水杨醛缩乙醇胺双氧钒席夫碱配合物的合成、晶体结构及热分解研究(英)

A new complex bis[(N-salicylidene-N′-aminoethanol)dioxovandium(Ⅴ)], [V(Ⅴ)O₂(SALAE)]₂, was synthesized by the reaction of salicylaldehyde and aminoethanol with vanadyl sulfate. It was characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The crystal of the title complex (C₁₈H₂₀N₂O₈V₂, M_r = 494.24) belongs to monoclinic, space group P2₁/c with the following crystallographic parameters: a= 1.7966(6) nm, b= 0.7587(3) nm, c= 2.1539(7) nm, β = 92.551 (6) °, V= 2.9329 (17) nm³, Z= 6, D_c= 1.679 g·cm^-3, μ(MoKα) = 1.006 mm^-1, F(000) =1512, and final R₁ = 0.0563, wR₂= 0.1243 for observed reflections 2861(I> 2σ(I)). The complex is a bis(μ-oxo)-bridged V(Ⅴ) schiff base dimer formed by two dioxovandium units, V(Ⅴ) is six-coordinated and forms a distorted octahedral structure. The thermal decomposition for the complex was studied by TG-DTG curves and the apparent activation energy was obtained by the Kissinger formula. CCDC: 211147.     

双水杨醛缩乙二胺氧钒配合物的合成和晶体结构

钒的化合物具有类胰岛素样活性,是新一代潜在的抗糖尿病药物。本文合成了水杨醛缩乙二胺氧钒席夫碱配合物[VO(SALEN)],并通过红外光谱、元素分析、X-射线单晶衍射和热重分析等手段进行了表征、结构测定及热分解研究。结果表明,它属于三斜晶系,与以前所报道的该配合物的单斜晶系结构不同。     

邻香草醛氧钒配合物的合成和晶体结构

钒是人体所必需的微量元素,钒化合物是新一代潜在的抗糖尿病药物。我们合成了邻香草醛氧钒配合物[VO(o-van)2(H2O)],并通过红外光谱,元素分析和X-射线单晶衍射等手段确定了其结构。     

含质子柠檬酸氧钒（V）配合物中间体的合成和晶体结构

合成了含质子柠檬酸氧钒（Ｖ）配合物中间体ＮａＫ３［ＶＯ２（Ｈｃｉｔ）］２·７Ｈ２Ｏ，用红外光谱和Ｘ射线衍射进行了结构表征。结果表明：晶体属单斜晶系，Ｐ２１／ｎ空间群。晶胞参数ａ＝１．１２５８（２）ｎｍ，ｂ＝１．５７７４（３）ｎｍ，ｃ＝１６５５９（１）ｎｍ，β＝９８．５６８（９）°，Ｖ＝２．９０８（１）ｎｍ＾３，Ｚ＝４，Ｄｃ＝１．８５１ｇ·ｃｍ＾－３，Ｆ（０００）＝１６４０，μ（Ｃｕ Ｋα）＝１０４     

钒氧多酸桥联大环铜配合物的合成及其晶体结构

以大环铜配合物［CuL］(ClO₄)₂(L=5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四-4,11-二烯)与NH₄VO₃反应合成了一个新的钒氧多酸桥联大环铜配合物［CuL］₂［H₂V₁₀O₂₈］·7H₂O(1),其结构经IR,元素分析和X-射线单晶衍射表征。1（CCDC: 1510831）属单斜晶系,P2(1)/n空间群,晶胞参数a=11.512(3) , b=18.170(4) , c=14.534(3) , β=102.997(4)°, V=2 962.3(11) ³, Dc=1.986 mg·cm^-3, Z=2, μ=2.300 mm^-1, R₁=0.047 2, wR₂=0.118 2。     

5-溴水杨醛缩乙醇胺Schiff碱Cu(II)配合物的合成和晶体结构

The title complex Cu(L)₂ [HL=N-(5-bromosalicylidene)-2-aminoethanol] was synthesized by the reaction of Cu(CH₃COO)₂·H₂O with N-(5-bromosalicylidene)-2-aminoethanol in the ethanol. It was characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The crystal of the title complex [Cu(C₉H₉BrNO₂)₂] belongs to monoclinic, space group P2₁/n with a=1.319 1(5) nm, b=0.444 58(16) nm, c=1.656 7(6) nm, β=91.226(5)°, V=0.971 46(6) nm³, Z=2, D_c=1.879 Mg·m^-3, μ=5.264 mm^-1, F(000)=542, and final R₁=0.045 6, wR₂=0.097 0. The complex comprises a four-coordinated copper(II) center, with an N₂O₂ planar coordination environment. The molecules are connected by hydrogen bonds to form two-dimensional layered structure. CCDC: 274180.     

含有羧基配体的蝎型钒氧配合物的合成、结构及其热分解动力学

设计合成了两种新型的以聚吡唑硼酸盐、氨基酸为配体的钒氧配合物VO[phCH2CH(NH2)COO][HB(pz)3](1)和VO(3,5-Me2pz)[HB(3,5-Me2pz)3](CH3COO)(2). 通过元素分析、红外光谱对配合物进行了表征, 并利用单晶X射线衍射技术解析了它们的结构. 非等温热分解动力学研究表明, 配合物1和2的热分解反应都是分两步进行的. 通过计算, 配合物1热分解的第一步反应的可能机理为成核与生长(n=1/4); 第二步反应的可能机理为化学反应. 其非等温动力学方程分别为, dα/dT=(A/β)e-E/RT(1/4)(1-α)[-ln(1-α)]-3 和dα/dT=(A/β)e-E/RT(1-α)2. 分解反应的表观活化能分别是223.52 和331.94 kJ·mol-1; 指前因子ln(A/s-1)分别是49.67 和57.50. 配合物2 热分解的第一步反应的可能机理为化学反应; 第二步反应的可能机理为成核与生长(n=1/2). 其非等温动力学方程分别为, dα/dT=(A/β)e-E/RT(1-α)2, 和dα/dT=(A/β)e-E/RT(1/2)(1-α)[-ln(1-α)]-1. 分解反应的表观活化能分别是300.56 和444.72 kJ·mol-1; 指前因子ln(A/s-1)分别是75.53 和92.50.     

含水杨醛缩对硝基苯甲酰腙的钒酰配合物和钴配合物的合成和晶体结构

本文合成了含水杨醛缩对硝基苯甲酰腙(简写为H2L)的钒酰配合物VOL(CH3OH)(CH3O)(1,C16H16N3O7V,Mr=413.26)和钴配合物[CoL(C5H5N)3]NO3C5H5N(2,C34H29N8O7Co,Mr=720.58)。配合物1属单斜晶系,空间群为P21/c,a=7.3253(3),b=18.8237(9),c=12.9014(5)?b=91.672(1),V=1778.2(1)3,Z=4,F(000)=848,m(MoKa)=0.603mm1,R=0.0470,wR=0.1312。配合物2属单斜晶系,空间群为P21/c,a=11.4196(8),b=17.157(1),c=17.081(1)?b=96.8233(9),V=3323.0(4)3,Z=4,F(000)=1488,m(MoKa)=0.578mm1,R=0.0455,wR=0.1311。在配合物1中,钒(V)原子由周围的酰氧基原子、配体L2的3个配位原子,去质子化甲醇的甲氧基原子和配位甲醇的氧原子配位,形成畸变的VO(ONO)(O)(O)八面体配位构型。晶体内每2个分子间通过氢键作用缔合成中心对称的分子对,OH…N氢键键长为2.861(4)?键角163.20。晶体中存在着弱p-p共轭作用。在配合物2中,钴(Ⅲ)原子由1个L2的3个配位原子和3个配位吡啶分子的3个氮原子配位,呈N4O2八面体配位构型。     

稀土与8-羟基喹啉三元配合物的合成研究Ⅱ.甲基丙烯酸稀土与8-羟基喹啉三元固态配合物的合成与表征

稀土与８－羟基喹啉三元配合物的合成研究Ⅱ．甲基丙烯酸稀土与８－羟基喹啉三元固态配合物的合成与表征王学智（安徽机电学院食品工程系芜湖２４１０００）关键词稀土甲基丙烯酸８－羟基喹啉三元配合物Ｂｉｒｙｕｌｉｎａ［１］首次报导了甲基丙烯酸稀土的合成与表征。８...     

Synthesis and Crystal Structure of a New Oxovanadium（V） Multicomponent Complex with Acylhydrazone and Benzoylhydrazine

A new oxovanadium（V） complex with the mixed ligand of 2-oxopropionic acid benzoylhydrazone （C10H10N2O3） and benzoylhydrazine （C7H8N2O）, VO（C7H7N2O）（C10H9N2O3）, has been synthesized. Its structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to monoclinic system with space group P21/n and cell parameters： a=1.1136（4） nm, b=0.6217（2） nm, c=2.6038（9） nm, β=97.182（6）°, V= 1.7887（11） nm^3, Z=4, F（000）=836, Mr=407.28, Dc= 1.512 g/cm^3,μ （Mo Kα） =0.592 mm^-1, R1 =0.0445, wR2= 0.1203. Vanadium atom is 6-coordinated by carboxyl and carbonyl O atoms and N atom of one tridentate C10H10N2O3 to form two stable five-membered rings with the same edge, and the other coordinated atoms of N and O come from one bidentate benzoylhydrazine C7H8N2O. The title complex has a six-coordinated V center [VO（N2O3）] with a distorted octahedral arrangement. In the crystal lattice, there are hydrogen bonding interactions between two molecules.     

Synthesis, Crystal Structure and Kinetic Mechanism of Thermal Decomposition of a Zinc(II) Complex with N-Salicylidene-p-toluidine

1 INTRODUCTION Over the past decades, considerable attention has been devoted to the synthesis, characterization and property studies of Schiff bases and their com- plexes because of their potential and developed appli- cations in the fields of conducting and magnetic ma- terials, dyes, non-linear optics, catalysis, analytical chemistry, biochemical research, agriculture and so on[1～7]. A large number of reports are available in the chemistry and biologic activities of transition metal co…     

N-（邻甲基苯基）二茂铁磺酰胺的制备、晶体结构及热分解研究

二茂铁磺酰氯与邻甲基苯胺反应合成了N-（邻甲基苯基）二茂铁磺酰胺,通过 元素分析、红外光谱和~1H NMR, ~（13）C NMR对产物结构进行了表征,并对晶体 结构进行了测定。结果表明该化合物为单斜晶系、空间群P2_l/c,晶胞参数a = 1. 0436(2) nm, b = 1.2377(3) nm, c = 1.2643(3) nm, β = 107.42(1)°, V = 1. 5581(6)°, Z = 4, D_c = 1.514 g/cm~3, μ = 1.106 mm~(-1), F(000) = 736, R_1 = 0.0470, wR_2 = 0.0580。采用Gaussian98W软件对此化合物的结构进行了 优化,得到理论结构模型,并与所测量的结构进行了比较。通过热分解实验研究了 该化合物的热稳定性。     

金刚乙胺水杨醛Schiff碱锌(Ⅱ)配合物的合成、表征、晶体结构和热分解动力学研究

A Zinc(Ⅱ) complex [ZnCl₂(HL)₂] with Schiff base HL derived from rimantadine and salicylaldehyde was synthesized and characterized by elemental analysis, infrared spectra, ¹H NMR spectra,molar conductance, ultraviolet and visible spectra, thermal analysis. Its structure was determined by single crystal X-ray diffraction method. The complex, C₃₈H₅₀Cl₂N₂O₂Zn, crystallizes in the orthorhombic system, space group Aba2 with a=1.381 7(3), b=2.275 0(5), c=1.145 0(2) nm, V=3.599(1) nm³, Z=4, M_r=653.79, F(000)=1 496, D_c=1.301 kg·m^-3, μ(Mo Kα)=0.866 mm^-1. The kinetic parameters were obtained from the analysis of TG curve by integral methods. The functions of thermal decomposition reaction mechanism are: F(α)=[1-(1-α)^1/3]², and kinetic compensation effect equation lnA=0.019 1E-0.142 7. CCDC: 253297.     

Synthesis,Crystal Structure and Thermal Decomposition of a New Energetic Potassium Salt of Bis（dinitromethyl）difurazanyl Ether

A new energetic organic potassium salt bis(dinitromethyl)difurazanyl ether potassium salt [K2(BDFE)] was synthesized, and structurally characterized by elemental analysis, IR spectra, 13 C NMR and single-crystal X-ray diffraction. K2(BDFE) crystallizes in monoclinic system, space group C2/c with a = 17.342(3), b = 12.6943(17), c = 8.0972(11), β = 110.630(2)°, V = 1668.3(4)3, Z = 4, Dc = 2.000 g/cm3, F(000) = 1000, μ = 0.675 mm-1, S = 1.058, the final R = 0.0499 and wR = 0.1452. The K ion is eight-coordinated with eight O atoms from one water molecule and four bis(dinitromethyl)difurazanyl ethers(BDFE), forming a distorted dodecahedral structure. Thermal decomposition of the title complex was studied by using DSC and TG-DTG. There are primarily two exothermic decomposition processes between 200 and 370 ℃.     

Synthesis, Crystal Structure and Thermal Property of a Manganese(II) 4-Carboxyphenoxyacetate Complex

1 INTRODUCTION Organic aromatic carboxylic acids which com-monly possess multiple coordination modes are ex-cellent candidates for constructing supramolecularmetal complexes[1～6]. 4-Carboxyphenoxyacetic acid(4-CPOAH2), widely used in biological activitystudies, is a multidentate flexible ligand that not onlyhas versatile binding possibilities but also can formregular hydrogen bonds as both hydrogen-bond donorand acceptor. However, there have been few reportson the coordination chemistr…     

一维链状镉配合物的合成及结构表征

在甲醇体系中合成了镉配合物[Cd(L)₂(H₂O)₂](ClO₄)₂·MeOH (1)[L=1,3,5-三(3-吡啶基甲氧基)苯]。通过元素分析及X-射线单晶衍射对其进行了表征。结构分析结果表明该化合物属于三斜晶系,P1空间群,晶胞参数为a=1.057 1(5) nm,b=1.059 0(5) nm,c=1.270 8(7) nm,α=87.460(16)°,β=81.895(17)°,γ=62.326(14)°,晶胞体积V=1.247 0(11) nm³,Z=1,D_calc=1.569 g·cm^-3,F(000)=604,μ=6.26 cm^-1,R=0.035 2,wR=0.066 4。在化合物1中,每个Cd(II)的配位环境为变形八面体,而每个配体L通过其两个吡啶基团连接2个Cd(II)形成一维链状结构,并进一步通过O-H…N,O-H…O和C-H…O氢键作用形成了一个具有三维结构的超分子化合物。     

Synthesis, Crystal Structure and Thermal Stability of (Diacetylacetone)(diimidazole)Nickel(II) Complex

1 INTRODUCTION Acetylacetone is well known as the intermediate product of organic synthesis reaction, which can be used as annexing agent in gasoline, lubricant and desiccant in paint. Also it has been found to possess fungicidal and insecticidal activi…     

酪氨酸希夫碱邻菲咯啉氧钒配合物的合成、结构及其与DNA相互作用研究

合成了一个新的L-酪氨酸萘酚醛希夫碱及邻菲咯啉混配氧钒配合物[VO(Naph-L-Tyr)(Phen)]•CH₃OH (Naph-L-Tyr＝2-羟基-1-萘甲醛与L-酪氨酸形成的希夫碱, Phen＝1,10-邻菲咯啉). 利用元素分析、红外光谱和X射线单晶衍射进行了表征. 晶体结构测定表明, 该晶体属于三斜晶系, P-1空间群, 其晶体学数据: a＝1.00023(11) nm, b＝1.13478(12) nm, c＝1.34076(15) nm, a＝108.118(2)o, b＝96.3920(10)o, g＝92.4010(10)o, V＝1.4326(3) nm³, Z＝2, D_c＝1.420 g/cm³, F(000)＝634, 最终的偏差因子为R₁＝0.0670, wR₂＝0.1324 [I＞2s (I)]. 以钒原子为中心形成了六配位变形的八面体构型, 晶体中相邻分子之间通过氢键和π-π相互作用形成一维链状结构. 利用紫外吸收光谱、荧光光谱、圆二色光谱和粘度测量等研究了配合物与小牛胸腺DNA (CT-DNA)的作用, 结果表明配合物以插入方式与CT-DNA作用. 琼脂糖凝胶电泳法研究表明, 配合物对质粒pBR322 DNA分子具有切割作用.