Syntheses,Structures and Spectroscopic Studies of Silver(I) Coordination Polymers Bridged by Flexible Bidentate Ligands

The reaction of Ag₂SO₄ and bpp (bpp = 1,3‐bis(4‐pyridyl)propane) in H₂O afforded the complex [Ag₂(bpp)₂(SO₄) · 6.5H₂O·CH₃OH]_n, 1. The IR and TGA have been recorded and the structure has been determined. Crystal data for 1: Space group C₂/c, a = 17.885(4), b = 25.230(6), c = 8.832(2) Å, β = 105.437(4)°. V = 3841(1) ų, Z = 8 with final residuals R1 = 0.0710 and wR2 = 0.1620. The complex shows a three‐dimensional supramoleclar structure constructed with two‐dimensional infinite [Ag₂(bpp)₂]_n sheetlike layers pillared by Ag‐Ag interactions and Ag····O (SO₄) interactions in the solid state.     

Determination of paeoniflorin, ferulic acid and baicalin in the traditional Chinese medicinal preparation Dang-Guei-San by high-performance liquid chromatography

A high-performance liquid chromatographic method for the determination of paeoniflorin, ferulic acid and baicalin in the traditional Chinese medicinal preparation Dang-Guei-San, which contains Paeoniae Radix, Swertiae Herba, Cnidii Rhizoma and Scutellariae Radix, was established. The samples were separated with a Cosmosil 5C₁₈-AR column by gradient elution with 0.03% (v/v) phosphoric acid- acetonitrile (0 min 96:4, 5 min 84:16, 7 min 82:18, 14–30 min 78:22) as the mobile phase at a flow-rate of 1.0 ml/min, with detection at 245 nm. Methylparaben was used as the internal standard and three equations were derived showing linear relationships between the peak- area ratios of marker components (paeoniflorin, ferulic acid and baicalin) to methylparaben and concentration. The recoveries of paeoniflorin, ferulic acid and baicalin were 27.86, 33.89 and 49.31%, respectively. The repeatability (relative standard deviation) was generally less than 5% (n = 5). The effects of various processes such as concentration by reduced-pressure evaporation, freeze-drying and spray-drying were studied and commercial concentrated herbal preparations containing Paeoniae Radix, Swertiae Herba, Cnidii Rhizoma and Scutellariae Radix were also analysed.     

Photoinduced 1,4-additions of indoles to enones

[reaction: see text] A photoinduced procedure for the 1,4-addition of indoles to enones is described. This reaction occurs with modest to excellent yield for cyclic and some acyclic enones. This reaction is experimentally simple, requiring only irradiation (UVA lamps, ca. 350 nm) of the reagents in a CH2Cl2 solution at room temperature, and avoids the necessity to use a Lewis acid. An important solvent effect was noticed, with CH2Cl2 and CHCl3 being the optimal solvents. Various substituents are tolerated on the indole moiety and an electronic trend was noticed, as electron-withdrawing groups can suppress this reaction. A mechanism involving single electron transfer between the enone triplet excited state and the indole is proposed and accounts for all experimental observations.     

Synthesis and Structures of Infinite Coordination Polymers from 1,3‐Bis(4‐pyridyl)propane Ligand and Zinc Salts

The reaction of Zn(NO₃)₂‐6H₂O, NH₄SCN and bpp (bpp = 1,3‐bis(4‐pyridyl)propane) in CH₃OH afforded the complex [Zn(NCS)₂(bpp)]_n, 1 , while the reaction of Zn(ClO₄)₂‐6H₂O and bpp in CH₃OH afforded the complex [Zn(ClO₄)₂(bpp)₂]_n, 2 . Both complexes have been characterized by spectroscopic methods and their structures have been determined by X‐ray crystallography. Crystal data for 1 : Orthorhombic, space group P2₁2₁2, a= 12.857(6), b = 14.822(7), c = 4.820(2) Å, β = 90°, V = 918.5(8) ų, Z = 2 with final residuals R1 = 0.0747 and wR2 = 0.1657. Crystal data for 2 : Tetragonal, space group I4/mcm, a = 11.612(1), b = 11.612(1), c = 23.247(9) Å, β = 90°, V = 3135(1) ų, Z = 4 with final residuals R1 = 0.0523 and wR2 = 0.1064. The coordination polymers display a variety of structural architectures, ranging from zigzag chains ( 1 ) and one‐dimensional channel‐type architectures ( 2 ). The effects of the orientation of the nitrogen atom in the pyridine rings on the resultant structures are discussed.     

Syntheses and Structures of Zinc(II) Co‐Ordination Polymers Bridged by Flexible Bidentate Nitrogen Ligands

The reaction of Zn(NO₃)₂·6H₂O and bpp (bpp = 1,3‐Bis(4‐pyridyl)pronpane) in CH₃OH afforded the complex [Zn(bpp)(NO₃)₂]_n, 1 . The IR has been recorded and the structure has been determined. Crystal data for 1: Space group P2(1)/n, a = 11.749(1), b = 11.413(1), c = 11.942(1) Å, β = 96.06(6)°. V = 1592.5(3) ų, Z = 4 with final residuals R1 = 0.0484 and wR2 = 0.0984. The complexes show supramolecular structure in the solid state by intermolecular hydrogen bonding interaction.     

An improvement on the adhesion‐strength of laminated ultra‐high‐molecular‐weight polyethylene fabrics: surface‐etching/modification using highly effective helium/oxygen/nitrogen plasma treatment

In this study, helium/oxygen/nitrogen (He/O₂/N₂)‐plasma was used to etch/modify the surface of ultra‐high‐molecular‐weight polyethylene (UHMWPE) fiber. After coated with polyurethane (PU), the plasma treated UHMWPE fabrics were laminated. It was found that the values of peeling strength between the laminated UHMWPE fabrics treated with He/O₂/N₂‐plasma were significantly higher (3–4 times) than that between pristine fabrics. The hydrophilic property and the value of the surface roughness of the UHMWPE fibers increased significantly after treated with He/O₂/N₂‐plasma. The mechanism of the oxidation/degradation of the polymers on the surface of the UHMWPE fiber during He/O₂/N₂‐plasma treatment was suggested. In addition, it was found that the higher content of functional groups (carbonyl, aldehyde, and carboxylic acid) on fiber surface and the higher value of surface roughness of the UHMWPE fiber treated with He/O₂/N₂‐plasma could significantly improve the adhesion‐strength of the laminated UHMWPE fabric. Especially, the micro‐aperture on the surface of UHMWPE fiber caused by the strenuous etching of He/O₂/N₂‐plasma treatment was also an important factor on improving the adhesion‐strength between the laminated UHMWPE fabrics. Copyright © 2010 John Wiley & Sons, Ltd.     

Synthesis, structural characterization and magnetic properties of RE2MgGe2 (RE=rare-earth metal)

A series of rare-earth metal–magnesium–germanides RE₂MgGe₂ (RE=Y, Nd, Sm, Gd–Tm, Lu) has been synthesized by reactions of the corresponding elements at high temperature. Their structures have been established by single-crystal and powder X-ray diffraction and belong to the Mo₂FeB₂ structure type (space group P4/mbm (No. 127), Z=2; Pearson symbol tP10). Temperature dependent DC magnetization measurements indicate Curie–Weiss paramagnetism in the high-temperature regime for all members of the family, excluding Y₂MgGe₂, Sm₂MgGe₂, and Lu₂MgGe₂. At cryogenic temperatures (ca. 60 K and below), most RE₂MgGe₂ phases enter into an antiferromagnetic ground-state, except for Er₂MgGe₂ and Tm₂MgGe₂, which do not undergo magnetic ordering down to 5 K. The structural variations as a function of the decreasing size of the rare-earth metals, following the lanthanide contraction, and the changes in the magnetic properties across the series are discussed as well.