Synthesis, growth, crystal structure and characterization of a new organic material: glycine glutaric acid

Glycine glutaric acid, a new organic compound has been synthesized and good quality single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal XRD. The presence of the functional groups was confirmed by using FT-IR spectroscopy. The optical transparency was studied by using UV-vis spectrophotometer and it was found that the crystal is having high optical transparency. The thermal stability of the crystal was studied by using thermo-gravimetric and differential thermal analyses and found that it is stable up to 150°C. The room temperature dielectric studies were also carried out over the wide frequency range: 10 mHz to 10 MHz.     

Synthesis, morphology, structure, and magnetic characterization of layered cobalt hydroxyisocyanates

New layered pink cobalt hydroxyisocyanates have been prepared by controlled hydrolysis of aqueous solutions of CoCl2.6H2O. Co(OH)(1.4)(NCO) 0.6.0.6H 2O ( 1) is formed when urea is used as the hydrolysis agent and mannitol as the stabilizer, while Co(OH)(1.25)(NCO)(0.75).0.2H2O ( 2) is formed when the hydrolysis agent is changed to hexamethylenetetramine and NaOCN is added to the solution. IR spectroscopy of 1 and 2 indicates that the OCN (-) is N-bonded to Co (2+). The X-ray powder data for 1 could be indexed using an intergrowth model consisting of both rhombohedral ( R3 m (166); a = 3.2031(1) A, c = 23.6876(11) A, hydrotalcite-like, 3 R 1) and hexagonal ( P 63/ mmc (194); a = 3.2005(2) A, c = 15.8303(5) A, Manasseite-like, 2H1) polytypes. Rietveld refinement of the X-ray powder data was performed using a two polytype model and 30% random substitution of the OH (-) ions by OCN (-). Although it is less crystalline, the XRD data for 2 can be indexed using a rhombohedral-symmetry cell with unit cell parameters, a = 3.158 A and c = 21.57 A. Both 1 and 2 exhibit magnetically ordered ground states with a saturation magnetization of ca. 2.0 mu B. The magnetization data is consistent with 3D ferromagnetic ordering of edge-share octahedral-Co (2+) layers with effective spin S' = 1/2.     

Synthesis, characterization, and crystal structures of three new divalent metal carboxylate-sulfonates with a layered and one-dimensional structure

Hydrothermal reactions of 5-sulfoisophthalic acid (HO(3)SC(6)H(3)-1,3-(CO(2)H)(2), H(3)L) with M(II) carbonate (or oxide) and 4,4'-bipyridine (4,4'-bipy) (or 2,2'-bipyridine, 2,2'-bipy) resulted in three new metal carboxylate-sulfonate hybrids, namely, [CdL(H-4,4'-bipy)] (1) and [Cd(3)L(2)(2,2-bipy)(4)(H(2)O)(2)].2H(2)O (2) with layered structures and [ZnL(H-4,4'-bipy)(H(2)O)].2H(2)O (3), whose structure features a one-dimensional double chain. The cadmium(II) ion in complex 1 is seven-coordinated by five carboxylate oxygen atoms and one sulfonate oxygen atom from four ligands and a unidentate 4,4'-bipyridine. The interconnection of the cadmium(II) ions through bridging carboxylate-sulfonate ligands resulted in the formation of a <002> double layer with the bipyridyl rings orientated toward the interlayer space. Complex 2 has a different layered structure. Cd(1) is seven-coordinated by two bidentate chelating carboxylate groups from two ligands, a bidentate chelating 2,2'-bipy and an aqua ligand, and Cd(2) is octahedrally coordinated by two bidentate chelating 2,2'-bipy's, a sulfonate oxygen, and an aqua ligand. The coordination geometry around Cd(3) is similar to that of Cd(1) with the aqua ligand being replaced by an oxygen atom from the sulfonate group. The carboxylate-sulfonate ligand acts as pentadentate ligand, bridging with three cadmium(II) ions. The bridging of cadmium(II) ions through the carboxylate-sulfonate ligands resulted in the formation of <006> and <003> layers; the 2,2'-bipy molecules and [Cd(2)(2,2'-bipy)(2)(H(2)O)] cations are orientated to the interlayer space. Complex 3 features a 1D metal carboxylate-sulfonate double chain along the diagonal of the a- and b-axes. The zinc(II) ion is octahedrally coordinated by four carboxylate O atoms from three ligands, a unidentate 4,4'-bipy, and an aqua ligand. Each pair of zinc(II) ions is bridged by two carboxylate groups from two ligands to form a dimer, and such dimeric units are interconnected by bridging ligands to form a double chain. The sulfonate group of the carboxylate sulfonate ligand remains noncoordinated and forms a number of hydrogen bonds with aqua ligands as well as lattice water molecules.     

Synthesis and characterization of a new layered lead borate

A new lead borate, Pb[B₈O₁₁(OH)₄], has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction, FTIR, powder X-ray diffraction and thermogravimetric analysis. The compound crystallizes in the monoclinic system, space group P2₁/n (No. 14), , , , β=90.327(2)°, , and Z=4. The structure consists of layers of 9-membered borate rings enclosing Pb²⁺ cations. Adjacent borate layers are interconnected via ionic Pb-O bonds and hydrogen bonding to form a 3D supramolecular network.     

Synthesis and structure of Ba6Co6ClO16, a new cobalt oxychloride with a layered perovskite-related structure

Well-developed single crystals of the title compound were prepared using a BaCl₂ flux and investigated by X-ray diffraction methods using Mo(Kα) radiation and a Charge Coupled Device (CCD) detector. The crystal structure was solved and refined in the hexagonal symmetry with space group, a=5.6698(2) Å and c=14.4654(5) Å to a final R₁=0.022 for 44 parameters with 1418 individual reflections. The structure of Ba₆Co₆ClO₁₆, which is related to the 6H-perovkite-type structure of BaMnO_2.88, is formed by the periodic stacking along [001] of five [BaO₃] layers separated by a [BaOCl] with a (hhhchc) stacking sequence. The [BaO₃] stacking creates tetranuclear face sharing octahedra units Co₄O₁₅ containing Co(III) connected by dimers of corner-sharing CoO₄ tetrahedra. This new oxychloride belongs to the family of compounds formulated as [BaOCl]M′₂[Ba_n+1M_nO_3n+3] where n represents the thickness of the octahedral string in hexagonal perovskite slabs.     

新型三维微孔砷酸铟InAsO4(H2O)2的合成及结构

首次以有机胺为结构导向剂,在水热条件下合成了微孔砷酸铟材料InAsO4-1,并对其进行了结构及性质表征。X射线单晶结构解析表明InAsO4-1分子式为InAsO4(H2O)2。晶体学数据为：Pbca,a=0.9090(4)nm,b=1.0344(4)nm,c=1.0468(4)nm,α=β=Υ=90°,V=0.9843(7)nm^3,Z=8,R=0.0480,Rw=0.1045。InAsO4-1具有三维结构,其a,b方向分别有4元环及6元环的一维孔道,结构中还含有一8^16^44^2笼,热重分析显示其结构水较稳定。     

Synthesis of a new PET/layered niobate hybrid material

A new organic/inorganic hybrid material was prepared by the polymerization of bis(hydroxyethyl) terephthalate (BHET) with a layered niobate compound, H₄Nb₆O₁₇, modified by 11-aminoundecanoic acid (AUA). The hybrid polymer films of BHET with H₄Nb₆O₁₇/AUA exhibited favorable characteristics, particularly of being optically clear, indicating the exfoliation and homogeneous dispersion of H₄Nb₆O₁₇ into the PET/niobate hybrid.     

Synthesis and powder X-ray diffraction analysis of new mixed rare-earth and selenium oxychlorides with composition LnSeO3Cl

A series of new mixed rare-earth and selenium oxychlorides with composition LnSeO₃Cl (Ln = La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb, or Y) were prepared by annealing together LnOCl and SeO₂ in sealed silica tubes. The resulting compounds were characterized by powder X-ray diffraction. The unit cell parameters of the phases were determined. Lanthanum—europium oxychlorides crystallized in the tetragonal system to give the Sillen phases analogously to tellurium compounds with the similar formula, whereas Tb—Yb and Y oxychlorides crystallized in the orthorhombic system. It is likely that the latter oxychlorides are not layered compounds.     

The molecular structure of selenium oxychloride as studied by electron diffraction

The molecular geometry of selenium oxychloride has been studied by electron diffraction. The internuclear distances (in terms of r_a) are: r(Se-O) 1.612 ± 0.005 Å, r(Se-Cl) 2.204 ± 0.005 Å, r(Cl β O) 3.064 ± 0.012 Å, r(Cl β Cl) 3.295 ± 0.016 Å. The bond angles are ∠Cl-Se-O 105.8 ± 0.7° and ∠ Cl-Se-Cl 96.8 ± 0.7°. The structural parameters of three simple selenium-oxygen compounds are compared with those of their sulphur analogs in terms of the valence shell electron pair repulsion model.     

A new cationic poly(ester-anhydride): Synthesis, structure characterization, and biological properties

To improve the cytotoxicity and biocompatibility of cationic polymers used as gene carriers, new cationic poly(ester-anhydride) copolymers (Pea-PAs) bearing a quaternary ammonium group in the backbone were synthesized through a reaction between an aminoester dicarboxylic acid with a tertiary amine in the backbone and excess acetyl chloride. Their structure was characterized by nuclear magnetic resonance (NMR), Fourier transform infrared spectrometry (FTIR), and gel permeation chromatography (GPC). They degraded hydrolytically in 20 mM HEPES buffer at pH 7.4 at 37°C with a half-life of more than 70 h. Their cytotoxicity was substantially lower than that of PEI. The blood clotting index (BCI) and haemolysis ratio (HR) also showed that these newly synthesized Pea-PA polymer are biopolymers with good blood compatibility.     

Synthesis and crystal structure of layered oxyhalides BaPbBi3Nb2O11X (X = Cl, Br, I)

Three new bismuth oxyhalides BaPbBi₃Nb₂O₁₁X (X = Cl, Br, I), including the first perovskite bismuth oxyiodide, were prepared by ceramic route. Their crystal structure is formed by intergrowth of Sillén (PbBiO₂X) and Aurivillius (BaBi₂Nb₂O₉) phases. The results of Rietveld refinements show that the peculiarities of the building blocks (in particular, the distribution of Ba²⁺ and Bi³⁺) remain intact upon formation of the intergrowth structure. The Ba²⁺ cations prefer pure-oxygen to mixed oxygen-halogen environment which can be explained on the basis of bond valence method.     

Synthesis, characterization and structure determination of two isotypes of a layered aluminophosphate with a new 2D network topology

Two isotypes of a new layered aluminophosphate, further denoted MDAP-3 and MDAE-1, have been synthesized under hydrothermal conditions using N-methyl-1,3-propanediamine and N-methyl-ethylenediamine, respectively. MDAP-3, with the empirical formula [Al₂(HPO₄)(PO₄)₂](C₄N₂H₁₄)(H₂O), crystallizes in the orthorhombic space group Pna2(1) (No. 33) with , , , Z=4, R₁=0.0498 and wR₂=0.1217. The second solid, MDAE-1, with the empirical formula [Al₂(HPO₄)(PO₄)₂](C₃N₂H₁₂)(H₂O), crystallizes in the same space group with , , , Z=4, R₁=0.0407 and wR₂=0.0954. The two compounds possess the same layer topology. Inorganic layers contain PO₃=O, PO₃OH, AlO₄ and AlO₆ polyhedra, linked together to generate a new 4×8 net. MDAP-3 and MDAE-1 represent the first examples of two-dimensional layered aluminophosphates with the Al₂P₃O₁₂ stoichiometry, and containing AlO₆ octahedra.     

Synthesis, characterization, and crystal structures of two divalent metal diphosphonates with a layered and a 3D network structure

Reactions of N-methyliminobis(methylenephosphonic acid), CH(3)N(CH(2)PO(3)H(2))(2) (H(4)L), with divalent metal acetates under different conditions result in metal diphosphonates with different structures. Mn(H(3)L)(2).2H(2)O (complex 1) with a layer structure was prepared by a layering technique. It is triclinic, P1 macro with a = 9.224(3) A, b = 9.780(3) A, c = 10.554(3) A, alpha = 82.009(6) degrees, beta = 74.356(6) degrees, gamma = 89.853(6) degrees, Z = 2. The Mn(II) ion is octahedrally coordinated by six phosphonate oxygen atoms from four ligands, two of them in a bidentate and two in a unidentate fashion. Each MnO(6) octahedron is further linked to four neighboring MnO(6) octahedra through four bridging phosphonate groups, resulting in a two-dimensional metal phosphonate (002) layer. These layers are held together by strong hydrogen bonds between uncoordinated phosphonate oxygen atoms. The zinc complex Zn(3)(HL)(2) (complex 2) was synthesized by hydrothermal reactions (4 days, 438 K, autogenous pressure). It is monoclinic, P2(1)/n with a = 7.7788(9) A, b = 17.025(2) A, c = 13.041(2) A, beta = 94.597(2) degrees, Z = 4. The structure of complex 2 features a 3D network built from ZnO(4) tetrahedra linked together by bridging phosphonate groups. Each zinc cation is tetrahedrally coordinated by four phosphonate oxygen atoms from four ligands, each of which connects with six zinc atoms, resulting in voids of various sizes. Magnetic measurements for the manganese complex shows an antiferromagnetic interaction at low temperature. The effect of the extent of deprotonation of phosphonic acids on the type of complex formed is discussed.     

Synthesis,structure, and physical properties of the new layered ternary chalcogenide NbNiTe5

The new ternary chalcogenide NbNiTe₅ has been prepared. NbNiTe₅ crystallizes with four formula units in a cell with dimensions a = 3.656(5), b = 13.075(16), c = 15.111(19) Å in the orthorhombic system in space group D¹⁷_2h-Cmcm. The structure has been refined to a final R index on F²_o of 0.037 for 25 variables and 1405 observations. NbNiTe₅ forms in a new layered structural type. Each layer consists of bicapped trigonal prismatic niobium atoms and octahedral nickel atoms coordinated by tellurium atoms. Electrical conductivity measurements indicate that NbNiTe₅ is a metal; its conductivity at room temperature is about 1.3 × 10⁴ Ω⁻¹ cm⁻¹. Magnetic susceptibility measurements show that NbNiTe₅ is paramagnetic (X_rt ≈ 1.04 × 10⁻³ emu mole⁻¹).     

KNa(3)In(9): a Zintl network phase built of layered indium icosahedra and zigzag chains. Synthesis,structure, bonding,and properties

This phase was discovered following direct fusion of the elements in welded Nb tubes at 550 degrees C and equilibration at 300 degrees C for 1 week. Single-crystal X-ray diffraction analysis reveals that KNa(3)In(9) crystallizes in an orthorhombic system (Cmca, Z = 8, a = 9.960(1) A, b =16.564(2) A, c = 17.530(2) A, 23 degrees C). The structure contains a three-dimensional indium network built of layers of empty In(12) icosahedra that are each 12-bonded and interconnected by 4-bonded indium atoms that also form zigzag chains. All cations bridge between cluster faces or edges, and their mixed sizes appear critical to the stability of this particular structure, which does not occur in either binary system. Both empirical electron counting and EHTB band structure calculations on the macroanion indicate that the bonding in this structure is closed-shell, whereas resistivity and magnetic susceptibility measures show that the compound is a moderately poor metal.     

Synthesis, growth, structure and characterization of a new semiorganic crystal

A new semiorganic single crystal, tris(allylthiourea)silver(I) nitrate was grown from an aqueous solution containing silver(I) nitrate and allylthiourea by slow evaporation solution growth technique at room temperature. The crystal belongs to trigonal system with centrosymmetric space group R3 and the cell parameters are, a = 12.5090(4) Å, b = 12.5090(4) Å, c = 21.7130(8) Å, V = 3348.89 Å³, and Z = 6. The various functional groups present in the molecule are confirmed by Fourier transformed infrared spectroscopy. High transmittance is observed in the visible region and band-gap energy is calculated by Kubelka–Munk algorithm. The structure and the crystallinity of the materials were further confirmed using powder X-ray diffraction analysis. Microhardness studies were also carried out to elucidate the mechanical behavior. Thermogravimetric and differential thermal analysis reveal the purity of the sample and no decomposition is observed up to the melting point.     

Synthesis, structure, and reactivity of a new Ti-containing microporous/mesoporous material

A new class of porous, mixed phase titanosilicate materials containing a microporous TS-1 phase and a mesoporous Ti-MCM-48 phase has been successfully synthesized. A novel, one-pot synthesis method was used in which the organic templates for the mesoporous and microporous phases were added sequentially to the same reaction mixture, followed by crystallization at 150 degrees C. The gemini surfactant 18-12-18 was used to form the Ti-MCM-48 mesophase; subsequent addition of tetrapropylammonium cation (TPA+) led to the formation of TS-1. The relative amounts of the two phases within the final products were controlled by optimizing the crystallization time. Crystallization times between 12 and 50 h gave materials containing both phases, with an increasing amount of microphase formed at longer crystallization times. These materials, called "Ti-MMM-2" (microporous/mesoporous materials) were characterized using powder XRD, N2 physisorption, TEM, FTIR, DR-UV/Vis spectroscopy, and 29Si MAS NMR. In the epoxidation of cyclohexene with tert-butyl hydroperoxide (TBHP), Ti-MMM-2 samples exhibited higher catalytic activity (approximately 61%) than either TS-1 (16%) or Ti-MCM-48 (42%), with a very high selectivity (97%) for formation of cyclohexene oxide.     

Synthesis,spectroscopic, thermal,crystal structure properties,and characterization of new Hofmann-Td-type complexes with 3-aminopyridine

In this study, synthesis of two new tetracyanocadmate(II) and tetracyanozincate(II) complexes based on 3-aminopyridine (3AP) and investigation of their structural properties were reported. These complexes were characterized by using vibration spectroscopy, elemental, thermal analysis and single crystal X-ray diffraction (SC-XRD) techniques. Investigation of the elemental, spectral and single crystal data of these complexes showed that the formulas [Cd(3AP)₂Zn(μ₄-CN)₄]_n (1) and [Cd(3AP)₂Cd(μ₄-CN)₄]_n (2) fully explained their crystal structure. General information about the structural and chemical properties of these complexes obtained in single crystal form was obtained by observing the changes in the characteristic peaks of the 3AP with the [Zn(μ₄-CN)₄]^2- and [Cd(μ₄-CN)₄]^2- structures that make up these complexes. The behaviors of these complexes against changes in temperature were obtained by examining the temperature-dependent changes of their mass. The asymmetric unit of the heterometallic complexes 1 and 2 consist of half Cd(II) ion, half M ion [M = Zn1 in 1 and Cd2 in 2], two cyanide ligands and one 3AP.