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971.
The hydrothermal reaction of YbCl(3) small middle dot6H(2)O with 1,2,4,5-benzenetetracarboxylic dianhydride resulted in [[Yb((b)btec)(1/4)((d)btec)(3/6)(H(2)O)(2)](4).6H(2)O](n)() (1) (H(4)btec = 1,2,4,5-benzenetetracarboxylic acid), and the solvothermal reaction of Er(NO(3))(3) small middle dot6H(2)O or TbCl(3).6H(2)O with 1,2,4,5-benzenetetracarboxylic dianhydride in H(2)O/acetic acid gave rise to [[Er(2)((c)btec)(2/4)((e)btec)(2/4)((f)btec)(2/4)(H(2)O)(4)].4H(2)O](n)() (2) and [[Tb(H(2)btec)(2/4)((f)btec)(3/6)(H(2)O)].2H(2)O](n)() (3), respectively. Complex 1 crystallizes in monoclinic space group C2/m with a = 20.8119(5) A, b = 17.6174(1) A, c = 5.7252(2) A, beta = 92.324(1) degrees, and Z = 1. 1 possesses a three-dimensional framework consisting of eight-coordinate ytterbium centers and two kinds of channels along the c axis. Complex 2 crystallizes in triclinic space group P with a = 9.6739(5) A, b = 11.0039(5) A, c = 11.5523 A, alpha = 104.8330(10) degrees, beta = 91.0000(10) degrees, gamma = 114.2570(10) degrees, and Z = 2. 2 has a three-dimensional framework comprising both eight- and nine-coordinate erbium centers and channels along the a axis. Complex 3 crystallizes in monoclinic space group P2(1)/n with a = 10.7246(12) A, b = 7.1693(9) A, c = 17.158(2) A, beta = 97.109(2) degrees, and Z = 4. 3 shows a three-dimensional framework containing nine-coordinate terbium centers and channels along the b axis. Uncoordinated water molecules occupy the channels in the three complexes. TGA and XRPD were determined for the three complexes, and the results illustrate that the framework of 1 is retained upon removal of uncoordinated and coordinated water molecules. 相似文献
972.
Oleg V. Mikhailov Marina A. Kazymova Tatyana A. Shumilova Galina A. Chmutova Svetlana E. Solovieva 《Transition Metal Chemistry》2005,30(3):299-304
The complexing process proceeding in the NiII–thiocarbohydrazide (H2N–H–NC(=S)–NH–NH2)–propanone triple system in EtOH solution and nickel(II)hexacyanoferrate(II) gelatin-immobilized matrix has been studied. It has been found that in the first case, template synthesis leading, as a minimum, to formation of three coordination compounds of NiII with (N,N,S,S)-donor tetradentate ligands having NiL1, NiL2 and NiL3compositions where L1 is 4,6,6-trimethyl-2,3,7,8-tetraazanonen-3-di(thiohydrazide)-1,9, L2 is 4,6,6,12-tetrametyl-1,9-dithio-2,3,7,8,10,11-hexaazatridekadien-3,11-hydrazide-1 and L3 is 2,8,10,10,16-pentamethyl-5,13-dithio-3,4,6,7,11,12,14,15-octaazaheptadekatrien-2,7,15 is observed, whereas in the gelatin-immobilized matrix, a complexing process in the system considered does not occur. 相似文献
973.
以互通多孔碳(IPC)为载体,水热条件下在碳表面原位反应生成纳米结构的二氧化锰(MnO2),制备互通多孔碳/二氧化锰纳米(IPC/MnO2)复合电极材料. 采用扫描电镜(SEM),透射电镜(TEM),X射线衍射(XRD),热重分析(TGA)对其结构进行表征;采用循环伏安法、恒流充放电和交流阻抗对其电化学性能进行研究. 结果表明:生成的MnO2均匀地负载在碳的表面,形成多层次结构,并且随着温度的升高IPC表面负载的MnO2由纳米颗粒变为纳米片状结构;MnO2纳米片具有典型的K-Birnessite 型晶体结构;复合物中MnO2的含量约为34%(w). 在100 ℃制备的IPC/MnO2复合材料在三电极系统中最高比电容达到了411 F·g-1;随着反应温度的升高,比容量先增长后基本保持不变. 以IPC/MnO2为正极,活性炭(AC)为负极,1 mol·L-1 Na2SO4溶液为电解液组装成IPC/MnO2//AC 混合超级电容器,发现IPC/MnO2电极的电容器其电位窗口从1 V扩展到1.8 V,容量可达86F·g-1,且表现出良好的电容特性和大电流放电性能. 相似文献
974.
A metal-organic coordination compound formulated as [Cd(MDPPz)(BDC)(H2O)]n 1 (MDPPz=11-methyldipyrido[3,2-a:2',3'-c]phenazine,BDC=1,4-benzenedicarboxylate) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system,space group C2/c,with a=30.673(8),b=9.623(3),c=20.784(6) ,β=98.646(3)o,V=6065(3)3,C27H17CdN4O5,Mr=589.85,Dc=1.292 g/cm3,μ(MoKα)=0.757 mm-1,F(000)=2360,Z=8,the final R=0.0381 and wR=0.0855 for 4191 observed reflections (I>2σ(I)). 1 exhibits blue fluorescence property at room temperature. 相似文献
975.
Yuan Ruo Cao ShuRui Chai YaQin Gao FengXian Zhao Qing Tang MingYu Tong ZhongQiang Xie Yi 《中国科学B辑(英文版)》2007,50(5):620-628
Alternate adsorption of positively charged colloid-Au nanoparticles (nano-Au⊕) and negatively charged hemoglobin (Hb) on L-cysteine (L-cys) modified gold electrode resulted in the assembly of {Hb/nano-Au⊕}n layer-by-layer films/L-cys modified gold electrode. The nano-Au⊕ was characterized by transmission electron micrograph (TEM) and microelectrophoresis. The modified electrode interface morphology was characterized by electrochemical impedance spectroscopy (EIS), atomic force mi- croscopy (AFM), cyclic voltammograms (CV) and chronoamperometry. Direct electron transfer between hemoglobin and gold electrodes was studied, and the apparent Michaelis-Menten constant ( km app) of the modified electrode was evaluated to be 0.10 mmol·L?1. Moreover, the higher activity of proteins in the nano-Au⊕ films could be retained compared with the electropolymerization membrane, since the pro- teins in nano-Au⊕ films retained their near-native structure. Direct electron transfer between hemoglo- bin and electrode and electrochemically catalyzed reduction of hydrogen peroxide on a modified elec- trode was studied, and the linear range was from 2.1×10-8 to 1.2 ×10?3 mol·L-1 (r = 0.994) with a detection limit of 1.1×10-8 mol·L-1 H2O2. 相似文献
976.
977.
An easily prepared and highly efficient monodentate phosphoramidite ligand derived from BINOL, (S)-2,2'-O,O-(1,1'-binaphthyl)-dioxo-N,N-diethylphospholidine, was examined in the hydrogenation of both enamides and alpha-dehydroamino acid derivatives. The catalyst provided remarkably high enantioselectivities (up to 99.6% ee for enamides and >99.9% ee for alpha-dehydroamino acid derivatives). 相似文献
978.
The biological effects of aluminium have received much attention in recent years. Speciation of Al is of basic relevance as it concerns its reactivity and bioavailability. A differential pulse voltammetry (DPV) procedure is proposed for speciation analysis of Al(III) in natural waters and biological fluids using six catechols (L-dopa, dopamine, epinephrine, norepinephrine, caffeic acid and o-benzenediol) as electroactive ligands. The decrease of the DPV anodic peak current for each catechol ligand is linear with the increase of Al concentration. This speciation analysis idea is based on the measurement of the complexation capacity, namely, different affinities of Al(III) for catechols and organic ligands under two pH conditions. The labile monomeric Al fraction (mainly inorganic aluminium) is determined at pH 4.6, while the total monomeric Al fraction is determined at pH 8.5. The principle for Al(III) speciation analysis by an electrochemical method is discussed. This sensitive and simple fractionation method is successfully applied to the speciation analysis of Al in natural waters and the results agree well with those of Driscoll's method. The speciation analysis of Al in biological fluids is also explored and the results are compared with those obtained by ultrafiltration and dialysis. Compared with other speciation protocols the electrochemical method possesses some remarkable advantages: rapidity, high sensitivity, cheap instrumentation and a simple operation procedure. 相似文献
979.
本文建立了2,2’-二羟基联苯(DHP)和4-羟基联苯(HP)的胶束增敏导数-可变角同步荧光同时分析方法,可变角同步扫描所得到的DHP和HP的谱峰位置均对应于常规光谱中的最佳激发-发射位置,经二阶求导后,消除分析谱带干扰,所得的二阶导数-可变角同步光谱即可用于两物质的同时测定,方法快速灵敏,DHP测定范围为0.05~0.5mg/L,HP测定范围为0.07~2mg/L。 相似文献
980.
Synthesis,photophysical and electrochemical studies of di-2-pyridyl ketone complexes of rhodium(III)
Huang Wen Liang Lee Jen Rong Shi Sheu Yuan Tsai Cheng Yuan 《Transition Metal Chemistry》2003,28(4):381-387
Complexes of rhodium(III) with di-2-pyridyl ketone (dpk), Rh(dpk)(MeCN)Cl3
(1) and cis-[Rh(dpk)2Cl2]+
(2), have been successfully prepared and characterized. At low temperature (77 K), complex (2) in EtOH/MeOH (4:1, v/v) shows a broad, symmetric and structureless red emission with a microsecond lifetime and, hence, is assigned as the dd* phosphorescence. Electrochemical data, including cyclic voltammetry, normal pulse voltammetry, triple pulse voltammetry and controlled potential electrolysis, have been obtained for the two dpk complexes of rhodium(III) in MeCN. On the basis of analysis of the electrochemical (1,2) and luminescence data (2), electron transfer mechanisms are proposed. For complex (1), two reduction processes occur at the metal-localized orbitals with elimination of chlorides during the first reduction step. This is followed by a one-electron reduction at the metal. For complex (2), three electrons are transferred to the metal in two successive reduction steps accompanied by elimination of two chlorides. After these two reduction steps another one-electron reduction occurs at the dpk ligand. 相似文献