Ti/Ru0.1Ti0.1Sn0.8O2电极电容性能研究

低温热分解法制备Ti/Ru0.1Ti0.1Sn0.8O2.XRD表征该样品结构特性,循环伏安和恒流充放电测定电极性能.结果表明,Ti/Ru0.1Ti0.1Sn0.8O2物相属细小的金红石相,在20 mV/s扫速下该电极比电容达933F/g.1000次充放电循环后,比电容衰减23.6﹪,显示良好的循环稳定性和可逆性.     

Synthesis and characterization of semicarbazone metal complexes of Sn(IV) and Zr(IV)

Three semicarbazonyl ligands were synthesized and used to form six novel organometallic complexes with Ph2SnCl2 and Cp2ZrCl2. All these complexes were characterized by IR,1H NMR,MS and elemental analysis.     

六氟磷酸二(2,2'-联吡啶)·(4,4'-二甲基-2,2'-联吡啶) 合钌(Ⅱ)的二维核磁共振谱分析

用一维NMR方法研究了电化学发光物质六氟磷酸二(2,2'-联吡啶)·(4,4'-二甲基-2,2'-联吡啶)合钌(Ⅱ)的立体结构,借助二维1H-1H COSY和1H-13C COSY实验技术对其氢谱和碳谱进行了完全的归属,并给出了其氢谱和碳谱的化学位移值.     

趋磁细菌(MTB)吸附Pd2+的实验研究

以趋磁细菌MTB作为吸附剂,吸附溶液中的Pd2 ,对影响吸附的因素进行了实验研究。结果显示,MTB对溶液中Pd2 的最佳吸附条件为:pH=1~5,菌体浓度在6g/L左右,Pd2 初始浓度为20mg/L~80mg/L,室温条件下吸附30min。吸附过程遵循准一级动力学方程和Langmuir等温吸附模型。     

Structures of Mn(II) complexes of bis(2-pyridylmethyl)amine (bpa) and (2-pyridylmethyl)(6-methyl-2-pyridylmethyl)amine (Mebpa): geometric isomerism in the solid state

The crystal structures of [Mn(bpa)₂](ClO₄)₂ (1), [bpa?=?bis(2-pyridylmethyl)amine], and Mn(6-Mebpa)₂(ClO₄)₂ (2), [6-Mebpa?=?(6-methyl-2-pyridylmethyl)(2-pyridylmethyl)amine] have been determined. In 1, two facial [Mn(bpa)₂]²⁺ isomers are observed in the same unit cell, one with C _i (1a) and the other with C₂ (1b) symmetries. In 2, only the isomer with C₂ symmetry is observed. The structure of [Mn(bpa)₂]²⁺ with only C₂ symmetry has been reported previously (Inorg. Chem., 31, 4611 (1992)). The bond length order Mn–N_amine?>?Mn–N_pyridyl, observed in the C₂ and the C _i isomers in the crystals of 1, is the reverse of the order observed in the structure of [Mn(bpa)₂](ClO₄)₂ which contains only the C₂ isomer in the unit cell. The structure of 2 in which only the C₂ isomer is found, also shows the bond length order Mn–N_pyridyl?>?Mn–N_amine. In cyclic voltammetric experiments in acetonitrile solutions, 1 and 2 show irreversible anodic peaks at E _p?=?1.60 and 1.90?V respectively, (vs. Ag/AgCl), assigned to the oxidation of Mn(II) to Mn(III). The substantially higher oxidation potential of 2 is attributable to a higher rearrangement energy in complex 2 due to the steric effect of the methyl substituent.     

Bis(diphenylphosphano)alkan- und 1-(Diphenylphosphano)-2-(2-pyridino)ethan-N-Arylsulfinylamin-Nickel(0)-Komplexe

Bis(diphenylphosphano)alkane- and 1-Diphenylphosphano-2-(2-pyridino)ethane-N-arylsulfinylamine Nickel(0) Complexes Synthesis and properties of the bis(diphenylphosphano)alkane-N-phenyl-sulfinylamine-nickel(0) complexes [Ni{Ph₂P(CH₂)_nPPh₂}(PhNSO)] (n = 2 dppe, n = 3 dppp, n = 4 dppb) as well as of the 1-(diphenylphosphano)-2-(2-pyridino)ethane nickel(0) complexes [Ni(dpppe)₂], [Ni(dpppe)(p-TolNSO)] and [Ni(dpppe)(PPh₃)₂] are described. These compounds have been characterized by i. r. and ³¹P n.m.r. spectroscopy. The N-arylsulfinylamine ligands are η²-(N, S)-side on coordinated.     

(±)-耳壳藻内酯的全合成研究(Ⅱ)

以2,6,6-三甲基环己-2-烯-1,4-二酮为原料, 经选择性羰基保护、Wittig反应、脱保护基、 腈基水解和还原等5步反应合成了目标化合物, 总产率可达6.0%.     

2-(Phenyltelluromethyl)tetrahydrofuran (L) and 2-(2-{4-methoxyphenyl}telluroethyl)-1,3- dioxolane (L) and their palladium(II) and platinum(II) complexes

The nucleophile [ArTe⁻] generated in situ borohydride solution of Ar₂Te₂, reacts with 2-(chloromethyl) tetrahydrofuran and 2-(2-bromoethyl)-1,3-dioxolane resulting in L¹ and L², respectively. The complexes of palladium(II) and platinum(II) with L¹/L² having stoichiometries [MCl₂·L₂], [ML₂](ClO₄)₂, [(DPPE)ML₂](ClO)₄)₂, [(PPh₃)₂ML₂](ClO₄)₂ and [(phen)ML₂](ClO₄)₂ (where L = L¹/L² DPPE = Ph₂PC H₂CH₂PPh₂, PHEN = 1,10-phenanthroline and M = Pd/Pt) have been synthesized. IR, ¹H, ¹²⁵Te{¹H} and ³¹P{¹H} NMR and UV-vis spectral data of these species in conjunction with their molar conductance and molecular weight data have been used to authenticate the new species. In all complexes (1–20) the ligands L¹ and L² are coordinated through tellurium and in the complexes of formula [ML₂](ClO₄)₂ (M = Pd, Pt) the ligand is bidentate with the oxygen atom used in complexation. In solution, complexes PtCl₂L₂ exist as a mixture of cis and trans isomers whereas only the trans isomer was observed for the palladium analogues. The [(phen)PdL₂](ClO₄)₂(Q) quenches ¹O₂ readily. The plot of log [Q] vs time is linear. Mechanism compatible with the experimental observations is proposed.     

Synthesis and Crystal Structure of 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

AN UNUSUAL RUTHENIUM(II) COMPLEX OF 2-(2-PYRIDYL)BENZOTHIAZOLE

Abstract

The ligand 2-(2-pyridyl)benzothiazole (L) can act both as an N-N and an N-S chelating donor. The latter coordination mode is expected to be preferred when it is involved in coordination to Ru(II) which is a soft acceptor centre However, in the title compound, chlorobis(acetonitrile)triphenylphosphino-2-(2-pyridyl)benzothiazole-N,N-ruthenium(II) chlride, [Ru(L)(PPh₃(CH₃CN)₂Cl]Cl, the ligand acts in N,N-bidentate manner and the Ru(II) ion is found to be present in an N₄PCl coordination environment. PPh₃ and Cl are trans to each other and the two CH₃CN ligands occupy cis positions facing the NN donor atoms of ligand L.     

Synthesis and Characterization of New Schiff Bases 2-(2-(2-(Aryl)Methyleneamino)Phenylthio) Ethylthio)-N-((aryl)Methylene)Benzeneamine

A series of Schiff bases containing four to six coordination sites N₂S₂ X₂(X = O,N) 2-(2-(2-(aryl)methyleneamino)phenylthio)ethylthio)-N-((aryl)methylene)benzeneamine (2c–f) were prepared from the reaction of 1,2-di(2-aminophenylthio)ethane (1) with aromatic aldehydes. All compounds were characterized by means IR, mass, ¹H and ¹³C NMR spectroscopy, and elemental analysis, and in the case of 2b with a single crystal X-ray diffraction. The X-ray crystal structure of 2b showed that the resonance occurs between aromatic rings, through the C=N bonds of the molecule.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

2-(2-喹啉偶氮)-1,5-苯二酚光度法测定钢铁样品中镍

合成了新试剂 2 (2 喹啉偶氮 ) 1,5 苯二酚 (QADHB) ,并研究了其与镍的显色反应 ,在pH 9.0的氯化铵 氨水缓冲介质中 ,CTMAB存在下 ,QADHB与镍反应生成 2∶1稳定络合物 ,λmax为 5 90nm ,ε为 1.0 5× 10 5L·mol- 1·cm- 1。镍含量在 0～ 10 μg/ 2 5ml内符合比耳定律 ,方法用于钢铁样品中镍含量的测定 ,结果满意。     

Solvent effects on the copolymerization kinetics of ionic (AMPS) and non-ionic (HEAm) acrylamide derivatives

The free-radical copolymerization of two N-substituted acrylamide monomers, the ionic AMPS (2-acrylamido-2-methyl-1-propanesulfonic acid) and the non-ionic HEAm (2-hydroxyethylacrylamide) is presented. Despite bearing similar polymerizable functionalities, HEAm is more reactive toward free-radical addition than AMPS in water. In a mixed aqueous solvent containing salt, (0.5 M LiNO₃, 50 wt%) and ethanol (50 wt%), the reactivity ratio was found to be r_AMPS = 0.53 and r_HEAm = 1.06 indicating that copolymers with a nearly random distribution of sulfonic and hydroxy functionalities can be prepared.     

Crystallographic report: Bis(tripyridyldiamine)zinc(II) tetrabromozincate(II) hydrate

The zinc(II) atom in the complex cation of [Zn(tpda)₂][ZnBr₄]·H₂O is octahedrally coordinated, whereas the zinc(II) atom in the anion is tetrahedrally coordinated. The cations and the anions are connected by hydrogen bonds, affording a two‐dimensional network. Copyright © 2005 John Wiley & Sons, Ltd.     

两种新型salen金属络合物WO2(salen)和MoO2-(salen)的合成

新合成了两种过渡金属salen络合物WO2(salen)和MoO2(salen).通过和已经有的文献比较,发现这两种络合物的分子结构是少见的β-cis构型.     

Synthesis and Structural Characterization of Bis(2,2'-bpy)bis(azide)cobalt(III) nitrate dihydrate

The title complex [CoIII(2, 2?-bpy)2(N3)2]@NO3@2H2O was obtained by an auto-oxidization reaction of cobalt nitrate with 2, 2?-bpy and sodium azide in aqueous solution at room temperature, and violet single crystals were prepared in ethanol solution. The structure was determined by X-ray crystallography. The crystal is of triclinic, space group P ī with a = 8.285(4), b = 11.990(8), c = 12.596(7) ?, ( = 86.630(3), ( = 86.280(5), ( = 71.130(10)°, C20H20CoN11O5, Mr = 553.40, Z = 2, V = 1180.6(12) ?3, F(000) = 568, Dc = 1.557 g/cm3, ( = 0.784 mm-1, R = 0.0403 and wR = 0.1008. The title complex consists of a [CoⅢ(2, 2?-bpy)2(N3)2]+ cation, a NO3- anion and two lattice water molecules. The center CoⅢ ion coordinated by two chelating 2, 2?-bpy ligands and two terminal azide groups with a CoN6 coordination environment exhibits a distorted octahedral geometry.     

2-(2-Thiazolylazo)-p-cresol(TAC) as a Reagent for the Spectrophotometric Determination of Lead(II)

Abstract

The reaction between lead(II) and 2-(2-Thiazolylazo)-p-Cresol(TAC) in the presence of TERGITOL NPX (4 mg/ml) at an apparent pH 9.0–10.0 results in an intensely colored complex which is stable for at least 4 hr.

The composition of the complex is 1:2 cation: TAC and the log of the formation constant is 11.92 ± 0. 40. Beer's law is obeyed up to 6.0μg.ml^?1 of lead(II) at 650nm.

The apparent molar absorptivity at 650 nm is 2.07 × 10⁴ 1. mole^?1.cm^?1 and the detection limit was obtained as 10.0 ng.ml^?1 of lead(II).

The method is applied to determination of lead(II) in copper-base alloy.     

配合物Cu(phen)2 (dca)2的合成及晶体结构

合成了配合物Cu(phen)2 (dca)2(phen=C12H8N2为1,10-邻菲啰啉,dca-为二氰基氨基阴离子),用IR对其结构进行了初步表征,并测定了配合物的晶体结构.该晶体属单斜晶系,空间群为P21/c;晶胞参数a=0.8869(2)nm,b=1.4691(2)nm,c=1.9298(2)nm,β=100.90(1)°;V=2.4691(8)nm3,Z=4,F(000)=1132.00,Dc=1.496g/cm3,R=0.051,RW=0.068.中心铜(Ⅱ)离子分别与两个phen中的四个N原子和两个dca-的两个N原子配位,形成六配位的变形八面体结构.     

Mg(NTf2)2催化Friedl(a)nder缩合反应合成喹啉衍生物

以Mg(NTf2)2为催化剂,在室温由2-氨基芳基酮和α-亚甲基酮通过Friedl(a)nder缩合反应合成了喹啉衍生物.该法操作简便,反应条件温和,产率高,反应时间短.     

配合物Ru(dcbpy)(phen)2(PF6)2的2D-NMR分析

用一维ＮＭＲ方法研究了新型电化学发光探针Ｒｕ（ｄｃｂｐｙ）（ｐｈｅｎ）２（ＰＦ６）２的立体结构,借助二维＾１Ｈ－＾１Ｈ ＣＯＳＹ和＾１Ｈ－＾１３Ｃ ＣＯＳＹ实验对其氢谱和碳谱进行了完全的归属,并给出了其氢谱和碳谱的化学位移值。