Synthesis and crystal structure of polymer cobalt(II) complex, 1,2,4,5-benzenetetracarboxylate hexaimidazole tetraaqua cobalt (II) tetrahydrate

The crystal structure of the title complex {[Co(TCB)2/2-(IMI)2(H2O)2][Co(IMI)4(H2O)2] } (H2O)4 (where TCB = 1,2,4,5-benzenetetracarboxylic anion; IMI = imidazole) has been determined by X-ray diffraction method. Crystal data for {[Co(TCB)2/2(IMI)2(H2O)2][Co(IMI)4(H2O)2]}-(H2O)4: triclinic, space group P 1, a = 1.0647(2) nm, b = 1.1165(1)nm,c = 1.00361(1)nm,α = 91.56(1)°,β = 111.34(1)°, γ = 115.642(10)°, V = 0.9772(3) nm5, Z = 1. The polymer cobalt (II) complex has a novel three-dimension network structure. Co(1) atom and Co(2) atom both are coordinated in an octahedral arrangement and located in the center of the coordination anion and the center of the coordination cation, respectively. Moreover four carboxyl groups of TCB are divided into two types, two para-carboxyl groups bridge Co(1) atom in monodentate fashion and other two para-carboxyl groups are in free.     

丁二酮肟双核铜配合物的合成、结构和性能表征

The structure of [Cu₂(Hdmg)₄] (Hdmg=dimethylglyoxime anion) has been determined by X-ray crystallog-raphy. It is monoclinic, space group P2₁/n, with Z=2. The lattice parameters: a=0.71601(14)nm; b=1.7044(3)nm; c=1.0126(4)nm; β=113.89(2)°; M_r=587.52 (C₁₆H₂₈Cu₂N₈O₈); V=1.1299(5)nm³. The copper atom lies in a distorted square-pyramidal environment. The four equatorial donors are four nitrogen atoms from bidentate chelate dimethylglyoxime anion ligands. The oxygen atom from the dimethylglyoxime ligand acts as a bridging atom occupying the apical position of the symmetry-related copper atom in the dimer structure. The two dimethylglyoximes bridge two copper atoms to form a six-member Cu₂O₂N₂ ring, respectively. The thermal gravity (TG) data indicate that the compound [Cu₂(Hdmg)₄] undergoes two exothermic reactions with loss of the organic ligand to give residue CuO. CCDC: 208729.     

Preparation and Molecular Structure of Binuclear Nickel (I) Complex Bridged by 1,2,4, 5‐Benzenetetracarboxylato Tetravalent Anion

The title complex [(H₂O)₂(IMI)₃Ni(TCB)Ni(IMI)₃‐(H₂O)₂] H₂O (TCB = 1,2,4,5‐benzenetetracarboxylato te‐travalent anion; IMI = imidazole) has been prepared by the reaction of Ni(IMI)₃(Ac)₂ and TCB in aqueous solution. The crystal structure has been determined by single‐crystal X‐ray diffraction method. It crystallizes in the monoclinic system, space group P2₁/c(# 14), a = 1.2714(4) nm, b = 0.9411 (3) nm, c = 1.5869(4) nm, β= 108.54(2)°, V= 1.8001(9) nm³, Z = 2. The main feature of the crystal structure is a symmetric binuclear unit made up of two slightly distorted coordination octahedrons, which are bridged by TCB in monodentate fashion to each metal ion. Moreover three nitrogen atoms from three imidazoles, three oxygen atoms from two water molecules and one carboxylate group of TCB coordinated to a nickel (I) ion are found on a face of the octahedron respectively, so the octahedron is a facial isomer.     

钒氧配合物[VOL(C9H6NO)]·CH2Cl2的合成与晶体结构

A oxovanadium(Ⅴ) complex of [VOL(C₉H₆NO)]·CH₂Cl₂[H₂L=2-hydroxy-1-naphthaldehyde 4-methoxy-benzoylhydrazone, C₉H₆NO^-=8-hydroxyquinoline anion] has been synthesized and characterized by elemental analyses, IR and single crystal X-ray diffraction. The crystal crystallizes in triclinic system, the space group is P1, with the crystal cell parameters a=1.087 0(2) nm, b=1.107 1(2) nm, c=1.269 3(3) nm, α=67.84(3)°, β=79.26(3)°, γ=73.85(3)° and V=1.353 1(6) nm³ , M_r=614.34, R=0.0503, wR=0.1409. The V(Ⅴ) atom is six-coordinated by one O atom of oxo group, two O atoms and one N atom of the tridentate hydrazone ligand, as well as one N atom and one O atom of 8-hydroxyquinoline ligand, thus defining a distorted octahedral VO(ONO)(NO) geometry. A two-dimensional supramolecular layer structure is formed through π-π stacking interactions. CCDC: 268672.     

Synthesis,Structure and Fluorescence of a Copper(II) Complex [Cu_2(bipy)_2(Hpht)_2Cl](Hpht)(bipy=2,2'-Bipyridine,H_2pht=o-Phthalic Acid)

1 INTRODUCTION o-Phthalic acid (H2pht) is a versatile ligand for co-ordinating to metal ions in various modes, such asmonodentate bonding through a carboxylic O atom[1],bidentate fashion via two carboxylic O atoms[2] andtriple coordination through its three carboxylic Oatoms[3], and bridging mode with two or four Oatoms of its carboxylate groups[4]. The coordinationproperties thus allow for the preparation of complex-es with a large variety of architectures, forming iso-lated mono-, di…     

一个二维钴配位聚合物的合成、结构及光催化性质

以N,N'-二(3-吡啶基)-吡啶-3,5-二甲酰胺(bppdca)和2-巯乙酸基烟酸(L)为混合配体,利用水热合成方法获得了一个二维的Co(Ⅱ)配位聚合物:{[Co(bppdca)(L)]·3H₂O}_n,并通过元素分析、IR和单晶X射线衍射等技术手段确定了其结构。该配合物分子式为C₂₅H₂₄N₆O₉SCo,单斜晶系,P2₁/c空间群,a=1.07419(9) nm,b=0.86166(6) nm,c=2.9853(2) nm,β=96.772(1)°,Z=4,V=2.743 9(4) nm³,M_r=643.49,D_c=1.558 g/cm³,F(000)=1324,μ=0.766 mm^-1,S=1.051,R=0.0406,wR=0.1160。 晶体结构分析表明,配合物中的CoⅡ与来自2个bppdca配体的2个N原子、1个L阴离子的单齿羧基O原子和S原子以及来自另一个L阴离子的一个羧基中的2个O原子配位形成八面体配位构型。 相邻的Co^Ⅱ通过L阴离子连接成一维螺旋链[Co(L)]_n,相邻的左、右螺旋链通过成对的bppdca配体拓展成二维配位网络。 最终,相互平行的二维网络通过氢键作用拓展成三维超分子框架。 另外,还研究了该化合物的热稳定性、电化学性质、荧光性质以及选择性光催化性质。CCDC: 1010786     

一维链状锌配位聚合物[Zn(apy)( μ-OH)NO3]n的合成、晶体结构及荧光性质

本文合成了1个新的配位聚合物[Zn(apy)(μ-OH)NO3]n(apy=2-氨基嘧啶),并且通过元素分析、红外、荧光、和单晶X-射线进行了表征。标题化合物属于单斜晶系,P21/c空间群,a=0.715 48(14)nm,b=1.850 5(4)nm,c=0.645 68(13)nm,β=110.24(3)°,V=0.802 1(3)nm3,Z=4,R=0.028 4。在化合物中,每个Zn(Ⅱ)离子与氨基嘧啶配体的1个N原子、硝酸根的1个O原子,以及2个羟基氧原子配位,并展示出扭曲的四面体几何构型。2个相邻的Zn(Ⅱ)四面体单元通过羟基氧原子连接形成一维链状结构,该一维链进一步通过氢键和π-π堆积作用形成三维网状结构。室温荧光光谱测定表明该化合物在392 nm处有强的荧光发射。     

对甲酰基苯氧乙酸和2-氨基苯并噻唑的新型三元铜配合物的合成、晶体结构及抗微生物活性

以对甲酰基苯氧乙酸和2-氨基苯并噻唑为原料,合成了一种三元铜配合物,并通过元素分析, 红外光谱以及X-射线衍射单晶结构分析对其进行了表征。该配合物晶体属单斜晶系,P2₁/c空间群,中心铜(Ⅱ)离子的配位数为4,分别与2个对甲酰基苯氧乙酸配体分子的羧基和2个2-氨基苯并噻唑配体分子的噻唑环上的氮原子发生配位。抑菌实验结果表明,配合物对新型隐球菌、粘性红圆酵母、桔青霉和黑曲霉具有很好的抑制作用,而对大肠杆菌和金黄色葡萄球菌的抑制效果一般。     

含柠檬酸配体的钼硫簇合物的合成与晶体结构的测定

合成了含有Mo—S簇阴离子 [Mo2 O2 ( μ S) 2 (C6H5O7) (C6H4 O7) ]5-柠檬酸簇合物 ,并通过元素分析、红外光谱、紫外 可见光谱和X射线光电子能谱对配合物进行了表征 ,用X射线衍射法测定了该化合物的晶体结构 .结果表明 ,该簇合物属于单斜晶系 ,空间群P2 1/c,a =2 3 766( 5)nm ,b =1 3 2 74 ( 3 )nm ,c =2 2 4 71 ( 5)nm ,α=γ =90°,β=1 1 8 2 1°,V =6 2 4 7( 2 )nm3 ,Z =8,一致性因子R =0 0 83 1 ,R2 ,w=0 1 536.该簇合物阴离子中每一个Mo原子都采取扭曲的八面体结构 ,柠檬酸通过羟基、α 羧基、一个 β 羧基与Mo配位 .晶体结构表明在一个结晶学上不对称的结构单元内有两个结晶学上独立的分子 .     

席夫碱大环双核锌配合物的合成与表征

本文用丙酮和乙二胺在高氯酸催化下合成了四氮杂十四环席夫碱(1),并用此化合物(1)与氧化锌和叠氮化钠反应,生成锌的双核大环配合物。通过X-射线单晶衍射和红外光谱对其进行了结构表征。该配合物属单斜晶系,C2/c空间群,晶胞参数为a=2.4914(2)nm,b=1.4 9748(13)nm,c=1.26800(11)nm;β=102.1900(10)°;v=4.6240(7)nm3,Z=4,Dc=1.482Mg/m3,Mr=1032.03,F(000)=2160,最终R=0.0506,wR=0.1434。该配合物中锌原子是五配位,它们分别和大环配体上的4个氮原子及叠氮根负离子两端的氮原子配位形成畸变的三角双锥构型。     

有机锡配合物{[(n-C8H17)2Sn(O2CCH2CS2NC4H8O)]2O}2的合成，表征及晶体结构

The title complex {[(n-C₈H₁₇)₂Sn(O₂CCH₂CS₂NC₄H₈O)]₂O}₂ has been synthesized by the reaction of (morpholinylthiocarbamoylthio)acetic acid with the di-n-octyltin oxide in 1∶1 molar ratio. The complex was characterized by elemental analysis, IR and ¹H NMR. The crystal and molecular structure of complex was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system with space group P1 and unit cell dimensions: a=1.201 5(9) nm, b=1.481 8(11) nm, c=1.894 1(14) nm, α=72.485(10)°, β=88.586(10)°, γ=66.893(9)°, and Z=1, μ=1.034 mm^-1, V=2.941(4) nm³, D_c=1.295 g·cm^-3, F(000)=1 196, R₁=0.058 8, wR₂=0.155 8. The complex is a centrosymmetric structure with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom. The endo-cyclic tin atoms and the exo-cyclic tin atom are all five-coordinate and have coordination geometry of distorted trigonal bipyramid with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are monodentate and connecting to each of exo-cyclic tin atoms by using one oxygen atom, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom. CCDC: 277048.     

稀土胺羧酸配合物的研究 I. {[MnGd(DTPA)(H2O)5]2·H2O}n配合物的合成和晶体结构

本文首次合成了{MnLn(DTPA)(H2O)5]·H2O}n异核链式配合物(Ln=Gd, Er, Y)单晶,测定了{[MnGd(DTPA)(H2O)5]2·H2O]n的单晶结构。     

Composition of a mixed-ligand gadolinium(III) complex in fluoride-dimethylformamide electrolyte

The gadolinium(III) complex formed in a fluoride-dimethylformamide (DMF) electrolyte was studied by linear-sweep voltammetry and IR spectroscopy. The composition of the mixed-ligand complex formed was found to correspond to the component ratios Gd: DMF: F = 1: 3: 4. It has been found that the coordination link in the complex is via two oxygen atoms and one nitrogen atom of dimethylformamide and involves four fluoride ions.     

Gadolinium acetylacetonate tetraphenyl monoporphyrinate complex and some of its derivatives: EXAFS study and molecular dynamics simulation

Many attempts to obtain single crystals appropriate for X-ray diffraction analysis of the Ln(tpp)(acac) derivatives (where Ln = Gd or Sm, tpp = tetraphenylporphyrin and acac = acetylacetonate) have failed so far. A suitable way to get structural parameters for these monoporphyrinates is to use extended X-ray absorption fine structure (EXAFS) spectroscopy. We recorded spectra of the monoporphyrins, Ln(tpp)(acac) and Gd(tpyp)(acac) (where tpyp = tetrapyridylporphyrin), and the bisporphyrin GdH(tpyp)2 in the solid state. We particularly focused our structural analysis on Gd(tpp)(acac), applying both molecular modeling and EXAFS, which allowed us to get accurate results about the local environment of the central atom. The Gd3+ ion of the complex at room temperature was found to be bonded to four monoporphyrin nitrogen atoms at an average distance R(Gd-N(av)) = 2.48 A and to three or four oxygen atoms at R(Gd-O(ac,w)) = 2.38 A from an acetylacetonato anion and a water molecule. The presence of the second water molecule in the coordination sphere was barely discernible by EXAFS analysis. Molecular modeling has provided further information about the coordination core geometry of the Gd(tpp)(acac) monoporphyrinate, including a bishydrated coordination sphere. Also, it has enabled the construction of a 3D structural model on which multiple scattering analyses were attempted. Monte Carlo simulation was used to validate the adjustments. EXAFS spectra analysis was carried out on the derivatives, displaying slight distortions in the lanthanide central-atom coordination geometry.     

一个新的超大铈锑钨酸盐阴离子Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)^1^9^-~4

合成了一超大铈锑钨酸盐[Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)~4](NH~4)~1~9.48H~2O,用X射线单晶衍射法及元素分析确定了其结构。其晶胞参数为：a=1.8908(6)nm,b=2.0032(14)nm,c=2.8653(12)nm,α=86.95(6)°,β=75.68(3)°,γ=67.52(5)°,V=9.706(9)nm^3,空间群P1。在杂多阴离子Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)^1^9^-~4中,四个β-B-(SbW~9O~3~3)^9^-是通过一个大的中心集团[Ce~3Sb~4W~2O~8(H~2O)~1~0]^1^7^+连接起来的,中心集团中含有两个桥连{WO~2(H~2O)}基,三个Ce(Ⅲ)离子和一个{Sb~4O~4}基团。三个Ce(Ⅲ)离子的配位数均为9,Ce(1)和Ce(3)的配位环境相同,但不同于Ce(2)的配位环境,四个{SbW~9O~3~3}中的三个参与了向Ce(Ⅲ)的配位。两个{SbW~9O~3~3}中的四个氧,三个水分子中的三个氧,{Sb~4O~4}中的一个氧及一个桥连{WO~2(H~2O)}中的一个氧向Ce(1)[或Ce(3)]配位;两个{SbW~9O~3~3}中的四个氧,两个水分子中的两个氧,{Sb~4O~4}中的一个氧及两个桥连{WO~2(H~2O)}中的两个氧向Ce(2)配位。在{Sb~4O~4}中,四个Sb原子的中心构成了一四面体。该离子属C~s点群,Sb(5),Sb(8)和Ce(2)所在的平面是其对称面。     

一种新颖钒.钨异金属八核簇合物[VW~3~4(O~2CEt)~8]~2Na~2的合成与结构

本文报道了一种钒.钨异金属八核簇合物[VW~3~4(O~2CEt)~8]~2Na~2(1)在恒温液相条件下的合成与结构研究,晶体属三斜晶系,P1空间群,a=1.2973(4),b=1.4063(3),c=1.2396(5)nm,α=1.09.92(2),β=117.32(2),γ=90.53(2)°,V=1.8513nm^3,D~c=2.29g/cm^3,Z=1对5499个可观测反射点[I>3σ(I)] 最终一致性因子为R=0.030.单晶结构分析表明,簇阴离子中两个[W~3O~4]^4^+单元通过两个"桥"金属V原子联接成一个奇特的环状结构,W-W平均键长为0.25328(6)nm,W...V间平均距离为0.3654nm,簇阴离子通过Na^+联成一个一维长链.Na 原子具有少见的五配位,Na-O距离仅为0.2314nm,Na-O间教情的相互作用以及无限长链的晶体结构很好地解释乐簇合物1的稳定性和不溶性.     

Synthesis and Crystal Structure of Potassium triaqua（ethyleneamin—N,N,N‘,N’—tetraacetate）gadolinium（Ⅲ）pentahydrate

1 INTRODUCTION The chemistry of lanthanide (Ⅲ) complexes has a considerable history. The stereochemistry of the lanthanide (Ⅲ) complexes with ethyleneamine- N, N, N, N-tetraacetate (Edta) has been investigated[1~10]. Up to now, many Ln-Edta complexes with the chemical formulae of M[Ln(Edta)(H2O)m]nH2O (M = Na+, K+, Cs+, NH4+, Guanium; m = 2, 3; n = 0, 1, 3, 5) have been reported and suggested that the coordination modes and crystal systems for the Ln-Edta complexes depend on …     

Octa-membered Water Ring Chain Based on Sulfonic Group in Ni(Ⅱ) Complex with 2-[(E)-(2-Oxidophenyl)methyleneamino]Ethanesulfonato and 2,2''-Bipyridinyl

The title compound, [Ni(tssb)(2,2-bipy)2]·5(H2O) 1 (tssbH2 =2-[(E)-(2-oxido-phenyl)methyleneamino]ethanesulfonato, 2,2-bipy = 2,2'-bipyridinyl), belongs to orthorhombic,space group Pbcn with a = 20.3983(18), b = 17.6929(15), c = 17.0897(15) nm, V = 6167.8(9) nm3,Mr= 688.38, Z = 8, Dc = 1.481 g·cm-3, F(000) = 2880, μ = 0.758 mm-1 and S =1.099. Each NiⅡ atom is six-coordinated by one N and one O atoms from one tssb2- anion and four N atoms from two 2,2-bipy ligands to give a distorted octahedral geometry. Noticeably, there exists a rare octa-membered water ring which presents a 1D chain by sulfonic group.     

四(4-乙烯基吡啶)硝酸铜(Ⅰ)配合物的结构、电化学和热稳定性能研究(英文)

The title complex Cu(Vpy)NO3 (Vpy=4-vinylpyridine) has been synthesized and structurally characterized by X-ray single crystal diffractometry. The complex crystallizes in triclinic system, P1 space group with the cell parameters of a=1.004 2(2) nm, b=1.631 7(3) nm, c=1.887 7(4) nm, α=81.54(2)°, β=77.44(2)°, γ=79.39(2)°, V= 2.948 9(11) nm3, Z=4, and Dc=1.230 g·cm-3, the final R1=0.075 2, wR2=0.139 1. The complex crystallizes with two molecules in the asymmetric unit. Each Cu(Ⅰ) ion is coordinated by four N atom from the Vpy ligands and one O atoms from the nitrate anion, resulted in a square pyramidal geometry. The electrochemical studies reveal that redox of Cu2+/Cu+ in the complex is a quasi-reversible process. CCDC: 736638.     

CRYSTAL STRUCTURE OF（η^5—C5H5）GdCl2（THF）3

<正> Compound (η5-C5H5)GdCl2(THF)3 was successfully prepared from action of GdCl3 and NaC5H5 in tetrahydrofuran (THF). X-ray diffraction data were collected at low temperature (about 210K). Its crystal belongs to the monoclinic space group P 21/n with a = 7. 821(2), b = 17.068(1), c=15. 057(1)(?), β=94. 76 (2)°, V = 2003. 2(10)(?)3, Z = 4, Dc=1. 69g/cm3, F(000)=1012, Mr=509. 6. The structure was solved by heavy-atom method. Least-squares refinement converged to a final R value of 0. 050. The coordination number of the Gd atom is 8. The centre of the cyclopentadienyl, the two Cl atoms and the three oxygen atoms of THF molecules form a distorted octahedron about the Gd atom.