Direct Synthesis, Crystal Structure and Thermal Kinetics of Supramolecular Complex [Co（H2O）6]·（Hnip）2·（H2nip）2·（DMA）2·（H2O）8 （nip=5-nitroisophthalate, DMA=CH3NHCH3）

The crystal of [Co（H2O）6]·（Hnip）2·（H2nip）2·（OMA）2·（H2O）8 has been cultured using direct method and characterized by X-ray single crystal diffractometry, elemental analysis and FTIR spectroscopy. It crystallizes in triclinic system, P-1 space group with the cell parameters of a=0.7012（1） nm, b=1.1378（2） nm, c=1.6612（3） nm, α= 84.92（3）°, β=85.19（3）°, γ=85.91（3）°, V= 1.3128（5） nm^3, Z=1, Dc= 1.573 g·cm^-3. Final R indices [1〉2σ（I）] are： R1 =0.0279, wR2=0.0765 while R indices for all data are： R1 =0.0327, wR2=0.0806. The Co coordination octahadra are each surrounded by two Hnip, two H2nip, two DMA and eight water molecules that are linked by hydrogen bonds and π-π stacking interactions. Thermal analyses of DSC and TG-DTG have been performed on the complex to predict its thermal decomposition mechanism and determine the most probable kinetic model function using Kissinger, Ozawa, integral and differential methods.     

一个新颖三维配位聚合物Pb(1，4-napdc)(DMF)的合成、结构及热稳定性研究

A novel 3D metal-organic coordination polymer Pb(1,4-napdc)(DMF) (1,4-napdc=naphthalene-1,4-dicarboxylate) was synthesized at room temperature using slow vapor diffusion method to grow single crystal that has been analyzed by X-ray diffraction. The crystal belongs to orthorhombic with space group P2₁2₁2₁. The unit cell parameters are as fellows: a=0.701 3(2) nm, b=1.407 6(3) nm, c=1.521 5(4) nm, V=1.501 8(6) nm³ and Z=4. In the crystal structure of Pb(1,4-napdc)(DMF), the square grids constructed with paddle-wheel units of Pb(Ⅱ) and 1,4-napdc links stack over each other to generate infinite 3D network, which has square apertures (1.158×1.158 nm²) along the crystallographic a-axis. The thermal stability of compound was investigated by differential scanning calorimetry and thermogravimetric analysis. CCDC: 293617.     

一维链状配位聚合物{[Cu(H2bttc)(H2O)3]·3H2O}n的非等温反应动力学和晶体结构

为研究配位聚合物{[Cu(H₂bttc)(H₂O)₃]·3H₂O}_n(H₂bttc=1，2，4，5-benzenetetracarboxylate)的热分解机理和非等温反应动力学进行了DSC和TG-DTG热分析。由热分析结果和FTIR光谱推测了其热分解机理；将Kissinger法、Ozawa法、积分法和微分法得到的动力学参数进行比较确定了第一个失重过程最可能的动力学模型函数。配位聚合物的X射线单晶结构分析表明它由 [Cu(H₂bttc)(H₂O)₃]_n分子链组成，并有客体水分子通过分子间氢键附着在分子链上。这一结构特点与热分析结果相一致。还有一种氢键将分子链连接起来形成二维框架，这一框架在失去配位水和结晶水后到553 K开始分解。     

Hydrothermal Synthesis of a 1D Paddle-wheel Cu(Ⅱ) Coordination Polymer {[Cu_2(NBDOA)_2·(H_2O)_2]·2(H_2O)}_n Constructed by Flexible Carboxylic Acid

A 1-D paddle-wheel copper (II) coordination polymer constructed by 2-nitro-benzene-1,4-di(oxyacetic) acid has been synthesized by hydrothermal reaction,and its crystal structure was determined by X-ray diffraction. The crystal is of triclinic,space group P1 with a=7.7257(12),b=8.3648(13),c=11.5516(18),α=76.654(2),β=82.088(2),γ=63.636(2)o,C20H22Cu2N2O20,Mr=737.48,V=650.27(18)3,Dc=1.883 g/cm3,F(000)=374,μ=1.737 cm-1 and Z=1. The final refinement gave R=0.0345 and wR=0.0995 for 1996 observed reflections with I > 2σ(I). The coordination polymer demonstrates a 1-D microporous structure,and the channel is formed by two NBDOA2-and two Cu2+ ions. The ligand NBDOAH2 displays a good flexible characteristic. The 1-D chains are connected to a 3-D supramolecular network by hydrogen bonds.     

超分子配合物[Co(H2O)6]·(Hnip)2·(H2nip)2·(CH3NHCH3)2·(H2O)8的直接合成，晶体结构和热分解反应动力学(nip=5-nitroisophthalate)

用直接法培养了配合物[Co(H₂O)₆]·(Hnip)₂·(H₂nip)₂·(DMA)₂·(H₂O)₈(DMA=CH₃NHCH₃)的晶体并用X射线单晶衍射，元素分析和傅里叶变换红外光谱进行了表征。该晶体属于三斜晶系，P-1空间群，晶胞参数为a=0.7012(1)nm, b=1.1378(2) nm, c=1.6612(3) nm, α=84.92(3)º, β=85.19(3)º,γ=85.91(3)º。晶胞体积V=1.3128(5) nm³, Z=1, 理论密度D_c=1.573 g/cm³. 最终R因子[I>2σ(I)]为: R₁=0.0279,wR₂=0.0765; 所有衍射点的R因子为: R₁=0.0327, wR₂=0.0806.衍射结果表明，在晶体结构中两个Hnip分子，两个H₂nip分子，两个DMA分子和八个水分子通过氢键和π-π堆积作用连接到每个Co配位八面体中心上。对配合物进行了DSC和TG-DTG热分析，根据热分析结果推测得到配合物的热分解机理，并且用Kissinger,Ozawa，积分法和微分法确定了最可能的动力学模型函数。     

三维网状结构配位聚合物[Cu(HCOO)2(H2O)2]∞晶体的热分解机理

用水热合成法得到了[Cu(HCOO)2(H2O)2]∞的晶体, 采用TG-DTG和DSC法对配合物[Cu(HCOO)2(H2O)2]∞进行了热分解机理和热分解动力学研究. 通过对DSC曲线用Kissinger、Ozawa、积分法和微分法处理的结果进行比较, 得到了脱水过程的动力学模型函数. 并用X射线单晶衍射、元素分析、FTIR光谱技术进行了表征. 结果表明该配位聚合物晶体为单斜晶系, 属P21/c空间群, 晶胞参数为a=0.8533(2) nm, b=0.7151(2) nm, c=0.9463(2) nm, β=96.94(0)°. 晶胞体积V=0.5732(2) nm3, Z=4, 计算得到的晶体密度Dc=2.197 g•cm−3. 在该配位聚合物中, 通过甲酸根作为连接配体将两种铜配位中心连接起来形成三维网状框架结构.     

纳米四氧化三铁(Fe3O4)的制备和形貌

纳米Fe₃O₄因其特殊的理化性质和在生物医学领域潜在的应用价值而得到广泛研究。本文综述了纳米Fe3O4的制备方法，包括直流电弧等离子体法、热分解方法、沉淀法、水热法、电化学法、微乳液法、溶胶-凝胶法、有机物模板法、回流法等，结合作者在Fe3O4纳米粒子制备方面的最新工作，介绍了Fe3O4纳米粒子的新颖形貌。对纳米级Fe3O4制备研究的发展趋势进行了展望。     

OBE教学理念下波谱分析课程教学改革的思考与实践

波谱分析作为应用化学专业的一门专业基础课,在学生毕业论文环节中起着重要的作用。基于成果导向教育(OBE)的教育理念,以我院应用化学专业学生在毕业论文环节的实际解谱需要为出发点,通过合理安排教学内容、改进课堂教学方式和建立有效的评价体系,对波谱分析课程进行初步改革探索,注重培养学生解析谱图的能力,提高课程的实用性。