bluuebunny/crossref_metadata_2025 huggingface dataset:
Review. Synthesis of Inorganic-Organic Hybrid Thiometallate Materials with a Special Focus on Thioantimonates and Thiostannates and in situ X-Ray Scattering Studies of their Formation
Authors: Seidlhofer Beatrix , Pienack Nicole , Bensch Wolfgang
Published: February 2015

A rich variety of inorganic-organic hybrid thioantimonates and thiostannates were prepared during the last few years under solvothermal conditions applying organic amine molecules or transition metal complexes as structure directors. In this review synthetic approaches to and structural features of these thiometallates are discussed. For thioantimonates(III) the structures range from well isolated thioanions to three-dimensional networks, whereas the structural chemistry of thiostannates(IV) is strongly dominated by the [Sn2S6]4− anion, and no three-dimensional thiostannate has been reported so far. In the structures of thioantimonates(III) several primary building units like the [SbS3] trigonal pyramid, the [SbS4] unit or even the [SbS5] moiety are joined by vertex- and/or edge-linkages to form building blocks of higher structural hierarchy like [Sb3S4] semi-cubes or SbxSx heterocycles. A pronounced difference between thioantimonate and thiostannate chemistry is the tendency of Sb(III) to enhance the coordination geometry via so-called secondary bonds. In most cases the environment of Sb(III) is better described as a 3+n polyhedron with n = 1 - 3. The thioantimonate(V) structural chemistry is less rich than that of thioantimonates(III), and the [SbS4]3− anion shows no tendency for further condensation. By applying suitable multidentate amine molecules, transition metal cations which normally prefer bonding to the N atoms of the amines can be incorporated into the thiometallate frameworks
Review. Solvothermal Synthesis of Multifunctional Coordination Polymers
Authors: Zhao Yonggang , Li Kunhao , Li Jing
Published: February 2015

This review focuses primarily on the past 10 years of our development of multifunctional coordination polymers with 1D, 2D and 3D structures employing low-temperature and cost-effective hydrothermal and solvothermal methods. The effects of the experimental conditions and parameters on the crystal formation and phase separation, including temperature and pressure, reaction pH, solvent and composition, are discussed. Our studies have shown that a variety of different types of network structures may be rationally designed and synthesized by deliberate selection and construction of metal building blocks and organic ligands, which lead to numerous interesting properties and multifunctionality that are promising for applications in gas storage and separation, catalysis and optical sensing
Review. New Trends in Solvothermal Crystal Growth at theMacro- and Nanoscale
Authors: Demazeau Gérard , Largeteau Alain , Darracq Stéphane
Published: February 2015

Solvothermal processes, as compared to hydrothermal processes, enlarge the scope of the employed solvents from aqueous to non-aqueous media, the objective being to extend the possibilities for the preparation and/or the crystal growth of non-oxide materials. During the last fifteen years solvothermal crystal growth of materials has been investigated at two different levels: (i) the macroscopic scale, with the preparation of large single crystals of functional materials for specific applications, (ii) the nanoscale, involving the elaboration of single-crystalline nanocrystallites well defined in size and morphology, and particularly adapted to nanodevices. In the first domain, two main factors have been studied: (i) the influence of the thermodynamical parameters governing the solvothermal processes, and (ii) the purity of the components (nutrient, solvent, etc.), the main objective being to reduce drastically the density of defects inside the single crystals. In the second domain, strong efforts have been made: (i) to control the nano-size, but mainly, (ii) to induce specific morphologies, in particular 1D, appropriate to the relative nanotechnologies
Hybridisation of Sebacic Acid on the Surface of γ-Alumina Nanoparticles in Sub- and Supercritical Water
Authors: Singh Varu , Takami Seiichi , Minami Kimitaka , Hojo Daisuke , Adschiri Tadafumi
Published: February 2015

The surface modification of γ -alumina nanoparticles by sebacic acid in super- and subcritical water was investigated. The modified alumina was characterised by Fourier-transform infrared spectra, X-ray diffraction patterns, transmission electron microscopy images, and thermogravimetric studies. The alumina nanoparticles were found to remain stable, and sebacic acid was bound to their surfaces at 200 ℃, but their crystallite structure was partially changed to that of boehmite above 200 ℃. Under supercritical conditions at 400 ℃, the alumina nanoparticles were totally changed to boehmite nanoparticles. The surface adsorption of sebacic acid is attributed to reactions between the surface -OH groups of alumina and the -COOH groups of sebacic acid. The modified alumina nanoparticles have -COOH groups on their surface, enabling hybridisation with various biomolecules, and thus allowing their application in several areas
Solvothermal Synthesis of Gallium and Indium Nitrides Using Lithium Amide
Authors: Chirico Pietro , Hector Andrew L.
Published: February 2015

Results of the investigation of the reactions of GaCl3, InCl3 and InI3 with LiNH2 under solvothermal conditions in benzene, which lead to metal nitrides, are reported. GaN is obtained as a cubic phase or as a mixture of cubic and hexagonal phases, depending on temperature. The effect of the addition of surfactants on the formation of GaN was explored. InN products were always contaminated with indium metal, even at low reaction temperatures. The addition of excess LiNH2 or the use of InI3 instead of InCl3 gave products with less In metal
Molybdenum-Boron Bonds in the Crystal – Structural Characterization of K[(η5-C5H5)Mo(CO)3] and[(η5-C5H5) (OC)3Mo-{B(NMe2)-B(NMe2)Br}]
Authors: Braunschweig Holger , Radacki Krzysztof , Kraft Katharina , Stellwag Sascha
Published: February 2015

Structural characterization of the solvent-free ionic complex K[(η5-C5H5)Mo(CO)3] and the molybdenum boryl complex [(η5-C5H5)(OC)3Mo-{B(NMe2)-B(NMe2)Br}] is reported.
Gold Nanoparticles Bearing an α-Lipoic Acid-based Ligand Shell: Synthesis, Model Complexes and Studies Concerning Phosphorescent Platinum(II)-Functionalisation
Authors: Siemeling Ulrich , Bretthauer Frauke , Bruhn Clemens , Fellinger Tim-Patrick , Tong Wah-Leung , Chan Michael C.W.
Published: February 2015

The surface functionalisation of gold nanoparticles (GNPs) with luminescent platinum complexes has been investigated, utilising α-lipoic acid derivatives for GNP stabilisation. Model complexes have been studied to mimic the chemisorption chemistry required to afford GNPs protected by an α-lipoic acid-based ligand shell with terminal functionalisation suitable for metal coordination, and the unambiguous binding of the cyclic disulfide moiety at a zero-valent precious metal core through oxidative addition has been confirmed by X-ray crystallography. Subsequently, gold nanoparticles bearing the α-lipoic acid-based ligand shell have been prepared and characterised, and a synthetic methodology for the immobilisation of PtII luminophores onto their surface has been established.
Seven-coordinate Manganese(II) Complex Formed with the Tripodal Tetradentate Ligand Tris(N-methylbenzimidazol-2-ylmethyl)amine
Authors: Wu Huilu , Yuan Jingkun , Qi Baoliang , Kong Jin , Kou Fan , Jiaa Fei , Fan Xuyang , Wang Yaoyu
Published: February 2015

A seven-coordinate manganese(II) complex with the tripodal tetradentate ligand tris(N-methylbenzimidazol- 2-ylmethyl)amine (Mentb), with composition [Mn(Mentb)(α-methacrylate)(DMF)]- (ClO4) · (DMF), was synthesized and characterized by elemental analysis, electrical conductivity, and IR and UV/Vis spectral measurements. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The MnII cation is bonded to a Mentb ligand, an α-methacrylate ligand and a DMF molecule through four N atoms and three O atoms, resulting in a seven-coordinate geometry. Cyclovoltammograms of the complex indicate a quasireversible Mn3+/Mn2+ couple. The X-band EPR spectrum of the complex exhibits a six-line manganese hyperfine pattern with g = 2, A = 91, and confirms that the material is high-spin Mn(II).
Morphology and Structure of Biomorphous Silica Isolated from Equisetum hyemale and Equisetum telmateia
Authors: Neumann Mike , Wagner Sandra , Noske Robert , Tiersch Brigitte , Strauch Peter
Published: February 2015

The family of horsetails (Equisetaceae) is characterized through their high content of silica (SiO2), which is the highest in known vascular plants. This work has focussed on two species of this family, Equisetum hyemale and Equisetum telmateia, where the biomorphous silica is deposited basically as amorphous SiO2 in the outer epidermis of the plants. As source of SiO2, the original plant material was air-dried and carved or powdered. For the isolation process the biomaterial was pre-treated with aceotropic HCl. This pre-treatment has the advantage of the extraction of high amounts of the natural inorganic matrix. In a second step the organic matrix was removed by a thermal oxidative process in the temperature range of 275 - 1200 ◦C to isolate the biogenic silicon dioxide from the perennial plant. Parameters of time, temperature and the thermal gradient were varied to optimize the process and to get products with the highest possible surface area. Furthermore, the particle morphology of the biogenic SiO2 from leaves and stems was examined separately. The silica deposits were characterized by optical microscopy, scanning electron microscopy, infrared spectroscopy, gravimetry, nitrogen sorption analysis, and sedimentation analysis.
Die rotationsfehlgeordnete Kristallstruktur von Tropyliumbromid C7H7
+Br– / The Rotationally Disordered Crystal Structure of Tropylium Bromide C7H7
+Br−
Authors: Hoffmann Florian , Fester Gerrit W. , Wagler Jörg
Published: February 2015

The crystal structure of tropylium bromide, C7H7
+Br−, was solved and refined in space group type R¯3m with rotationally disordered C7 rings. Restraints of identical 1,2- and 1,7-C-C bond lengths as well as identical 1,3- and 1,6-C-C separations within a flat C7H7 moiety were applied. The refinement converged to a regular C7 heptagon with C-C bond lengths of 139.1(1) pm. C7H7
+Br− reacts with Mo(CO)3(CH3CN)3 to form C7H7Mo(CO)2Br.
Cyclic Oxalylation of Primary N-Substituted Anthranilamides: 1H-Benzo[e][1,4]diazepine-2,3,5(4H)-triones and 11a-Chlorobenzo[ e]oxazolo[3,2-a][1,4]diazepine-2,3,5,11(10H,11aH)-tetraones
Authors: Köllner Maria Anna , Geffken Detlef
Published: February 2015

In dependence on the molar ratio, the reaction of primary anthranilamides 3 with oxalyl chloride produced 1H-benzo[e][1,4]diazepine-2,3,5(4H)-triones 4 or 10-substituted 11a-chloro-benzo[e]- oxazolo[3,2-a][1,4]diazepine-2,3,5,11(10H, 11aH)-tetraones 5, the structures of which were unambiguously proven by X-ray diffraction analysis.
Synthesis and Crystal Structure of the Praseodymium Orthoborate λ -PrBO3
Authors: Haberer Almut , Kaindl Reinhard , Huppertz Hubert
Published: February 2015

The praseodymium orthoborate λ -PrBO3 was synthesized from Pr6O11, B2O3, and PrF3 under high-pressure / high-temperature conditions of 3 GPa and 800 °C in a Walker-type multianvil apparatus. The crystal structure was determined on the basis of single-crystal X-ray diffraction data, collected at room temperature. The title compound crystallizes in the orthorhombic aragonite-type structure, space group Pnma, with the lattice parameters a = 577.1(2), b = 506.7(2), c = 813.3(2) pm, and V = 0.2378(2) nm3, with R1 = 0.0400 and wR2 = 0.0495 (all data). Within the trigonal-planar BO3 groups, the average B-O distance is 137.2 pm. The praseodymium atoms are ninefold coordinated by oxygen atoms.
Two Supramolecular Architectures Containing Dinuclear Thiostannate [Sn2S6] Units
Authors: Zhou Jian , Liu Xing , Chen Guang-Quan , Zhang Feng , Li Li-Rong
Published: February 2015

Two thiostannates [Co(dien)2](H2dien)Sn2S6 (1) (dien = diethylenetriamine) and [Zn(tren)]2Sn2S6 (2) (tren = tris(2-aminoethyl)amine) were prepared under solvothermal conditions and structurally characterized. Both 1 and 2 contain dinuclear [Sn2S6]4− anions built from two SnS4 tetrahedra sharing a common edge. 1 consists of discrete [Sn2S6]4− anions with rare u-fac-[Co(dien)2]2+ and H2dien2+ as counterions, while 2 consists of neutral centrosymmetric [Zn(tren)]2Sn2S6, in which the [Sn2S6]4− anion connects two coordinatively unsaturated complex [Zn(tren)]2+ cations as a bidentate ligand via trans terminal S atoms. The different cations act as structure-directing agents that have a significant influence on the arrangement of the [Sn2S6]4− anions in their crystal structures. 2 exhibits fluorescence properties at room temperature.
Synthesis, High-resolution Crystal Structure Refinement and Magnetic Properties of the Manganese-rich Cementite-type Mn1.8Fe1.2C
Authors: Stork Ludwig , Müller Paul , Speldrich Manfred , Kögerler Paul , Appen Jörg von , Dronskowski Richard
Published: February 2015

The manganese-rich ternary cementite phase Mn1.8Fe1.2C has been synthesized by a ceramic route in an almost quantitative yield, and the crystal structure refinement on the basis of high-resolution X-ray powder diffraction data using MoKα1 radiation has been performed. The carbon atom is found in a slightly distorted trigonal prism composed of Mn and Fe atoms, with a rather narrow bond length range from 1.95 to 2.09 Å . The magnetic susceptibility data clearly indicate long-range ordering phenomena, in particular dominant antiferromagnetic interactions, as predicted by density-functional theory.
Syntheses and Structures of [nBu4N][nBu2SbCl4] and [Et3SbMe]2[(MeSbCl3)2]
Authors: Breunig Hans Joachim , Koehne Tim , Lork Enno , Moldovan Ovidiu , Poveleit Jörn , Raţ Ciprian Ionuţ
Published: February 2015

[nBu4N][nBu2SbCl4] (1) is synthesized by reaction of nBu4NCl and nBu2SbCl3. [Et3SbMe]2- [(MeSbCl3)2] (2) is formed from [Et3SbMe]I and Me2SbCl3. The structures of 1 and 2 were determined by single-crystal X-ray diffractommetry.
Study on Chemical Constituents and Cytotoxic Activities of Salacia chinensis Growing in Vietnam
Authors: Minh Tran Thi , Hoang Anh Nguyen Thi , Thang Vu Dao , Van Sung Tran
Published: February 2015

Two new triterpenoids, named 7α,21α-dihydroxyfriedelane-3-one (1) and 7α,29-dihydroxyfriedelane- 3-one (2) have been isolated from the ethyl acetate extract of the stems of Salacia chinensis besides the known triterpenoid 21α,30-dihydroxyfriedelane-3-one (3). The structures of the isolated compounds were elucidated on the basis of spectral analysis. Eight triterpenoids from this plant have been tested against the four cancer cell lines Hep-G2, LU, KB, and MCF-7. The new compound 1 showed good activity against all four tested cell lines.
Crystal Structure of La3OBr[AsO3]2
Authors: Yahia Hamdi Ben , Pöttgen Rainer , Rodewald Ute Ch.
Published: February 2015

Colorless needles of the arsenite bromide La3OBr[AsO3]2 were synthesized from ammonium dihydrogen arsenate, ammonium bromide and lanthanum oxide in an NaBr/KBr flux at 900 °C. La3OBr[AsO3]2 crystallizes with the centrosymmetric tetragonal La3OCl[AsO3]2 type, space group P42/mnm. The structure was refined from single-crystal diffractometer data: a = 13.0431(15), c = 5.6127(7) Å , wR2 = 0.0454, 945 F2 values, and 39 variables. It consists of chains of trans-edge-sharing OLa4/2 tetrahedra which are coordinated by [AsO3]3− units via the oxygen atoms
Metal Benzenesulfonates/Acetic Acid Mixtures as Novel Catalytic Systems: Application to the Protection of a Hydroxyl Group
Authors: Wang Min , Gao Jingjing , Song Zhiguo
Published: February 2015

A surprising synergistic effect has been discovered in mixtures of metal benzenesulfonates (Co, Al, Ni, Zn, Cd, Pr, La, Cu, Mn) and acetic acid, leading to active catalytic systems for the tetrahydropyranylation of alcohols and phenols to produce tetrahydropyranyl ethers. All reactions proceed mildly and efficiently with moderate to high yields at room temperature without solvent. After the reaction, the metal benzenesulfonate can be easily recovered and reused many times. The efficiency of these systems might result from the “double activation” by Brønsted and Lewis acid catalysis.
Synthesis of Some Fused Triazole Derivatives Containing 4-Isobutylphenylethyl and 4-Methylthiophenyl Moieties
Authors: Kumsi Manjunatha , Poojary Boja , Lobo Prajwal L. , Fernandes Jennifer , Chikkanna Chandrashekhar
Published: February 2015

A series of substituted [1,3]thiazolo[3,2-b][1,2,4]triazole derivatives 4 were synthesized in good yield by condensing 2-substituted-1,2,4-triazole-5-thiols 3 with various N-aryl-maleimides in acetic acid media. All structures of the newly synthesized compounds were elucidated by elemental analyses and spectral data.
Synthesis, in vitro Antiproliferative and Anti-HIV Activity of New Derivatives of 2-Piperazino-1,3-benzo[d]thiazoles
Authors: Al-Soud Yaseen A. , Al-Sa’doni Haitham H. , Saber Sadeekah O. W. , Al-Shaneek Reem H. M. , Al-Masoudi Najim A. , La Colla P.
Published: February 2015

A series of N-{2-oxo-2-[4-(1,3-benzothiazol-2-yl)piperazin-1-yl]}-(het)arenecarboxamides 4a - l, sulfonamide derivatives 8a - i as well as benzothiazole-containing N1-(2-oxoethyl)-N1-arylthioureas 9a - c have been synthesized. Compounds 4a - l and 9a were evaluated, in vitro, for their antiproliferative activity against a large panel of human tumor-derived cell lines. Compounds 4l and 9a were the most potent analogs in this series, showing remarkable effects on human splenic B-lymphoblastoid cells (WIL-2NS) and human acute B-lymphoblastic leukemia (CCRF-SB) cell lines (4l: CC50 = 5.1 and 7.3 μM, respectively), and compound 5 against CCRF-SB cell lines with CC50 = 2.3 μM. These compounds are leading candidates for further development. Compounds 6 - 7a - i were screened as inhibitors against HIV-1 and HIV-2, and no activity has been witnessed.
Ziziphorins A and B. New Flavonoids from Ziziphora tenuior
Authors: Mehmood Rashad , Imran Muhammmad , Malik Abdul , Tareen Rasool Bakhsh
Published: February 2015

Ziziphorins A (1) and B (2), new flavonoids, have been isolated from the chloroform-soluble fraction of Ziziphora tenuior along with 1-hentetracontanol, β -sitosterol-3-O-β -D-glucoside, ursolic acid, oleanolic acid, and apigenin. Their structures were assigned from spectral studies including 1D and 2D NMR spectroscopic data
Two New Phytoecdysteroids from the Needles of Taxus canadensis
Authors: Fang Yu , Ni Zhi-Yu , Yamada Teiko , Wang Yu-Fang , Zhang Man-Li , Dong Mei , Cong Bin , Sauriol Françoise , Huo Chang-Hong , Shi Qing-Wen , Kiyota Hiromasa
Published: February 2015

Two new phytoecdysteroids with a 20,22-acetal group were identified for the first time from the needles of the Canadian yew, Taxus canadensis. Their structures were characterized as ponasterone A 20,22-p-hydroxybenzylidene acetal (1) and ponasterone A 20,22-acetonide (2) on the basis of 1D, 2D NMR evidence and high-resolution FABMS analysis
Crystal Structures of New Alkali Metal-rich Oxometallates: Rubidium Aluminate Tetrahydroxide, Rb9(AlO4)(OH)4, Rubidium Orthogallate, Rb5GaO4, Cesiumbis-Chromate(IV) Oxide, Cs10(CrO4)2O, and Cesium Diindate, Cs8In2O7
Authors: Bender Johannes , Wohlfarth Andreas , Hoch Constantin
Published: February 2015

Several new alkali metal oxometallates with anions built up from tetrahedral [MO4] units were obtained in reactions aimed at the formation of alkali metal suboxometallates or by thermally decomposing the latter. Rubidium orthoaluminate tetrahydroxide Rb9(AlO4)(OH)4 crystallizes with a new structure type (space group P21/c, a = 13.116(1), b = 6.9266(5), c = 18.934(2) A , β = 92.05(1)°, V = 1719.0(3) Å3, Z = 4, R1 = 0.0352) and contains orthoaluminate anions [AlO4]5− and isolated hydroxide anions. Rubidium orthogallate Rb5GaO4 crystallizes with the Na5GaO4 structure type (space group Pbca, a = 6.9318(5), b = 21.309(2), c = 11.740(1) Å, V = 1734.2(3) Å3, Z = 8, R1 = 0.0423) with isolated orthogallate anions [GaO4]5−. Cesium chromate oxide Cs10(CrO4)2O adopts the Cs10(GeO4)2O structure type (space group P21/c, a = 12.903(1), b = 11.4523(8), c = 19.074(3) Å , β = 127.903(8)°,V = 2223.9(4) Å3, Z = 4, R1 = 0.0326) with orthochromate(IV) anions [CrO4]4− and isolated oxide anions. In all orthometallates the anions [MO4]n− deviate only slightly from ideal tetrahedral symmetry. Cesium diindate Cs8In2O7 crystallizes with the Cs8Fe2O7 structure type (space group P21/c, a = 7.4307(6), b = 18.6181(14), c = 7.2639(6) Å , β = 119.225(8)°, V = 877.0(1) Å3, Z = 2, R1 = 0.0349). A single-crystal structure investigation at r. t. has shown linear diindate units, but the temperature dependence of the libration angles from TLS studies for the bridging oxygen atom suggests a slightly bent and dynamically disordered diindate anion.
Mechanothermal Solid-state Synthesis of Cobalt(II) Ferrite and Determination of its Heat Capacity by MTDSC
Authors: Berbenni Vittorio , Milanese Chiara , Bruni Giovanna , Girella Alessandro , Marini Amedeo
Published: February 2015

Cobalt ferrite (CoFe2O4) has been synthesized by a solid-state mechanothermal process, and its molar heat capacity has been determined. A stoichiometric mixture of CoC2O4 ・ 2H2O and FeC2O4 ・ 2H2O was subjected to a combination of mechanical activation (by high-energy milling) and thermal activation (by annealing at temperatures between 300 and 700 °C). The process was followed by thermogravimetric analysis and high-temperature X-ray powder diffraction. It has been shown that CoFe2O4 forms at all temperatures, though with different degrees of crystallization, while Co3O4 and Fe2O3 are the only products formed when starting from unmilled mixtures. The molar heat capacity of CoFe2O4 has been determined in the temperature range 60 - 400 °C by MTDSC. It has been shown that the molar CP values of CoFe2O4 samples produced at T ≥ 500 °C are close to each other while those of the samples produced at 300 and 400 °C are lower. Furthermore the CoFe2O4 samples prepared at T ≥ 500 °C show very similar microstructures.
A Novel Keggin Tungstocobaltate Framework Supported by Copperbipyridyl Complexes: [Cu(I)(2,2' -bipy)2]{[Cu(II)(2,2' -bipy)2]2[HCoW12O40]} · 4H2O
Authors: Sha Jingquan , Xin Li , Zhou Baibin , Yu Decheng , Qu Youle , Li Shuxian , Liu Fenghua
Published: February 2015

A new organic-inorganic hybrid compound based on Keggin tungstocobaltate units supported by copper complexes, [Cu(I)(2,2’-bipy)2]{[Cu(II)(2,2’-bipy)2]2[HCoW12O40]} ・ 4H2O (bipy = bipyridine), has been synthesized under hydrothermal conditions and characterized by elemental, IR, TG, and XPS analyses and X-ray single-crystal structure determination. The crystal structure is built up from bi-supported Keggin tungstocobaltate polyoxoanions {[Cu(II)(2,2’-bipy)2]2[HCoW12O40]}−, [Cu(I)(2,2’-bipy)2]+ cations and water molecules. The title compound possesses a 1D tangled helical structure composed of {[Cu(II)(2,2’-bipy)2]2[HCoW12O40]}− polyoxoanions via π・ ・ ・π interactions along the c axis. The electrochemical behavior of the title compound was studied.
Anthracenylporphyrins
Authors: Davis Mia , Senge Mathias O. , Locos Oliver B.
Published: February 2015

We report the synthesis and characterization of meso-anthracenylporphyrins with zinc and nickel metal centers. A variety of novel aryl and alkyl meso-substituted anthracenylporphyrins were synthesized via step-wise Suzuki cross-coupling reactions using anthracenyl boronates. This method was compared to standard syntheses based on condensation reactions to yield anthracenylporphyrins of the A2B2- and A3B-type. The work was complemented by the synthesis of a number of the functionalized anthracene derivatives via Suzuki couplings. Selected systems were subjected to single-crystal X-ray analysis which revealed an unusual close packing for nickel(II) anthracenylporphyrins.
Synthesis, Characterization and Biological Studies of Some Bioactive Thiazolotriazole Derivatives
Authors: Kumsi Manjunatha , Poojary Boja , Lobo Prajwal Lourdes , Kumari Nalilu Suchetha , Chullikana Anoop
Published: February 2015

The key precursor rac-2-(4-isobutylphenyl)ethyl-1,2,4-triazole-5-thione (3) was synthesized in good yield from Ibuprofen (1). One-pot three-component reactions of 3 with 5-aryl-furan-2-carboxaldehydes/ substituted aromatic aldehydes and monochloroacetic acid in acetic acid in the presence of acetic anhydride and anhydrous sodium acetate afforded substituted thiazolo[3,2-b][1,2,4]triazole derivatives 4 and 5. The structures of the newly synthesized compounds were elucidated by elemental analyses and spectral data. The compounds were tested for their in-vitro antimicrobial activities.
Single-crystal Structure and Solid-state NMR of Ga2–xScxO3 (x = 0.83)
Authors: Yahia Hamdi Ben , Wüllen Leo van , Balamurugan Sarkarainadar , Rodewald Ute Ch. , Eckert Hellmut , Pöttgen Rainer
Published: February 2015

Colorless needles of Ga2−xScxO3 (x = 0.83) were isolated during the crystal growth of La3Ga3Sc2O12 in a K2WO4 flux. The structure was refined from X-ray single-crystal data: β -Ga2O3 type,C2/m, Z = 4, a = 12.716(4), b = 3.1566(6), c = 5.928(5) Å , β = 102.57(3)◦,V = 232.2 Å3, wR2 = 0.0618, 429 F2 values, 32 variables. The structure is based on infinite double chains of edge-sharing Sc/GaO6 octahedra running along the b axis. The GaO4 tetrahedra connect these chains by sharing corners and form a three-dimensional framework. The oxygen atoms form a distorted ccp pattern. The 45Sc NMR spectra confirm the presence of a single scandium site, while 71Ga NMR data clearly prove the partial occupancy of the scandium site by gallium atoms. The nuclear electric quadrupolar parameters of 45Sc and 71Ga are discussed in relation to the crystallographic atomic environments
Crystal Structure and NQR Studies of Compounds (RH)[ZnBr3(R)], (RH)2[ZnBr4] and [ZnBr2(R)2] (R = Py, n-MePy: n = 2, 3, 4); on the Dominant Stability of the Monoanionic Complexes over the Dianionic and Neutral Species
Authors: Ishihara Hideta , Nakashima Michio , Nakashima Hisayo , Tateno Ryuichi , Shibamura Yuki , Makino Toshio , Kikuchi Aika , Kii Daisuke , Horiuchi Keizo , Svoboda Ingrid , Fuess Hartmut , Terao Hiromitsu
Published: February 2015

The monoanionic complexes (C5H5NH)[ZnBr3(C5H5N)] (1) and (n-CH3C5H4NH)[ZnBr3(n- CH3C5H4N)] (n = 2 (2), 3 (3), 4 (4)) were prepared by crystallization from ethanol solutions through redistribution reactions between the corresponding dianionic complexes (C5H5NH)2[ZnBr4] (5) and (n-CH3C5H4NH)2[ZnBr4] (n = 2, 3 (6), 4 (7)) and the neutral complexes [ZnBr2(C5H5N)2] (10) and [ZnBr2(n-CH3C5H4N)2] (n = 2 (8), 3, 4 (9)). The crystal structures of 1, 4, 9, and 10 were determined; 1: triclinic, P1, a = 7.6957(5), b = 7.7975(4), c = 12.4768(8) Å , α = 90.857(5), β = 95.917(5), γ = 107.899(6)°, Z = 2, 150 K; 4: monoclinic, P21/c, a = 14.8369(6), b = 13.9504(5), c = 8.0041(3) Å , β = 96.318(4)°, Z = 4, 299 K; 9: monoclinic, P21/c, a = 14.2883(5), b = 8.0269(3), c = 13.6031(5) Å , β = 100.581(4)°, Z = 4, 150 K; 10: monoclinic, P21/c, a = 8.7388(5), b = 17.9730(10), c = 8.5452(5) Å , β = 100.024(6)°, Z = 4, 300 K. The cation and anion are paired up via bifurcated hydrogen bonds in the structure of 1 and via a normal N-H· · ·Br hydrogen bond in the structure of 4. 81Br NQR resonance lines coinciding in number with the Br atoms in the chemical formulae were observed for the compounds 1 - 5 and 7 - 9 throughout the temperature range from 77 to ca. 320 K. The comparison between the net charges on the Br atoms obtained by the Townes-Daily analysis or by the Mulliken population analysis seems to indicate that the formation of the intermolecular N-H· · ·Br hydrogen bonds and the π-π and the CH3-π interactions in the crystal structures of the monoanionic complexes are the driving forces to the redistribution reactions
An Efficient Ultrasound-assisted Method for the Synthesis of 1,4-Disubstituted Triazoles
Authors: Jiang Yuqin , Chen Xiaolan , Qu Lingbo , Wang Junliang , Yuan Jinwei , Chen Senshen , Li Xu
Published: February 2015

An efficient method for the synthesis of 1,4-disubstituted triazoles has been developed with the help of ultrasound irradiation in water at room temperature. Under the optimized conditions, a novel series of 1,4-disubstituted 1,2,3-triazoles was synthesized in high yields
Synthesis and Characterization of a Cubic Iron Hydroxy Boracite
Authors: Neumair Stephanie C. , Knyrim Johanna S. , Oeckler Oliver , Kaindl Reinhard , Huppertz Hubert
Published: February 2015

The cubic iron hydroxy boracite Fe3B7O13OH・1.5H2O was synthesized from Fe2O3 and B2O3 under high-pressure/high-temperature conditions of 3 GPa and 960 °C in a modified Walker-type multianvil apparatus. The crystal structure was determined at room temperature by X-ray diffraction on single crystals. It crystallizes in the cubic space group F4̄3c (Z = 8) with the parameters a = 1222.4(2) pm, V = 1.826(4) nm3, R1 = 0.0362, and wR2 = 0.0726 (all data). The B-O network is similar to that of other cubic boracites.
New Pyridylene-bridged Bisoxazoles – Synthesis and Structural Study
Authors: Felsmann Marika , Hübscher Jörg , Eißmann Frank , Seichter Wilhelm , Weber Edwin
Published: February 2015

The bisoxazoles 1a - 1c that feature structures with two oxazole moieties connected to a 2,6- pyridylene central linker and contain different aryl substituents in 4- and 5-positions of the oxazole rings have been synthesized. Single-crystal X-ray structure determinations of the free ligand 1a, containing the NiCl2 complex of 1c as the CH3COOH solvate as well as the 1,4-dioxane-solvated diester intermediate 2a are reported, which show specific molecular conformations and packings in the crystals. The conformation of 1a is syn with reference to the oxazole nitrogen atoms and anti with reference to the oxazole and pyridine nitrogen atoms. In the Ni2+ complex, the metal ion is in an octahedral coordination environment with the nitrogens of 1c and an oxygen of an acetic acid molecule in the basal plane, while two chloride ions occupy the axial positions of three additional acetic acid molecules one is hydrogen-bonded to a chloride and two form a carboxylic dimer, thus giving rise to a 1 : 1 : 4 (1c: NiCl2 :HOAc) stoichiometric ratio. The crystalline 1 : 1 inclusion compound of 2a with 1,4-dioxane suggests a typical clathrate owing to the bulkyness of the host molecule.
A Metal-Organic Framework Constructed of 1,4-Di(pyridin-4-yl)- buta-1,3-diyne and Nickel(II) Nitrate
Authors: Albrecht Marcel , Nieger Martin , Schmidt Andreas
Published: February 2015

A metal-organic framework (MOF) was prepared from 1,4-di(pyridin-4-yl)buta-1,3-diyne and nickel(II) nitrate hexahydrate in methanol and dichloromethane at room temperature. The crystals are orthorhombic, space group C2221, Z = 4. The rhombic cavities of the MOF are occupied by disordered molecules of dichloromethane
Application of n-Dodecyltrimethylammonium Chloride for the Oxidation of Intermetallic Phases
Authors: Böhme Bodo , Hoffmann Stefan , Baitinger Michael , Grin Yuri
Published: February 2015

The thermal decomposition products of ionic liquids based on n-dodecyltrimethylammonium chloride (DTAC) were used for the preparation of the metastable allotrope Ge(cF136) by oxidation of Na12Ge17 in gas-solid reactions. This method of preparation provides a promising low-temperature route for the synthesis of intermetallic phases and elemental modifications. In order to explore the reaction mechanism, we investigated the thermal decomposition of DTAC as well as of the ionic liquids DTAC/MgCl2 and DTAC/AlCl3 by in-situ mass spectrometry and by powder X-ray diffraction. The results have revealed HCl, CH3Cl and 1-chlorododecane to act as oxidizing agents in the gas-solid redox reactions.
Mössbauer-spectroscopic Characterization of the Local Surrounding of Tin Dopant Cations in the Bulk and on the Surface of YCrO3 Crystallites
Authors: Afanasov Mikhail I. , Wattiaux Alain , Labrugère Christine , Fabritchnyi Pavel B. , Delmas Claude
Published: February 2015

119Sn Mössbauer spectra of tin-doped YCrO3, obtained by annealing in air of an YCr(119Sn4+)0.003(OH)6·xH2O precursor, provide evidence for the location of Sn4+ on the Cr3+ site in the bulk of crystallites. Below the Néel point of YCrO3 (TN = 141 K), Sn4+ ions are spinpolarized, the majority exhibiting a hyperfine field H of 80 kOe at 4.2 K. Analysis of the 119Sn spectra of another sample, obtained by impregnation of polycrystalline YCrO3 with a solution of 119SnCl4, shows that annealing in H2 results in the location of the dopant, in the divalent state, on the surface of the crystallites. The parameters of an in situ 119Sn spectrum at 295 K (isomer shift δ = 2.76 mm s−1 and quadrupole splitting EQ = 1.95 mm s−1) reveal the presence of Sn2+ ions on sites with a coordination number CN < 6. At 100 K these Sn2+ ions exhibit no spin polarization. Upon contact with air they are rapidly oxidized to the tetravalent state, as demonstrated by their modified isomer shift value δ = 0.06 mm s−1. For the large majority of both the residual “parent” Sn2+ ions and the “daughter” Sn4+ ones no spin polarization is observed down to 4.2 K. This means that surface-located tin dopant cations, regardless of their oxidation state, occupy the Y3+ sites with an equal number of Cr3+ neighbors having mutually opposite spin orientations.
Separation of Different Types of Monosaccharides by Polyacrylamide Column Chromatography
Authors: Bystrický Slavomír , Medovarská Izabela , Machová Eva
Published: February 2015

A high-throughput polyacrylamide gel chromatography was effectively tested to separate different types of monosaccharides. These occur for example in the complex bacterial LPS (lipopolysaccharide) structures as well as in other compounds. Here, a Bio-Gel P-2 column eluted only with water at ambient temperature afforded a convenient separation of the main structural types of neutral, charged, or highly polar hexoses, as well as N-acetylated hexose derivatives. These can be easily isolated on the semi-preparative scale by this method. The method was evaluated with a mixture of all basic types of monosaccharides, and repeatedly an efficient resolution was achieved. As an example of a complex structure, the monosaccharide constituents of the delipidated bacterial lipopolysaccharides (dLPS) of V. cholerae O135 were effectively separated after acid hydrolysis.
Synthesis, Reactions and Antibacterial Activity of 3-Acetyl[1,2,4]triazolo[3,4-a]isoquinoline Derivatives using Chitosan as Heterogeneous Catalyst under Microwave Irradiation
Authors: Hassaneen Hamdi M. , Hassaneen Huwaida M. E. , Mohammed Yasmin Sh. , Pagni Richard M.
Published: February 2015

3-Acetyl[1,2,4]triazolo[3,4-a]isoquinolines were prepared using chitosan as a catalyst. These compounds were used to prepare a novel series of enaminones 5, and their reactions with hydrazonoyl halides 1 and 11 gave triazoloisoquinolines 8 and 13, respectively, with a carbonylpyrazole side chain. Hydrazinolysis of 8 and 13 gave the pyrazolopyridazines 10 and pyrazolopyridazinones 14. Reaction of 5 with hydroximoyl halides 15 led to triazoloisoquinoline 16 with a carbonylisoxazole side chain. Antibacterial effects of compounds 8 and 10 were studied.
Orthoborate Halides with the Formula (M+II)5(BO3)3X: Syntheses, Crystal Structures and Raman Spectra of Eu5(BO3)3Cl and Ba5(BO3)3X (X = Cl, Br)
Authors: Reckeweg Olaf , Schulz Armin , DiSalvo Francis J.
Published: February 2015

Single crystals of Eu5(BO3)3Cl were obtained by serendipity by reacting Eu2O3 and Mg with B2O3 at 1300 K in the presence of an NaCl melt for 13 h in silica-jacketed Nb ampoules. Ba5(BO3)3X (X = Cl, Br) crystals were formed by direct synthesis from appropriate amounts of Ba(OH)2, H3BO3 and the respective barium halide (hydrate) in alumina crucibles kept in the open atmosphere at 1300 K for 13 h. The crystal structures of the title compounds were determined with single-crystal X-ray diffraction. All compounds crystallize isotypically to Sr5(BO3)3Cl in the orthorhombic space group C2221 (no. 20, Z = 4) with the lattice parameters a = 1000.34(7), b = 1419.00(9), c = 739.48(5) pm for Eu5(BO3)3Cl, a = 1045.49(5), b = 1487.89(8), c = 787.01(4) pm for Ba5(BO3)3Cl, and a = 1048.76(7), b = 1481.13(9) and c = 801.22(5) pm for Ba5(BO3)3Br. The Raman spectra of all compounds were acquired and are presented and compared to literature data. The incremental volume of the orthoborate (BO3)3− anion has been determined and is compared to the Biltz volume
Orthoamide und Iminiumsalze, LXXI [1]. Zur Fixierung von Kohlendioxid mit organischen Basen (Teil 2) – Reaktionen von Guanidinen und ω-Aminoalkyl-guanidinen mit Kohlendioxid/ Orthoamides and IminiumSalts, LXXI [1]. Capturing of Carbon Dioxidewith OrganicBases (Part 2) – Reactions of Guanidines and ω-Aminoalkyl-guanidines with Carbon Dioxide
Authors: Tiritiris Ioannis , Mezger Jochen , Stoyanov Edmont V. , Kantlehner Willi
Published: February 2015

The guanidines 1, 4, 6, 8, 10, and 12 react with carbon dioxide in the presence of traces of water to give the guanidinium hydrogen carbonates 3, 5, 7, 9, 11, and 13. The crystal structures of the salts reveal the presence of centrosymmetric hydrogen carbonate ion dimers, which are connected by O-H・ ・ ・O hydrogen bonds. Additionally the cations are associated with the anions via N-H・ ・ ・O hydrogen bonds. The reaction of the N-(aminoalkyl)guanidine 14 with CO2 in the presence of traces of water affords a stable hygroscopic carbamic acid as the hydrogen carbonate salt 15. In the crystal structure of 15 the hydrogen carbonate ion is connected with the carbamic acid moiety by strong O-H・ ・ ・O hydrogen bonds
Dendrophen, a Novel Glycyrrhetyl Amino Acid from Dendronephthya hemprichi
Authors: Shaaban Mohamed , Shaaban Khaled A. , Abd-Alla Howaida I. , Hanna Atef G. , Laatsch Hartmut
Published: February 2015

Chemical investigation of the extract of Dendronephthya hemprichi, collected from the Red Sea, Egypt, delivered dendrophen (1), the first 3β -acetoxy-glycyrrhetyl amino acid conjugate obtained from nature. Additionally, a new polyhydroxy sterol, dendrotriol (2), together with cholesterol and hexitol were isolated. Chromatographic separation of the low-polarity components of the D. hemprichi extract afforded 4-oxo-pentanoic acid, 2-methyl-acrylic acid 2-diethylaminoethyl ester (3), juniper camphor (4), and 2-octadecanone. The structures of 1 and 2 were confirmed by 1D and 2D NMR studies and mass spectrometry.
Aminkomplexe von Silber(I)-disulfonylamiden, Teil I: Sekund¨are Amine [1]
Authors: Zerbe Eva-Maria , Wölper Christoph , Jones Peter G.
Published: February 2015

We report the crystal structures of five amine-complexed silver(I) disulfonylamides of composition L2AgX (L = secondary amine, X = disulfonylamide anion) [1: bis(2,2,6,6-tetramethylpiperidine)- silver(I) dimesylamide, 2: bis(2,2,6,6-tetramethylpiperidine)(1,1,3,3-tetraoxo-1,3,2-benzodithiazolido) silver(I), 3: bis(diethylamine)(dimesylamido)silver(I), 4: bis(diethylamine)silver(I) 1,1,3,3-tetraoxo- 1,3,2-benzodithiazolide, 5: bis(dicyclohexylamine)silver(I) 1,1,3,3-tetraoxo-1,3,2-benzodithiazolide]. In the solid state 1, 4 and 5 are ionic compounds, whereas 2 and 3 appear to be molecular, but with long Ag-Ndisulfonylamide bonds (ca. 2.5 Å ), almost linear Namine-Ag-Namine bond angles (171, 158°) and S-N bond lengths more typical of purely ionic disulfonylamides. The packing of these complexes is governed by the formation of chains via motifs of Ag・ ・ ・O contacts and classical hydrogen bonds. The interaction motifs vary slightly depending on the steric demand of the amine substituents. For the molecular compounds, either new motifs appear (3) or intramolecular classical hydrogen bonds are formed, and linear arrays of molecules are generated by non-classical hydrogen bonds (2)
Drei neue Koordinationsverbindungen mit komplexen Metallkationen [M(X)6]n+ (M = Co: X = H2O, NH3 und n = 3; M = Ni: X = H2O und n = 2) und Hydrogenacetylendicarboxylat als Anion / Three New Coordination Compounds with Complex Cations [M(X)6]n+ (M = Co: X = H2O, NH3 and n = 3; M = Ni: X = H2O and n = 2) and Hydrogenacetylenedicarboxylate Anions
Authors: Stein Irena , Ruschewitz Uwe
Published: February 2015

From an aqueous solution containing acetylenedicarboxylic acid (H2ADC) and [Co(NH3)6]Cl3 or Ni(O2CCH3)2 ・ 4H2O single crystals of [Co(H2O)6][(ADC)(HADC)] ・2H2O (1), [Co(NH3)6]- [Cl2(HADC)] ・H2O (2) and [Ni(H2O)6](HADC)2 ・ 2H2O (3) precipitated upon slow evaporation of the solvent. In their crystal structures slightly distorted octahedral coordination spheres of the metal ions ([Co(H2O)6]3+, [Co(NH3)6]3+ and [Ni(H2O)6]2+) are found. These complex cations are further connected via weak hydrogen bonds to structural units of higher dimensionality. All compounds contain mono-protonated acetylenedicarboxylate anions (HADC−). In 1 strong hydrogen bonds (O・ ・ ・O = 2.524(5) Å ) form ADC・ ・ ・HADC− dimers, whereas in 2 (H2O・ ・ ・HADC−)∞ ribbons (O・ ・ ・O = 2.496(4) Å and 2.676(3) Å , respectively) and in 3 (HADC−)∞ chains (O・ ・ ・O = 2.489(3) Å ) are found. 1 and 2 represent new structure types, whereas 3 is isotypic to the known Mg and Zn compounds
Synthesis of Substituted Benzoxazolinones by the Curtius Rearrangement: Crystal Structures of Intermediates and By-Products
Authors: Laus Gerhard , Kahlenberg Volker , Wurst Klaus , Nerdinger Sven , Schottenberger Herwig
Published: February 2015

3-Substituted salicyloyl chlorides were converted to salicyloyl azides (R = Br, NO2) which underwent thermal rearrangement and intramolecular cyclization to benzoxazolinones. The crystal structures of 7-substituted benz[d]oxazolin-2-ones (R = Br, NH2), intermediate salicyloyl azides and byproducts, i. e. 3-(2-hydroxy-3-nitrophenyl)-8-nitrobenz[e][1,3]oxazine-2,4-dione and 2-hydroxy-N- (2-hydroxy-3-nitrophenyl)-3-nitrobenzamide, have been determined. 7-Aminobenzoxazolinone was obtained by catalytic hydrogenation of the nitro compound as the hemihydrate or in anhydrous form, depending on the temperature of the crystallization
Synthesis, Experimental and Theoretical Study on the Structure of Some Semicarbazides with Potential Antibacterial Activity
Authors: Pitucha Monika , Karczmarzyk Zbigniew , Kosikowska Urszula , Malm Anna
Published: February 2015

A series of 1,4-disubstituted semicarbazide and 4,4’-bis[1-substituted semicarbazide]diphenylmethane derivatives were synthesized to explore their antibacterial activity. New compounds were characterized by elemental analysis and spectroscopic data. In order to find the tautomeric equilibrium for the molecules energy calculations for each possible tautomeric form of model compound 2, and for the most antibacterially active compound 7 in the investigated series, were calculated for the gas phase at the RHF/SCF/6-31G** level of theory
Synthesis and Antitumor Activity of Ring A-modified Glycyrrhetinic Acid Derivatives
Authors: Csuk René , Schwarz Stefan , Siewert Bianka , Kluge Ralph , Ströhl Dieter
Published: February 2015

The pentacyclic triterpene glycyrrhetinic acid is an interesting natural product exhibiting various biological activities. Especially its ability to induce apoptosis in tumor cells is of high scientific interest. In this study we altered the lipophilicity in ring A by derivatization at positions C-2 and C-3. The consequences of these variations on the cytotoxicity were investigated applying a colorimetric sulforhodamine B assay using 8 different human tumor cell lines. An acridine orange/ethidium bromide (AO/EB) test and a trypan blue test were used to determine the extent of apoptotic activity of some of these compounds
Imidazolium Dicyanoargentates
Authors: Mallah Eyad , Abu-Salem Qutaiba , Sweidan Kamal , Kuhn Norbert , Maichle-Mößmer Cäcilia , Steimann Manfred , Ströbele Markus , Walker Michael
Published: February 2015

New imidazolium dicyanoargentate salts were synthesized by treatment of 2-chloro-1,3-diisopropyl-4,5-dimethylimidazolium chloride (2a) with an excess of silver cyanide in acetonitrile to afford 2-chloro-1,3-diisopropyl-4,5-dimethylimidazolium dicyanoargentate (3) and its conversion into the corresponding 2-cyano-1,3-diisopropyl-4,5-dimethylimidazolium dicyanoargentate (4) by reaction with an excess amount of potassium cyanide. The crystal structures of 3 and 4 are reported
Cd4 Tetrahedra and Condensed RE6Rh Trigonal Prisms as Building Units in the Rare Earth-rich Compounds RE15Rh5Cd2 (RE = La, Ce, Pr, Nd)
Authors: Tappe Frank , Rodewald Ute Ch. , Hoffmann Rolf-Dieter , Pöttgen Rainer
Published: February 2015

The rare earth-rich compounds RE15Rh5Cd2 (RE = La, Ce, Pr, Nd) were synthesized by induction melting of the elements in sealed tantalum tubes and characterized by X-ray powder diffraction. The structure of La15Rh5Cd2 was refined from single-crystal diffractometer data: new type, R3m, a = 1016.4(2), c = 4418.7(9) pm, wR2 = 0.0417, 2258 F2, 95 variables. Striking structural motifs in the RE15Rh5Cd2 intermetallics are rhodium-centered trigonal prisms RE6Rh which are condensed via common corners and edges to a complex three-dimensional network which leaves cavities for Cd4 tetrahedra and RE6 octahedra. The structural relationship with the recently discovered structure types Gd4RhIn and Pr23Ir7Mg4 is discussed.
Chemical Constituents of Pedicularis densispica Franch
Authors: Chu Hong Biao , Zeng Guang Zhi , Zhu Mei Ju , He Wen Jun , Zhang Yu Mei , Tan Ning Hua
Published: February 2015

An ethanol extract of the dried aerial of Pedicularis densispica Franch (Scrophulariaceae) afforded a new lignan, densispicoside (1), and two new iridoids, densispicnin C and D (14, 15), together with four lignans, (+)-isolarisiresinol 3a-O-β -D-glucopyranoside (2), (-)-pinoresinol-β - D-glucopyranoside (3), syringaresinol mono-β -D-glucopyranoside (4), longifloroside B (5), eight phenylpropanoids, 4-O-β -D-glucopyranosyl-sinapic acid methyl ester (6), 3-(4-hydroxy-3-methoxyphenyl)- 1,2,3-propantriol (7), citrusin C (8), robustaside B (9), verbascoside (10), martynoside (11), 2ʺ-O-acetylverbascoside (12), cis-martynoside (13), and two iridoid glycosides, shanzhiside methyl ester (16), and 8-epiloganin (17). Their structures were established on the basis of chemical and spectroscopic studies. Bioactivity results indicate that P. densispica shows activity on PAI-1 antithrombus assay in vitro and antifatigue activities in vivo.
Synthesis and Crystal Structure of a New Pb(II) Coordination Polymer Constructed by a 1,10-Phenanthroline Derivative and a Flexible Dicarboxylate
Authors: Wang Xiu-Yan , Guo Jia , Wang Hui-Lian , Wang Qing-Wei
Published: February 2015

The new coordination polymer, [Pb(L)(trans-1,4-chdc)] 1 (L = 1-(1H-imidazo[4,5-f][1,10]phenanthrolin-2-yl)- naphthalen-2-ol and trans-1,4-H2chdc = trans-1,4-cyclohexanedicarboxylic acid), has been hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal data: C31H24N4O5Pb, monoclinic, space group P21/c, a = 13.579(2), b = 9.7831(15), c = 19.958(3) Å, β = 105.058(2)°, V = 2560.3(7) Å3, Z = 4. The Pb(II) atoms are bridged by the flexible trans-1,4-chdc ligands to form a zigzag chain. The ligands L are located on both sides of the zigzag chains, where π-π interactions among neighboring zigzag chains give rise to a two-dimensional supramolecular network. In addition, O-H···O and N-H···O hydrogen bonding interactions further stabilize the supramolecular network structure of 1.