Nanocomposites Based on Poly(Amide-Imide) Matrix with Na–Mg Triple Chain Hydrosilicate

Crystallography Reports - A new polymer-inorganic nanocomposite composed of fibrous Na–Mg triple chain hydrosilicate with a poly(amide-imide) matrix was developed. Its structure, morphology,...     

PL Quenching of Poly(3-hexylthiophene) by 2,2′,7,7′-Tetradiphenylamino-9,9′-Bifluorenylidene

2,2′,7,7′-Tetradiphenylamino-9,9′-bifluorenylidene, TDPABF, was synthesized by reductive dimerization using Lawesson's reagent. It is soluble in common organic solvents such as dichloromethane, chloroform, and 1,2-dichlorobenzene. Its synthesis was confirmed by ¹H-, ¹³C- NMR, MALDI-TOF, and FT-IR spectroscopy. Its HOMO and LUMO energy levels were –5.33 eV and –2.98 eV, respectively, using photoelectron spectroscopy and UV-Vis absorption spectra. Its fluorescence quenching properties were investigated through a Stern-Volmer quenching experiment. The PL intensity significantly decreased on increasing the concentration of TDPABF in a P3HT chloroform solution. The calculated Stern-Volmer quenching constant was 9.1 × 10⁴ M^?1, which is higher than that reported for PC₆₁BM.     

Poly (Isonicotinic Acid N-Oxide–Isonicotinate-N-Oxide-Chloro-Uranyl): The Interpenetrating Grids Created by Coordination and Hydrogen Bonds

Abstract  

The building blocks of the title compound, [UO₂ ²⁺·Cl⁻·(C₆H₄NO₃)⁻ · (C6H5NO3)]_n–uranyl fragment, chloride ion, one deprotonated isonicotinate N-oxide and one isonicotinic acid N-oxide, are arranged in the complicated three dimensional network by means of both coordination and hydrogen bonds. The uranium ion is seven-coordinated, in the fashion intermediate between the pentagonal bipyramid and capped octahedron. The coordination one-dimensional polymer chains are connected by strong carboxyl—carboxyl hydrogen bonds into two dimensional grids. These grids interpenetrate each other like the chain-links.     

Antimicrobial Activity of Composite Hydrogels in the Poly(N-vinylpyrrolidone)–RE(NO3)3 · xH2O (RE Are Rare-Earth Ions) System

Crystallography Reports - The bactericidal and bacteriostatic properties (in darkness) of salts RE(NO3)3 · xH2O (RE = La, Ce, Gd, Yb, Y) and composite hydrogels with poly(N-vinylpyrrolidone)...     

Adsorption Capacity of Poly[4-Methacroyloxy-(4’-Carboxy-3-СHloro)-Azobenzene], In Situ Immobilized on the Silica Gel Surface to Toxic Metals Ions

Abstract

By mean of heterophase polimarzation on the silica gel surface has been made in situ immobilization of poly[4-methacroyloxy-(4’-carboxy-3-Сhloro)-azobenzene] and has been received new organic-mineral composit material. The fact of polymer immobilization has been confirmed by IR spectroscopic method and thermogravimetric analysis combined with mass spectrometry. According to the results of thermogravimetric analysis, has been found the mass of the immobilized polymer is 13.33%.

The synthesized composite revealed sorption activity to the ions of Cu (II), Pb (II) and Fe (III) micro quantities in a neutral water environment. Maximum sorption ions Cu (II), Pb (II) and Fe (III) degree is reached during first contact hour in static sorption condition. According to the results of isotherms sorption treatment has been determined the silica gel surface poly [4-methacryloxy- (4'-carboxy-3-chloro)-azobenzene] modification led to the sorbtion volum Cu (II) ions more than 1.5 times, for ions Pb (II) - 3.6 times, but for Fe (III) ions - almost 2 times.     

Synthesis,Crystal Structures and Physicochemical Properties of Poly[bis(<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>-Dimethylformamide)tetra(thiocyanato)metal(II) Mercury(II)] (Metal = Cadmium and Manganese)

Abstract  

Two novel single crystals, poly[bis(N,N-dimethylformamide)tetra(thiocyanato)metal(II)mercury(II)] (metal = cadmium and manganese, abbreviated as DTCM and DTMM, respectively) were prepared. The characterizations of DTCM and DTMM were performed by elemental analyses, infrared, X-ray single crystal diffraction. The two title complexes crystallized in the same monoclinic crystallographic system and P2₁/n space group with unit cell parameters: a = 9.2515(2) Å, b = 14.1670(3) Å, c = 16.5898(3) Å, β = 93.0320(10)°, z = 4, D _x  = 2.115 g/cm³ for DTCM, and a = 9.24580(10) Å, b = 14.1110(2) Å, c = 16.4937(2) Å, β = 92.9120(10)°, z = 4, D _x  = 1.960 g/cm³ for DTMM, respectively. The two structures are isostructural. The thermal decomposition processes of the two crystals were investigated by means of thermogravimetric analysis and differential thermal analysis measurements in air.     

Crystal structure of (3-aminopropionato)bis(ethylenediamine)cobalt(III) catena-di(μ-chloro)dichloroplumbate(II) monohydrate

Crystals of [Co(C₂H₈N₂)₂(C₃H₆NO₂)]PbCl₄ · H₂O [a = 7.627(1) Å, b = 11.238(1) Å, c = 11.444(1) Å, α = 99.125(1)°, β = 103.80(1)°, γ = 94.739(1)°, V = 933.09(1) ų, Z = 2, and space group $P\bar 1$ ] contain the octahedral PbCl₆ groups that share edges to form infinite [Cl₂Pb(μ-Cl)₂] _n ²ⁿ chains, in which the terminal Cl atoms occupy the cis positions. The Pb-Cl bond lengths are 2.763(1)–3.180(3) Å. In the discrete cationic complexes, the Co atom is coordinated by two ethylenediamine molecules and the 3-aminopropionate anion. In the enantiomeric complex with the Δ absolute configuration, the ethylenediamine rings have the λ and δ configurations and the aminopropionate ring has the λ configuration.     

Crystal structure of chloro(dicarbonyl) bis(acetonitrile) (π-2-methallyl) molybdenum(II)

The title compound crystallizes in the monoclinic spacegroup P2₁/m with a = 6.796(9), b = 12.145(14), c = 7.749(8)Å, = 101.86(1)°, and Z = 2. The crystal structure consists of molecules of [MoCl(CO)₂(NCMe)₂(³-C₃H₄Me-2)] with crystallographically imposed C_s symmetry and has a pseudo-octahedral geometry, with the -allyl group trans- to the chloro group and the two cis-carbonyl and acetonitrile groups occupying the equatorial plane.     

K_4CuNb_8O_(23)掺杂对K_(0.44)Na_(0.52)Li_(0.04)Nb_(0.86)Ta_(0.10)Sb_(0.04)O_3压电陶瓷性能的影响

采用固相反应法制备了K_(0.44)Na_(0.52)Li_(0.04)Nb_(0.86)Ta_(0.10)Sb_(0.04)O_3+x mol ;K_4CuNb_8O_(23)(0≤x≤2)(简称LF4-KCN)无铅压电陶瓷,使用XRD、SEM、 Agilent 4294A精密阻抗分析仪等对该体系的相组成、显微结构、压电及介电等性能进行表征.XRD分析表明,随着KCN含量的增加,室温时样品由四方相向正交相转变,且当x≥1时,出现K_6Li_4Nb_(10)O_(30)杂相.SEM分析表明,掺入KCN后,样品晶粒尺寸减小,晶粒轮廓清晰.随着KCN含量的增加,在100 ℃附近的介电常数温度曲线上出现第二介电常数极大值,即正交→四方铁电相变温度T_(O-T),同时居里温度TC向低温方向移动.KCN掺杂量对LF4的电性能有很大影响,表现为"硬性"掺杂,其压电常数d_(33),平面机电耦合系数k_p,1kHz频率下的介电损耗tanδ和介电常数ε_r均随着 KCN含量的增加而降低,而机械品质因素Q_m整体提高,样品的密度也显著增大.     

Complexes in the Ni2+-imidazole-RN(CH2COO−)2 systems. The crystal structures of tris(imidazole)iminodiacetatonickel(II) monohydrate, hexa(imidazole)nickel(II) bis(N-methyliminodiacetato)nickelate(II) hexahydrate, and tetra(aqua)bis(imidazole)nickel(II) bis(N-benzyliminodiacetato)nickelate(II)

Crystals of different compositions, namely, [Ni(Ida)(Im)₃] ? H₂O (I), [Ni(Im)₆][Ni(Mida)₂] ? 6H₂O (II), and [Ni(Im)₂(H₂O)₄][Ni(Bida)₂] (III), have been precipitated from aqueous solutions of the Ni²⁺-Lig ^2?-Im systems, where Lig ^2? is Ida, Mida, and Bida, respectively. The crystal structures of I–III are determined by X-ray diffraction analysis (R = 0.0307, 0.0348, and 0.0302 for 3061, 4706, and 2882 reflections, respectively). Crystals I are built of monomeric mixed-ligand complexes and molecules of crystallization water, which are interlinked by hydrogen bonds into a three-dimensional framework. In II and III, the ligands Lig ^2? and Im form charged complexes separately. In II, the cationic and anionic layers of the complexes alternate along the c-axis. Numerous hydrogen bonds involving molecules of crystallization water link the layers into a three-dimensional framework. In III, the cationic and anionic complexes, which serve as proton donors and acceptors, respectively, are bound into layers parallel to the xy plane.     

Synthesis, spectral, and single crystal X-ray structural studies on (2,2′-bipyridyl)bis(dimethyldithiocarbamato) zinc(II) and (1,10-phenanthroline) bis(dimethyldithiocarbamato)zinc(II)

Synthesis, spectral, and single crystal X-ray structural studies on (2,2-bipyridyl)bis (dimethyldithiocarbamato)zinc(II) (1) and (l,10-phenanthroline)bis(dimethyldithiocarbamato)zinc(II) (2) complexes are reported in this paper. The complex (1) crystallizes in the orthorhombic lattice, space group Pcca, a = 18.456(3), b = 6.529(2), and c = 17.092(2) Å. The complex (2) crystallizes in the monoclinic space group C2/c, a = 13.372(2), b = 13.850(2), c = 24.680(3) Å, and = 102.71(4)°. IR spectra of the complexes (1) and (2) show the thioureide (C-N) bands at 1489 and 1510 cm^–1, respectively, which are lower than the value observed for the parent bisdithiocarbamate. Reduction in the thioureide stretching frequency is due to the increase in coordination around the zinc ion and the resultant increase in electron density. Thermal studies indicate that the 1,10-phenanthroline adduct is marginally more stable than the other complex. X-ray crystal structures of the two adducts show them to be octahedrally coordinated and monomeric in nature. The Zn-S distances are longer than those observed in the parent bisdithiocarbamate. The thioureide C-N bond distances in (1) and in (2) indicate the partial double bond character. The most important structural changes as a result of the adduct formation are observed in the Zn-S bond distances and S-Zn-S bond angles, in terms of very significant increases in Zn-S bond distances and reductions in S-Zn-S angles, compared to the parent bisdithiocarbamate. The observed changes are indicative of a strong steric force in operation in the adducts rather than electronic effects.     

柠檬酸络合法制备La_(0.8)Sr_(0.2)CoO_(3-δ)的研究(英文)

采用柠檬酸络合法制备了La0.8Sr0.2CoO3-δ,通过TG-DSC、SEM和XRD对产物进行表征。研究了各因素对其制备的影响,并对其合成机理作了分析。结果表明,平均晶粒尺寸随着柠檬酸量的增加而逐渐减小;pH值对La0.8Sr0.2CoO3-δ主晶相的生成没有影响,但影响凝胶过程中的胶体状态和La0.8Sr0.2CoO3-δ相的平均晶粒尺寸;80℃左右是较好的成胶温度;水是较好的溶剂,没有杂相产生。     

BaCo_(0.02)~IICo_(0.04)~IIIBi_(0.94)O_3/BaSb_(0.04)Sn_(0.96)O_3复合热敏厚膜电学性能研究

采用丝网印刷工艺制备了BaCoII0.02CoIII0.04Bi0.94O3/BaSb0.04Sn0.96O3复合热敏厚膜。借助X射线衍射仪、扫描电子显微镜和阻温测试仪对复合热敏厚膜的微结构、电学性能进行了表征分析。结果表明复合热敏厚膜主相仍为钙钛矿结构的BaCoII0.02CoIII0.04Bi0.94O3和BaSb0.04Sn0.96O3,厚膜表面随BaCoII0.02CoIII0.04Bi0.94O3含量增加趋于致密均匀。复合热敏厚膜的烧结温度、室温电阻率(ρ25)、热敏常数(β25/85)和活化能(E a)随BaCoII0.02CoIII0.04Bi0.94O3含量的增加呈现下降趋势,其烧结温度、ρ25、β25/85和E a分别处于870~1000℃、2.5 kΩ·cm~2.35 MΩ·cm、2764~4030 K和0.238~0.348 eV范围内。     

Crystal structure of bis(η5-methylcyclopentadienyl)-bis(4-methylbenzenesulfonato-O)-molybdenum(IV)

The compound bis(⁵-methylcyclopentadienyl)-bis(4-methylbenzenesulfonato-O)-molybdenum (IV) crystallizes in space-group P2₁/c, a = 8.2956(5), b = 26.896(3), c = 11.4196(11) Å, = 96.101(7)°, Z = 4. The sulfonate ligands are monodentate and the molybdenum atom has pseudotetrahedral coordination geometry, with angles O–Mo–O 72.0(1)° and Cp–Mo–Cp 134.9(1)° (Cp = ring centroid).     

Crystal structures of bis(cyanido)bis(N,N′-diethylthiourea-κS) mercury(II) and bis(cyanido)bis(N,N′-dipropylthiourea-κS) mercury(II)

Two mercury(II) complexes containing cyanide and, N,N′-diethylthiourea (detu) and N,N′-dipropylthiourea (dprtu) ligands, [(detu)₂Hg(CN)₂] (1) and [(dprtu)₂Hg(CN)₂] (2), respectively, have been prepared and characterized by X-ray crystallography. In the both complexes Hg atom lies on a 2-fold rotation axis, and is coordinated to the sulfur atoms of two thiourea ligands and to two cyanide carbon atoms. Both have a distorted tetrahedral environment with bond angles about the Hg atoms in the range of 93.41(4)°–146.75(19)°. In the crystal structures symmetry related molecules are linked via N-H-N hydrogen bonds resulting in the formation of a two-dimensional network in 1, while in 2 a double stranded one-dimensional chain is formed.     

Structure of lithium (picrate) (2,2′-bipyridyl)

The title compound C₁₆H₁₀N₅O₇Li is triclinic, witha=14.51(1),b=6.90(2),c=9.10(1) Å,=101.5(1),=67.1(2), =105.6°(1),Z=2 and space groupP¯1. Data were measured by photographic methods. The structure was solved by direct methods, and refined by full matrix least-squares. The refinement, based on 1337 reflections, gave the rather highR value of 0.11 because of poor quality data. The complex is dimeric. The coordination around the cation is distorted square-pyramidal. Two coordination sites are occupied by the nitrogen atoms of the bipyridyl ligand, two by the phenolic oxygen and oxygen ofo-nitro group, and the fifth coordination site is occupied by the phenolic oxygen belonging to the symmetry-related molecule (1–x,–y,1–z). Both oxygens act as bridges to form the dimer. The bridging is unsymmetrical, with Li-O (phenolic)=1.84(2) Å and Li¹-O (phenolic)=2.16(2) Å (whereI=1–x,–y, 1–Z).     

Molecular structure of N-(2-phenylethyl)amide of α-(1,1-ethylenedioxy)-ethyl γ-hydroxybutyric acid (I) and1H NMR spectra of (I) and N-(p-methoxybenzyl)derivative (III)

The spectroscopic and X-ray investigation of the N-(2-phenylethyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are reported. The¹H NMR spectra for the title structure and for the N-(p-methoxybenzyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are given. The N-(2-phenylethyl)amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid, C₁₆H₂₃O₄N, crustallizes in the monoclinic space groupP2 ₁/c witha=21.547(5),b=6.333(2),c=11.822(3) Å and =101.01(2)°. The dioxolane ring has a half-chair conformation with C₂(O3)=2.4° and ||_av=18.2°. The inconsiderable deviations from planarity of the six atoms of the amide group are caused mainly by twist around the C4–N1 bond and out-of-plane bending at the N1 atom ((C4–N1)=4°, X_N =7°, X_c =0.4° ). The amide group plane is nearly coplanar with the phenyl ring. The molecules are connected by two intermolecular hydrogen bonds.     

Na_(0.5)Bi_(0.5)TiO_3-K_(0.5)Na_(0.5)NbO_3无铅陶瓷介电性能研究

采用固相反应法制备了(1-x)Na0.5Bi0.5TiO3-K0.5Na0.5NbO3体系陶瓷,研究了KNN含量对Na0.5Bi0.5TiO3-xK0.5Na0.5NbO3陶瓷的晶体结构、显微结构和介电性能的影响。XRD分析结果表明,KNN进入NBT形成固溶体,该体系陶瓷均为钙钛矿结构。扫描电镜分析显示KNN的引入有利于细化晶粒,提高陶瓷致密度。测试了样品在不同频率(1 kHz,10 kHz,100 kHz,1 MHz)下的的介电温谱(室温~500℃),结果表明随着KNN含量的增加,介电峰逐渐变宽,弛豫性逐渐增强,铁电-反铁电相变温度Td和反铁电-顺电相变Tm都明显降低,当x≥0.25时,Td降至室温或更低;室温(1 kHz)下,KNN和NBT相对介电常数分别为675和575,而KNN和NBT形成的固溶体介电常数明显增大,当x=0.25时,达到最大值εr=1653。在NBT中掺入KNN得到了介电峰明显宽化、在较宽温度范围内具有低电容温度系数的致密弛豫铁电体。     

Reaction of bis(dimethoxyphosphino)dimethylhydrazine (dmpdmh) with Ru3(CO)12: Evidence for facile ligand fragmentation in Ru3(CO)10(dmpdmh) to give Ru4(CO)12[μ-N(Me)N(Me)], Ru3(CO)11[P(OMe)3], and Ru3(CO)9[μ-P(OMe)3]

Thermolysis of the cluster Ru₃(CO)₁₂ with the bis(phosphanyl)hydrazine ligand (MeO)₂PN (Me)N(Me)P(OMe)₂ (dmpdmh) in toluene at 75°C furnishes the known clusters Ru₄(CO)₁₂ [-N(Me)N(Me)] (2) and Ru₃(CO)₁₁[P(OMe)₃] (3), in addition to the new cluster Ru₃ (CO)₁₀(dmpdmh) (1) and the phosphite-tethered cluster Ru₃(CO)₉[-P(OMe)₃] (4). The simple substitution product Ru₃(CO)₁₀(dmpdmh), a logical intermediate to clusters 2–4, was synthesized by treating Ru₃(CO)₁₂ with Me₃NO in CH₂Cl₂ at room temperature, and independent thermolysis reactions using cluster 1 was shown to yield clusters 2–4. The solid-state structure of clusters 2 and 4 were unequivocally established by X-ray diffraction analysis. Ru₄(CO)₁₂[-N(Me)N(Me)] crystallizes in the orthorhombic space group Pnna (#52), a = 12.913(1), b = 13.3238(6), c = 12.5690(8) Å, V = 2162.5(2) ų, Z = 4, and d _calc = 2.452 g/cm³. Ru₃(CO)₉[-P(OMe)₃] crystallizes in the triclinic space group P a = 9.586(1), b = 14.354(1), c = 14.997(2) Å, = 89.82(1)°, = 98.36(1)°, = 92.010(8)°, V = 2040.4(4) ų, Z = 4, and d _calc = 2.212 g/cm³. The coordination of the dimethylazo linkage to the four ruthenium atoms in 2 and the phosphorus atom and one of the oxygen atoms of the methoxy groups to the three ruthenium centers in 4 are confirmed by X-ray analysis.