双核铕-间甲基苯甲酸邻菲罗琳[Eu(m-MBA)_3PHEN](H_2O)_2三元配合物的晶体结构和荧光光谱

标题配合物晶体属Cc空间群,a=1.5955(6)nm,b=1.8508(6)nm,c=2.2595(9)nm,β=97.79(4)°,Z=4,Dx=1.52g/cm~3,T=295K.用I>3σ(I)的7316个可观察衍射数据对92个非氢原子的原子坐标和各向异性温度因子进行全矩阵最小二乘法精修,最终的偏离因子R=0.043.中心Eu(Ⅲ)离子与周围6个氧和一对氮原子配位,配位多面体属四方反棱柱体,其点对称性为C_1.以Eu(Ⅲ)离子为荧光探针,77K下测得配合物多晶样品的高分辨激光激发光谱和发射光谱,激发光谱表明配合物中Eu(Ⅲ)离子仅有一种晶格格位.~5D_0→~7F_J(J=0～2)跃迁光谱表明中心Eu(Ⅲ)离子在77K下具有C_1对称性.     

3-硝基-1,2,4-三唑-5-酮镱配合物的制备及其晶体结构

３硝基１，２，４三唑５酮（ＮＴＯ）的锂盐水溶液与Ｙｂ２Ｏ３的稀硝酸溶液反应，制备了标题配合物，其化学式为Ｙｂ（ＮＴＯ）３·１０Ｈ２Ｏ。用Ｘ射线衍射法测定配合物的晶体结构，其分子式为［Ｙｂ（ＮＴＯ）３（Ｈ２Ｏ）４］·６Ｈ２Ｏ。属单斜晶系，空间群为Ｃ２／ｃ。晶胞参数如下：ａ＝３６９３１（５）ｎｍ，ｂ＝０６６８３（１０）ｎｍ，ｃ＝２５６５６（３）ｎｍ，β＝１３０９７４（５）°，Ｖ＝４７８１１（１１）ｎｍ３，Ｚ＝８，Ｄｃ＝２０１３ｇ·ｃｍ－３，μ＝４０１７ｍｍ－１，Ｆ（０００）＝２８５０。镱离子的配位数为７，其配位多面体为五角双锥。     

Li2EuSiO4, ein Europium(II)-dilithosilicat: Eu[(Li2Si)O4]

Li₂EuSiO₄, an Europium(II) Litho-Silicate: Eu[(Li₂Si)O₄] Single crystals of Li₂EuSiO₄ were first obtained by reaction of Eu₂SiO₄ with a melt of LiCl at 800 °C in a sealed tantalum tube. It crystallizes with the trigonal space group P3₁21, Z = 3, with a = 502.70(5), c = 1247.0(2) pm. The tetrahedra [LiO₄] and [SiO₄] are connected via common corners and thereby build up a three-dimensional network that leaves space for Eu²⁺ which is in an eightfold coordination. Li₂SrSiO₄ is isotypic with a = 502.59(4) and c = 1247.1(1) pm.     

A New Europium(II) Oxide Iodide: Eu2OI2

Red single crystals of Eu₂OI₂ were obtained from a reaction mixture of barium metal, EuI₂, Eu₄OI₆ and some NH₄I in a tantalum tube at 780/500 °C. The crystal structure (orthorhombic, Imcb, Z = 4, a = 648.93(11), b = 742.85(13), c = 1307.1(3) pm, R1(all) = 0.0605) contains {Eu₄O} tetrahedra connected via trans‐edges to infinite chains. The iodide ions surround and connect these chains to a three‐dimensional structure.     

Synthesis and Characterizaion of a New Inorganic-organic Sulfate Compound--Crystal Structure of [Ni(H2O)6][H2N(C2H4)2NH2](SO4)2

[Ni(H2O)6][H2N(C2H4)2NH2](SO4)2 is an inorganic-organic compound with a new open framework synthesized by hydrothermal method, and characterized by means of single-crystal diffraction and spectroscopic data. The compound crystallized in a monoclinic space group P21/n with a=1.29089(2) nm, b=1.06301(3) nm, c=1.33202(4) nm, β=114.0870(10)°, V=1.67127(8) nm3, Z=4, and was solved by using the direct method and the least-squares refinement converged at R=0.0214[I>2σ(I)]. The structure consists of isolated Ni(H2O)6 octahedra and SO4 tetrahedra, with both of them hydrogen-bonded to piperazine cations.     

Synthesis and Crystal Structure of Lithium Tetrametaphosphimate Tetrahydrate Li4(PO2NH)4 · 4 H2O

Single crystals of Li₄(PO₂NH)₄ · 4 H₂O were obtained by dissolving LiOH and H₄(PO₂NH)₄ · 2 H₂O in water and subsequent precipitation with acetone and ethanol followed by slow evaporation of the solvents. The structure of Li₄(PO₂NH)₄ · 4 H₂O was solved by single‐crystal X‐ray methods ( (No. 2), a = 489.2(2), b = 853.2(2), c = 880.5(2) pm, α = 101.71(3), β = 102.39(3), γ = 94.88(3)°, Z = 1). The structure is composed of LiO₄ tetrahedra and (PO₂NH)₄^4? ions. The P₄N₄ rings of the anions exhibit a slightly distorted chair–1 conformation, which is supported by IR data and has been described by torsion angles, displacement asymmetry parameters and puckering parameters. Via Li⁺ ions and hydrogen bonds, the tetrametaphosphimate anions are connected forming a three‐dimensional network.     

Eu2(3,4-DMBA)6(PHEN)2的晶体结构及HRS研究

合成了铕（Ⅲ）与３,４－二甲基苯甲酸（３,４－ＨＤＭＢＡ）、邻菲咯啉（ＰＨＥＮ）形成的晶体配合物Ｅｕ２（３,４－ＤＭＢＡ）６（ＰＨＥＮ）２．测定其分子量Ｍ＝１５５９．３５,晶体属三斜晶系,Ｐ１空间群,ａ＝１．２６６５（４）ｎｍ,ｂ＝１．３５６７（４）ｎｍ,ｃ＝１．０７５５（４）ｎｍ,α＝９８．８７（３）°,β＝１０８．２５（３）°,γ＝８７．９８（２）°,Ｚ＝１,最终的偏离因子Ｒ＝０．０３１．以Ｅｕ（Ⅲ）离子为荧光探针,在７７Ｋ下测定了配合物的高分辨光谱（ＨＲＳ）．铕配合物的激发光谱、发光光谱、时间分辨光谱和发光寿命测定结果表明,该配合物中存在两种化学环境不同的Ｅｕ（Ⅲ）离子格位     

Synthesis,crystal structure,and luminescence of a quaternary binuclear europium complex [Eu2(phth)2(Hphth)2(phen)2(H2O)4]

A quaternary binuclear europium complex [Eu₂(phth)₂(Hphth)₂(phen)₂(H₂O)₄] (H₂phth?=?phthalic acid, phen?=?1,10-phenanthroline) has been synthesized. The structure was determined by X-ray crystallography which reveals that it is binuclear with each europium nine-coordinate. Intermolecular hydrogen bonds link the complex units to form a 3D supermolecular network. Its properties have been studied by means of luminescence spectrum and thermal analysis. Fluorescence spectra show that the complex exhibits strong red emission.     

A Novel Route to Triphenylgermyl Europium Complexes. Crystal Structure of (Ph3Ge)2Eu(DME)3

(Ph₃Ge)₂Eu(THF)₄ ( 1 a ) and (Ph₃Ge)₂Eu(DME)₃ ( 1 b ) have been synthesized by reacting Ph₃GeH with europium naphthalene, C₁₀H₈Eu(THF)₂, in THF or DME, respectively. The reaction of Ph₃GeH with C₁₀H₈[EuI(DME)₂]₂ in DME yielded Ph₃GeEuI(DME)₂ ( 2 ). The addition of two equivalents of CH₃I to a solution of 1 b in THF produced Ph₃GeMe and EuI₂(DME)₂ with almost quantitative yields. Complex 2 easily disproportionates forming mixtures of 1 b and EuI₂(DME)₂. The molecular structure of 1 b was determined from X-ray diffraction data.     

Synthesis,Structural, and Optical Characterization of a New Europium(II) Tin Selenide,Eu8(Sn4Se14)(Se3)2 with a (Sn4Se14)12– Building Block

A new phase in europium‐tin‐chalcogenide chemistry has been prepared using the reactive flux method: Eu₈(Sn₄Se₁₄)(Se₃)₂. The compound crystallizes in the orthorhombic space group P2₁2₁2 with cell parameters a = 11.990(2) Å, b = 16.425(4) Å, c = 8.543(1) Å, and Z = 2. Eu₈(Sn₄Se₁₄)(Se₃)₂ is a three dimensional structure with Eu^II cations linked together with an unusual (Sn₄Se₁₄)^12– anionic unit and (Se₃)^2– chains. UV‐VIS‐NIR band‐gap analysis shows that these black metallic crystals are likely semiconductors with an optical band‐gap of 1.07 eV.     

Synthesis and Crystal Structure of Dinuclear Copper Complex[Cu（CH2O（C6H4）N=C（C6H4）O）（Py]2

1 INTRODUCTION Synthesis of transition metal complexes with Schiff-base has been a subject of considerable importance [1,2]. They are not only good complexing agents for Schiff-base, but also good bactericide and antitumour agent [3,4]. At present, there is a spectacular growth in this field. Recently, some bridged binuclear complexes have received much attention on account of their biological relevance and condensed-phase magnetic properties[5,6]. Especially, the complexes containin…     

Synthesis, Crystal Structure and Properties of Complex VO（C12H12N2O2） （C13H10NO2）

IntroductionAsthevanadate dependentenzyme ,ahaloperox idase,andvanadiumnitrogenasehavebeenfoundinsuccession ,somescientistsareinterestedinthecoor dinationchemistryandthebiochemistryofvanadi um[1] .Thereactivecenterofvanadiumbromoperoxi dasecontainstheoxovanadiumVO3+ coordinatedbyoxygenandnitrogenatoms[2 ] .However,thestudiesaboutoxovanadiumVO3+ coordinationcompoundscontainingbioactiveligandsarerarelyfound[3— 8] .Hydroximicacidthatcanbeconsideredtobethederivativeofthecarboxylicacid ,theamide…     

Dicarboxylatgruppen als Liganden und Anionen in Aquamagnesiumkomplexen: Kristallstrukturen von [Mg (C4H2O4)(H2O)4] · H2O und [Mg(H2O)6](C4HO4)2 · 2H2O ((C4H2O4)2— = Fumarat; (C4HO4)— = Hydrogenacetylendicarboxylat)

Dicarboxylate Groups as Ligands and Anions in Aquamagnesium Complexes: Crystal Structures of [Mg (C₄H₂O₄)(H₂O)₄] · H₂O and [Mg(H₂O)₆](C₄HO₄)₂ · 2H₂O ((C₄H₂O₄)^2— = Fumarate; (C₄HO₄)^— = Hydrogenacetylenedicarboxylate) Crystals of tetraaqua(fumarato)magnesium‐hydrate ( 1 ) and hexaaquamagnesium‐bis(hydrogenacetylenedicarboxylate)‐dihydrate ( 2 ) were prepared by reacting MgCl₂ with sodium fumarate and acetylenedicarboxylic acid, respectively. In 1 cis‐Mg(H₂O)₄ units are bridged by α, Ö‐bonded fumarate groups. The resulting zig zag chains exhibit the maximum symmetry compatible with space group symmetry C2/c. 2 consists of layers of voluminous [Mg(H₂O)₆]²⁺ cations alternating with layers of C₄HO₄^— anions. The nearly planar anions are held together by parallel stacking and by short hydrogen bonds. Both structures contain efficient H bridging systems. 1 : Space group C2/c, Z = 4, lattice constants at 20 °C: a = 5.298(1), b = 13.178(2), c = 13.374(2)Å; ß = 94.79(2)°, R₁ = 0.024. 2 : Space group P1, Z = 1, lattice constants at 20 °C: a = 5.985(1), b = 6.515(1), c = 11.129(1)Å; α = 105.24(2), ß = 91.87(3), γ = 90.92(1)°, R₁ = 0.034.     

Synthesis and Crystal Structure of[Ni(C5H2N2O4)(2, 2'-bipy)(H2O)2]·2H2O

The crystal structure of [Ni(C5H2N2O4)(2, 2?-bipy)(H2O)2]·2H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P ī with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) (A。）, α = 84.771(1), β = 77.375(2), γ = 68.993(2)°, C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) (A。）3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, ((MoK() = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2((I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2'-bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and (-( stacking interaction of aromatic rings from 2, 2'-bipy results in a 3D structure.     

金属有机盐[CpFe(C6H6)]2·[Ni(mnt)2]的合成及晶体结构

通过[CpFe(C6H6)]PF6与Na2[Ni(mnt)2]复分解反应合成了金属有机盐[CpFe(C6H6)]2·[Ni(mnt)2],用元素分析、红外光谱和1H NMR进行了鉴定,并用X射线测定了晶体结构.结构分析表明,该化合物属于三斜晶系,空间群P1.晶胞参数:α=0.838(2)nm,b=1.084(6)nm,c=1.816(7)nm,α=83.41(4)°β=89.30(3)°,γ=80.22(3)°Z=2.晶体中混式夹心的阳离子处于几乎互相垂直的取向.配阴离子平面也存在两种取向,它们形成75.4°的二面角.测试表明,化合物表现半导体属性,其粉末压片室温电导率为4.1×10-S·cm-1.     

[Cu(PTA)(Phen)2](p-MBA)(H6O)配合物的合成、晶体结构及电化学分析

The crystal structure of the title complex with the stoichiometric formula [Cu(PTA)(Phen)₂](p-MBA)(H₆O) (Phen=1,10-phenanthroline, PTA=terephthalic acid, p-MBA=p-toluic acid) has been determined by single-crystal X-ray diffraction. The crystal (C₄₈H₄₀CuN₄O₁₀, M_r=896.38) belongs to the monoclinic space group C2/c, with the following crystallographic parameters: a=1.778 6(3) nm, b=1.912 5(3) nm, c=1.389 9(2) nm, β=114.686(2)°, V=4.295 7(12) nm³, D_c=1.386 g·cm^-3, Z=4, μ(Mo Kα)=0.574 mm^-1, F(000)=1 860, final GooF=1.019, R=0.054 0, wR=0.148 3 for 2 644 observed reflections (I>2σ(I)). The crystal structure shows that the copper(Ⅱ) ion is coordinated with two oxygen atoms from one terephthalic acid molecule and four nitrogen atoms from two 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 298809.     

锌(Ⅱ)与2,2′-联吡啶胺(dpa)和3-苯丙酸(HPPr)混配配合物的合成、晶体结构及性质表征

合成了锌（Ⅱ）与２，２′－联吡啶胺（ｄｐａ）和３－苯丙酸（ＨＰＰｒ）混配配合物［Ｚｎ（ｄｐａ）（ＰＰｒ）２］·２Ｈ２Ｏ，并测定其晶体结构．晶体属三斜晶系，Ｐ１空间群，晶胞参数ａ＝１０．５４１（１）ｎｍ，ｂ＝１１．３３３（１）ｎｍ，ｃ＝１１．６９８（１）ｎｍ，α＝９１．００（１）°，β＝９０．９６（１）°，γ＝８８．３８（１）°，Ｚ＝２，２个ＰＰｒ－１羧基上的４个氧原子、１个ｄｐａ上的２个氮原子分别与中心离子Ｚｎ（Ⅱ）配位，构型为畸变八面体．２个结晶水与配体间可能存在着分子内氢键．通过元素分析、ＩＲ、摩尔电导和热重分析表征了配合物的结构．     

Ni(Ⅱ)牛磺酸缩水杨醛席夫碱·2,2'-联吡啶三元配合物的合成及晶体结构

合成了标题化合物。该化合物的分子式[Ni(TSSB)(Bipy)H2O]4H2O(C19H27NiN3O9S),分子量532.21,采用单色化的MoK?(=0.71073?射线测定,共收集15601个数据,其中独立衍射点5371个(Rint=0.0316),I>2(I)可观测点数3537个,结果表明该化合物属单斜晶系,空间群P21/c,其晶胞参数为:a=16.406(2),b=15.409(2),c=9.252(1)?β=90.373,V=2338.9(6)?,Z=4,Dc=1.511g/cm3,=0.973mm-1,F(000)=1112,该配合物是六配位的变形八面体构型。     

Synthesis and Crystal Structure of Cobalt(II) Complex [Co(H2O)2(bpe)(OAc)2](4,4''-dpdo

The reaction of Co(OAc)2 with bpe and 4,4'-dpdo in an aqueous-alcohol solution affords the formation of red crystals of [Co(H2O)2(bpe)(OAc)2](4,4'-dpdo (bpe = trans-1,2-bis(4- pyridyl)ethylene, 4,4'-dpdo = 4,4'-dipyridyl N,N'-oxide). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 7.6146(9), b = 8.6691(11), c = 10.344011 A, α = 88.311(3), β = 76.992(3), γ = 75.809(3)°, V = 644.7613 A3, Z = 1, C26H28CoN4O8, Mr = 583.45, Dc = 1.503 g/cm3, μ = 0.724 mm-1, F(000) = 303, T = 223(2) K, the final R = 0.0477 and wR = 0.1177 for 3199 observed reflections with I > 2σ(I). In the crystal the cobalt atom is six-coordinated by oxygen atoms from two carboxylic molecules, two nitrogen atoms from the bpe ligands and two water molecules, completing an octahedral geometry. The structure of the title complex consists of neutral chains containing cobalt(II) ions bridged by mutually trans bpe molecules. The adjacent chains are connected through weak hydrogen bonds to form a two-dimensional structure.