Structure and Thermal Stability of a Novel 2‐D Layered Copper(II) Coordination Polymer with the Bidentate Ligand 1, 2, 4‐Triazol‐5‐one

Single crystals of {[Cu(TO)₂(H₂O)₂](NO₃)₂}_n (TO: 1, 2, 4‐triazol‐5‐one) were grown by slow evaporation from aqueous solution. It crystallizes in the orthorhombic space group Pbca, with a = 7.082(1), b = 10.285(1), c = 17.911(3)Å, V = 1304.6(3)ų, Z = 4. The Cu^II distorted octahedra are bridged by bidentate TO ligands into infinite 2‐D interlaced rhombic grid‐like network planes, {[Cu(TO)₂(H₂O)₂]²⁺}_n. Hydrogen bonds, electrostatic interactions, and weak van der Waals' forces assemble these planes and the NO₃^— anions to a layered structure. The title compound decomposes at 153.4 °C to the final products, Cu(CN)₂ and CuO.     

High-performance liquid chromatography of tyrosine-containing peptides by pre-column derivatization involving formylation followed by fluorescence reaction with 1,2-diamino-4,5-dimethoxybenzene

A pre-column fluorescence derivatization method is described for the high-performance liquid chromatographic determination of tyrosine-containing peptides. A tyrosyl residue in the peptide is first formylated in an alkaline medium in the presence of chloroform, and the resulting aldehyde is then converted into a fluorescent derivative by reaction with 1,2-diamino-4,5-dimethoxybenzene. The derivative is separated on a reversed-phase column (LiChrosorb RP-18) by isocratic elution with an aqueous acetonitrile-containing potassium chloride-hydrochloric acid buffer (pH 2.2) and sodium 1-hexanesulphonate. The method is selective and fairly sensitive; the lower limits of detection for the tyrosine-containing peptides tested are in the range 3.4-26.2 pmol in a 100-microliter injection volume.     

Crystal structure of a methyl(methoxy)carbene complex of nickel(II), trans-[Ni(C6Cl5)(PMe2Ph)2{C(OMe)Me}]BF4

The structure of a nickel(II) complex, trans-[Ni(C₆Cl₅)(PMe₂Ph)₂{C(OMe)Me}]BF₄, containing the simplest alkyl(alkoxy)carbene ligand has been determined by X-ray crystallography (R = 0.091). The geometry around the nickel atom is square-planar. The comparatively short NiC(1) bond length of 1.843(10) Å showed the presence of π-bonding in the nickel-carbene bond.     

Influence of drying procedure on the mesoporosity and surface fractal dimensions of silica xerogels prepared with different agitation methods

Silica xerogels were prepared by thermal drying wet gels in an electric oven (70 degrees C) after certain duration of ambient drying, and the relevant effect is investigated on the mesopore structures and surface fractal dimensions of the resultant xerogels. The silica gels were derived from a hydrochloric acid-catalyzed TEOS (tetraethylorthaosilicate) system, and both magnetic stirring and ultrasonic vibration were adopted during sol preparation. The percentage mesoporosity and surface fractal dimensions are evaluated using image analysis methods, based on FE-SEM (field emission gun-scanning electron microscopy) images. The results show that the mesoporosity of the resultant xerogels decreases with the duration of ambient drying for samples prepared using magnetic stirring and low-intensity ultrasonic vibration, while samples subjected to high-intensity ultrasound show a somewhat reverse trend. Samples prepared with magnetic stirring have almost constant surface fractal dimensions (nearly 3), irrespective of the ambient drying before thermal drying. The surface fractal dimensions of samples prepared using ultrasound increase with the duration of ambient drying.     

Selective Transport of Alkali—Metal Cations through Liquid Membranes by Non—Cyclic Carriers

The emission spectra of a series of naphthalene end-labeled oligo-oxyethylene(N-Pn-N) and their facilitated transport of cations across liquid membranes have been investigated.Alkali-metal cations enhance or inhibit the intramolecular excimer formation of N-Pn-N remarkably,suggesting that the polyether chain of N-Pn-N in solution complexes with the cations,and the orientation of the terminal chromophores depends on the cation size and the length of the polyether chain. These compounds are able to act as carriers to facilitate transport of alkali-metal cations through organic liquid membranes.The transport efficiencies are comparable with those of cyclic carriers such as crown ethers,and show remarkable selectivity.     

Studies of the reaction of dimethyltin dichloride with mercaptoacetic acid in the presence of amines and crystal structure of [(n-Pr)3NH][Me2Sn(μ-SCH2COO)Cl]

A series of new five-coordinated ionic organotin(IV) complexes with general formula [Q][Me₂Sn(μ²-SCH₂COO)Cl](Q = diethylammonium, triethylammonium, di-i-propylammonium, tripropylammonium, tri-n-butylammonium, pyrimidium, 3-picolinium, methylphenylammonium, dimethylphenylammonium) were synthesized by the reaction of mercaptoacetic acid with dimethyltin dichloride in the presence of an organic base. These complexes have been characterized by elemental analyses, IR and ¹H NMR spectroscopies. The crystal structure of [(n-Pr)₃NH][Me₂Sn(μ²-SCH₂COO)Cl] was determined by X-ray crystallography. The structure consists of an anion part, and a tri-n-propylammonium cation part as a counterion. The tin atom has a distorted cis-tbp geometry with two carbon and one sulfur atoms occupying the equatorial positions and the O atom and Cl atom occupying the axial positions. The organotin anion and its counterion are connected through a hydrogen bond between the N atom in the ammonium and the O atom of the carbonyl group with a N-O length of 2.766 Å.     

Syntheses and Crystal Structures of Two Metal Succinates Modified by Bipyridines

Two new metal succinates modified by rigid bipyridines, Cd(4, 4′‐bpy)(C₄H₄O₄)·1/4H₂O ( 1 ) and Cu(2, 2′‐bpy)(C₄H₄O₄)_0.5(NO₃)(H₂O) ( 2 ) (bpy = bipyridine), have been synthesized by hydrothermal reactions and structurally determined. Complex 1 crystallizes in the orthorhombic space group Cmca with the cell parameters a = 11.696(2), b = 15.554(2), c = 15.874(3) Å, α = β = γ = 90.00°, V = 2888(3) ų, Z = 8. Complex 2 crystallizes in the triclinic space group with a = 7.077(1), b = 9.838(2), c = 10.461(2) Å, α = 71.941(3)°, β = 73.078(3)°, γ = 74.502(3)°, V = 649.8(2) ų, Z = 2. In complex 1 , a 2‐D network was formed by Cd‐succinato bonding. The 2‐D networks are pillared by 4, 4′‐bpy ligands, forming a 3‐D grid framework. The 2‐fold interpenetration of the resulting 3‐D frameworks completes the molecular structure. In complex 2 , the Cu^II atom adopts a distorted octahedral in which the Cu^II atoms are bridged by two H₂O molecules into an infinite zigzag chain, [Cu₂(H₂O)₂(C₄H₄O₄)]_n. The neighboring chains are further linked by π‐π stacking interactions into a 2‐D network, and the interlayer hydrogen bonds lead to the final 3‐D crystal structure.     

A New Activation Method for Electroless Metal Plating：Palladium Laden via Bonding with Self—Assembly Monolayers

A new activation method has been developed for electroless copper plating on silicon wafer based on palladium chemisorption on SAMs of APTS without SnCl2 sensitization and roughening condition.A closely packed electroless copper film with strong adhesion is successfully formed by AFM observation.XPS study indicates that palladium chemisorption occurred via palladium chloride bonding to the pendant amino group of the SAMs.     

掺溴聚-4-甲基-1-戊烯的合成研究

 液溴与聚-4-甲基-1-戊烯（PMP）的四氯化碳溶液反应，在光照条件下得到溴代PMP，通过红外与元素分析确证了其结构。并通过热重分析对其性能进行了初步的研究。研究发现，在光照条件下溴原子很容易与PMP中叔丁基上的氢原子发生取代反应，得到化学掺杂溴原子的聚合物。该聚合物在150℃以下比较稳定，在150℃以上就会失去HBr。采用此种方法，可得到掺杂均匀的低密度材料。     

铁掺杂PMP泡沫制备工艺研究

 以聚-4-甲基-1-戊烯为泡沫骨架，二茂铁为掺杂材料，通过热诱导倒相技术制备出铁掺杂聚合物泡沫。掺杂泡沫的实际密度均高于理论密度，且沿轴向从上至下逐渐增大。在理论密度不变的情况下，掺杂泡沫实际密度随掺杂元素原子百分含量的升高而呈降低趋势。与PMP泡沫相比，掺杂泡沫的孔洞直径分布变宽且网络骨架尺寸有变大的趋势。