Synthesis and structure of bismuth(III)-containing noncentrosymmetric phosphates, Cs3KBi2M4(PO4)6Cl (M = Mn, Fe). Monoclinic (Cc) and tetragonal (P43) polymorphs templated by chlorine-centered Cl(Bi2Cs) acentric units.

Single crystals of three new noncentrosymmetric (NCS) phosphates, α (1) and β (2) forms of Cs(3)KBi(2)Mn(4)(PO(4))(6)Cl and α-Cs(3)KBi(2)Fe(4)(PO(4))(6)Cl (3), were grown in a reactive CsCl/KCl molten-salt media. Their structures were determined by single-crystal X-ray diffraction methods showing that the α form crystallizes in the space group Cc (No. 9), which is in one of the 10 NCS polar crystal classes, m (2/m) while the β form crystallizes in P4(3) (No.

Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine.

Synthesis, characterization, and preliminary studies of vanadium(IV) complexes with a Schiff base and thiosemicarbazones as mixed-ligands.

[VO(Sal--tryp)(HO)] (where sal--tryp = -salicylidene--tryptophanate) was used as a precursor to produce the novel complexes, [VO(Sal--tryp)(MeATSC)].1.5CHOH (where MeATSC = 9-Anthraldehyde-N(4)-methylthiosemicarbazone), [VO(Sal--tryp)(-Ethhymethohcarbthio)].

Symmetry preservation in a new noncentrosymmetric lattice comprised of acentric POM clusters residing in bowls of Cs(+)-based half SOD β-cage.

In light of ever growing interests in noncentrosymmetric materials, a fascinating reticular chemistry is illustrated via the structure of a new family of solids where the acentric symmetry of the well-known [V(4+)(14)As(3+)(8)O(42)Cl](5-) POM cluster is manifested through the network construction of counter cations featuring slabs of Cs(+)-based half SOD β-cages.

The diselanylbis(1,3-dimethyl-1H-imidazol-3-ium) dication stabilized by the polymeric catena-pentachloridotricuprate(I) anion.

In the title compound, catena-poly[diselanylbis(1,3-dimethyl-1H-imidazol-3-ium) [μ(3)-chlorido-tetra-μ(2)-chlorido-tricuprate(I)]], {(C(10)H(16)N(4)Se(2))[Cu(3)Cl(5)]}(n), the diselenide dication is stabilized by catena-[Cu(3)Cl(5)](2-) anions which associate through strong Cu-Cl bonds [average length = 2.3525 (13) Å] to form polymeric chains. The polymeric [Cu(3)Cl(5)](2-) anion contains crystallographically imposed twofold rotation symmetry, with distorted trigonal-planar and tetrahedral geometries around the two symmetry-independent Cu atoms.

Synthesis of internal fluorinated alkenes via facile aryloxylation of substituted phenols with aryl trifluorovinyl ethers.

Nucleophilic addition-elimination of ortho- or para-substituted phenols to aryl trifluorovinyl ethers (TFVEs) in N,N-dimethylformamide was studied. Using sodium hydride as a base afforded vinyl substitution products R-Ar-O-CF=CF-O-Ar-R', where R or R' = H, Br, OMe, tert-Bu, or Ph. The vinyl substitution products produced mixtures of (Z)/(E)-isomers and this isomer ratio was influenced by substitution with more sterically encumbered phenol nucleophiles.

Probing the antioxidant action of selenium and sulfur using Cu(I)-chalcogenone tris(pyrazolyl)methane and -borate complexes.

Hydroxyl radical generated from the reaction of Cu(+) with hydrogen peroxide results in oxidative DNA damage, and this damage is implicated in aging, cancer, and many other diseases. Selenium- and sulfur-containing compounds can act as antioxidants, and coordination of selenium and sulfur to copper is one explanation for this antioxidant activity. To determine how copper coordination results in antioxidant activity, biologically relevant tris(pyrazolyl)methane and borate Cu(+) complexes of the formulas Tp*Cu(L) and [Tpm(R)Cu(L)](+), where (L = N, N'-dimethylimidazole selone, dmise; N, N'-dimethylimidazole thione, dmit; Tp* = hydrotris(3,5-dimethylpyrazolyl)borate; Tpm(R) = tris(pyrazolyl)methane, R = H; Tpm, R = Me; Tpm*, R = iPr; Tpm(iPr)), have been synthesized and characterized.

In vitro biological studies and structural elucidation of fluoro-substituted phenyl acrylic acids.

Background: Synthesis, characterization, and biological significance of different substituted phenyl acrylic acids have been studied. These acids are contributing a key role during synthesis of antimicrobial drugs.

Method: The acids were prepared by condensation of various substituted phenyl acetic acids and aldehydes.

K(3)(Sc(0.875)Nb(0.125))Nb(2)O(9)H(1.75): a new scandium niobate with a unique cage structure.

Potassium scandium niobate hydroxide, K(3)(Sc(0.875)Nb(0.125))Nb(2)O(9)H(1.

Synthesis and characterization of N-(Arylcarbamothioyl)-cyclohexanecarboxamide derivatives: the crystal structure of N-(naphthalen-1-ylcarbamothioyl)cyclohexanecarboxamide.

A number of N-(arylcarbamothioyl)cyclohexanecarboxamide derivatives (aryl substituents: phenyl, 2-chlorophenyl, 3-chlorophenyl, 4-chlorophenyl, o-tolyl, p-tolyl, 3-methoxyphenyl, 4-methoxyphenyl and naphthalen-1yl) have been synthesized. The compounds obtained were characterized by elemental analyses, IR spectroscopy and (1)H-NMR spectroscopy. N-(naphthalen-1-ylcarbamothioyl)cyclohexanecarboxamide, H(2)L(9), was also characterized by a single crystal X-ray diffraction study.

Khayanolides from African mahogany Khaya senegalensis (Meliaceae): A revision.

Five khayanolides (1-O-acetylkhayanolide B 1, khayanolide B 2, khayanolide E 3, 1-O-deacetylkhayanolide E 4, 6-dehydroxylkhayanolide E 5) were isolated from the stem bark of African mahogany Khaya senegalensis (Meliaceae). Their structures and absolute configurations were determined through extensive spectroscopic analyses including MS, NMR, and single-crystal X-ray diffraction experiments. The results established that two previously reported khayanolides, 1alpha-acetoxy-2beta,3alpha,6,8alpha,14beta-pentahydroxy-[4.

1-(1H-Benzimidazol-1-ylmeth-yl)-3-[2-(di-isopropyl-amino)eth-yl]-1H-benzimid-azolium bromide 0.25-hydrate.

The title N-heterocyclic carbene derivative, C(23)H(30)N(5) (+)·Br(-)·0.25H(2)O, was synthesized using microwave heating and was characterized by (1)H and (13)C NMR spectroscopy and a single-crystal X-ray diffraction study. The structure of the title compound are stabilized by a network of intra- and inter-molecular C-H⋯Br hydrogen-bonding inter-actions.

Dichlorido[1-(2-methyl-benz-yl)-3-(η-2,4,6-trimethyl-benz-yl)-1H-2,3-dihydro-benzimidazol-2-yl-idene]ruthenium(II) dichloro-methane solvate.

The title complex, [RuCl(2)(C(25)H(26)N(2))]·CH(2)Cl(2), is best thought of as containing an octa-hedrally coordinated Ru center with the arene occupying three sites. Two Ru-Cl bonds and one Ru-carbene bond complete the distorted octa-hedron. The carbene portion of the ligand is a benzimidazole ring.

1,3-Bis(4-tert-butyl-benz-yl)-4,5-dihydro-imidazolium chloride monohydrate.

In the title compound, C(25)H(35)N(2) (+)·Cl(-)·H(2)O, the imidazolidine ring adopts a twisted conformation, with a pseudo-twofold axis passing through the N-C-N carbon and the opposite C-C bond. The N-C-N fragment of the imidazolidine ring shows some degree of both double- and single-bond character due to partial electron delocalization. One of the tert-butyl groups is disordered over two conformations with occupancies of 0.

1,3-Bis(2-thienylmeth-yl)-4,5-dihydro-imidazolium trichlorido(η-p-cymene)ruthenate(II).

The asymmetric unit of the title compound, (C(13)H(15)N(2)S(2))[RuCl(3)(C(10)H(14))], contains a 1,3-(2-thienylmeth-yl)-4,5-dihydro-imidazolium cation and a trichlorido(η(6)-p-cymene)ruthenate(II) anion. The thio-phene rings of the cation are disordered by an 180° rotation about the thio-phene-CH(2) bonds with occupancies of 0.847 (5)/0.

The molecular structure and vibrational spectra of N-(2,2-diphenylacetyl)-N'-(naphthalen-1yl)-thiourea by Hartree-Fock and density functional methods.

N-(2,2-Diphenylacetyl)-N'-(naphthalen-1yl)-thiourea (PANT) has been synthesized and characterized by elemental analysis, IR spectroscopy and (1)H NMR spectroscopy. The crystal and molecular structure of the title compound has been determined from single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1, Z=2 with a=10.

Fluoroalkylation of imidazoles by hypervalent iodonium salts.

N-1H,1H-perfluoroalkylation and regioselective C-perfluoroalkylation of imidazoles were obtained using the corresponding hypervalent iodonium salts.

1-(4-tert-Butyl-benz-yl)-3-(3,4,5-tri-methoxy-benz-yl)benzimidazolium bromide monohydrate.

A novel N-heterocyclic carbene derivative, C(28)H(33)N(2)O(3) (+)·Br(-)·H(2)O, was synthesized and characterized by elemental analysis, (1)H and (13)C-NMR and IR spectroscopy and a single-crystal X-ray diffraction study. Ions of the title compound are linked by π⋯π stacking inter-actions (face-face separation 3.441 Å) and C-H⋯Br and O-H⋯Br inter-actions.

1-(2-Phenyl-benz-yl)-3-(2,4,6-trimethyl-benz-yl)imidazolidinium bromide.

In the title salt, C(26)H(29)N(2) (+)·Br(-), which may serve as a precursor for N-heterocyclic carbenes, the imidazolidine ring adopts a twist conformation with a pseudo-twofold axis passing through the N-C-N carbon and the opposite C-C bond. The N-C-N bond angle [113.0 (4)°] and C-N bond lengths [1.

1,3-Bis[4-(dimethyl-amino)benz-yl]-4,5,6,7-tetra-hydro-1H-1,3-diazepan-2-ium chloride.

The title N-heterocyclic carbene derivative, C(23)H(33)N(4) (+)·Cl(-), has been synthesized and characterized by elemental analysis, (1)H and (13)C NMR, IR spectroscopy and a single-crystal X-ray diffraction study. Ions of the title compound are linked by three C-H⋯Cl inter-actions. The seven-membered 1,3-diazepane ring has a form inter-mediate between twist-chair and twist-boat.

Bromido[1-(η-4-tert-butyl-benz-yl)-3-(2,4,6-trimethyl-benz-yl)benzimidazol-2-yl-idene]chloridoruthenium(II).

A new ruthenium complex, [RuBrCl(C(28)H(32)N(2))], has been synthesized and characterized by elemental analysis, (1)H NMR, (13)C NMR, IR-spectroscopy and a single-crystal X-ray diffraction study. The Ru atom in this complex is best described as having a considerably distorted octa-hedral coordination environment with the arene occupying three coordination sites. Two further coordination sites are occupied by chloride and bromide ligands, while the sixth site is occupied by the carbene.

1,3-Bis(thio-phen-2-ylmeth-yl)-3,4,5,6-tetra-hydro-pyrimidinium trichlorido(η-p-cymene)ruthenate(II).

The asymmetric unit of the title compound, (C(14)H(17)N(2)S(2))[Ru(C(10)H(14))Cl(3)], contains a 1,3-bis-(thio-phen-2-ylmeth-yl)-3,4,5,6-tetra-hydro-pyrimidinium cation and a trichlorido(η(6)-p-cymene)ruthenate(II) anion. The Ru atom exhibits a distorted octa-hedral coordination with the benzene ring of the p-cymene ligand formally occupying three sites and three chloride atoms occupying the other three sites. The N-C bond lengths of the N-C-N unit of the pyrimidinium cation are shorter than the average single C-N bond length of 1.

A two-dimensional organic-inorganic hybrid compound, poly[(ethylenediamine)tri-μ-oxido-oxidocopper(II)molybdenum(VI)].

A new organic-inorganic two-dimensional hybrid compound, [CuMoO(4)(C(2)H(8)N(2))], has been hydro-thermally synthesized at 443 K. The unit cell contains layers composed of CuN(2)O(4) octa-hedra and MoO(4) tetra-hedra. Corner-sharing MoO(4) and CuN(2)O(4) polyhedra form CuMoO(4) bimetallic sites that are joined together through O atoms, forming an edge-sharing Cu(2)Mo(2)O(4) chain along the c axis.

Tetra-μ-aqua-octaaqua-bis(μ-4-chloro-pyridine-2,6-dicarboxyl-ato)bis-(4-chloro-pyridine-2,6-dicarboxyl-ato)tri-cobalt(II)disodium(I) bis-[triaqua-bis(4-chloro-pyridine-2,6-dicarboxyl-ato)cobalt(II)] hexa-hydrate.

The title compound, [Co(3)Na(2)(C(7)H(2)ClNO(4))(4)(H(2)O)(12)][Co(C(7)H(2)ClNO(4))(H(2)O)(3)](2)·6H(2)O, consists of a centrosymmetric dimer of [Co(II)(dipicCl)(2)](2-) complex dianions [dipicCl is 4-chloro-pyridine-2,6-dicarboxyl-ate] bridged by an [Na(2)Co(II)(H(2)O)(12)](4+) tetra-cationic cluster, two independent [Co(dipicCl)(H(2)O)(3)] complexes, and six water mol-ecules of crystallization. The metals are all six-coordinate with distorted octahedral geometries. The [Co(II)(dipicCl)(H(2)O)(3)] complexes are neutral, with one tridentate ligand and three water molecules.

Synthesis and cytotoxicity of epoxide and pyrazole analogs of the combretastatins.

Twenty-six epoxide and corresponding pyrazole derivatives, of the structurally related chalcones and combretastatin A-4 (CA-4), were synthesized and tested for in vitro cytotoxicity. These molecules were synthesized by epoxidation of the relevant chalcones, followed by reaction with hydrazine. The structures of epoxides 3 and 7, and pyrazole 17, were confirmed by X-ray diffraction studies.