Hydrothermal Synthesis and Crystal Structure of a Novel Hexanuclear Copper（Ⅱ） Complex：[Cu_6（DPPZ）_4（btc）_4（H_2O）_8]·5H_2O

A new hexanuclear copper(Ⅱ) complex,[Cu 6 (DPPZ) 4 (btc) 4 (H 2 O) 8 ]·5H 2 O (1,DPPZ=dipyrido[3,2-a:2,3-c]phenazine,H 3 btc=1,3,5-benzenetricarboxylic acid),has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analyses,IR,and thermogravimetric analysis.Its crystal structure is of triclinic system,space group P1 with a=12.489(4),b=14.234(5),c=14.484(5),α=82.848(4),β=79.399(4),γ=73.646(4)°,V=2421.2(13) 3,Z=1,Cu 6 C 108 H 78 N 16 O 37,M r=2573.17,D c=1.752 g/cm 3,μ=1.398 mm-1,F(000)=1308,GOOF=1.011,the final R=0.0495 and wR=0.1030 for 5420 observed reflections with I > 2σ(Ⅰ).In 1,four btc 3ligands act as bridges between six neighboring Cu atoms to form an unusual hexanuclear copper cluster.The clusters are further connected by two types of O-H···O and O-H···N hydrogen bonds,generating a three-dimensional supramolecular structure.In addition,intermolecular and intramolecular π-π stacking interactions further consolidate the three-dimensional supramolecular framework of 1.     

A 3-fold Interpenetrated lvt Cd(Ⅱ) Network Constructed from 4-[(3-pyridyl)methylamino]benzoate Acid

A new three-dimensional(3D) coordination polymer, [Cd(L)2H2O]n·5nH2O 1 with 4-[(3-pyridyl)methylamino]benzoate acid(HL), has been synthesized by slow evaporation solvent at room temperature, and structurally characterized by elemental analysis, IR spectrum, thermal analysis, fluorescence spectrum and single-crystal X-ray diffraction. Compound 1 crystallizes in the tetragonal system, space group I-4, with a = 20.7937(16), c = 13.515(2), V = 5843.5(11) 3, C26H34CdN4O10, Mr = 674.97, Dc = 1.534 g/cm3, μ(MoKα) = 0.808 mm-1, F(000) = 2768, Z = 8, the final R = 0.0276 and wR = 0.0691 for 5323 observed reflections(I 2σ(I)). The result of thermal analysis shows that 1 is stable under 290 ℃. Moreover, it exhibits blue photoluminescence at room temperature.     

Bi_2MoO_6/BiVO_4异质结的水热合成和可见光催化活性(英文)

采用一步水热法制备Bi2MoO6/BiVO4复合光催化剂.利用X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、高分辨透射电子显微镜(HRTEM)等手段对其晶体结构和微观结构进行了表征.结果表明,Bi2MoO6纳米粒子沉积在BiVO4纳米片表面从而形成异质结结构.紫外-可见漫反射光谱(UV-Vis DRS)表明所制备的Bi2MoO6/BiVO4异质结较纯相Bi2MoO6和BiVO4对可见光吸收更强.由于形成异质结结构及其光吸收性能使Bi2MoO6/BiVO4光催化活性有较大提高.可见光下(λ420 nm)光催化降解罗丹明B(RhB)实验结果表明,Bi2MoO6/BiVO4光催化活性较纯相Bi2MoO6和BiVO4高.Bi2MoO6/BiVO4样品光催化性能提高的原因是Bi2MoO6和BiVO4形成异质结,从而有效抑制光生电子-空穴对的复合,增大了可见光吸收范围及比表面积.     

一个由4,4′-(丁烷-1,4-二氧基)-二苯甲酸和双咪唑配体构筑的三重穿插金属有机骨架化合物(英文)

采用水热法合成了1个二维缠结金属有机框架化合物[Cu(bbi)0.5(boba)]n(1)(bbi=1,1′-(1,4-丁烷基)-二(咪唑);H2boba=4,4′-(丁烷-1,4-二氧基)-二苯甲酸),并通过元素分析、红外光谱和单晶X-射线衍射对其进行了结构表征。结构分析显示:化合物1是具有聚轮烷和聚锁烃结构特征的三重平行穿插网络。此外还研究了它的荧光和热稳定性。     

Hydrothermal Synthesis and Crystal Structure of a New Manganese（Ⅱ） Complex with 2,4-Pyridine-dicarboxylic Acid and 2,2′-Bipyridine Ligands

A new metal-organic complex [Mn2（PDC）2（bipy）2（H2O）2] （H2PDC = 2,4-pyridine-dicarboxylic acid, bipy = 2,2′-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The compound crystallizes in triclinic, space group P ^-1 with a = 7.376（3）, b = 9.990（4）, c = 11.950（5） A^°, α= 75.217（5）, β = 78.052（5）, γ = 70.655（5）°, V = 796.0（5）A^°3, C34HE6Mn2N6O10, Mr = 788.49, De = 1.645 g/cm^3,μ（MoKa） = 0.866 mm^-1, F（000） = 235, Z = 1, the final R = 0.0425 and wR = 0.0700 for 1971 observed reflections （I 〉 2σ（I））. In the crystal structure, the manganese atom is six-coordinated by two carboxylate oxygen atoms from two different PDC ligands, one aqua ligand, and three nitrogen atoms from 2,2′-bipy and PDC ligands, giving a distorted octahedral geometry. It exhibits a three-dimensional supramolecular network defined by O-H…O hydrogen-bonding interactions.     

Synthesis and Crystal Structure of a New Zinc(Ⅱ) Coordination Polymer Assembled by 4-Nitrophthalic Acid and Bis(imidazol) Ligands

A new complex [Zn(4-nph)(bib)]_(2n)·nH_2O(1) has been obtained by the reaction of metal(Zn(Ⅱ)),1,4-bis(imidazol-1-yl)-butane(bib) with 4-nitrophthalic acid(4-H_(2nph)).The crystal structure of 1 has been determined by single-crystal X-ray diffraction analysis.Compound 1 is of triclinic system,space group P1 with a = 10.3251,b = 12.4503,c = 16.6497 ?,α = 88.487(3),β = 72.529(3),γ = 79.991(3)°,V = 2009.8(5) ?~3 and Mr = 945.47.Complex 1 shows a three-dimensional(3 D) framework.Moreover,through intermolecular hydrogen bonds,compound 1 is assembled into a supramolecular structure.The thermal stability and luminescent properties of 1 are also investigated.     

纳米Ag/TiO_(2)纳米管阵列基底构建及表面增强拉曼散射光谱检测与降解盐酸四环素北大核心CSCD

将阳极氧化与光还原法结合,在TiO_(2)纳米管阵列(TiO_(2)NTAs)表面修饰Ag纳米粒子,获得一种均匀有序、稳定性高且可循环的TiO_(2)NTAs/Ag活性基底。采用X射线粉末衍射(XRD)、X射线光电子能谱(XPS)、紫外可见漫反射光谱(UV-Vis DRS)、表面增强拉曼散射光谱(SERS)和扫描电子显微镜(SEM)等手段对TiO_(2)NTAs/Ag的组成和结构进行了表征。进一步研究了该TiO_(2)-NTAs/Ag阵列对盐酸四环素(TC-HCl)的SERS响应,结果表明,该复合基底对TC-HCl具有较高的检测灵敏度,在水中检测限可达1×10^(−14) mol/L,而TiO_(2)-NTAs与Ag之间的协同效应对其检测性能的提高起着关键作用。此外,TiO_(2)NTAs/Ag基底在光照下对TC-HCl展示了优异的降解活性,且至少可循环使用8次。表明该TiO_(2)NTAs/Ag基底在环境中有机污染物的SERS检测和降解领域具有潜在的应用前景。     

高精度胶束毛细管电动色谱法测定牛磺酸滴眼液中牛磺酸和羟苯乙酯的含量

建立了高精度胶束毛细管电动色谱法同时测定牛磺酸滴眼液中牛磺酸和羟苯乙酯含量的方法。移取牛磺酸滴眼液样品5.0 mL,用水定容至10 mL,超声混匀,经0.22μm微孔滤膜过滤,取续滤液,得到待测样品溶液。选择带隔离槽的石英毛细管柱（内径75μm,总长度65 cm,有效长度45 cm）,以含20 mmol·L^-1十二烷基硫酸钠的硼砂-硼酸缓冲液(pH 9.0,15 mmol·L^-1)的混合液为分离缓冲液,在分离电压为-15 kV,检测波长为210 nm的条件下进行电泳分离。结果显示：牛磺酸的质量浓度在5.02～40.80 g·L^-1内,羟苯乙酯质量浓度在0.050～0.333 g·L^-1内与其各自对应的峰面积呈线性关系,检出限分别为1.2,0.005 g·L^-1;牛磺酸和羟苯乙酯混合标准溶液的日内精密度（n=6）均小于2.0%,日间精密度（n=6）均小于4.0%;对实际样品进行加标回收试验,牛磺酸的回收率为93.9%～111%,羟苯乙酯的回收率为85.3%～107%。方法用于3批...     

由草酸及双咪唑基配体构筑的二维锰(Ⅱ)配位聚合物的水热合成及晶体结构

通过水热法合成了一个新的金属-有机配位聚合物[Mn(C2O4)(bimb)]n.0.25nH2O(H2C2O4=草酸,bimb=1,4-双(咪唑基-1-基)丁烷)。并对其进行了元素分析、红外光谱、紫外光谱、热重和X-射线单晶衍射测定。该配合物属于三斜晶系,P1空间群。在晶体结构中,锰原子为六配位与来自2个不同的C2O42-配体上的4个羧基氧原子和来自2个bimb配体上的2个氮原子配位,呈现畸变的八面体几何构型。     

两个由5-硝基间苯二甲酸和双咪唑基配体构筑的锰、钴配合物的合成及晶体结构

通过水热法合成了2个新的配合物[Mn(NIPH)(mbix)]_n (1)和[Co(NIPH)(mbix)(H₂O)₃]_2n·2nH₂O (2)(H₂NIPH=5-硝基间苯二甲酸,mbix=1,3-双(咪唑基-1-基)苯)。并对其进行了元素分析、红外光谱、紫外光谱、热重和X-射线单晶衍射测定。这两个配合物通过氢键和π-π相互作用形成了三维超分子网状结构。