Synthesis,Structural Characterization and Magnetocaloric Effect of a Butterfly [Co~Ⅱ_2Gd~Ⅲ_2] Cluster

2-(2,3-Dihydroxpropyliminomethyl)6-methoxyphenol(H_3L), trimethylacetic acid(Hpiv), Gd(NO_3)3·6 H_2O and Co(NO_3)2·6 H_2O were reacted in Me OH to obtain a heterometallic tetranuclear cluster [Gd_2Co_2(L)_2(μ_3-OH)_2(piv)_6]·2 Hpiv·2 CH_3OH(1). X-ray crystallographic analysis reveals that compound 1 was found to be a butterfly heterometallic tetranuclear cluster. The crystal(C_(64)H_(108)Co_2Gd_2N_2O_(28), Mr = 1785.88) belongs to the triclinic crystal system, space group P1 with a =11.9798(6), b = 12.0877(5), c = 15.0367(7) ?, α = 67.320(4)°, β = 81.583(4)°, γ = 75.201(4)°, V =1939.62(18) ?3, Z = 1, T = 293.15 K, R = 0.048 and w R = 0.144 for 16299 observed reflections with I 2σ(I). In magnetization study, heterometallic 1 exhibits magnetocaloric effect(MCE) of 14.75 J·kg~(-1)·K~(-1) at 2 K for ΔH = 5 T, while it does not show non-linear response of the ac-susceptibilities.     

玻碳电极界面的阻抗谱数学表达及定量分析

玻碳电极（GCE）是各类电化学传感器常用的基础电极,其界面特征直接影响检测性能。本文详细考察了电极体系的电化学过程,针对GCE传感界面,探讨了一个等效电路中电解质电阻、电荷输运电阻、扩散阻抗、电化学（氧化/还原）反应阻抗、表面吸附阻抗和双电层电容等电学元件的物理意义,并给出了对应的数学模型。通过改变模型中5个参数值,模拟了不同状态下的阻抗谱,分析了电极系统各参数对GCE阻抗谱的贡献规律。最后,采用该数学模型对裸GCE和修饰GCE在铁氰化钾溶液中的阻抗谱进行分析,拟合结果与实验数据吻合度高;基于拟合获得参数,定量对比分析了修饰前后电极表面的特征变化。     

Synthesis, Crystal Structure, Thermal Stability and Luminescent Properties of a New 2D Zinc Complex

A new coordination polymer associated with zinc ion,[Zn(Tda)(bpp)] n (1,H 2 tda=thiophene-2,5-dicarboxylic acid,bpp=1,3-bis(4-pyridyl)propane),was prepared under solvothermal conditions,and characterized by single-crystal X-ray diffraction,elemental analysis and IR spectra.The complex belongs to monoclinic,space group P2 1 /c with a=9.8799(4),b=12.0430(6),c=15.4269(9),β=95.424(5) o,V=1827.33(16) 3,Z=4,D c=1.577 g/cm 3,S=1.074,μ=1.486 mm-1,F(000)=888,M r=433.80,R=0.0359 and wR=0.0968 for 2685 observed reflections (I > 2σ(Ⅰ)).Complex 1 displays an interesting 2D lattice structure.In 1,four coordinated zinc ions were bridged by Tda and bpp ligands to generate a (4,4) two-dimensional layer.The thermogravimetric analysis,powder X-ray diffraction (XRD) and luminescent properties for 1 also have been explored.     

Crystal Structure and Luminescent Properties of a Zn(Ⅱ) Coordination Polymer Assembled by Mixed-ligand

A Zn(Ⅱ) coordination polymer [Zn(NIP)(3,3'-bpt)]·H2O(1, NIP = 5-nitroisophthalate, 3,3'-bpt = 1H-3,5-bis(3-pyridyl)-1,2,4-triazolate) has been synthesized by the hydrothermal reaction at 140 ℃ and structurally characterized by IR spectroscopy, X-ray diffraction, thermal analysis, single-crystal X-ray diffraction and luminescent properties. In complex 1, the zinc atom is five-coordinated with three carboxylate oxygen atoms from three H2 NIP and two nitrogen atoms from two 3,3'-bpt, respectively, forming a distorted trigonal bipyramidal geometry and showing a 1D chain structure, which is further bridged by NIP to form a 3D supramolecular network via self-assembly of hydrogen bonds.