Structural elucidation of the Bi(2(n + 2))Mo(n)O(6(n + 1)) (n = 3, 4, 5 and 6) family of fluorite superstructures by transmission electron microscopy.

The cationic framework structure of a whole new family of compounds with the general formula Bi(2(n + 2))Mo(n)O(6(n + 1)) (n = 3, 4, 5 and 6) has been elucidated by transmission electron microscopy (TEM) methods. High-resolution transmission electron microscopy (HRTEM) has been used to postulate heavy-atom models based on the known structure of the n = 3 phase, Bi(10)Mo(3)O(24). These models were tested by HRTEM image simulation, electron diffraction and powder X-ray diffraction simulation methods which agreed with the experimental results. The four known phases of this family correspond to n = 3, 4, 5 and 6 members and all show fluorite superstructures. They consist of a common delta-Bi(2)O(3) fluorite-type framework, inside of which are distributed ribbons of {MoO(4)} tetrahedra which are infinite along b, one tetrahedron thick along c, and of variable widths of 3, 4, 5 or 6 {MoO(4)} tetrahedra along a depending on the family member (n value). These {MoO(4)} tetrahedra are isolated, i.e. without sharing any corner as in the [Bi(12)O(14)] columnar structural-type phase Bi[Bi(12)O(14)][MoO(4)](4)[VO(4)]. The structure of all these family members can be described as crystallographic shear derivatives from Aurivillius-type phases such as Bi(2)MoO(6), the n = infinity end member. All these compounds are good oxygen-ion conductors.

Relaxor behavior, polarization buildup, and switching in nanostructured 0.92 PbZn1/3Nb2/3O3-0.08 PbTiO3 ceramics.

The relaxor-type behavior, electrical polarization buildup, and switching in 0.92Pb(Zn(1/3)Nb(2/3))O(3)-0.08PbTiO(3) nanostructured ceramics with a grain size of approximately 20 nm is reported for the first time. This composition presents the highest-known piezoelectric coefficients, yet phase stability is an issue. Ceramics can only be obtained by the combination of mechanosynthesis and spark-plasma sintering. The results raise the possibility of using nanoscale, perovskite-relaxor-based morphotropic-phase-boundary materials for sensing and actuation in nanoelectromechanical systems.

Synthesis and antileishmanial activity of 6-mono-substituted and 3,6-di-substituted acridines obtained by acylation of proflavine.

Two new series of diaminoacridinic derivatives obtained from proflavine and N-(6-amino-3-acridinyl)acetamide were synthesised and assessed for their cytotoxic and antileishmanial activities. Two compounds, N-[6-(acetylamino)-3-acridinyl]acetamide and N-[6-(benzoylamino)-3-acridinyl]benzamide demonstrated highly specific antileishmanial properties against the intracellular amastigote form of the parasite. Structure-activity relationships established that the antiproliferative activity against human cells was greatly enhanced by the presence of a benzoylamino group in 6-mono-substituted acridines, while the presence of two acetylamino or benzoylamino groups in 3,6-di-substituted acridines strongly increased the specificity of the molecules for Leishmania parasite, suggesting that symmetric conformations could preferentially interfere with Leishmania metabolism.

Synthesis and antileishmanial activity of (1,3-benzothiazol-2-yl) amino-9-(10H)-acridinone derivatives.

(1,3-Benzothiazol-2-yl) amino-9-(10H)-acridinone derivatives were synthesized via a procedure based on the Ullman reaction and were assessed for their in vitro antileishmanial and anti-HIV activities. Two derivatives, 4-(6-nitro-benzothiazol-2-ylamino)-10H-acridin-9-one and 1-(6-amino-benzothiazol-2-ylamino)-10H-acridin-9-one, revealed a selective antileishmanial activity, mainly due to amastigote-specific toxicity. Results suggested that:the addition of a benzothiazole group on a parent amino-9-(10H)-acridinone ring could enhance antileishmanial abilities, the presence of a 6-amino-benzothiazole group on position 2 amino chain or a 6-nitro-benzothiazole group on position 4 amino chain was essential for specific anti-amastigote properties.

Tetrahydroacridin-9-ones, 9-chlorotetrahydroacridines, 9-amino-tetrahydroacridines and 9-(pyrazol-1-yl)-tetrahydroacridines derived from chiral cyclanones.

A series of tetrahydroacridines related to tacrine have been synthesized starting from 3-methylcyclohexananone, menthone, pulegone, carvone and dihydrocarvone (both racemic and chiral). In many cases, the yields and purity of the compounds have been improved by the use of a microwave oven. These compounds have been characterized by (1)H and (13)C NMR data. To establish their relative configuration, the structure of (1R,4R)-(+)-9-chloro-1-methyl-4-isopropyl-1,2,3,4-tetrahydroacridine (cis-10b), derived from (2S,5R)-(-)-menthone, has been determined by X-ray. The chemical shifts of cis-10b and trans-10b have been calculated at the GIAO/B3LYP/6-31G* level and compared successfully with the experimental data.

Characterization of ammonium chloride derivatives by salt clustering in electrospray mass spectrometry.

Clustering of ammonium chloride salts was studied using an electrospray source to characterize the form, mono- vs. dihydrochloride, of organic compounds by mass spectrometry. This new way of taking advantage of cluster formation is applied to aminomethylacridines as their storage requires the synthesis of such derivatives. Both positive and negative cluster mass spectra were obtained and allowed the determination of the nature of the hydrochloride forms as the salt mass is straightforwardly derived from the mass of the cluster monomer, calculated from singly and multiply charged ion distributions. The identity of the counterion is confirmed from the mass of the ionic moieties in the clusters.

A new aquahydroxidocopper(II) oxovanadium(IV) vanadate, Cu(H2O)(OH)VO(VO4).

Single crystals of the title compound have been prepared hydrothermally. Vanadate tetrahedra and distorted oxovanadium octahedra form layers, linked by two independent Cu atoms located on inversion centres. Each Cu atom is surrounded by six O atoms, forming an octahedron distorted by Jahn-Teller elongation. One of the two independent interlayer spaces bridged by the Cu atoms is significantly more compact than the other.

In vitro activities of 7-substituted 9-chloro and 9-amino-2-methoxyacridines and their bis- and tetra-acridine complexes against Leishmania infantum.

9-Chloro and 9-amino-2-methoxyacridines bearing different substituents in position 7, as well as their corresponding unsubstituted dimeric and tetrameric complexes, were investigated for in vitro antiproliferative properties against Leishmania infantum compared to toxicity towards human monocytes. The results clearly confirmed that several compounds of the 2-methoxyacridine series, together with their corresponding dimeric and tetrameric derivatives, had strong in vitro antiparasitic properties. Antileishmanial activity was shown to depend on the nature of both 7- and 9-substituted groups in monoacridines, while it varied according to the nature of the 9-substituted group and the length of the linker among bis- and tetra-acridines. The effects of acridine derivatives on DNA synthesis raised the hypothesis that DNA metabolism constituted their main target in Leishmania promastigotes; however, secondary effects on other biochemical pathways, including protein and lipid metabolism, were observed, suggesting that acridine compounds could be considered multitarget drugs.

CH3CN: X-ray structural investigation of a unique single crystal. beta --> alpha phase transition and crystal structure.

The phase transition from the low- (beta) to the high-temperature (alpha) form of acetonitrile, CH(3)CN, has been directly observed and studied on a unique single crystal. Both the beta and alpha structures have been determined at temperatures close to the transition temperature (206 K and 201 K), taking advantage of the hysteresis. A single crystal of the beta form was obtained for the first time.

A neodymium(III)-ammonium complex involving oxalate and carbonate ligands: (NH4)2[Nd2(C2O4)3(CO3)(H2O)].H2O.

The title compound, diammonium aqua-mu-carbonato-tri-mu-oxalato-dineodymium(III) hydrate, (NH(4))(2)[Nd(2)(CO(3))(C(2)O(4))(3)(H(2)O)].H(2)O, involving the two ligands oxalate and carbonate, has been prepared hydrothermally as single crystals. The Nd atoms form a tetranuclear unit across the inversion centre at (1/2, 1/2, 1/2). Starting from this tetranuclear unit, the oxalate ligands serve to develop a three-dimensional network. The carbonate group acts as a bis-chelating ligand to two Nd atoms, and is monodentate to a third Nd atom. The oxalate groups are all bis-chelating. The two independent Nd atoms are ninefold coordinated and the coordination polyhedron of these atoms is a distorted monocapped antiprism.

KVTeO5 and a redetermination of the Na homologue.

A single crystal of KVTeO(5), potassium vanadium tellurite, has been grown. The present structure determination has been conducted together with the refinement of the NaVTeO(5) homologue, sodium vanadium tellurite, for the sake of precise comparison. The network consists of [VTeO(5)](n) ribbons built up by VO(4) tetrahedra linking centrosymmetric Te(2)O(6) groups and stacked along the [010] direction; the alkali cations are intercalated in between. The Te(IV) atom exhibits a typical one-sided coordination number (CN) of 4, completed by a lone pair, which forms a distorted triangular bipyramid with the four O atoms.

In vitro activities of position 2 substitution-bearing 6-nitro- and 6-amino-benzothiazoles and their corresponding anthranilic acid derivatives against Leishmania infantum and Trichomonas vaginalis.

6-Nitro- and 6-amino-benzothiazoles bearing different chains in position 2 and their corresponding anthranilic acid derivatives were investigated for their in vitro antiparasitic properties against parasites of the species Leishmania infantum and Trichomonas vaginalis compared to their toxicity towards human monocytes. Biological investigations established that the antiprotozoal properties depended greatly on the chemical structure of the position 2 substitution-bearing group. Compound C1, 2-[(2-chloro-benzothiazol-6-yl) amino] benzoic acid, demonstrated an interesting antiproliferative activity towards parasites of the species T. vaginalis, while compound C11, 2-([2-[(2-hydroxyethyl) amino]-benzothiazol-6-yl] amino) benzoic acid, exhibited a promising activity against parasites of the species L. infantum in their intracellular amastigote form. Additional experiments established that compound C11, which was poorly toxic against the promastigote and the extracellular amastigote forms of the parasite, could improve host-protective mechanisms against Leishmania by preventing parasite internalization by macrophages and stimulating NO production, by means of a mechanism synergistically enhanced by the presence of gamma interferon.

AsCl(3): from the crystalline to the liquid state. XRD (176 < T (K) < 250) and WAXS (295 K) studies.

This paper presents structural studies on crystalline and liquid AsCl(3), performed using X-ray diffraction (XRD) and wide-angle X-ray scattering (WAXS) in the 176-250 K temperature range and at 295 K for the crystalline and liquid samples, respectively. The XRD results, collected using a single-crystal diffractometer, show that AsCl(3) crystallizes in the orthorhombic system with P2(1)2(1)2(1) space group and the unit cell parameters a = 9.475(3) A, b = 11.331(2) A, and c = 4.2964(8) A at 221 K. This structure is stable in the temperature range 176-243 K. Above the melting point, at 257 K, transition to the liquid state is observed. The WAXS data were recorded up to a maximum scattering vector K(max) = 16 A(-1) and then converted to real space by the sine Fourier transform, yielding to the reduced radial distribution function (RRDF). For a series of models, based on the crystalline AsCl(3) structure, the intensity and RRDF functions have been computed and compared with the experimental data. These simulations indicate that the model consisting of six AsCl(3) molecules, arranged along the y axis, accounts satisfactorily for the experimental observation. The results of the structure analysis in both crystalline and liquid states are discussed in relation to the influence of the As lone electron pair.

The mixed oxide MoVAlO7.

A single crystal of MoVAlO7, vanadium aluminium molybdate, has been grown. The present structure determination is more precise than a previous powder-pattern investigation [Knorr, Jacubus, Dabrowska & Kurzawa (1998). Eur. J. Solid State Inorg. Chem. 35, 519-530]. A three-dimensional [MoAlO6](3n-)n network surrounds infinite strings of [VO]3+ groups [V-O = 1.586 (4) A] lying in the mirror planes.