三元混合配合物Cu(C10H8N2O3)·(C5H5N)·(H2O)的合成和晶体结构

The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C₁₀H₈N₂O₃)·(C₅H₅N)·(H₂O) (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm³, Z= 2, D_c= 1.547 Mg·m^-3, μ(MoKα) = 1.417 mm^-1, F(000) = 374. The final R₁ = 0.030 6, wR₂= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C₁₀H₈N₂O₃^2- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.     

配合物Ni(C14H10N2O3)(C5H5N)的合成和晶体结构

A novel nickel(Ⅱ) complex with 2,4-dihydroxybenzalidene benzoylhydrazone and pyridine ligands, Ni(C₁₄H₁₀N₂O₃)(C₅H₅N), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pbca. The cell parameters are: a=1.580 20(19) nm, b=1.362 18(16) nm, c=1.616 50(19) nm, and V=3.479 5(7) nm³, Z=8, D_c=1.497 Mg·m^-3, μ(MoKα)=1.139 mm^-1, F(000)=1 616, R=0.032 9 and wR=0.077 0 for 2 772 observed reflections (I>2σ(I)) out of 3810 unique ones. The nickel(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone schiff base ligand and one nitrogen atom of the pyridine ligand. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 244668.     

[Co(HOC10H6COO)2(H2O)4]配合物的合成、晶体结构和性质研究

Complex [Co(HOC₁₀H₆COO)₂(H₂O)₄] was synthesized by reaction of hydroxy-2-naphthoic acid with CoCl₂·6H₂O. The compound was characterized by elemental analysis, IR and the structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n with a=0.675 8(2) nm, b=0.518 15(14) nm, c=2.962 9(9) nm, β=94.925(8)°. V=1.033 6(5) nm³, Z=2, D=1.624 Mg·m^-3, F(000)=522. The Co atom has an octahedron coordination geometry and was six-coordinated with two oxygen atoms from two carboxylate ligands and four oxygen atoms from four water molecules. The complex molecules were linked by different hydrogen bonds to form a 2D network. The complex has thermal stability and shows a strong fluorescent emission at 421 nm (λ_ex=342 nm). CCDC: 250903.     

配合物[Cu(HPHAc)2(py)2](H2PHAc=苯羟乙酸，py=吡啶)的合成和晶体结构

The novel copper(Ⅱ) complex with α-hydroxyphenylacetic acid (H₂PHAc) and pyridine (py) ligands, [Cu(HPHAc)₂(py)₂], has been synthesized and characterized by elemental analysis and IR spectroscopy. Its crystal structure was determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group C2/c. The cell parameters are: a=1.712 5(3) nm, b=1.533 2(2) nm, c=0.963 42(14) nm, β=111.866(2)°, V=2.347 6(6) nm³, and D_c=1.483 Mg·m^-3, Z=4, F(000)=1 084. The structure was refined to final R₁=0.071 4, wR₂=0.166 1. The complex has a six-coordinated distorted octahedral geometry, in which copper(Ⅱ) ion coordinates with two carboxylic oxygen atoms and two hydroxyl oxygen atoms from the two α-hydroxyphenylacetic acid ligands, two nitrogen atoms from the two pyridine ligands. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 255346.     

杂-双核配合物[CaCu(C3H2O4)2(H2O)4]n的合成、晶体结构及热稳定性

The title complex， [CaCu(C₃H₂O₄)₂(H₂O)₄]_n， with a formula of C₆H₁₂CaCuO₁₂ and M_r=379.78 has been sy-nthesized and characterized by single crystal X-ray diffraction structure analysis， elemental analysis， IR spectra and TG-DTG techniques. The results show that the crystal is Orthorhombic， space group Pbcn with a=0.669 21(5) nm， b=1.370 23(5) nm， c=1.322 39(10) nm， V=1.212 59(16) nm³， D_c=2.080 g·cm^-3， μ=2.288 mm^-1， F(000)=772 and Z=4. The final R=0.054 0 and wR=0.112 8 for 1 189 observed reflections with I>2σ(I). The structure of the title complex consists of CaO₈ polyhedra and CuO₆ elongated octahedra linked together by malonate ligands. The Ca(Ⅱ) cation， on a twofold axis， is coordinated by two water molecules and six malonate O atoms. The Cu(Ⅱ) cation， which lies in a centre of symmetry in an octahedral arrangement， is coordinated by four malonate O atoms and two water molecules. The structure comprises alternating layers along the [101] plane， with the shortest Cu…Cu distance of 0.762 46(6) nm. The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds. Its thermo gravimetric analysis was determined by TG-DTG techniques. CCDC: 663184.     

三核锌配合物的合成及结构表征

A trinuclear Zn(Ⅱ) complex [Zn₃(L)₂(Cl)₂(OSO₃)₂(H₂O)₂]·2H₂O (1) (L=N¹-(2-aminoethyl)-N¹-(2-imidazolethyl)-ethane-1,2-diamine) was synthesized by reaction of ligand L with ZnSO₄·7H₂O at pH=9 in air. The complex has been characterized by elemental analysis, FTIR and X-ray single crystal diffraction. It reveals that the crystal of complex 1 belongs to monoclinic C2/c space group, a=3.516 9(7) nm, b=0.676 57(14) nm, c=1.502 2(3) nm, β=110.955(4)°, V=3.337 9(12) nm³, Z=4. In complex 1, two ligands L bridge three Zn(Ⅱ) centers to form trinuclear structure which was further connected by hydrogen bonding to form two-dimensional structure. CCDC: 609515.     

一维链状的2-氧-1(4H)-吡啶氮乙酸钴配位聚合物{[Co(2-OPA)2(4，4′-bipy)(H2O)2]·6H2O}n的合成、结构及性能研究

A coordination polymer of {[Co(2-OPA)₂(4，4′-bipy)(H₂O)₂]·6H₂O}_n (2-OPA^-=2-oxo-1(4H)-pyridineacetate anion) was synthesized and characterized by elemental analysis， IR， TG， fluorescence and X-ray single crystal diffraction. The title complex crystallizes in triclinic space group P1， with a=0.856 66(17) nm， b=0.859 58(17) nm， c=1.142 2(2) nm， α=69.64(3)°， β=68.35(3)°， γ=74.88(3)°， and V=0.724 4(3) nm³， Z=1， R=0.064 4， wR=0.159 8. Each Co atom occupies a special position of inversion center and has an octahedral coordination environment， defined by two carboxyl O atoms from two 2-OPA^- ligands， two N atoms from two 4，4′-bipy ligands and two water molecules. Adjacent Co(Ⅱ) atoms are bridged by 4，4′-bipy ligands， forming a one-dimensional linetype chain structure. The closest Co…Co distance is 1.142 2(2) nm. The results of TG and fluorescent analysis show that the title coordination polymer is stable under 90.2 ℃ and has three emission peaks at 368， 422 and 484 nm. CCDC: 643626.     

混配配合物[Zn(acac)2(C5H4NOH)]的合成、晶体结构及表征

The complex [Zn(acac)₂(C₅H₄NOH)] was synthesized based on the reaction of zinc(Ⅱ) acetate, acetylaceton and 3-hydroxypyridine(C₅H₄NOH) in methanol medium. The structure of the complex was confirmed by IR, ¹H NMR, elemental analysis, thermal analysis and X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P2₁/n, and a=0.743 7(3) nm, b=0.829 5(3) nm, c=2.612 5(9) nm, β=95.026(6)°, V=1.605 4(9) nm³; D_c=1.484 g·cm^-3; Z=4; F(000)=744; μ=1.551 mm^-1. Zinc(Ⅱ) atom lies at the center of an coordination of the distorted square pyramidal formed by four O atoms which come from two different acetylaceton ions and one N atom from the 3-hydroxypyridine molecule. CCDC: 600232.     

四(1-乙基咪唑)二异硫氰酸锰的晶体结构和热性能

A complex [Mn(NCS)₂(Eim)₄] (where Eim=1-ethylimidazole) has been synthesized and structurally cha-racterized by X-ray diffraction single-crystal structure analysis. The compound crystallizes in the Orthorhombic space group Pbca with the cell parameters: a=1.618 9(3) nm, b=1.787 4(4) nm, c=1.999 4(4) nm, and V=5.786(2) nm³, Z=8. In the structure, each Mn atom is coordinated by four Eim ligands and a pair of monodentate isothiocyanic groups, affording a compressed octahedral MnN₆ core. The NCS^- anions are trans and four N atoms from the Eim ligands define the equatorial plane. The C-H…π supramolecular interactions between C-H and imidazole rings of Eim link the molecules into independent chains running along the c-axis. The thermal gravity(TG) data indicates that thermal decomposition of the title complex takes place in two steps, the residue is Fe. CCDC: 646113.     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

一维链状酰基吡唑啉酮配合物Zn(C26H15N3O2Cl)2的合成、晶体结构及热稳定性

A one-dimensional chain complex bis{4-[(Z)-(4-chlorophenylamino)(2-furyl)methylene]-3-methyl-1-phenylpyrazol-5-onato}zinc(Ⅱ) Zn(C₂₆H₁₅N₃O₂Cl)₂ has been synthesized. Its structure was characterized by elemental analysis, IR, UV, thermal analysis and X-ray diffraction single crystal structure analysis. The title complex crystallizes in triclinic system, space group P1 with a=0.903 58(18) nm, b=1.359 8(3) nm, c=1.757 0(4) nm; α=102.42(3)°, β=101.24(3)°, γ=109.2(4)°, V=1.906 3(10) nm³. The final R factors are R=0.051 3 and wR=0.133 9. The zinc atom is four-coordinate involving two oxygen atoms and two nitrogen atoms forming a distorted tetrahedral geometry. The intermolecular hydrogen bonds C-H…N, C-H…Cl, C-H…π, together with intramolecular π…π stacking in the large congujate system, leading to the formation of a one-dimensional supramolecular chain. The results of TG-DTA analysis show that the title complex was stable under 323 ℃. CCDC: 299690.     

Zn的3，5-二溴水杨醛水杨酰腙配合物的合成、表征及晶体结构

The title complex [Zn(C₁₄H₈N₂O₃Br₂)(C₅H₅N)₃] was synthesized in DMF and pyridine. It has been characterized by IR, element analysis and X-ray diffraction analysis. The crystal structure of the title complex belongs to monoclinic space group P2₁/c with cell parameters: a=0.999 78(6) nm, b=1.951 11(13) nm, c=1.496 02(10) nm, β=97.126 0(10)°, and V=2.895 7(3) nm³, Dc=1.639 g·cm^-3, Z=4, F(000)=1 424, μ=3.647 mm^-1, the final R=0.061 0 and wR=0.140 2 for 3 528 observed reflections with I>2σ(I). The X-ray crystal structure analysis revealed that the center zinc(Ⅱ) is bonded to two oxygen atoms and one nitrogen atom from a tridentate ligand and three nitrogen atoms from three solvent pyridine molecules to form a six-coordinate octahedron. CCDC: 261047.     

3-甲基-4-对甲基苯基-5-(2-吡啶基)-1，2，4-三唑双核铜(Ⅱ)配合物的合成、晶体结构及磁性

A dinuclear Cu(Ⅱ) complex [Cu₂(MMBPT)₂Cl₄(H₂O)_2.5] (I) [MMBPT=3-Methyl-4-(4-Methylphenyl)-5-(2-pyridyl)-1,2,4-triazole] was synthesized by reaction of MMBPT with CuCl₂·2H₂O and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group P2₁/c with a=1.273 4(3) nm, b=1.237 5(3) nm, c=2.403 2(5) nm, β=90.51(3)°. V=3.786 6(13) nm³, Z=2, D_c=1.429 Mg·m^-3, μ=1.445 mm^-1, F(000)=1 660, and final R₁=0.055 5, wR₂=0.129 7. The crystal structure shows that the dinuclear Cu₂N₆ unit is almost planar in which each Cu(Ⅱ) ion was five-coordinated by one nitrogen atoms from MMBPT and two chlorine in the basal positions and two nitrogen atoms from two MMBPTs respectively in the axial one, to form a distorted trigonal bipyramidal geometry. Magnetic measurements reveal a relatively strong antiferromagentic interaction in the complex. CCDC: 720011.     

超分子钴(Ⅱ)配合物[CoL(H2O)2]n的合成与结构表征

A mononuclear Cobalt(Ⅱ) complex [CoL(H₂O)₂]_n (H₂L: 4,4′,6,6′-Tetrabromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction single crystal structure analysis. The crystal of the complex belongs to monoclinic space group P2₁/c with a=2.516 8(3) nm, b=1.023 43(18) nm, c=0.789 17(14) nm, β=91.375(2)°, V=2.032 1(5) nm³, Z=4, D_c=2.317 Mg·m^-3, μ(Mo Kα)=8.747 mm^-1, F(000)=1 356, R₁=0.049 7, wR₂=0.110 4. The crystal structure of [CoL(H₂O)₂]_n indicates that the complex consists of one cobalt(Ⅱ) atom, one L^2- unit and two coordinated water molecules, and the coordination number of the cobalt(Ⅱ) atom is six. One-dimensional chain supramolecular structure is formed by intermolecular hydrogen bonds and π-π stacking of neighboring benzene rings. CCDC: 652649.     

一维链状超分子化合物[Zn(dafo)2(H2O)2](NO3)2(dafo=4，5-二氮芴-9-酮)的合成、表征和晶体结构

A novel one-dimensional chain complex [Zn(dafo)₂(H₂O)₂](NO₃)₂ was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a= 0.702 7(14) nm, b= 0.828 95(17) nm, c= 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.     

Cu(Ⅱ)-2′-(2-噻吩亚甲基)水杨酰腙Schiff碱配合物的合成、表征、晶体结构及抑菌活性研究

In ethanol, the copper(Ⅱ) complex with the 2′-(2-thienylidene)-h ydroxybenzoylhydrazide, Cu(C₁₂H₁₀N₂O₂S)₂, was synthesized, and it′s structure was characterized by IR, UV and elemental analysis. The single crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with cell constants, a=2.273 6(4) nm, b=0.592 12(9) nm, c=1.828 1(3) nm, β=109.735(5)°, V=2.316 4(7) nm³, Z=4, μ=1.164 mm^-1, D_c=1.595 g·cm^-3, F(000)=1 140, R=0.048 6, wR=0.101 6. In the compound copper(Ⅱ) atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. Their biological activities have been measused. The results show that the anti-bacterial activity of the coordination compound is much better that of the ligand. CCDC: 272938.     

一个新的双核锌配合物Zn2(dhaash)2(py)4的合成及晶体结构

The crystal of binuclear zinc complex Zn₂(dhaash)₂(py)₄ was obtained in DMF and pyridine, where H₂dhaash is 2,4-dihydroxy-5-acetylacetophenone-N-salicylhydrazone. It has been characterized by IR, UV, element analysis and X-ray single crystal diffraction. The crystallographic data were as follows: monoclinic system, space group P2₁/c, a=1.108 98(11) nm, b=1.640 84(16) nm, c=1.445 14(14) nm, β=108.617(2)°, Z=2, V=2.492 1(4) nm³, D_c=1.466 g·cm^-3, M_r=1 099.74, μ=1.031 mm^-1, F(000)=1 136 and the final R=0.044 8 and wR=0.105 8 for 4 143 observed reflections with I≥2σ(I), respectively. The X-ray crystal structure analysis revealed that, in the centrosymmetric binuclear complex molecule, two zinc(Ⅱ) centers are linked by two oxygen atoms (O(3) and O(3A)), respectively. Zn(1)…Zn(1A) distance is 0.314 81(6) nm, O(3)…O(3A) distance is 0.270 4(2) nm. Every zinc(Ⅱ) ion has an elongated octahedral coordination. For example, the two pyridine nitrogen atoms, one oxygen atom and one nitrogen atom from salicylhydrazone, one oxygen atom from 2,4-dihydroxy-5-acetylacetophenone in one dhaash^2- ligand and one oxygen atom from 2,4-dihydroxy-5-acetylacetophenone in another dhaash^2- ligand coordinated to zinc(Ⅱ) ion, respectively. Two zinc(Ⅱ) ions and all the 72 non-hydrogen atoms in the two dhaash^2- ligands are in the same plane. CCDC: 261929.     

3-甲基-4-对甲基苯基-5-(2-吡啶基)-1，2，4-三唑双核锰(Ⅱ)配合物的合成及晶体结构

A dinuclear Mn(Ⅱ) complex [Mn₂L₂(μ-Cl)₂Cl₂(H₂O)₂] (1) was synthesized by reaction of ligand L with MnCl₂ ·4H₂O and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group C2/c with a=2.018 0(15) nm, b=0.894 0(6) nm, c=1.932 1(14) nm, β=97.506(12)°. V=3 456(4) nm3, Z=4, D_c=1.515 Mg·m^-3, μ=1.081 mm^-1, F(000)=1 608, and final R₁=0.043 8, wR₂=0.109 9. The result shows a Mn(Ⅱ) ion was six-coordinated by a bidentate 3-methyl-4-( p-methylphenyl)-5-(2-pyridyl)-1,2,4-triazole, one chlorine and one bridging chlorine atom in the basal positions and one chloride atom and one water molecule in the axial one, to form a distorted octahedral-pyramidal geometry. CCDC: 713047.     

氢键构筑具有三维结构的配合物[Cu(N-phthgly)2(H2O)2]·C2H5OH的合成及晶体结构

A copper(Ⅱ) complex [Cu(N-phthgly)₂(H₂O)₂]·C₂H₅OH(N-Hphthgly=N-phthaloylglycine) has been synthesized and characterized by elemental analysis, infrared spectroscopy and X-ray crystallography. The complex crystallizes in triclinic space group P1 with a=0.472 90(7) nm, b=1.080 01(13) nm, c=1.154 02(15) nm, α=74.360 0(10)°, β=79.151 0(10)°, γ=87.918(2)°, V=0.557 37(13) nm³, Z=1. The central copper atom allows the formation coordination environment with two O(5) atoms of two water ligands and two O(1) atoms of two N-phthgly ligands. The complex forms a step-like 3D structure through the three types of O-H…O hydrogen bonds and the Cu…O weak interaction. CCDC: 712945.     

草酸根桥联的双核铜(Ⅱ)配合物[Cu2(phen)2(H2O)2(μ2-C2O4)](NO3)2的合成及晶体结构

A new binuclear copper(Ⅱ) complex, [Cu₂(phen)₂(H₂O)₂(μ₂-C₂O₄)](NO₃)₂, has been synthesized and characterized by elemental analysis, IR and UV-Vis spectrum. Its crystal structure was determined by single crystal X-ray diffraction techniques. Crystal data: monoclinic, space group P2₁/c, a=0.712 21(8) nm, b=1.170 93(14) nm, c=1.783 7(2) nm, β=111.828(2)°, and V=1.380 8(3) nm³, D_c=1.769 Mg·m^-3, Z=2, F(000)=744, R₁=0.025 4, wR₂=0.069 5, Gof=1.077, Δρ=328～-455 e·nm^-3. The complex is packed by one centrosymmetry binuclear copper(Ⅱ) unit, oxalate dianion and NO₃^- anion. In the molecule structure of the title complex, two Cu(Ⅱ) ions are bridged by oxalate dianion and each Cu(Ⅱ) ions coordinates with two nitrogen atoms from 1,10-phenanthroline ligand and one oxygen atom from water to form a five-coordinate distorted square-pyramidal configuration. The hydrogen bonds are observed between coordinated water molecules and NO₃^- anions. The analysis of the crystal structure indicates that the complex has a two-dimensional stacking network structure, which is formed by intramolecular hydrogen bonds, intermolecular hydrogen bonds and stacking effect of aromatic ring. CCDC: 255345.