配合物[Cu2(phen)2](SiW12O40)(H2O)7的合成、晶体结构及电化学分析

The title complex has been synthesized by the reaction of silicotungstic acid, 1,10-phenanthroline (phen) monohydrate and cupric acetate. The crystal structure belongs to triclinic system, space group P1 with a=1.158 46(15) nm, b=1.658 8(2) nm, c=1.664 4(2) nm, α=82.090(2)°, β=76.001(2)°, γ=86.531(2)°, and V=3.072 6(7) nm³, D_c=3.887 g·cm^-3, Z=2, F(000)=3 196. R₁=0.086 7, wR₂=0.185 8. The structure shows that the copper(Ⅱ) atom is coordinated with two nitrogen atoms from the one phen and three oxgygen atoms from three water, forming a distorted square-pyramid configuration The cyclic voltametric behavior of the complex is also reported. CCDC: 298807.     

[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.     

一维链状锰配位聚合物[Mn(3,5-Me2PhCO2)2(phen)]n的合成与晶体结构

A manganese coordination polymer [Mn(3,5-Me₂PhCO₂)₂(phen)]_n(phen=1,10-phenanthroline) has been synthesized by hydrothermal methods. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a=0.770 3(4) nm, b=1.145 2(6) nm, c=1.537 0(9) nm, α=78.182(9)°, β=77.170(9)°, γ=89.784(9)°, V=1.292 8(12) nm³, Z=2, M_r=533.47, D_c=1.370 g·cm^-3, μ=0.549 mm^-1, F(000)=554, R_int=0.043 4, R=0.060 8 ,wR=0.148 4. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from phen and four oxygen atoms from four 3,5-dimethylbenzolate molecules, completing an octahedral geometry. And the title complex forms one-dimensional chain structure through bridging 3,5-dimethylbenzolate molecules. CCDC: 642920.     

混合配体配合物[Cd2(phen)4(bmal)2]·3H2O的合成与晶体结构研究

A novel binucleus mixed-ligand[Cd₂(phen)₄(bmal)₂]·3H₂O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure analysis was carried out to determine the crystal structure of the title complex. The crystal of the title complex belongs to monoclinic system with space group P2₁/c, a=1.119 1(8) nm, b=2.480 5(17) nm, c=1.063 4(8) nm, β=142.042(12)°, Z=4, V=2.887(3) nm³, D_c=1.613 g·cm^-3, R₁=0.046 2, wR₂=0.115 6, F(000)=1 424. One carboxyl of bmal is coordinated to Cd(1) with monodentate form, the others are coordinated to Cd(2) with bidentate form. The complexes form a 1-D chain structure bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in bmal, the 2-D network structure was formed by π-π interaction of neighbouring phen. CCDC: 257080.     

配合物[Co(phen)2(m-chlorobenzoic acid)2·(H2O)]·(H2O)2的水热合成、晶体结构电化学分析

The title complex has been synthesized with m-chlorobenzoic acid, 1,10-phenanthroline and cobalt perchlorate anhydrous in the solvent mixture of water and methanol. Crystal data for this complex: triclinic, space group P1, a=0.870 7(3) nm, b=1.284 4(4) nm, c=1.692 9(5) nm; α=75.430(5)°, β=77.562(5)°, γ=86.346(5)°, V=1.789 4(9) nm³, D_c=1.456 g·cm^-3, Z=2, F(000)=806. Final GooF=1.065, R₁=0.068 4, wR₂=0.127 5. The crystal stru-cture shows that the Cobaly ion is coordinated with four nitrogen atoms from two 1,10-phenanthroline molecules and two oxygen atoms from one m-chlorobenzoic acid molecule and one water molecule respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619087.     

一维链状配位聚合物[Cd(N-MeIM)2(SCN)2]n的结构表征和电化学性能研究(英)

A novel cadmium(Ⅱ) isothiocyanate complex [Cd(N-MeIM)₂(SCN)₂]_n(N-MeIM=N-methylimidazole) has been prepared and characterized by spectroscopic analysis and crystallographic method. The title compound crystallize in the Triclinic system, space group P1, with lattice parameters a=0.589 50(12) nm, b=0.785 70(16) nm, c=0.882 00(18) nm, α=110.98(3)°, β=106.49(3)°, γ=95.08(3)°, and Z=1. The title compound exhibits an infinite chain structure in which each pair of Cd atoms is bridged by two η-1,3-SCN^- groups. The unique Cd atom lies on an inversion centre and the coordination sphere is completed by two N-MeIM N atoms to form a CdS₂N₄ octahedron. The polymeric chains are further extended into three-dimensional network via π…π stackings interactions between the imidazole rings. The cyclic voltammetry behaviors of the compound on glass carbon electrode showed a typical irreversible process. CCDC: 265283.     

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.     

甲酸桥联四核锰配合物[Mn4(O2CH)4(phen)8](ClO4)4·6H2O的水热合成和晶体结构

The title compound, [Mn₄(O₂CH)₄(phen)₈](ClO₄)₄·6H₂O(1), where phen=1,10-phenanthroline, was synthes-ized and its crystal structure was determined by X-ray diffraction structure analysis. The crystal is of monoclinic, space group P2/c with a=1.928 0(16) nm, b=1.297 0(11) nm, c=2.126 4(18) nm, V=5.242 2(8) nm³, Z=2, M_r=2 347.36, D_c=1.487 g·cm^-3, μ=0.659 mm^-1, F(000)=2 400, R_int=0.043 7, R=0.052 3, wR=0.118 6. The Mn atoms are octahed-rally coordinated by two O atoms of two ligands and four N atoms of two 1,10-phenanthroline molecules. The carboxyl group coordinates to Mn(Ⅱ) in the bridging bidentate mode. CCDC: 675520.     

配合物{CdI(phen)(H2O)[C8H11O2(COO)]}·H2O的水热合成、晶体结构及电化学性质

One Complex{CdI(phen)(H₂O)[C₈H₁₁O₂(COO)]}·H₂O with bicycle[2.2.1]hept-2-en-5,6-dicarboxylic acid [C₇H₈(COOH)₂], hydriodic acid and 1,10-phenanthroline(phen) has been synthesized by means of hydrothermal way and characterized. It crystallizes in the triclinic space group P1, with a=0.975 4(2) nm, b=0.990 0(2) nm, c=1.319 1(3) nm, α=89.146(4)°, β=69.800(3)°, γ=68.718(3)°, V=1.105 0(4) nm³, D_c=1.914 g·cm^-3, Z=2, F(000)=620, Final R₁=0.033 2, wR₂=0.085 7, GooF=1.092. The crystal structure shows that the cadmium ion is coordinated with two oxygen atoms from one C₇H₁₀(COOH)₂ molecule, two nitrogen atoms from the 1,10-phenanthroline, one oxygen atom from one water molecule and one iodine ion, respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 648242.     

二聚体配合物[Cd(5-oxo-4-oxa-tricyclo[4.2.1.0]nonane-9-carboxylic radical)2(phen)]2的合成、晶体结构及荧光性质

A seven-coordinate dimmer has been synthesized with 5-oxo-4-oxa-tricyclo[4.2.1.0]nonane-9-carboxylic acid and 1,10-phenanthroline. The crystal structure was determined by single-crystal X-ray structural analysis. The crystal belongs to a monoclinic system, space group P2₁/n, with a=1.552 08(12) nm, b=1.065 52(8) nm, c=1.626 57(12) nm, β=100.100(10)°, V=2.648 3(3) nm³, D_c=1.643 g·cm^-3, Z=2, F(000)=1 328, Final GooF=1.026, R₁=0.026 2, wR₂=0.059 2. The crystal structure shows that the cadmium ion is coordinated with five oxygen atoms and two nitrogen atoms, forming a distorted capped octahedral coordination geometry. There exist two types of coordinated 5-oxo-4-oxa-tricyclo[4.2.1.0]nonane-9-carboxylic acid anions: the tridentate-chelating-bridging ones and the bidentate-chelating ones. The Cd(Ⅱ)…Cd(Ⅱ) distance is 0.373 7 nm. The luminescence property of the complex is also studied. CCDC: 7299551.     

邻-(4-甲基苯甲酰基)-苯甲酸双核镉(Ⅱ)配合物的水热合成、晶体结构及热稳定性

<正>羧酸因其具有多样的配位方式、羧基氧原子易参与形成氢键以及本身能减缓抗衡离子效应的负电性而被广泛应用于配合物的合成中[1-4]。目前,研究主要集中于苯甲酸及其衍生物构筑的配合物,而其     

2，6-二氯苯甲酸桥联的双核锰配合物的水热合成与晶体结构

A dinuclear manganese(Ⅱ) complex, [Mn₂(L¹)₂(phen)₄]·(ClO₄)₂ (1), has been synthesized and structurally characterized (HL¹=2,6-dichlorobenzoic acid, phen=1,10-phenanthroline). It crystallizes in triclinic system, space group P1 with a=1.112 3(4) nm, b=1.378 2(4) nm, c=2.085 7(3) nm, α=93.768(2)°, β=90.606(10)°, γ=95.606(3)°, V=3.174 8(15) nm³, Z=2, C₆₂H₃₈C₁₆Mn₂N₈O₁₂, M_r=1 409.58, D_c=1.475 g·cm^-3, μ=0.718 mm^-1, F(000)=1 428, R=0.064 3, wR=0.138 3. In the crystal the manganese atom is six-coordinated by two oxygen atoms from two different 2,6-dichlorobenzolate molecules and four nitrogen atoms from two 1,10-phenanthroline molecules, completing an octahedral geometry. CCDC: 692296.     

Hydrothermal Synthesis,Crystal Structure and Electrochemical Properties of Complex [Cd(phen)_3]·(ClO_4)_2·(p-MBA)_2·(H_2O)_2

One new cadmium complex [Cd(phen)3]·(ClO4)2·(p-MBA)2·(H2O)2 has been hydro-thermally synthesized by reacting p-methylbenzoic acid (p-MBA),1,10-phenanthroline (phen) and cadmium perchlorate. It crystallizes in the triclinic system,space group P1,with a=1.2809(3),b= 1.3431(3),c=1.3734(3) nm,α=84.259(4),β=71.603(3),γ=74.424(3)o,V=2.1594(8) nm3,Dc= 1.532 g/cm3,Z=2,F(000)=1008,μ=0.697 mm-1,R=0.0646 and wR=0.1648. The crystal structure shows that the cadmium ion is coordinated with six nitrogen atoms from three 1,10-phenanthroline molecules,forming a distorted octahedral coordination geometry. The result of electrochemical property analysis shows that the electron transfer in the electrode reaction is irreversible.     

Synthesis, Crystal Structure and Electrochemical Properties of a Cadmium(II) Complex with α-Furoic Acid and 1,10-Phenanthroline

A new cadmium complex [Cd(phen)3]·(ClO4)2·(α-FRA)·(H2O)3 was prepared by self-assembly of α-furoic acid, 1,10-phenanthroline (phen), and cadmium perchlorate. It crystal- lizes in the monoclinic system, space group P21/n, with a = 1.28130(15), b = 2.5957(3), c = 1.35449(16) nm, β = 109.395(2)o, V = 4.2492(9) nm3, Dc = 1.491 g/cm3, Z = 4, F(000) = 1926, GOOF = 1.023, the final R = 0.0729 and wR = 0.2086. The crystal structure analysis indicates that the cadmium ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the com- plex was also investigated.     

由亚甲基丁二酸根桥联的新颖双U形四核铜配合物[Cu_4(IA)_2(phen)_4(H_2O)_4](NO_3)_4(H_2O)_6

亚甲基丁二酸、邻菲啰啉(phen)和硝酸铜在甲醇-水中反应合成了一种由亚甲基丁二酸根(IA)桥联的新颖双U形四核铜配合物[Cu4(IA)2(phen)4(H2O)4](NO3)4(H2O)6(1),其结构经UV,IR,元素分析和单晶X-射线衍射分析表征。1属三斜晶系,Pī空间群,晶胞参数a=1.2262(3)nm,b=1.282 4(3)nm,c=1.3551(3)nm,α=63.236(2)°,β=75.555(2),°γ=73.126(2)°,Z=2,F(000)=844,R=0.059 6,wR=0.166 2。IA通过8个羧基O将两个U形双核亚单元联接成具有一个对称中心的双U形四核结构,其中每个U型亚单元包含晶体学上不对称的两个Cu(Ⅱ)离子。每个Cu(Ⅱ)离子均处于畸变的四方锥配位环境,除与IA和phen的O,N配位形成锥底平面外,Cu(Ⅱ)还与水配位。     

4-甲基苯硫乙酸与含氮配体构筑的两个化合物的合成，晶体结构，热稳定性与发光性质的研究

合成了2个配合物[ZnL₂(Him)₂] (1)和[ (Cu₂L₂(phen)₂( μ₂-Cl)₂)·(Cu₂( μ₂-L)₂(phen)₂Cl₂)] (2)(L=4-甲基苯硫乙酸,Him=咪唑,phen=1,10-邻菲咯啉),进行了元素分析、红外、热重等表征,并测定了其晶体结构。配合物1晶体属于单斜晶系,空间群为C2/c。配合物2晶体属于三斜晶系,空间群为P1。配合物1是由N-H…O氢键作用形成的一维带状结构。配合物2的单胞中含有2个分别由氯原子与羧基氧原子桥联的双核独立分子,通过C-H…O,C-H…Cl氢键以及C-H…π作用而构成三维结构。室温固体荧光分析显示配合物1具有较强荧光吸收。     

含氮螯合配体过渡金属配合物修饰的缺位型Keggin多酸盐

在常温条件下合成了铜-邻菲啰啉修饰的结构独特的多酸衍生物H₄[Cu(phen)(H₂O)][Cu(phen)][α-SiW₁₁O₃₉]·3H₂O(1). 该化合物分子中2个独立的非二聚体的铜-邻菲啰啉平行地与缺位多酸空穴外的氧配位键合, 通过元素分析、红外光谱、热重分析和X射线单晶衍射对其结构进行了表征. 结果表明, 该化合物属三斜晶系, P1空间群, 晶胞参数a=1.3624(2) nm, b=1.4133(2) nm, c=2.0470(3) nm, α=97.840(3)°, β=95.117(3)°, γ=112.483(3)°.     

之字链聚合物[Zn(o-bda)(phen)(H2O)]n·nH2O的结构

[Zn(o-bda)(phen)(H₂O)]_n·nH₂O (C22H20N2O6Zn) (1) [where o-bda is o-phenylenediacetic acid dianion and phen is 1,10-phenanthroline] crystallizes in triclinic system, space group P1 with a=0.826 5(4) nm, b=1.042 4(5) nm, c=1.238 1(6) nm, α=76.987(9)°, β=70.987(9)°, γ=78.281(8)°, V=0.9728(8) nm³, Z=2, D_c=1.617 g·cm^-3, μ=1.308 mm^-1 and F(000)=488. Zn(Ⅱ) ion has a distorted trigonal bipyramid coordination geometry formed by two carboxyl O atoms from two different o-bda groups, two N atoms from the phen ligand and one terminal water molecule. Adjacent Zn(Ⅱ) ions are interlinked by o-bda groups into a infinite zigzag chain structure with a Zn…Zn distance of 0.825 6(4) nm. The adjacent zigzag chains may also be paired under direction of supramolecular recognition and attraction through both π-π stacking and hydrogen bonding interactions into molecular zippers, which further interlinked into a three-dimensional supramolecular network by these noncovalent interactions. CCDC: 600935.     

双环[2.2.1]-2-庚烯-5，6-二甲酸镍配合物的合成、晶体结构及热稳定性

The nickel complex Ni(phen)(H₂O)₃[C₈H₁₁O₂(COO)] has been synthesized with bicycle[2.2.1]hept-2-en-5,6-dicarboxylic acid [C₇H₈(COOH)₂] by means of solvent way. It crystallizes in the triclinic space group P1, with a=0.780 58(16) nm, b=1.189 9(2) nm, c=1.214 8(2) nm, α=66.20(3)°, β=88.28(3)°, γ=86.33(3)°, V=1.030 3(4) nm³, D_c=1.554 g·cm^-3, Z=2, F(000)=502. Final GOF=1.107, R₁=0.026 4, wR₂=0.070 2. The crystal structure shows that the nickel ion is coordinated with four oxygen atoms from one bicycle[2.2.1]-2-hepten-5,6-dicarboxylic acid molecule and three water molecules, respectively, with two nitrogen atoms from the 1,10-phenanthroline molecule, forming a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex was stable under 210.0 ℃. CCDC: 741933.     

含Br…π及Br…Br相互作用的1-溴-3，5-二(1-咪唑基-亚甲基)苯-镉(Ⅱ)配合物的合成和晶体结构

利用双齿含氮有机配体1-溴-3,5-二(1-咪唑基-亚甲基)苯(bib)与不同的镉盐反应合成了2个配合物[Cd(bib)₂(NO₃)₂] (1)和[Cd(bib)Br₂] (2)。利用元素分析及X-射线衍射单晶结构分析对其进行了表征。晶体结构表明标题化合物1晶体属于三斜晶系,P1 空间群。化合物2晶体属于单斜晶系,P2₁/c空间群。在化合物1中,一维链状结构通过Br…π相互作用连接成为二维网状结构;而化合物2的二维结构通过卤素…卤素相互作用形成一个三维结构。