2)(ox)(2)(4,4'-bipy)]n (1), [Pd(2)(ox)(2)(bpe)](n) (2) and [Pd(2)(ox)(2)(pz)](n) (3) {ox = oxalate, bipy = 4,4'-bipyridine, bpe = 1,2-bis(4-pyridyl)ethane, pz = pyrazine}. TG experiments reveal that compounds 1-3 undergo thermal decomposition in three steps. Metal palladium was the final product of the thermal decompositions, which was identified by X-ray powder diffraction.