双核银络合物[Ag_2(dppm)_2(Py)_2(μ-Cl)]ClO_4的合成与结构

二-(二苯基膦)甲烷(dppm)是一种易与金属形成多核络合物的有机膦配体。我们用dppm作为配体合成了一系列银的多核络合物,并对其结构进行了研究。本文报导了其中一个双核化合物[Ag_2(dppm)_2(Py)_2(μ-Cl)]ClO_4的合成及晶体结构、分子结构的测定。     

Study of a molecular imprinting polymer coated BAW bio-mimic sensor and its application to the determination of caffeine in human serum and urine

A bio-mimic bulk acoustic wave (BAW) sensor was fabricated by coating the caffeine (CAF) template molecular imprinting polymer (MIP). This sensor exhibited high selectivity and a sensitive mass response to CAF. The response range of the sensor was between 5.0 x 10(-9) and 1.0 x 10(-4) M with a detection limit of 5.0 x 10(-9) M at pH 8.0. Recoveries were 96.1-105.6%. Influencing factors were investigated in detail and optimized. When employed to detect real samples, the proposed method proved to be a convenient method with the advantages of high sensitivity, good selectivity and ease of handling.     

Hydrothermal synthesis and crystal structure of a layered vanadium oxide with an interlayer metal coordination complex: [Co(phen)3][V10O26]·H2O

A novel compound, [Co(phen)₃][V₁₀O₂₆]·H₂O, was hydrothermally synthesized and characterized by single-crystal X-ray diffraction. This compound crystallizes in the orthorhombic space group Ccca with a=13.447(3), b=29.936(6), c=23.252(5) Å, V=9360(3) Å³, Z=8 and R=0.0285. Data were collected on a Rigaku R-AXIS RAPID IP diffractometer at 293 K in the range of 1.36<θ<24.99°. The structure of the compound consists of vanadium oxide layers, which are built up from the infinite VO₄ chains by corners and edges sharing. The [Co(phen)₃]²⁺ complexes occupy the interlayer space and contact each other via π−π stacking interactions of the phen groups to form infinite one-dimensional chains.     

Synthesis of triphenylamine-cored dendritic two-photon absorbing chromophores

[structure: see text]. A new series of dendritic two-photon absorbing chromophores containing triphenylamine moiety as a core or branching points have been synthesized through a convergent synthetic strategy. One-photon and two-photon optical properties of these molecules were characterized. In the nanosecond time domain, these molecules exhibited large two-photon absorption (TPA) cross sections up to 7.56-12.2 x 10(-44) s cm(4) at 800 nm, indicating that these molecular structures were viable candidates for various two-photon related applications.     

The first mu3-oxalato-bridged copper complex with tridentate Schiff base ligand N-ethyl-N'-salicylidene-1,2-diaminoethane: synthesis,structure, and magnetic properties

The first mu(3)-oxalato-bridged copper(II) complex, [[Cu(3)(L)(3)(mu(3)-C(2)O(4))][Cu(L)(H(2)O)](ClO(4))(2)] x 0.5(H(2)O) x 0.5(CH(3)OH), where HL = N-ethyl-N'-salicylidene-1,2-diaminoethane, has been synthesized and characterized by variable-temperature magnetic susceptibility measurement. The complex exhibits ferromagnetic coupling between the oxalato-bridged copper atoms and antiferromagnetic coupling between the oxygen-bridged copper atoms.     

The structures of Langmuir-Blodgett films of fatty acids and their salts

Recent advances in several experimental techniques have enabled detailed structural information to be obtained for floating (Langmuir) monolayers and Langmuir-Blodgett films. These techniques are described briefly and their application to the study of films of fatty acids and their salts is discussed. Floating monolayers on aqueous subphases have been shown to possess a complex polymorphism with phases whose structures may be compared to those of smectic mesophases. However, only those phases that exist at high surface pressures are normally used in Langmuir-Blodgett (LB) deposition. In single LB monolayers of fatty acids and fatty acid salts the acyl chains are in the all-trans conformation with their long axes normal to the substrate. The in-plane molecular packing is hexagonal with long-range bond orientational order and short-range positional order: known as the hexatic-B structure. This structure is found irrespective of the phase of the parent floating monolayer. The structures of multilayer LB films are similar to the structures of their bulk crystals, consisting of stacked bilayer lamellae. Each lamella is formed from two monolayers of fatty acid molecules or ions arranged head to head and held together by hydrogen bonding between pairs of acids or ionic bonding through the divalent cations. With acids the acyl chains are tilted with respect to the substrate normal and have a monoclinic structure, whereas the salts with divalent cations may have the chains normal to the substrate or tilted. The in-plane structures are usually centred rectangular with the chains in the trans conformation and packed in a herringbone pattern. Multilayer films of the acids show only a single-step order-disorder transition at the melting point. This temperature tends to rise as the number of layers increases. Complex changes occur when multilayer films of the salts are heated. Disorder of the chains begins at low temperatures but the arrangement of the head groups does not alter until the melting temperature is reached. Slow heating to a temperature just below the melting temperature gives, with some salts, a radical change in phase. The lamellar structure disappears and a new phase consisting of cylindrical rods lying parallel to the substrate surface and stacked in a hexagonal pattern is formed. In each rod the cations are aligned along the central axis surrounded by the disordered acyl chains.     

Synthesis and magnetic properties of poly(p‐phthaloyl‐disacetylaceton‐ethylenediimine) metal complexes

Macrocyclic Schiff‐base ligand, bisacetylaceton‐ethylenediimine (BAE) and its transition metal complexes M(BAE) (M = Cu²⁺, Ni²⁺) were synthesized. The complexes having characteristics of aromatic systems and well‐defined one‐dimensional structures, reacted with p‐phthaloyl chloride, to obtain polymer complexes. The complexes were characterized by elemental analysis, inductively coupled plasma (ICP), FT‐IR, and thermal analysis and show good thermal stability. ESR spectra analysis discovered that there are free radicals in the chain of polymers, indicating that a weak magnetic spin‐exchange interaction operates between the metal ions and free radicals. It is found that, as the bridging p‐phthaloyl group is able to propagate the magnetic exchange interaction, the polymer complexes show paramagnetic properties by measurement of temperature dependence of the magnetic property, and obey Curie–Weiss law. Copyright © 2001 John Wiley & Sons, Ltd.     

Redox Polymerization of Methyl Methacrylate in the Fluorous Triphasic System

Fluorous-phase chemistry is currently a topic of considerable interest1-6. Since fluoroustriphasic reactions were first described by the Curran and co-workers7, this triphasicsystem has been widely used for detagging7,8 and phase-vanishing reactions9-11. …     

流动注射—在线分离富集与原子光谱检测联用技术

现代分析化学发展的重要特征之一是分析方法从离线/手动操作向在线/自动操作方向转化。流动注射(FI)作为非均匀和非平衡状态下的溶液处理和微量进样技术,是实现上述转化的有力工具。FI可与不同的分离富集和检测手段结合,具有很强适应性和实用性。在众多联用技术中,FI—在线分离富集与原子光谱检测联用技术特别受到分析化学界的青睐。这种联用不仅可以克服常规离线操作费时、污染环境和试样/试剂消耗大的缺点,而且可大大提高分析效率,显著改善分析方法的灵敏度与选择性,进行多种成分同时检测(对ICP—AES,DCP—AES     

Anomalous behavior of the Nd1.84Ce0.16CuO4 superconductor

The as-prepared electron-doped system Nd_2–xCe_xCuO₄ (where x0.16) is not superconducting. It becomes superconducting only after removal of a minuscule amount of extraneous oxygen (0.02 of O per unit formula). Mössbauer effect studies were carried out for oxygenated and deoxygenated Nd_2–xCe_xCu(⁵⁷Co)O₄ with x=0.14, 0.16, and 0.18. The spectra show evidence of oxygen anions attaching to the probe⁵⁷Co in apical positions, to form 5- and 6-coordinated species. A conventional procedure for deoxygenation brings about little change in the Mössbauer spectra both above and below the optimal superconducting concentration; however, for x=0.16, a dramatic change is observed—a major fraction of the magnetically split five-coordinated species manifests itself as a paramagnetically relaxed doublet upon deoxygenation, which costitutes a microscopic measure of the superconducting volume fraction. This apparently anomalous behavior at x0.16, where the extraneous oxygen is more readily desorbed, may be related to an electronic and/or local structural change in the CuO₂ plane.