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1.
采用水热方法合成出一种稀土配位聚合物[Eu2(Suc)0.5(BC)3(OH)2]n(Suc=琥珀酸根离子,BC=苯甲酸根离子),并通过X射线单晶结构分析、元素分析以及红外光谱对该配合物进行了表征。结构分析表明标题配合物的晶体属于三斜晶系,P^-1空间群。金属铕离子、OH和“Eu-O-C.0.Eu”形成无限的无机带,无机带之间通过琥珀酸和苯甲酸连接形成二维开放骨架结构。本文对标题配合物的荧光性质和热稳定性也做了详细的分析。  相似文献   

2.
由Cu(Ⅱ)的硝酸盐与四氟对苯二甲酸(H2tfbdc)的自组装得到标题配合物.用元素分析、红外光谱、热重分析、X-衍射单晶结构分析等对其进行了表征.晶体结构表明,标题配合物的晶体属单斜晶系,空间群为C2/c,晶胞参数:a=3.3739(5)nm,b=1.5696(2)am,c=1.641 9(2)nm,β=1 17.527(2)°.每个铜离子与来自4个四氟对苯二甲酸分子的4个氧原子和1个N,N-二甲基甲酰胺分子中的氧原子配位,形成四方锥的配位构型.四氟对苯二甲酸根桥连铜离子形成具有孔穴的二维层状结构,相邻的层状结构又通过氢键形成三维的超分子网络结构.配合物中一些苯环上的-CF基团具有无序结构.变温磁化率数据(300~1.8 K)显示配合物中分别存在反铁磁性和铁磁性相互作用.  相似文献   

3.
合成了一种新的双核倒反中心的稀土镧配合物{La[o-C6H4(NO2)(CO2)]3·(DMF)2}2. 通过元素分析、 核磁共振谱和红外光谱对配合物的组成和结构进行了表征,  用热重分析研究了该配合物的热稳定性,  用X射线单晶衍射法测定了其晶体结构. 镧配合物{La[o-C6H4(NO2)(CO2)]3·(DMF)2}2晶体属三斜晶系, 空间群P1,  晶胞参数a=1.902(2) nm, b=1.245 0(2) nm, c=1.298 7(2) nm, α=64.555(2)°, β=66.348(2)°, γ=71.920(2)°, V=1.569 5(5) nm3, Dc=1.658 Mg/m3, Z=2, μ=1.437 mm-1, F(000)=784. 配合物中有2个La(Ⅲ)被4个邻硝基苯甲酸的羧酸根的负氧离子桥联, 每个La(Ⅲ)的中心离子配位数为9,  配位原子分别来自于7个邻硝基苯甲酸的羧酸根的负氧离子和2个DMF的羰基氧原子. 化合物中的氢键和π…π堆积作用使其成为三维立体结构. 同时发现了标题化合物固体具有光致发光现象, 发光性能测试表明, 配合物具有很好的荧光性质.  相似文献   

4.
赵明星  高颖  孟跃  倪生良 《化学通报》2014,77(11):1116-1119
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   

5.
在乙醇和水的混合溶剂中以间硝基苯甲酸(m-nitrobenzoic acid)、邻菲咯啉(phen)为原料合成了一个新的配合物[Cd(m-nitrobenzoic acid)2(phen)2]·(H2O)2,该配合物晶体属三斜晶系,空间群P1。配合物中镉原子与2个phen的4个N原子和2个间硝基苯甲酸根的3个羧基氧原子配位形成七配位的五角双锥结构。电化学性质研究表明:标题配合物  相似文献   

6.
合成了乙酰丙酮缩邻氨基苯甲酸Schiff碱(HAAABA)(HAAABA=acetylacetone-o-aminobenzoic acid),获得了其锌和锰的配合物单晶[M(AAABA)2(py)2(H2O)2,M=Zn,1;Mn,21.产物经IR、核磁共振谱、元素分析、X-射线单晶结构分析等表征.两晶体均属于单斜晶系,空间群为P21/m.用Guassian 03W程序,在B3LYP/6-31G等水平上对标题化合物进行了几何全优化,并对其成键情况、自然键轨道(NBO)及键能进行了分析.在DMF中测定了Schiff碱配体及其锌配合物的荧光性质.  相似文献   

7.
黄春芳  陈华龙 《无机化学学报》2007,23(12):2035-2038
合成了一个Mn(Ⅱ)的配合物[Mn(NPA)2(Phen)(H2O)2](NPA=N-苯基代邻氨基苯甲酸,Phen=邻菲咯啉),经红外光谱、紫外光谱、元素分析、差热,X射线单晶衍射等表征,其晶体结构为单斜晶系,C2/c空间群。标题配合物中的Mn原子与2个N-苯基代邻氨基苯甲酸的2个氧原子、1个Phen的2个N原子,2个水分子的氧原子形成六配位八面体结构。  相似文献   

8.
以异烟酸和邻菲咯啉(phen)为原料,采用水热合成方法,合成了一个新的配位聚合物{[Cd2(phen)2(H2O)2(C6H5NO2)2]·(ClO4)}n,测定了其晶体结构.结果表明:该配合物晶体属单斜晶系,空间群P21/n.与中心镉(Ⅱ)离子配位的3个氧原子分别来自2个异烟酸根和1个水分子,3个氮原子分别来自1个异烟酸根和1个邻菲咯啉,形成六配位变形八面体结构.由于异烟酸的桥联作用及氢键作用,配合物堆积成三维网状结构;同时配合物通过异烟酸的羧基双齿桥联配位以及邻菲咯啉和水分子作为端基配位.形成了双核笼状结构,其Cd(Ⅱ)…Cd(Ⅱ)距离为0.8798 nm.此外,还研究了该聚合物的荧光性质.  相似文献   

9.
采用水热方法,合成出一种新颖的刚柔混合多羧酸稀土配位聚合物[Gd(bta)0.5(ad)0.5(H2O)]n(H2ad=己二酸,H4bta=1,2,4,5-均苯四甲酸),并通过元素分析、红外光谱、X射线单晶结构分析对标题配合物进行了表征。标题配合物属于单斜晶系,P21/n空间群,晶胞参数a=0.77765(18)nm,b=0.72405(17)nm,c=1.7351(4)nm,β=91.649(3)°,V=0.9766(4)nm3,Dc=2.533 g·cm-3,Z=4。结构分析表明:标题配合物结构中含有沿[100]方向的无限一维Tb-O-Tb聚合链。此Tb-O-Tb聚合链通过桥连配体1,2,4,5-均苯四甲酸与己二酸连接,最终形成复杂的三维开放网络结构。此外,我们还对标题化合物的热稳定性做了研究。  相似文献   

10.
[Eu2(BA)6(bipy)2]的晶体结构和荧光光谱   总被引:6,自引:0,他引:6       下载免费PDF全文
标题配合物晶体属单斜晶系,P21/n空间群,晶胞参数a=1.4162(3) nm,b=1.5377(5) (nm), c=2.6017(5) nm, β=103.56(3°), Z=4。标题配合物是双核分子,4个苯甲酸的羧基桥联两个中心Eu(Ⅲ)离子。它们又分别与1个苯甲酸的羧基的两个氧原子和一个联吡啶分子的两个氮原子螯合配位,形成4,4′-双帽三角棱柱体。两个Eu(Ⅲ)离子的Eu-O和Eu-N平均键长不等。两个Eu(Ⅲ)离子的化学环境略有不同。在配合物的 7F05D0激发光谱里,580.17和580.31 nm处呈现两个锐峰,可以认为配合物具有两种Eu(Ⅲ)格位,选择激发配合物的 5D0能级,得到的 5D07F1,2发光光谱表明配合物中Eu(Ⅲ)离子有不同的化学环境,这与晶体结构分析结果一致。  相似文献   

11.
Crystal structures of Pb(MoO2)2(PO4)2 and Ba(MoO2)2(PO4)2 were determined. Both compounds contain the molybdyl group MoO2. The monoclinic unit-cell parameters are a = 6.353(7), b = 12.289(4), c = 11.800 Å, β = 92°56(6), and Z = 4 for the lead salt and a = 6.383(8), b = 7.142(7), c = 9.953(8) Å, β = 95°46(8), and Z = 2 for the barium salt. P21c is the common space group. The R values are respectively R = 0.027 and R = 0.031 for 1964 and 1714 independent reflections. The frameworks built up by a three-dimensional network of monophosphate PO4 and molybdyl MoO2 groups are similar, characterized mainly by corner-sharing PO4 and MoO6 polyhedra. Two oxygen atoms of each MoO6 group are bonded to the molybdenum atom only as in other molybdyl salts.  相似文献   

12.
The title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X-ray analysis revealed that the copper(Ⅱ) atom is coordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu-O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354.  相似文献   

13.
The reactions of lanthanide tris(borohydrides) Ln(BH4)3(thf)3 (Ln = Sm or Nd) with 2 equiv. of lithium N,N′-diisopropyl-N′-bis(trimethylsilyl)guanidinate in toluene produced the [(Me3Si)2NC(NPri)2]Ln(BH4)2Li(thf)2 complexes (Ln = Sm or Nd), which were isolated in 57 and 42% yields, respectively, by recrystallization from hexane. X-ray diffraction experiments and NMR and IR spectroscopic studies demonstrated that the reactions afford monomeric ate complexes, in which the lanthanide and lithium atoms are linked to each other by two bridging borohydride groups. The complexes exhibit catalytic activity in polymerization of methyl methacrylate. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 441–445, March, 2007.  相似文献   

14.
The observed difference in transition strength for (SF6)2, (SiF4)2 and (SiH4)2 IR-predissociation spectra is explained by induction effects (μ012/R126) which have to be included in the interaction Hamiltonian in addition to the dominant dipole-dipole term (μ012/R123).  相似文献   

15.
Molecular beam deflection studies on (CO2)2 and (OCS)2 indicate that both these species are polar molecules. Structural implications of this are explored in light of previous studies of these systems.  相似文献   

16.
The reactivity of bis(dimethylamido) complexes of phenyl- and hydridogallium with ammonia, dimethylamine and 1,1-dimethylhydrazine is described. Synthesis of the starting gallium hydride, [HGa(NMe2)2]2, was achieved in nearly quantitative yield from the reaction of HGaCl2(quinuclidine) with LiNMe2. In neat ammonia or methylamine at room temperature both dimethylamido ligands in [HGa(NMe2)2]2 were substituted by a single equivalent of NH3 or MeNH2 to produce amorphous (HGaNH)n or (HGaNMe)n, respectively. In contrast, the reaction of [PhGa(NMe2)2]2 with neat Me2NNH2, at room temperature consumed two equivalents of the substituted hydrazine to form [PhGa(NHNMe2)2]2 in a 73% yield. Single crystal X-ray crystallographic analyses of [HGa(NMe2)2]2 and [PhGa(NHNMe2)2]2 establish that in the solid state both compounds adopt a cyclic Ga-N-Ga-N structure with a crystallographic center of symmetry located at the center of the ring.  相似文献   

17.
[(ZrO2)0.92(Y2O3)0.08]0.9(TiO2)0.1 (titania-doped yttria stabilized circonia, 10TiYSZ) samples were prepared by solid state reaction from mixtures of 8 mol% yttria-doped ZrO2 (YSZ) and TiO2 and characterized in terms of structure, microstructure, and electrical properties. [(ZrO2)0.97(Y2O3)0.03]0.9(TiO2)0.1 (titania-doped tetragonal zirconia polycrystalline, 10TiTZP) was also prepared for comparison in some specific studies. Ionic transport properties were measured by impedance spectroscopy in air as a function of temperature. DC techniques including electromotive force (EMF) and Ion Blocking measurements (IB) were carried out in order to determine the electronic contribution to the total conductivity. The addition of titania to YSZ induces the tetragonal zirconia phase formation, thus [(ZrO2)0.92(Y2O3)0.08]0.9(TiO2)0.1 is a composite material and is constituted by two solid solutions, titania-doped yttria-stabilized zirconia (67.7 mole fraction) and titania-doped tetragonal zirconia (32.3 mole fraction). A decrease in bulk ionic conductivity, of one order of magnitude, when TiO2 is added to YSZ is observed in the whole temperature range. Furthermore, in the bulk conductivity vs the reciprocal of the temperature plot, a bending (from 550°C to higher temperatures) toward higher activation energies was detected. The bending could indicate the existence mainly of Ti4+-Vö associated pairs with an association energy of 0.43±0.02 eV. It could mean that Ti-O bonds become stronger and shorter and could produce the formation of microdomains of a ZrTiO4-like structure. The addition of titanium is effective in increasing the electronic conductivity under reducing conditions. Conductivity as a function of Po2 and IB results cannot be related to the formation of small polarons during the reduction process. Furthermore, according to the calculations based on the small polaron theory, inconsistent values for the radius of a small polaron (rp) are obtained in both 10TiYSZ and 10TiTZP. However, large polarons can explain the transport properties in these materials under reducing conditions in agreement with the experimental data.  相似文献   

18.
Compound [Ni(hmt)2(SCN)2(H2O)2][Ni(SCN)2(H2O)4](H2O)2 (hmt=hexamethylenetetramine) was pre-pared and structurally characterized by means of X-ray single crystal diffraction. The two neutral units [Ni(hmt)2(SCN)2(H2O)2] and [Ni(SCN)2(H2O)4] are joined together through hydrogen bonds N…H-O, O…H-O and S…H-O. In the solid state, the compound has three-dimensional network structure. The determination of its variable-temperature magnetic susceptibilities (5~300K) shows that the magnetic behavior obeys the Curie-Weiss law over the whole temperature ranges.  相似文献   

19.
Phase equilibria in the Ba3(VO4)2-K2Ba(MoO4)2 and Pb3(VO4)2-K2Pb(MoO4)2 systems have been investigated. In the first system, a continuous series of substitutional solid solutions with the palmierite structure is formed, and in the second one, the polymorphic transition in lead orthovanadate at 100°C restricts the extent of the palmierite-type solid solution to 10–100 mol % K2Pb(MoO4)2. Original Russian Text ? V.D. Zhuravlev, Yu.A. Velikodnyi, A.S. Vinogradova-Zhabrova, A.P. Tyutyunnik, V.G. Zubkov, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 10, pp. 1746–1748.  相似文献   

20.
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