共查询到20条相似文献,搜索用时 187 毫秒
1.
在140℃下,以3-溴-4-甲基苯甲酸和咪唑为配体,通过水热法在甲醇/水混合溶剂中反应24 h合成了锌(Ⅱ)配合物Zn(C3H4N2)2(C8H6O2Br)2。通过元素分析、红外光谱、热重分析和X射线粉末衍射对配合物进行了结构表征,同时用X射线单晶衍射分析确定了其晶体结构。结果表明,其晶体属单斜晶系,空间群为C2/c,晶胞参数:a=13.257(3),b=9.765(2),c=20.494(4),β=107.79(3)°,V=2526.3(9)3,Dc=1.655g·cm-3,μ=4.170mm-1,F(000)=1248,Z=4,最终残差因子R1=0.0552,wR2=0.1378。配合物为单核结构,中心锌(Ⅱ)离子与来自2个3-溴-4-甲基苯甲酸根的2个O原子及2个咪唑分子的2个N原子配位,形成了畸变的四方锥几何体。晶体内,分子间则通过N—H…O氢键作用在ab面形成了层状结构。研究了配合物的发光性质。 相似文献
2.
在无水乙醇中, 使低水合氯化稀土 (RE = Ho, Er, Tm, Yb, Lu) 与吡咯烷二硫代氨基甲酸铵 (APDC)和1,10-菲咯啉 (o–phen•H2O) 反应, 制得其三元固态配合物. 用化学分析和元素分析确定它的组成为RE(C5H8NS2)3(C12H8N2) (RE = Ho, Er, Tm, Yb, Lu). IR光谱说明RE3+ 分别与3个PDC–的6个硫原子双齿配位, 同时与o–phen的2个氮原子双齿配位, 配位数为8. 用精密转动弹热量计测定了它们的恒容燃烧热△cU分别为(-16788.46 ± 7.74), (-15434.53 ± 8.28), (-15287.80 ± 7.31), (-15200.50 ± 7.22)和(-15254.34 ± 6.61) kJ•mol-1; 并计算了它们的标准摩尔燃烧焓△cHmθ和标准摩尔生成焓△fHmθ分别为( -16803.95 ± 7.74), (-15450.02 ± 8.28), (-15303.29 ± 9.28), (-15215.99 ± 7.22), (-15269.83 ± 6.61) kJ • mol-1和 (-1115.42 ± 8.94), (-2477.80 ± 9.15), (-2619.95 ± 10.44), (-2670.17 ± 8.22), (-2650.06 ± 8.49) kJ•mol-1. 相似文献
3.
C4H8N2H4·Zn(HPO3)2的水热合成和结构表征 总被引:5,自引:5,他引:5
在过去的十几年中 ,人们对含有机模板的、由 Zn O4 四面体和 PO4 四面体基本结构单元组成的磷酸锌盐进行了深入广泛的研究 ,发现其结构具有多样性 [1] .近年来 ,人们又开始探索用亚磷酸氢根( HPO3)替代磷酸根 ( PO4 ) ,形成结构新颖的含有机模板的亚磷酸盐 .与磷酸根相比 ,亚磷酸氢根只能与 3个邻近的阳离子通过 P— O— M( M=Zn等 )键相连 ,结构同 [PO3( OH) ]相似 .鉴于此 ,HPO3完全可以作为搭建空旷骨架化合物的结构基元 .与磷酸盐的研究相比 ,以有机胺为模板的过渡金属亚磷酸盐合成研究相对较少 .Harrison等 [2 ,3] 报道了通过… 相似文献
4.
H. Chen X. L. Wu L. Shi G. Huang X. J. Lin D. W. Meng 《Russian Journal of Coordination Chemistry》2011,37(10):725-729
The novel 3D coordination polymer {Cd2(C4H2O4)2(C4H6N2)2(H2O)2 · 2H2O}
n
(I) has been synthesized and characterized by standard solid state methods including single-crystal X-ray crystallography. The
compound crystallizes in triclinic space group P
[`1]\bar 1 with a = 8.589(4), b = 10.585(3), c = 13.094(1) ?, α = 84.91(4)°, β = 79.21(0)°, γ = 83.76(4)°, V = 1159.5(1) ?3, Z = 2. The fumaric acid acts as a multimodal bridging ligand in the polymer unit. One of the fumaric acid ligands tridentately
chelates to two Cd2+ cations in the same dinuclear unit, while the other bidentately chelates to two Cd2+ cations in another dinuclear unit. The two metal centers possess slightly distorted pentagonal bipyramid geometry with four
Cd {(μ4-fumarato)-(μ2-fumarato)-bis(2-methylimidazolyl)-diaqua} units joining together to form a 28-membered ring. The whole molecule exhibits a through channel
along y-axis and 2D layers in xz plane. With hydrogen bond and π-π interaction, the 2D layers construct a 3D microporous network. 相似文献
5.
Eu2(p-ClC6H4COO)6(C12H8N2)2配合物热分解机理及非等温动力学 总被引:2,自引:0,他引:2
The thermal decomposition behaviour of europium p-chlorobenzoate complex with 1, 10-phenanthroline and its kinetics were studied in nitrogen by non-isothermal thermogravimetry.Its thermal decomposition occurs mainly in three steps..The intermediate and residue for each step of decomposition were identified from TGcurve.The kinetic parameters were obtained from analysis of the TG-DTG curves by the Achar method.the Madhusudanan- Krishnan-Niman (MKN) method and Ozawa method respectively.The most probable mechanisms function for the first and second stage were suggested by comparing the kinetic parameters. 相似文献
6.
The complex [Co(Im)6](Cin)2 (Im=imidazole,Cin=cinnamate) was prepared by reaction of Co(PhCHCHCOO)2 with imidazole in ethanol. It has been determined by single crystal X-ray analyses. The crystals are triclinic, space group P, with a=9.7601(3),b=10.5935(3),c=11.3269(2)(A),α =69.948(1),β =71.027(1),γ =62.803(1)°, and Z=1. The crystal structure of the title complex consists of monomeric [Co(Im)6]2+ cations and cinnamate anions in which the cobalt(Ⅱ) ion assumes a centrosymmetric octahedral geometry with the CoN6 chromophore. In the solid state, the complex forms a three dimensional network through N-H… O hydrogen bonds, the intermolecular hydrogen bonds connect the [Co(Im)6]2+ cations and cinnamate anions.The cinnamate anions are nearly planar. 相似文献
7.
The complex has been synthesized and characterized by spectroscopic techniques and single-crystal X-ray analysis. The crystal is orthorhombic , space group P212121 with a=1.6620(3)nm, b=1.7300(4)nm, c=0.5450(1)nm and Z=4. In the crystal lattice, the molecules create a two-dimensional network structure through hydrogen bonds. The C-H…O intermolecular hydrogen bonds connect the title complex to form layer super-molecular plane structure perpendicular to the axis b, with the layers stacked by the Van der Waals interaction. CCDC: 195309. 相似文献
8.
9.
配合物[Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N的结构与磁性研究 总被引:4,自引:0,他引:4
The complex [Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N has been synthesized and characterized by X-Ray diffraction, IR and variable temperature (~10 to ~278K) magnetic susceptibility. X-Ray diffraction result for the single crystal shows that the crystal belongs to monoclinic, space group P21/c, a=1.0969(3)nm, b=2.0903(5)nm, c=2.0481(6)nm, β=97.366(6), V=4.657(2)nm3, Z=4, Dc=1.47g·cm-3。 相似文献
10.
T. M. Polyanskaya E. A. Ilinchik V. V. Volkov M. K. Drozdova O. P. Yureva G. V. Romanenko 《Journal of Structural Chemistry》2008,49(3):494-503
A novel compound of {[(C6H5)NH]2C=NH(C6H5)}[B(C6H5)4]·C2H5OH is prepared and examined by single crystal X-ray diffraction. Crystal data: C45H44BN3O, M = 653.64, monoclinic, space group P21/c, unit cell parameters: a = 24.375(2) Å, b = 17.5829(15) Å, c = 18.090(1) Å, β = 105.277(2)°, V = 7479.0(11) Å3, Z = 8, d
calc = 1.161 g/cm3, T = 293 K, R
1 = 0.064. The structure contains two crystallographically independent cations, two anions, and two solvate ethanol molecules.
Three types of interactions occur between them: interionic N-H(N)⋯π and N(H)⋯π⋯H(C), π-delocalized system of Ph rings of the
anions, and interaction of ions with ethanol molecules N-H⋯O-H(O)⋯π. The compound is characterized by IR and luminescence
spectra. At room temperature, the emission intensity grows with time of exposure to UV irradiation.
Original Russian Text Copyright ? 2008 by T. M. Polyanskaya, E. A. Il’inchik, V. V. Volkov, M. K. Drozdova, O. P. Yur’eva,
and G. V. Romanenko
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 3, pp. 512–521, May–June, 2008. 相似文献
11.
在水乙醇混合溶剂中,首次得到了2-羰基丙酸水杨酰腙、1,10-菲啰啉与硝酸钆形成的配合物[Gd(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O,并测试了其单晶结构。该配合物属三斜晶系,空间群为P-1。每个配合物分子中有两个九配位的钆的结构单元,每个钆离子与两个三齿配体2-羰基丙酸水杨酰腙(分别以负一价和负二价形式)和三个水分子配位。每个钆单元在空间呈扭曲的单帽四方反棱柱。同时还有一个游离的1,10-菲啰啉存在于晶格中,通过氢键与配位水作用。生物活性试验表明该配合物对三种病原菌有一定的抑菌活性。 相似文献
12.
[Eu2(o-ClC6H4OCH2COO)6(C12H8N2)2(H2O)2]·(CH3)2SO的晶体结构和荧光光谱 总被引:1,自引:0,他引:1
标题配合物M=1892.01,单斜晶系,空间群P21/c, a=1.2975(3) nm, b=2.6591(9) nm, c=1.2118(3) nm, β=96.95(1)°, Z=2, Dc=1.577 g/cm3, T=293(2)K。最终的偏离因子R=0.0583。该配合物以二聚体形式存在,通过其中的桥联羧基形成了双核分子。该分子中羧基具有桥联双齿、桥联三齿和单齿三种配位模式,Eu-Eu之间的距离为0.4019(1) nm。在77K下测得配合物中Eu(Ⅲ)离子仅有一种格位。 5D0→ 7FJ(J=0~2)跃迁光谱说明Eu(Ⅲ)离子格位具有C2对称性。 相似文献
13.
14.
合成了高氯酸镨和咪唑(C3H4N2), DL-α-丙氨酸(C3H7NO2)混配配合物晶体. 经傅立叶变换红外光谱、化学分析和元素分析确定其组成为[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3. 使用具有恒温环境的溶解-反应量热计, 以2.0 mol•L-1 HCl为量热溶剂, 在T=(298.150±0.001) K时测定出化学反应PrCl3•6H2O(s)+2C3H7NO2(s)+C3H4N2(s)+3NaClO4(s)=[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s)+3NaCl(s)+5H2O(1)的标准摩尔反应焓为ΔrHmө=(39.26±0.11) kJ•mol-1. 根据盖斯定律, 计算出配合物的标准摩尔生成焓为ΔfHmө{[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s), 298.150 K}=(-2424.2±3.3) kJ•mol-1. 采用TG-DTG技术研究了配合物在流动高纯氮气(99.99%)气氛中的非等温热分解动力学, 运用微分法(Achar-Brindley-sharp和Kissinger法)和积分法(Satava-Sestak和Coats-Redfern法)对非等温动力学数据进行分析, 求得分解反应的表观活化能E=108.9 kJ•mol-1, 动力学方程式为dα/dt=2(5.90×108/3)(1-α)[-ln(1-α)]-1exp(-108.9×103/RT). 相似文献
15.
合成了高氯酸镨和咪唑(C3H4N2), DL-α-丙氨酸(C3H7NO2)混配配合物晶体. 经傅立叶变换红外光谱、化学分析和元素分析确定其组成为[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3. 使用具有恒温环境的溶解-反应量热计, 以2.0 mol•L-1 HCl为量热溶剂, 在T=(298.150±0.001) K时测定出化学反应PrCl3•6H2O(s)+2C3H7NO2(s)+C3H4N2(s)+3NaClO4(s)=[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s)+3NaCl(s)+5H2O(1)的标准摩尔反应焓为ΔrHmө=(39.26±0.11) kJ•mol-1. 根据盖斯定律, 计算出配合物的标准摩尔生成焓为ΔfHmө{[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s), 298.150 K}=(-2424.2±3.3) kJ•mol-1. 采用TG-DTG技术研究了配合物在流动高纯氮气(99.99%)气氛中的非等温热分解动力学, 运用微分法(Achar-Brindley-sharp和Kissinger法)和积分法(Satava-Sestak和Coats-Redfern法)对非等温动力学数据进行分析, 求得分解反应的表观活化能E=108.9 kJ•mol-1, 动力学方程式为dα/dt=2(5.90×108/3)(1-α)[-ln(1-α)]-1exp(-108.9×103/RT). 相似文献
16.
L. Mei C. Jie H. B. Yang Z. S. Ming Y. Hao T. H. Ming 《Journal of Structural Chemistry》2011,52(4):748-754
(C8H11N)2·Zn(OAc)2 (1a), (C8H11N)2·Cu(OAc)2 (1b), and (C8H11N)2·CuCl2 complexes are synthesized by a simple one-pot method. The crystal structures of 1a, 1b, and 1c are determined by X-ray crystallography. The complexes are also characterized by NMR, IR, MS, and elemental analysis and
used as the catalysts applied to the Henry reaction; moderate to high yields are obtained at room temperature. 相似文献
17.
以5-硝基间苯二甲酸,1,10-邻菲啰啉,硫酸锰(MnSO4.H2O)为原料合成了一种结构新颖的金属配位聚合物——[Mn2(C8H3NO6)2(C12H8N2)2]n(1),其结构经IR,XRD,TG-DTG和元素分析表征。X-射线单晶衍射测试结果表明,1属三斜晶系,空间群Pī,晶胞参数a=10.060 2(1),b=14.343 5(2),c=14.663 7(2),α=104.052(1)°,β=102.633(1)°,γ=110.460(1)°,Mr=888.52,V=1 812.69(4)3,Z=2,Dc=1.628 g.cm-3,F(000)=900。以30%H2O2为氧化剂,初步研究了1在苯乙烯氧化反应中的催化氧化性能。 相似文献
18.
A novel binuclear praseodymium(III) complex with N-(2-propionyl)salicyloylhydrazone (C10H10N2O4, H3L) and p-hydroxybenzoic acid (C7H6O3, Phba) was prepared in a H2O-C2H5OH mixed solution, and the crystal structure of [Pr2(H2L)2(Phba)4(H2O)2] · 2H2O (I) was determined by X-ray single crystal diffractometry. Complex I crystallizes in the monoclinic system, space group P21/c, a = 1.1050(4), b = 1.9534(7), c = 1.2376(4) ?, β = 94.955(7)°, and Z = 4. In the structure each Pr3+ ion lies in a single capped square antiprism geometry coordinated by carboxyl O and acyl O atoms and azomethine N atom of
one ligand (H2L− form), which coordinates via the keto form, four carboxyl O atoms from two Phba, and O atoms of two water molecules. In each
molecule, two tridentate ligands were coordinated by the H2L− form, and each Pr3+ ion was chelated by the carboxyl group from Phba. The carboxyl groups of H2L− and other two Phba were coordinated via μ2-bridging form and bidentate bridging form, respectively. Complex I and ligands Phba and H3L were also searched for biological activity against Valsa mali by the growth rate method. The result showed that the inhibitory
rate of ligands Phba and H3L is better than complex I, especially Phba. 相似文献
19.
[Ce(NO3)5H2O]·(C3H5N2)2的合成、晶体结构及热分析 总被引:2,自引:0,他引:2
Colorless crystal, [Ce(NO3)5H2O]·(C3N2H5)2, has been obtained from the reaction of Ce(NO3)3 with imdazole in the aqueous solution and its crystal structure has been determined by single crystal X-ray diffraction techniques.The crystal belongs to triclinic, space group P1. The cell parameters are: a = 0.7489(1) um, b = 0.7914(2) nm, c = 1.8139(3) nm, a = 89.39(2)°, β = 89.37(l) °,γ = 63.18(2)°, Dc = 2.1g·cm-3, Z = 2, R = 0.0319.In the compound, all of five nitrates are bidentate and one molecule of water is monodentate, the coordination number of Ce (Ⅲ) is 11.The processes of thermal decomposition of the compound was proposed by its TGcurve. 相似文献