Electronic structure, growth mechanism and photoluminescence of CaWO4 crystals

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

Quartz crystal microbalance as a tool for kinetic enzymatic assays by variation of pH

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

Loading of praziquantel in the crystal lattice of solid lipid nanoparticles Studies by DSC and SAXS

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

Study of zinc hexacyanoferrate-modified platinum electrodes using electrochemical quartz crystal microbalance

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Structural study of thin films prepared from tungstate glass matrix by Raman and X-ray absorption spectroscopy

Thin films were prepared using glass precursors obtained in the ternary system NaPO(3)-BaF(2)-WO(3) and the binary system NaPO(3)-WO(3) with high concentrations of WO(3) (above 40% molar). Vitreous samples have been used as a target to prepare thin films. Such films were deposited using the electron beam evaporation method onto soda-lime glass substrates. Several structural characterizations were performed by Raman spectroscopy and X-ray Absorption Near Edge Spectroscopy (XANES) at the tungsten L(I) and L(III) absorption edges. XANES investigations showed that tungsten atoms are only sixfold coordinated (octahedral WO(6)) and that these films are free of tungstate tetrahedral units (WO(4)). In addition, Raman spectroscopy allowed identifying a break in the linear phosphate chains as the amount of WO(3) increases and the formation of P-O-W bonds in the films network indicating the intermediary behavior of WO(6) octahedra in the film network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed identifying the presence of W-O and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO(3) concentrated samples (above 40% molar) attributed to the formation of WO(6) clusters. (C) 2008 Elsevier B.V. All rights reserved.

Vibrational spectra of pilocarpine hydrochloride crystals

Pilocarpine is a natural substance with potential application in the treatment of several diseases. In this work Fourier Transform (FT)-Raman spectrum and the Fourier Transform infra red (FT-IR) spectrum of pilocarpine hydrochloride C11H17N2O2+.Cl- were investigated at 300 K. Vibrational wavenumber and wave vector have been predicted using density functional theory (B3LYP) calculations with the 6-31 G(d,p) basis set. A comparison with experiment allowed us to assign most of the normal modes of the crystal.

Crystal structure of myotoxin-II: A myotoxic phospholipase A2 - Homologue from Bothrops moojeni venom.

The crystal structure of Myotoxin-II (MjTX-II), a Lys49 PLA(2)-homologue from Bothrops moojeni venom has been determined and refined at 2.0 Angstrom to a crystallographic residual of 19.7% (R-free = 28.1%). MjTX-II is a dimer in the crystal, with the monomers in the asymmetric unit related by a two-fold symmetry axis running through the dimer interface. The dimers of MjTX-II and the Lys49 PLA(2) from B. asper venom are similar, however the relative orientations of the monomers suggests a flexible dimer interface, which serves as a hinge between the two molecules.

Synthesis, electrochemical behavior and X-ray crystal and molecular structures of [Fe(diene)(CO)(2)PPh3] (diene = chalcone, sorbic acid)

The compounds [Fe(ch)(CO)(2)PP3] (1) (ch = chalcone) and [Fe(sba)(CO)(2)PPh3] (2) (sba = sorbic acid) were prepared by irradiating the tetracarbonyltriphenylphosphineiron(0) complex in benzene in the presence of ch or sba. The compounds were characterized by infrared and P-31 NMR spectroscopies. Their electrochemical behavior was investigated by cyclic voltammetry and the results suggest that their oxidations occur by more than one electrochemical step, producing free ch and sba, free PPh3 and solvated Fe(III). It was observed that sba ligand contributes more effectively to the stabilization of metal center in these complexes, the X-ray crystal and molecular structures of 1 and 2 were determined; it was shown that the Fe atom adopts a distorted octahedral coordinated geometry in which three of the sites are occupied by the ch or sba ligand. The [Fe(ch)(CO)(2)PPh3] complex is a monomer and the unit cell of complex 2 contains exist two identical and crystallographically independent molecules of [Fe(sba)(CO)(2)PPh3] which are linked by short hydrogen bonds O-H . . .O (C) 2001 Published by Elsevier B.V. Ltd.

1,3-dipolar cycloaddition of CS2 to the coordinated azide in the cyclopalladated [Pd(bzan)(mu-N-3)](2). Crystal and molecular structure of di(mu-N,S-1,2,3,4-thiatriazole-5-thiolate)bis[(benzylideneaniline-C-2,N)palladium(II)]

The compound [Pd(bzan)(mu -N-3)](2) 1, bzan = benzylideneaniline, was prepared from [Pd(bzan) (mu -OOCCH3)](2) by an anion exchange reaction. The 1,3-dipolar cycloaddition of carbon disulfide to the bridged coordinated azide in the cyclometallated compound I was investigated. The species resulting from this reaction, di(mu -N,S-1,2,3,4-thiatriazol-5-thiolate)bis[(benzylideneaniline)palladium(II)] 2, was characterized by IR spectroscopy and X-ray diffraction. The compound 2 is a dimer containing two [Pd(benzylideneaniline)] moieties connected by two vicinal bridging N,S-1,2,3,4-thiatriazole-5-thiolate anions in a square-planar coordination geometry for the palladium atoms.

REACTIONS OF MERCURIC ACETATE WITH PENTACARBONYLIRON IN ALCOHOLS - CRYSTAL AND MOLECULAR-STRUCTURES OF HG[FE(COOR)(CO)(4)](2) (R=CH3, C2H5)

Reactions of Hg(CH3COO)(2) with [Fe(CO)(5)] in MeOH and EtOH lead to the compounds Hg[Fe(COOR)(CO)(4)](2) (I for R = CH3 and II for R = C2H5). Crystals of I are triclinic, P (1) over bar, with a = 6.272(2), b = 6.441(3), c = 11.703(4) Angstrom, a = 92.94(3)degrees, beta = 103.77(3)degrees, gamma = 96.10(2)degrees, and Z = 1. Crystals of II are tetragonal, I4(1)/a, with a = 17.906(3) Angstrom, c = 12.756(2) Angstrom, and Z = 8. The geometry around Hg is linear for compound I and approximately linear for compound II. The Hg-Fe distances are 2.5716(8) and 2.575(4) Angstrom for compounds I and II, respectively. The geometry around the Fe in both compounds is approximately octahedral. The carboalkoxy group is cis to Hg in both compounds with Fe-C distances equal to 2.034(6) and 2.05(4) Angstrom for compounds I and II, respectively.

cDNA cloning and 1.75 angstrom crystal structure determination of PPL2, an endochitinase and N-acetylglucosamine-binding hemagglutinin from Parkia platycephala seeds

Parkia platycephala lectin 2 was purified from Parkia platycephala (Leguminosae, Mimosoideae) seeds by affinity chromatography and RP-HPLC. Equilibrium sedimentation and MS showed that Parkia platycephala lectin 2 is a nonglycosylated monomeric protein of molecular mass 29 407 +/- 15 Da, which contains six cysteine residues engaged in the formation of three intramolecular disulfide bonds. Parkia platycephala lectin 2 agglutinated rabbit erythrocytes, and this activity was specifically inhibited by N-acetylglucosamine. In addition, Parkia platycephala lectin 2 hydrolyzed beta(1-4) glycosidic bonds linking 2-acetoamido-2-deoxy-beta-D-glucopyranose units in chitin. The full-lengthamino acid sequence of Parkia platycephala lectin 2, determined by N-terminal sequencing and cDNA cloning, and its three-dimensional structure, established by X-ray crystallography at 1.75 angstrom resolution, showed that Parkia platycephala lectin 2 is homologous to endochitinases of the glycosyl hydrolase family 18, which share the (beta alpha)(8) barrel topology harboring the catalytic residues Asp125, Glu127, and Tyr182.

Crystal structure of bis(acetylacetonato)bis(quinoline)nickel(II), Ni(C5H14O2N)(2)(C9H7N)(2)

C28H28N2NiO4, triclinic, P (1) over bar (no. 2), a = 7.9202(6) angstrom, b = 8.0496(6) angstrom, c = 10.246(1) angstrom, alpha = 97.15(1)degrees, beta = 106.68(1)degrees, gamma = 94.686(9)degrees, V = 616.1 angstrom(3), Z = 1, R-gt(F) = 0.028, wR(ref)(F-2) = 0.078, T = 293 K.

New crystal forms of Diocleinae lectins in the presence of different dimannosides

Studying the interactions between lectins and sugars is important in order to explain the differences observed in the biological activities presented by the highly similar proteins of the Diocleinae subtribe. Here, the crystallization and preliminary X--ray data of Canavalia gladiata lectin (CGL) and C. maritima lectin (CML) complexed with Man(alpha 1-2)Man(alpha 1)OMe, Man(alpha 1-3)Man(alpha 1)OMe and Man(alpha 1-4)Man(alpha 1)OMe in two crystal forms [the complexes with Man(alpha 1-3)Man(alpha 1)OMe and Man(alpha 1-4)Man(alpha 1)OMe crystallized in space group P3(2) and those with Man(alpha 1-2)Man(alpha 1)OMe crystallized in space group I222], which differed from those of the native proteins (P2(1)2(1)2 for CML and C222 for CGL), are reported. The crystal complexes of ConA-like lectins with Man(alpha 1-4)Man(alpha 1)OMe are reported here for the first time.

Revisiting the addition reaction of TeCl4 to alkynes: the crystal structure and docking studies of 1-chloro-2-trichlorotelluro-3-phenyl-propen-2-ol

Tellurium tetrachloride adds to alkynes via two pathways: a concerted syn addition, that yields Z-tri- and tetra-substituted alkenes or by an anti addition that yields E-alkenes. The mechanistic aspects of these divergent pathways have been reevaluated at the light of crystallographic data. The molecules, of the title compound, in the crystal, are associated in a helical fashion with a Te...Te pitch of 6.3492(6) angstrom. As it exhibits inhibitory activity for cathepsin B and in order to gain more insight of the inhibition mechanism, a docking study was undertaken providing insight on why organic telluranes are more efficient inhibitors than inorganic ones as AS-101. (c) 2006 Elsevier B.V. All rights reserved.

THE CRYSTAL-STRUCTURE OF BENZOYL-HISTIDINE MONOHYDRATE

The crystal structure of benzoyl-histidine monohydrate (BYLH hereafter), C-13H-12N-3O-3. H2O was determined from three dimensional data of 3012 independent reflections measured on a Enraf-Nonius (CAD4) single crystal diffractometer. The compound crystallizes in the orthorhombic space group P2(1)2(1)2(1) with cell dimensions alpha = 7.102(1) angstrom, b = 13.783(3) angstrom, c = 14.160(4) angstrom, V = 1385.92 angstrom-3, F.W. = 277.28, F(000) = 584 Q(calc) = 1.32 g cm-3 and Z = 4.The structure was solved with direct methods. All positional and anisotropic thermal parameters were refined by full-matrix least-squares calculations. The final reliability factor was R = 0.040, while the weighted one was Rw = 0.034. The H atoms found in the difference Fourier map were refined isotropically.The compound consists of a histidine molecule bound to a benzoyl group. There is also a cocrystallized water molecule stabilized through a hydrogen bridge.The 5-membered ring of the histidine has its tautomeric form, after the transfer of the H atom from the N(delta) to the N(epsilon) atom of the ring. There is an sp2 conformation around C6 while the conformation around C3 is that of sp3. The histidine ring forms with the benzene ring a dihedral angle of 109.8(1)-degree.All angle values and bond distances agree very well with the expected values in the literature.