Supramolecular isomerism in the hydrogen-bonded network of (5<Emphasis Type="Italic">R</Emphasis>,10<Emphasis Type="Italic">R</Emphasis>)-3,8-dihydroxy-5,10-diethoxy-5,10-dihydrochromeno[5,4,3-<Emphasis Type="Italic">cde</Emphasis>]chromene monohydrate

A new compound (5R, 10R)-3,8-dihydroxy-5,10-diethoxy-5,10-dihydrochromeno[5,4,3-cde]chromene monohydrate was obtained from 3,4-dihydroxybenzaldehyde in aerobic basic aqueous ethanol solution in the presence of manganese chloride and triethylamine and crystallized in orthorhombic P2₁2₁2₁ space group (denoted as 1). When 1 was recrystallized from aqueous methanol, it was transformed to another crystal (2) with the same composition but in P2₁/n space group. The drastic difference in the extensive hydrogen bond network makes 1 a 3D and 2 a 2D infinite supramolecular structure, respectively.     

Lysine peroxycarbamates: free radical-promoted peptide cleavage

Strategies are reported that combine in one step a predictable chemical-based protein digestion with mass spectrometry. Lysine residue amino groups in peptides and proteins are modified by reaction with a peroxycarbonate derived from p-nitrophenol, and tert-butyl hydroperoxide. The peroxycarbonate reacts with lysine residues in peptides and proteins, and the resulting lysine peroxycarbamates undergo homolytic fragmentation under conditions of low-energy collision-induced dissociation (CID). Observed fragmentation of the peptides involves apparent free radical processes including Hofmann-L?ffler-type rearrangements that lead to peptide chain fragmentation. Strategies for directed cleavage of peptides by free radical promoted processes are feasible, and such strategies may well simplify schemes for protein analysis.     

Differential determination of arsenic (III) and total arsenic with L-cysteine as prereductant using a flow injection non-dispersive atomic absorption device

Speciation of arsenic in environmental samples gains increasingly importance, as the toxic effects of arsenic are related to its oxidation state. A method was developed for the determination of trace amounts of arsenic (III) and total arsenic by flow injection hydride generation coupled with an in-house made non-dispersive AAS device. The total arsenic is determined after prereduction of arsenic (V) to arsenic (III) with L-cysteine in a low concentration of hydrochloric, acetic or nitric acid. The conditions for the prereduction, hydride generation and atomization were systematically investigated. A quartz tube temperature of 800 degrees C was found to be optimum in view of peak shape and baseline stability. Pb(II), Ni(II), Fe(III), Cu(II), Ag(I), Al(III), Ga(II), Se(IV), Bi(III) were checked for interfering with the 2 microg/L As(V) signal. A serious signal depression was only observed for Se(IV) and Bi(III) at a 150-fold excess. With the above system, arsenic was determined at a sampling frequency of about 1/min with a detection limit (3sigma) of 0.01 microg/L using a 0.5 mL sample. The reagent blank was 0.001+/-0.0003 absorbance units and the standard deviation of 10 measurements of the 2 microg/l As signal was found to be 1.2%. Results obtained for standard reference materials and water samples are in good agreement with the certified values and those obtained by ICP-MS     

Acetonitrile derivatives as carbonyl synthons. One-pot preparation of diheteroaryl ketones via a strategy of sequential SNAr substitution and oxidation

The anion of 2-aryl acetonitrile derivatives reacted with a variety of heteroaryl chlorides or bromides in an S(N)Ar manifold to afford intermediate anions which were susceptible to oxidation. The addition of sodium peroxide and aqueous NH(4)OAc solution effected oxidation to afford aryl heteroaryl ketones in good yields. Aryl acetonitrile derivatives are thus umpolung-type synthons of the corresponding aryl carbonyl functionality.     

三苄基锡二硫代氨基甲酸酯的合成

三苄基锡二硫代氨基甲酸酯的合成尹汉东马春林＊张如芬（聊城师范学院化学系聊城２５２０５９）关键词三苄基氯化锡，二硫代氨基甲酸盐，合成１９９７－０７－１０收稿，１９９７－０９－０９修回山东省自然科学基金资助项目三烃基锡衍生物是一类具有较强生物活性的有机锡...     

Controlled morphology synthesis of β-FeOOH and the phase transition to Fe2O3

The hexagram and arrayed β-FeOOH nanorods were first synthesized free of surfactants through the solvent-thermal method. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectrum (EDAX) and thermal gravimetric analysis (TGA) were used to characterize the as-prepared products. The TEM and FESEM images showed that hexagram β-FeOOH and arrayed rod-like β-FeOOH with an average diameter of 10-15 nm and an average length of 100 nm (aspect ratio is about 10) were prepared. Electrochemical tests show that these nanorods deliver a large discharge capacity of 277 mA h g⁻¹ versus Li metal at 0.1 mA cm⁻² (voltage at 1.5-4.2 V). Treated the as-synthesized rod-like β-FeOOH by annealing, rhombus hematite was obtained.     

含杂环羧酸基二苄基锡(Ⅳ)配合物的合成与表征

以二苄基二氯化锡和杂环羧酸钠为原料合成了十种新的有机锡配合物(PhCH₂)₂Sn(O₂CR)_nCl_2-n(n=1或2，R=杂环)。用元素分析、IR、 ¹H NMR和TG表征了配合物的组成和结构。     

Self-assembly of electron donor-acceptor dyads into ordered architectures in two and three dimensions: surface patterning and columnar "double cables"

We report the synthesis and characterization of covalent dyads and multiads of electron acceptors (A) and donors (D), with the purpose of exploiting their nanophase separation behavior toward (a) two-dimensional (2D) surface patterning with well-defined integrated arrays of dissimilar molecular electronic features and (b) bulk self-assembly to noncovalent columnar versions of the so-called "double cable" systems, the likes of which could eventually provide side-by-side percolation pathways for electrons and holes in solar cells. Soluble, alkylated hexa-peri-hexabenzocoronenes (HBCs) bearing tethered anthraquinones (AQs) are shown by scanning tunneling microscopy (STM) to self-assemble at the solution-graphite interface into either defect-rich polycrystalline monolayers or extended 2D crystalline domains, depending on the number of tethered AQs. In the bulk, the thermal stability of the room-temperature HBC columnar phase is increased, which is attributed to the desired nanotriphase separation of HBC columns, insulating alkyl sheaths, and AQ units. Homeotropic alignment (columns normal to surfaces), predicted to be ideal for potential exploitation of such "double cables" in photovoltaic devices, is demonstrated.     

Co3{CH3C(NH3)(PO3H)(PO3)}2 {CH3C(NH3)(PO3H)2}2(H2O)4·2H2O: A cobalt 1-aminoethylidenediphosphonate with a layer structure

This paper describes the structure and magnetic properties of a novel cobalt 1-aminoethylidenediphosphonate compound, namely Co₃{CH₃C(NH₃)(PO₃H)(PO₃)}₂{CH₃C(NH₃)(PO₃H)₂}₂(H₂O)₄·2H₂O (1). The structure contains a trimer unit of Co₃{CH₃C(NH₃)(PO₃H)(PO₃)}₂ in which two equivalent phosphonate ligands chelate and bridge the three cobalt ions. Each trimer unit is further linked to its four equivalent neighbors through corner-sharing of CoO₆ octahedra and CPO₃ tetrahedra, forming a two-dimensional layer in the bc-plane which contains 12-membered rings. These layers are connected to each other by extensive hydrogen bonds. Magnetic studies show that weak antiferromagnetic interactions are mediated between the cobalt ions. Crystal data for 1: monoclinic, space group C2/c, a=27.727(4), b=7.1091(11), , β=118.488(3), , Z=2.