配合物[Cu(NPA)2(Im)2(H2O)]·H2O的合成、晶体结构及电化学性质

A novel copper(II) complex [Cu(NPA)₂(Im)₂(H₂O)]·H₂O has been synthesized (NPA=N-phenylanthranilic acid and Im=imidazole) and characterized by IR, elemental analysis and X-ray single crystal diffraction methods. It Crystallizes in Triclinic system, space group P1 with a=0.987 9(2) nm, b=1.075 7(3) nm, c=1.559 7(5) nm, α=104.18(10)°, β=108.14(10)°, γ=92.69(10)°, V=1.513 39(7) nm³, Z=2, D_c=1.447 g·cm^-3, F(000)=684, R₁=0.028 0, wR=0.083 1. The Cu(II) ion in the title complex is coordinated with two oxygen atoms from two N-phenylanthranilic acid in monodenate mode, two nitrogen atoms form two imidazole, and one oxygen atom from water, forming a distorted square-pyramid coordination geometry. CCDC: 638653.     

配位聚合物[Mn(4，4′-bpy)1.5(H2O)3](ClO4)·(4，4′-bpy)(L)·H2O的水热合成和晶体结构

The title compound, [Mn(4,4′-bpy)_1.5(H₂O)₃](ClO₄)·(4,4′-bpy)(L)·H₂O(1), where L=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 0(1) nm, α=105.300(2)°, β=97.495(2)°, γ=91.118(2)°, V=1.884 0(4) nm³, Z=2, M_r=780.10, D_c=1.375 g·cm^-3, μ=0.483 mm^-1, F(000)=812, R=0.055 4, wR=0.135 2. The Mn atoms are octahedrally coordinated by three N atoms of three 4,4′-bipyridine ligands and three O atoms of water. The complex shows a one-dimensional chain structure bridged by water and 4,4′-bipyridine molecules. CCDC: 615707.     

{[Co(4，4′-bipy)(H2O)4]·(α-Furacrylic acid)2·(H2O)}n的水热合成、晶体结构及电化学分析

A complex {[Co(4,4′-bipy)(H₂O)₄]·(α-Furacrylic acid)₂·(H₂O)}_n with α-furacrylic acid, 4,4′-bipy and cobaltous chloride hexahydrate has been synthesized by means of hydrothermal way and characterized. Crystal data for this complex: monoclinic, space group P2₁/c, a=1.147 0(2) nm, b=1.099 9(2) nm, c=1.111 1(2) nm, β=97.829(3)°, V=1.388 7(5) nm³, D_c=1.429 g·cm^-3, Z=2, μ(Mo Kα)=0.682 mm^-1, F(000)=622, S=1.025, R₁=0.035 8, wR₂=0.086 1. The crystal structure shows that the cobalt(Ⅱ) ion is coordinated with two nitrogen atoms of two 4,4′-bipy molecules and four oxygen atoms from four water molecules, respectively, giving a distorted octahedral coordination geometry. Adjacent cobalt(Ⅱ) ions are bridged by 4,4′-bipy groups, resulting in a 1D chain structure. The adjacent Co(Ⅱ)-Co(Ⅱ) distance is 1.147 0 nm. The cobalt(Ⅱ) ion isn′ t coordinated with α-Furacrylic acid. The complex molecules form 2D structure through hydrogen bonds. The cyclic voltametric behavior of the complex was also investigated. CCDC: 648243.     

［Eu2(o-ClC6H4OCH2COO)6(C12H8N2)2(H2O)2］·(CH3)2SO的晶体结构和荧光光谱

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, D_c=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→ ⁷F_J(J=0～2)跃迁光谱说明Eu(Ⅲ)离子格位具有C₂对称性。     

不对称大环双核铜(Ⅱ)配合物[Cu2(C23H26Cl2N4O2)](ClO4)2的合成、晶体结构及磁性

大环双核铜(Ⅱ)配合物由N,N′-二甲基-N,N′-二(3-甲酰基-5-氯水杨醛)乙二胺和1,3-丙二胺,与铜(Ⅱ)反应形成的,经过X-射线单晶衍射结果表明：a=0.871 05(16) nm,b=0.957 78(18) nm,c=1.810 4(3) nm,β=100.761(18)°,V=1.483 8(5) nm³,Z=2,D_c=1.762 Mg·m^-3,μ=1.85 mm^-1,F(000)=796,and final R₁=0.061,wR₂=0.126。晶体结构表明：两个铜离子位于双核大环中间,与大环的胺、亚胺以及酚羟基的氧进行配位。磁性结果表明配合物为反铁磁性。     

一维链状钴配位聚合物{[Co(4，4′-bipy)(C9H8O3N)2](H2O)4}n的溶剂热合成、晶体结构及热稳定性

One novel coordination polymer {[Co(4,4′-bipy)(C₉H₈O₃N)₂](H₂O)₄}_n with p-acetamidobenzoic acid and 4,4′-bipy has been synthesized. It was characterized as crystallizing in the triclinic space group P1, with: a=1.138 1(2) nm, b=1.165 2(2) nm, c=1.223 3(2) nm, α=88.47(3)°, β=88.00(3)°, γ=65.78(3)°, V=1.478 4(4) nm³, D_c=1.446 g·cm^-3, Z=1, F(000)=670. Final GooF=1.106, R₁=0.041 5, wR₂=0.110 4. The crystal structure shows that the cobalt(Ⅱ) ion is lined with one 4,4′-bipy molecule, forming a one-dimension chain with Z-type structure, which coordinated with two nitrogen atoms of two 4,4′-bipy molecules and four oxygen atoms from two p-acetamidobenzoic acid molecules, giving a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex was stable under 230.0 ℃. CCDC: 741932.     

{(n-Bu4N)2[Mo2O2S6Cu6Br4(4，4′-bipy)3]·0.5H2O}n的合成与晶体结构

Cluster coordination polymer {(n-Bu₄N)₂[Mo₂O₂S₆Cu₆Br₄(4,4′-bipy)₃]·0.5H₂O}_n (4,4′-bipy=4,4′-bipyridine), has been synthesized and characterized by X-ray crystallography. The polymeric anion {[Mo₂O₂S₆Cu₆Br₄(4,4′-bipy)₃]^2-}_n is composed of secondary building units (SBUs) [MoOS₃Cu₃], Br atoms and 4,4′-bipy ligands. Two secondary building units [MoOS₃Cu₃] and a double parallel 4,4′-bipy ligands form an octanuclear rectangular metallamacrocycle with the dimension of 1.13×0.39 nm², which is further connected by single bridging 4,4′-bipy ligands to form a 1D zigzag structure. Crystal data for compound 1: C₆₂H₉₇N₈O_2.50S₆Br₄Cu₆Mo₂, M=2 079.68, Triclinic, P1, a=0.982 40(10) nm, b=1.293 70(10) nm, c=1.737 4(2) nm, α=97.810(10)°, β=101.390(10)°, γ=108.520(10)°, V=2.005 1(4) nm³, Z=2, D_c=1.722 g·cm^-3, F(000)=1 039, μ(Mo Kα)=4.055 mm^-1, the final R=0.040 7, wR₂=0.097 2. CCDC: 236407.     

异双桥二维镍(Ⅱ)配位聚合物 ∞2[Ni(μ-4，4′-bpy)2/2(μ-L)4/2](HL=2-indolyl-formic acid)的水热合成和晶体结构

The allo-bisbridge 2D coordination polymer _∞²[Ni(μ-4，4′-bpy)_2/2(μ-L)_4/2](HL=2-indolyl-formic acid) has been obtained by using hydrothermal synthesis, and the results of X-ray single crystal diffraction analysis show that the compound crystallizes in monoclinic system, space group C2/c (No.15) with a=2.300 2(5) nm, b=1.129 1(2) nm, c=0.974 0(2) nm, β=109.85(3)°, V=2.379 2(8) nm³, D_c=1.494 g·cm^-3, Z=4, F(000)=1 104, μ=0.860 mm^-1, R=0.032 2, wR=0.088 8. The crystal structure consists of the [Ni(μ-4,4′-bpy)_2/2(μ-L)_4/2] complex molecules, in which the Ni atom is octahedrally coordinated by two N atoms from two different 4,4′-bpy molecule ligands and four O atoms from four different L- anion ligands. TG analysis indicate that title coordination polymer possesses relatively high thermal stability. CCDC: 252833.     

［Cu2(BpheO)4(bpy)2］·2H2O的合成晶体结构及性质研究

N-苯甲酰苯丙氨酸(BpheO)与Cu(bpy)Cl₂发生取代反应，在水中合成了双核铜(Ⅱ)配合物［Cu₂(BpheO)₄(bpy)₂］·2H₂O(bpy:2,2′-联吡啶)。晶体属三斜晶系，P1空间群，晶胞参数：a=10.681(2)?,b=12.320(2)?,c=16.525(2)?；α=110.23(1)°，β=76.98(1)°，γ=105.49(1)°,V=1945.0(6)?³,Z=1,F(000)=786,D_c=1.291 g/cm³, μ=0.61 mm^-1。Cu与bpy的二个氮原子和BpheO的三个氧原子构成五配位略有畸变的四方锥多面体。经元素分析、IR、ESR和TG-DTA对配合物的性质进行了研究。     

二维配位聚合物[Mn(FA)2(4，4′-bipy)]n的合成、晶体结构及量子化学研究

A novel manganese coordination polymer [Mn(FA)₂(4，4′-bipy)]_n(HFA=2-furancarboxylic acid, 4,4′-bipy=4,4′-bipyridine) has been synthesized by hydrothermal methods. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a=1.698 4(3) nm, b=1.168 6(2) nm, c=1.009 5(17) nm, β=109.455(11)°, V=1.889 2(6) nm³, Z=4, D_c=1.523 g·cm^-3, M_r=433.27, F(000)=884, μ=0.740 mm^-1, R₁=0.028 2 and wR₂=0.071 0. In the crystal, the manganese atom is six-coordinated by two nitrogen atoms from 4,4′-bipyridine and four oxygen atoms from furancarboxylic acid molecules, completing an octahedral geometry. The 4,4′-bipyridine molecules are connected to the infinite chain [Mn(FA)₂]_n to form a two-dimensional layer. The quantum chemistry calculation on the title complex has been performed by means of G98W package and taking Lanl2dz basis set. CCDC: 296763.     

［Mn2(CHZ)4(H2O)2］(PA)4·10H2O的制备和分子结构研究

本文论述了苦味酸(PA,三硝基苯酚)锰与碳酰肼(CHZ, NH₂NHCONHNH₂)反应制备目标配合物的方法及该配合物的晶体结构。该配合物的结构式为［O,O′-μ-Mn₂(CHZ)₄(H₂O₂)］(PA)₄·10H₂O。晶体属三斜晶系,P1 空间群。晶体学参数为：a=0.8269(1) nm, b=1.2812(1) nm, c=1.5915(1) nm; α=109.58(1)°, β=95.19(1)°, γ=92.76(1)°, V=1.5765(2)nm³; Z=1, Dc=1.580 g·cm^-3, μ(Mo K_α)=520 m^-1。晶体结构经全矩阵最小二乘法修正,最终偏离因子R=0.0557。该化合物为具有中心对称的双核配合物,以两个碳酰肼分子中羰基氧为桥原子将两个锰离子结合起来,与锰离子形成配位键的原子是碳酰肼分子第一、五氮原子,羰基氧原子和水分子中的氧原子,锰离子的配位数为七。若味酸根作为外界离子以库伦力和氢键与内界离子结合成配合物分子。     

一维链状铽配位聚合物{[Tb(p-MBA)2(H2O)2]2·(4，4′-bipy)2}n的合成、晶体结构及荧光分析

A novel one-dimensional chain coordination polymer of terbium(Ⅲ) with p-methylbenzoic acid, 2,2′-bi-pyridine and 4,4′-bipyridine has been synthesized and characterized. The crystal data of this complex C₃₉H₃₇N₃O₈Tb are as follows: monoclinic system, space group P2₁/n, a=0.974 01(10) nm, b=2.605 8(3) nm, c=1.457 77(14) nm, β=96.108(2)°, V=3.678 9(6) nm³, D_c=1.507 g·cm^-3, M_r=834.64, Z=4, μ(Mo Kα)=1.978 mm^-1, F(000)=1 684, R₁=0.032 4, wR₂=0.063 4. The crystal structure of the complex shows that the terbium(Ⅲ) ion is coordinated with eight oxygen atoms, six from five p-methylbenzoic acid molecules and two from two water molecules, respectively, forming the distorted tetraprism geometry. The luminescent property of the complex is also studied. CCDC: 619216.     

镧与β-丙氨酸配合物{[La2(β-ala)6(H2O)4](ClO4)6·H2O}n的合成及晶体结构

The complex, {[La₂(β-ala)₆(H₂O)₄](ClO₄)₆·H₂O}_n, was synthesized in aqueous solution and its crystal structure was determined by X-ray diffraction method .The crystal is triclinic with space group of .The cell pa-rameters are a=0.946(1)nm, b=1.2917(1)nm, c=2.1726(3)nm,α=76.79(1)°, β=80.85(1)°,γ=83.35(1)°, V=2.5429(5)nm³, Z=2, D_c=1.958g·cm^-3.The complex is an one-dimensional infinite chain. The coordination number of lanthanum ion is nine, forming a distorted tricapped trigonal prism.     

一维链状镉(Ⅱ)配位聚合物{[Cd(PAc)2(4，4′-bipy)(H2O)]·4H2O}n的合成、晶体结构及热稳定性研究

A novel one-dimensional coordination polymer, {[Cd(PAc)₂(4,4-bipy)(H₂O)]·4H₂O}_n (HPAc=phenyl acetic acid, 4,4′-bipy=4,4′-bipyridine) was synthesized and characterized by element analysis, IR, TG and X-ray single diffraction crystal structure determination. It crystallizes in the monoclinic space group C2/c with a=2.088 5(4) nm, b=0.839 05(17) nm, c=1.683 5(3) nm, β=105.45(3)° and V=2.843 5(10) nm³, Z=4, M_r=628.94, F(000)=1 288, μ=0.820 mm^-1, R=0.019 9, wR=0.056 5. Each cadmium(Ⅱ) atom is seven-coordinated by four oxygen atoms from two different phenyl acetate groups and two nitrogen atoms from two 4,4′-pyridine ligands and one water molecule, forming a distorted pentagonal bipyramid coordination geometry. Adjacent cadmium(Ⅱ) atoms are bridged by 4,4′-pyridine ligand, constructing a infinite chain along the diagonal direction of ac plane. The Cd…Cd separation within the polymer is 1.164 6(4) nm. The three-dimensional supramolecular structures of the title complexes are constructed by hydrogen bonding interactions and π-π stacking interactions between the benzene rings of HPAc and 4,4′-bipy. CCDC: 616697.     

三苯基锡(Ⅳ)N-烃基哌嗪氨荒酸酯配合物的合成、表征、性质和Ph3SnS2CN(C2H4)2NCH3的晶体结构

Six triphenyltin(Ⅳ)N-alkylpiperazinyldithiocarbamates have been synthesized by the reaction of triphenyltin chloride with N-alkylpiperazinyldithiocarbamates and characterized by elemental analysis, UV, IR and ¹H NMR. The crystal structure of Ph₃SnS₂CN(C₂H₄)₂NCH₃(1) has been determined by X-ray single crystal diffraction. The crystal of the compound 1 belongs to triclinic with space group P1, a=1.033 56(18) nm, b=1.148 8(2) nm, c=1.191 6(2) nm, α=66.282(2)°, β=78.756(2)°, γ=67.476(2)°， Z=2, V=1.195 2(4) nm³, D_c=1.460 g·cm^-3, μ=1.256 mm^-1, R=0.025 1, wR=0.058 3. The structure shows a distorted tigonal bipyramidal configuration with five-coordination for the central tin atom. CCDC: 240375.     

新颖无限三股螺旋钴配位聚合物{[Co(4,4′-bipyridine)(4,4′-azobispyridine)2(NCS)2]·H2O}n的合成、结构和性质的研究

The novel complex {[Co(bipy)(azpy)₂(NCS)₂]·H₂O}_n (where bipy=4,4′-bipyridine, azpy=4,4′-azobisp- yridine) has been synthesized and characterized by elemental analyses, IR, UV, thermal analyses, and vari-able-temperature magnetic susceptibility. The crystal (C₃₂H₂₆CoN₁₂OS₂, M_r=717.70) belongs to the orthorhombic, space group Pnna, a=2.21312(16)nm, b=1.40403(10)nm, c=1.14237(8)nm, V=3.5497(4)nm³, Z=4, D_c=1.343g·cm^-3, μ=0.645mm^-1, F(000)=1476, and final R₁=0.0691, wR₂=0.1129 for 231 parameters and 1674 observed reflections [I >2.00σ(I)]. The Co(Ⅱ) atom is, in a distorted octahedral geometry, coordi-nated by six nitrogen atoms from two bridging bipy, two monodentate azpy, and two thiocyanate groups. The bridging ligand bipy links Co(Ⅱ) atoms to form the infinite “rod＂ with terminal coordination azpy ligand acting as sidearms. Unprecedented three parallel interpenetrating two-dimensional (4,4) networks and novel infinite triple helices are formed via hydrogen-bonding interactions. CCDC: 155588.     

配合物[Cu2(m-MBA)4(2，2′-bipy)2(H2O)]·H2O的水热合成、晶体结构及电化学分析

A copper(Ⅱ) complex [Cu₂(m-MBA)₄(2，2′-bipy)₂(H₂O)]·H₂O with m-methylbenzoic acid (m-MBA), 2,2′-bipyridine (2,2′-bipy) and water molecule has been synthesized by means of hydrothermal way and characterized. Crystal data for this complex: monoclinic, space group C2/c, a=2.591 8(5) nm, b=1.414 2(3) nm, c=1.790 8(4) nm, β=131.80(3)°, V=4.893 3(17) nm³, D_c=1.379 g·cm^-3, Z=4, F(000)=2 104 , Final GooF=1.034, R₁=0.065 6, wR₂=0.197 6. The crystal structure shows that two neighboring copper(Ⅱ) ions are linked together by two bridging-chelating m-methylbenzoic acid groups, one bridging water molecule, forming a cage structure and the Cu(Ⅱ)-Cu(Ⅱ) bond distance is 0.366 7 nm. Each copper(Ⅱ) ion is coordinated with two nitrogen atoms of one 2,2′-bipyridine molecule and four oxygen atoms from three m-methylbenzoic acid molecules and one water molecule, repectiveley, forming a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the Complex was also investigated. CCDC: 648619.     

[Mn(H2O)(phen)2(PAc)](ClO4)的合成、红外光谱及晶体结构

The complex [Mn(H₂O)(phen)₂(PAc)](ClO₄) was synthesized and investigated by elemental analysis, molar conductivity, IR spectrum and X-ray diffraction methods, where phen=1,10-phenanthroline and PAc=phenylac-etate group. The complex crystallizes in the triclinic space group,P1 , with a=0.9289(2)nm,b=1.2425(2)nm,c=1.4791(3)nm,α=114.34(3)°,β=91.25(3)°,γ=104.65(1)°,V=1.4893(4)nm³,Z=2,F(000)=686,D_c=1.489g·cm^-3,μ=0.589mm^-1. The Mn(Ⅱ) ion has a six-coordinate distorted-octahedral geometry with the four nitrogen atoms of two phen ligands,a coordinated-water oxygen atom, and a carboxylate oxygen atom of PAc^-. There is π-π stacking interaction between two phen rings from two neighbor molecules.     

[Pb2(TNR)(NO3)2(H2O)]的制备和晶体结构研究

[Pb₂(TNR)(NO₃)₂(H₂O)] was prepared by reaction of the aqueous solution of lead nitrate and magnesium styphnate. The crystal structure of Pb₂(TNR)(NO₃)₂(H₂O)was determined by single crystal diffraction analysis. The crystal is triclinic, space group P1 with crystal parameters a=0.7279(2)nm,b=1.0698(2)nm,c=1.0738(2)nm;α=86.82(1)°,β=89.52(2)°,γ=83.50(2)°;V=0.8295(3)nm³,Z=2,D_c=3.201g·cm^-3, F(000)=716. The final R value is 0.0358.In the crystal structure, one lead ion was represented by nine coor-dination geometry; the other was showed as ten coordination geometry.     

[Cu(TO)2(H2O)4](PA)2的合成和晶体结构

[Cu(TO)₂(H₂O)₄](PA)₂ was prepared by mixing the aqueous solution of 1,2,4-triazol-5-one(TO) and Cu(PA)₂. The molecular structure and crystal structure of the title complex was determined by X-ray single crystal diffraction method. The crystal is triclinic, space group with a=0.7321(1)nm,b=0.7474(2)nm,c=1.3649(3)nm;α=88.65(2)°,β=85.63(1)°,γ=63.35(1)°;V=0.6655(2)nm³,Z=1. The Cu²⁺ coordinated with two TO molecule through its 2-nitrogen atom and four water molecules and showed an octahedral configuration.