三维锌基金属有机框架材料的合成及其晶体结构与热性能

以1,1'-双(二苯基膦)二茂铁氯化钯为催化剂,2,5-二溴苯甲醛和4-吡啶苯硼酸经"一锅法"反应合成了新化合物2,5-二(吡啶-4-基)苯甲醛(L)。以L和反式-4,4'-二苯乙烯二甲酸(H2SDA)为配体,与Zn(NO3)2·6H2O经溶剂热反应合成了一个四重穿插的三维金属有机框架材料[Zn2L(SDA)2]·2DMA(1),其结构和热性能经IR,元素分析,X-射线粉末衍射和TGA表征。1属四方晶系,P4(1)2(1)2空间群,晶胞参数a=17.452 0(9),b=17.452 0(9),c=18.360 6(14),V=5 592.1(6)3,Z=8,Dc=1.303 mg·cm-3,F(000)=2 268,μ=1.557 mm-1,R1=0.040 6,ωR2=0.114 7。1的结构中轮浆型双核Zn2(CO2)4单元被四个SDA分子连接形成一个二维层状结构,进而通过配体L桥连形成一个三维的网状结构,其热稳定性高达320℃。     

新型手性希夫碱镍配位聚合物的合成及其晶体结构

以手性对称的Schiff碱为配体,合成了手性镍配合物[Ni2(salen)2(1)],其结构经X-单晶射线衍射和元素分析表征。1属单斜晶系,C2空间群,晶胞参数a=25.060(5)A,b=13.508(3),c=11.938(2),α=90(3)°,β=104.82(3)°,γ=90(3)°,V=3 906.7(14)3,Z=4,Mr=828.24,Dc=1.429 g.cm-3,F(000)=1 808,μ=1.027 mm-1,GOF=1.068,R1=0.051 0,wR2=0.128 9。在1的分子结构中,环己胺和苯环之间通过分子间CH┈π作用形成二维结构。     

连二-2-吡啶酮三核钴簇合物的溶剂热合成及其晶体结构

用二-2-吡啶酮作为配体与羧酸钴在溶剂热中反应,得到两个新型连二-2-吡啶酮三核钴簇合物--Co3(Py2CO2H)2(PhCO2)5]·MeCN(1)和Co3(Py2CO)2(PhCO2)6(2),其结构经XRD, IR和元素分析表征.1属单斜晶系,P(2)1空间群,晶胞参数:a=1.068 7(3) nm, b=2.258 0(5) nm, c=1.163 9(3) nm, α=90.000°, β=104.805(5)°, γ=90.000°, V=2 715.6(4) nm3, Z=2, Dc=1.497 g·cm-3.2属三斜晶系,P-1空间群,晶胞参数:a=1.133 5(3) nm, b=1.140 8(3) nm, c=1.181 8(3) nm, α=85.59 8(6)°, β=75.973(5)°, γ=69.519(5)°, V=1 388.8(2), Z=1, Dc=1.521 g·cm-3.     

Synthesis and Characterization of Nickel(II) and Copper(II) Complexes with Schiff Base (1R,2R)-(-)-Diaminocyclohexane-N,N'-bis(3-tert-butyl-5-(4'-benzoic acid)-salicylidene)

Two homochiral metallosalen complexes, Ni(salen) (salen = (1R,2R)-(-)-diaminocyclohexane-N,N'-bis(3-tert-butyl-5-(4'-benzoic acid)-salicylidene) 1 and Cu(salen) 2, have been synthesized and characterized by IR, microanalysis, TGA, powder and single-crystal X-ray crystallography. Both 1 and 2 crystallize in orthorhombic space group P21212 with Z = 4. For 1, a = 12.082(2), b = 15.447(3), c = 18.784(4) , V = 3505.7(12) 3, Mr = 731.50, Dc = 1.386 g/cm3, μ = 0.606 mm–1, F(000) = 1544, the final GOOF = 1.043, R = 0.0496 and wR = 0.1248 for 4791 observed reflections with I > 2σ(I). For 2, a = 12.181(2), b = 15.501(3), c = 18.877(4) , V = 3564.3(12) 3, Mr = 736.33, Dc = 1.372 g/cm3, μ = 0.665 mm–1, F(000) = 1548, the final GOOF = 1.062, R = 0.0575 and wR = 0.1508 for 4562 observed reflections with I > 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. An infinite two-dimensional network is generated by hydrogen bonding interactions and intermolecular π···π interactions.     

Synthesis and Crystal Structure of {η~5:η~1-[(2-Methoxyphenyl)-isopropyl]-indenyl}(dimethoxyethylene)lithium1

1 INTRODUCTION The applications of alkali metal cyclopentadi- enides or their benzoanellated analogues in organo- metallic and organic syntheses are still the interest of chemists[1–3]. The structures of known indenyl li- thium are the supersandwich or oligomeric indenyl lithium[4], and 2-aminoindenyl lithium[5] was charac- terized by high-resolution X-ray powder diffraction and single-crystal X-ray diffraction, respectively. The trigonal planar structure of TMEDA (tetra-methyl- ethyle…     

核心素养导向下中考化学试题特点分析及对命题的思考——以2018年安徽省中考化学试卷第15题为例

以2018年安徽省初中学业水平考试化学试卷第15题为例,对核心素养导向下的中考化学试题的特点进行分析,从试题的情境、知识、问题等要素分析如何体现学科素养的测试宗旨,并阐述对命题素材的遴选及问题设计的方式等方面的思考。     

对“空气中氧气含量测定实验”的改进

通过文献研究和实验研究，得出用吸氧腐蚀原理测量空气中氧气含量，比传统用红磷燃烧测量空气中氧气含量的方法更加科学、准确，并提出改进方案。     

手性不对称希夫碱铜配位聚合物的合成及其晶体结构

以手性不对称希夫碱为配体与铜离子在温和条件下合成了新的一维链状铜配位聚合物C54H68N6O8Cu2(1),其结构经IR,热重分析,元素分析和X-单晶射线衍射表征.1属单斜晶系,P2(1)空间群,晶胞参数为:a=11.268(5)(A), b=13.682(6)(A), c=17.604(7)(A), β=106.739(5) °, V=2 598.9(18) (A)3, Z=2, Mr=1 056.22, Dc=1.350 g·cm-3, F(000)=1 112, R1=0.037 0, wR2=0.095 9.1具有一维zigzag链结构.     

Synthesis and Characterization of Nickel（Ⅱ） Complex Bearing 2,9- di-tert-butyl-1,10-phenanthroline Ligand

The complex DtbpNiCl2(Dtbp = 2,9-di-tert-butyl-1,10-phenanthroline) was synthe- sized and characterized by X-ray single-crystal structure analysis. For the complex: C20 H24 Cl2 N2 Ni CH2 Cl2, Mr = 506.95, monoclinic, space group P21 /c, a = 9.5905(3), b = 13.7587(3), c = 17.3364(5), β = 94.244(2)°, V = 2281.31(11)3, Z = 4, Dc = 1.476 g/cm3, λ = 1.54184, μ = 5.606 mm-1, F(000) = 1048, S = 1.079, R = 0.0402 and wR = 0.1010 for 3223 observed reflections with I 2σ(I). In complex DtbpNiCl2, the nickel adopts a distorted tetrahedral geometry coordinated by two nitrogen atoms of Dtbp and two chlorine ions. The complex is connected by intermolecular C–H···Cl hydrogen bonds to form a 1D structure in the solid state.     

含茂基稀土金属有机络合物催化剂在有机合成中的应用

综述了含茂基稀土金属有机络合物催化下的不饱和烃（或其取取衍生物）转化反应及其在有机合成中的作用。重点阐述了含茂基稀土金属有机络合物催化的烯烃氧化，氢化环化；烯烃和炔烃的氢化硅化，1，5－或1，6－二烯或烯炔的氢化硅化／环化，氨基取代烯烃，炔烃，丙二烯等的氢化胺化／环化等反应在有机合成中的主要用途，这些反应在形成碳－杂原子键，碳－碳键，碳环和杂环等方面具有广泛的应用前景。讨论了这些反应的催化循环机制，区域稳定性，对映选择性，非对映选择性及其影响因素。