The self-assembly reactions of AgNO3, Ln(NO3)(3) (Ln = La, Eu, and Tb), D-penicillamine (D-pen, H2L), and NiCl2 (or CoCl2) lead to the formation of six new compounds: (H3O)(3)[LnNi(6)Ag(8)L(12)Cl(Ac)(H2O)(4)]-(H2O)(28) (Ln = La (1); Eu (2); and Tb (3)) and (H3O)(2)[LnCo(2)Ag(3)L(6)](H2O)(3) (Ln = La (4); Eu (5); and Tb (6)). Single crystal X-ray analyses show that 1, 2, and 3 are isomorphous and have a 3D anionic framework in which the nodes are octahedral {Ni6Ag8S12Cl} clusters, and Ln(3+) ions and the connectors are the CCHCOO chains of the D-pen ligands. Moreover, 4, 5, and 6 are also isomorphous, possessing a 3D anionic framework with trigonal dipyramidal {Co2Ag3S6} clusters, Ln(3+) as nodes, and the CCHCOO chains of the D-pen ligands as connectors. Topology analysis indicates that the two series of 3d-4d-4f heterotrimetallic frameworks have (3,3)-connected utg and (6,6)-connected pcu networks, respectively. The frameworks are rigid and stable. The porosity is retained after the guest molecules are removed and can take back guest molecules again. Solid-state UV-vis spectroscopy experiments show that compounds 1-6 are all medium gap semiconductors with band gaps of 1.82, 1.80, 1.83, 1.68, 1.71, and 1.72 eV, respectively.
A series of rigid imidazolate/carboxylate functionalized ligands, X-(5,7-dioxopyrrolo[3,4-f]benzimidazole-6-yl)benzoic acid (X=4, H24-DPBB; X=3, H23-DPBB; X=2, H22-DPBB) were designed and used for the assemble reactions with Zn2+/Cd2+/Cu2+ ions. Four compounds, [Zn(4-DPBB)(H2O)]·DMSO·0.5MeOH (1), [Cd(3-DPBB)(DMA)1.8(H2O)0.2] (2), [Cu(3-DPBB)(DMSO)(DMA)] (3) and [Cd(2-DPBB)(DMA)2] (4) have been synthesized and structurally characterized (where DMSO=dimethylsulfoxide, DMA=dimethyl acetylamide). Single crystal X-ray analyses show that the four compounds are all based on 3-connected single metal nodes and 3-connected spacers. Compounds 1 and 2 bear a 2D (6, 3)-net structure, while 3 and 4 have a 2D (4, 8)-net. Compared with 2, 3 and 4, 1 exhibits a relatively high thermal stability which is up to ∼550°C. Luminescent analysis indicates that 1 and 2 exhibit linker-localized emissions while 4 has ligand-to-metal charge transfer (LMCT) emission. The effect of the torsion of the ligands on the crystal structures and properties of the four compounds is discussed.
A rigid imidazolate/sulfonate functionalized ligand, 6-(4-sulfonatopheny)imidazo[4, 5-f]isoindole-5, 7-dione (SPID) was designed and used for assembling reactions with Mn2+ and Cu2+ ions. Two 2D frameworks compounds, [Mn(H-1SPID)2(DMAC)2] (1) and [Cu(H-2SPID)(H2O)2]center dot 0.7DMAC center dot 0.3H2O (2) (DMAC = N,N-dimethylacetamide) were obtained. Single crystal X-ray analyses show that 1 has a 2D (4, 4)-net based on 4-connected Mn2+ nodes and mu 2-coordinated H-1SPID spacers, whereas compound 2 has a 2D (6, 3)-net built of 3-connected Cu2+ nodes and mu 3-coordinated H-2SPID spacers. Additionally, the thermal behavior of 1 and 2 is presented.
The assembly reactions between a rigid imidazole/carboxylate functionalized ligand, 2-(5, 7-dioxopyrrolo[3, 4-f]benzimidazole-6-yl)benzoic acid (H22-DPBB) and Mg2+(Li+) ions led to the formation of two 2D layered compounds, [Mg(H2-DPBB)2(DMF)2] (1) and [Li(H2-DPBB)(DMF)] (2) (DMF = N,N-dimethylformamide). Single crystal structural analyses show that compound 1 has a 2D (4, 4)-net structure based on 4-connected mononuclear Mg2+ nodes and HDPBB spacers. Compound 2 also has a 2D (4, 4)-net structure but based on dinuclear {Li2} nodes and HDPBB spacers. Interesting hydrogen bond and interactions are observed in the structures. Additionally, the IR spectra and thermal behaviors of 1 and 2 are presented.
With formate as ligand, two 1-D 3d-4f compounds (linear and zigzag) based on pyramidal {TbCu(4)} unit were obtained. Chair-like [(H(2)O)(2)(ClO(4))(2)](2-) clusters and μ(5)-η(1):η(4) bridging mode of formate were observed in the linear one which also displays slow relaxation of the magnetization.
介绍一个综合性研究型实验——Y型沸石分子筛的制备及表征。该实验以水热条件下溶胶-凝胶法合成分子筛为理论基础,采用导向剂法合成Y型沸石分子筛,并采用XRD、IR等手段对产物进行表征。该实验时间和步骤安排合理,可操作性强,可以在本科及研究生实验教学中推广。
Title compound (II) crystallizes in the monoclinic space group P21/c with Z = 4 (single crystal XRD).
AbstractThe title compound is hydrothermally synthesized from a mixture of MgCl2, B2O3, H3PO4, pyridine, HCl, and H2O (autoclave, 170 °C, 3 d, 10% yield).
A new protonated borophosphate (H3O)Mg(H2O)(2)[BP2O8]center dot H2O (1) was synthesized under mild hydrothermal conditions and characterized by single-crystal X-ray diffraction, FTIR spectroscopy and TG-DTA. The compound crystallizes in the hexagonal system, space group P6(1)22 (No 178), a = 9.4462(7) angstrom, c = 15.759(2) angstrom, V = 1217.8(2) angstrom(3), and Z = 6. There exist infinite helical (1)(infinity){[BP2O8](3-)} ribbons built up from corner-sharing PO4 and BO4 tetrahedra, which are connected by MgO4(H2O)(2) leading to an infinite three-dimensional open-framework. The H3O+ ions are located at the free thread of the helical ribbons, whereas crystallized water occupy the channels of the helical ribbons. The dehydration of the compound occurs at a higher temperature which is presumably due to the anisotropic hydrogen bonds in the crystal structure. The luminescent properties of the compound were studied.
The cobalt (II)-exchanged zeolite A (NaCoA) was prepared by cation exchange process with zeolite A (NaA) and Co(NO3)2 in aqueous solution. A static volumetric system was employed to evaluate the N2 and O2 adsorption properties of NaCoA at 298K. It was found that the N2 adsorption capacity of NaCoA increased rapidly with the rising pressure, and the adsorption isotherm of N2 became nonlinear in low pressure region. The O2 adsorption capacity of NaCoA increased slightly with pressure. The introduction of Co2+ into the NaA enhanced the N2 adsorption capacity and N2/O2 selectivity, which could be contributed to the π-complexation between N2 and Co2+. This strong interaction brought about a series of high value for Henry's constant, Langmuir constant, adsorption selectivity and adsorption capacity of N2 in NaCoA. Infrared spectra were also carried out to illustrate that the N2 were bonding with Co2+.
Reactions between CoO, ZnCl2 (or ZnBr2), and molten citric acid (Hcit) led to the formation of two 3d-3d heterometallic coordination frameworks: [ZnCo(licit)Cl] (1) and [ZnCo(Hcit)Br] (2). X-ray structure analyses show that both compounds 1 and 2 crystallize in the monoclinic space group P2(1)/n [1: a = 5.8699(5) angstrom, b = 17.7963(13) angstrom, c = 9.2152(8) angstrom, beta = 106.806(4)degrees, Z = 4, V = 921.53(13) angstrom(3); 2: a = 5.909(3) angstrom, b = 17.798(8) angstrom, c = 9.302(5) angstrom, beta = 106.374(7)degrees, Z = 4, V = 938.6(8) angstrom(3)]. The structures of the two compounds are almost the same except for the terminal halogen ligand. Both of them are 3D frameworks based on citric acid bridging ligands and a ID backbone chain built of corner-shared {CoO6} and {ZnO3Cl} polyhedra. Photoluminescence and thermal stabilities of the compounds were studied.
In order to offer a reference for the university teachers and researchers,the common troubles and resolutions in the use of optical mouse are introduced in detail based on the authors' experiences.
Intruduction Though hydrogen is a clean fuel giving water as the only byproduct on its combustion in air, on-board storage of hydrogen is still a challenge. Various methods for storing hydrogen including gaseous, liquid and solid state storage have been suggested [1, . The storage of hydrogen via adsorption, including physisorption, using porous materials is one of these several methods currently being investigated. Porous materials such as carbons , zeolites , and hybrid inorganic–organic framework materials have been studied as potential hydrogen sorbents. Recent studies have shown that zeolites can be alternative for reversible hydrogen storage . These researches demonstrate that optimum pore size or small pore is stated to be important to enhance the hydrogen uptake . Development of open or coordinatively unsaturated sites (CUS) of metal atoms is also helpful to increase the adsorption strength . Jhunga et al. have reported that coordinatively unsaturated nickel sites of porous nickel phosphate [14] or nickel-5-sulfo isophthalate [15] lead to an adsorption of hydrogen. During the past decade or so, numerous experimental studies on the incorporation of small palladium clusters inside pores of FAU zeolites have been reported. In the study the clathrate sodalite (SOD) is chosen as the model compound because of it large void volume and large number of six-rings per cage, and to the best of our knowledge, hydrogen storage experiments using sodalite have only thus far been performed for alumina–silica–sodalite . Thouth the metals palladium and ruthenium are known to absorb hydrogen , which has similar characterations with nickel. The present investigation therefore has been undertaken with an objective to study the effect of nickel clusters loading in porous materials on the hydrogen sorption properties, expecially adsorption capacity, using SOD-supported nickel clusters in low temperatures of 77K and pressure up to about 1 bar. These experiments show a hydrogen storage capacity of 24.7327cm/g at 77K for sample 52 with a Ni:Si:Al ratio of 0.5:1.1:1 after a loading time of 8 hours at 333K.
Administrators often deal with many small failures that influence chemical experiment course. This article introduces solutions to 12 kinds of failures to help to the teachers and administrators of university.
As one of the motsly widely used instruments in chemical plants,Agilent 6890 GC is common chemical analysis and exactitude measure apparatus.In this paper,in order to give a reference for the maintainer and user,the frequent troubles and maintenance are introduced on the basis of the authors'experiences.
ZSM-5 crystals, of which granule size is about 120 pm along c axis, are employed as a good host material for TiO2 loading. Optical microscopy photographs, X-ray powder diffraction spectra and surface area calculated from nitrogen adsorption data at -196 degrees C have been carried out and show that the titanium dioxide clusters are infiltrating into the pores of ZSM-5. TiO2/ZSM-5 host-guest material, regardless of whether being prepared by microwave and water bath heating, shows similar features except for the TiO2 contents. The materials have a photoluminescence emission peak at 2.85 eV, which is ascribed to the band edge emission. A red shift was observed on the photoluminescence emission spectra when NH3 adsorbed into the pores of TiO2/ZSM-5 material. (C) 2009 Elsevier B.V. All rights reserved.
针对化工专业实验教学目前存在的弊端,从实验教材、实验教学内容、教师队伍建设以及教学方法进行改革与实践,开放大型仪器的使用等,使学生从被动学习变为主动学习,激发学生实验热情,提高学生分析和解决问题能力以及开拓创新能力。
普通化学实验是高等院校化学教育的重要组成部分。根据目前普通化学实验教学的状况,对其教学教学内容、教学方法、教学手段和实验考核方法等方面进行改革,从而提高学生的实验理论知识、操作技能和创新能力,以促使普通化学实验教学在培养高素质创新人才中发挥应有的作用。
电光分析天平是一种能够测量物质质量的精密仪器,是高等院校实验室化学分析和物质精密测量常用的仪器,在使用中其光学部分出现故障是最常见的。文章主要对电光分析天平光学系统在使用中出现的常见问题及解决方法详细介绍,兼顾其他故障。
文章介绍了绿色化学的定义和内涵,就实现化学实验绿色化问题提出了一系列措施,强调树立绿色化学的思想观念,增强环境保护意识;认识不到位,投资不足是其产生的主要原因;采用推广微型化学实验,推广连续合成实验和回收再利用,分类收集、区别处理等多种途径,探索出一套简便易行的实验室废弃物综合治理方法。