镧-锌杂多核配合物的合成和晶体结构

A new heteronuclear complex, [LaZnL₅(C₂H₅OH)(phen)]₂ (HL=α-methylacrylic acid, phen=1, 10-phen- anthroline), was synthesized and characterized by elemental analysis, infrared absorption spectra (IR) and single crystal X-ray diffraction analysis. The complex crystallizes in space group P1 with the cell dimensions a=12.614(3), b=14.485(4), c=12.148(2)?, α=109.68(2), β=115.65(1), γ=66.87(2)°. The complex mole- cule is a discrete tetranuclear molecule bridging by α-methylacrylate groups.     

高氯酸二水邻菲咯啉合铜配合物的合成和晶体结构

Crystal structure of the title compound， Cu(phen)(H₂O)₂·ClO₄(phen=1，10-phenanthroline)， was deter-mined by X-ray crystallography. It crystallizes in the monoclinic system， space group C2/c with lattice parameters a=1.49071(4)nm， b=1.38594(4)nm， c=0.70292(1)nm， β=108.509(1)° and Z=4; The Cu(Ⅰ) ion is chelated by a phen ligand and two aqua ligands in cis arrangement and assumes a C2 symmetric square-planar geometry with the CuN₂O₂ core. Eight Cu(phen)(H₂O)₂·ClO₄ molecules are interconnected by strong hydrogen bonds between coordinated water molecules and uncoordinated perchlorate anions to form a molecular scale cavities along c axis. The bond distances of Cu-N and Cu-O are 0.2003(4)nm and 0.1973(3)nm， respectively. CCDC： 197600.     

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.     

混配配合物[Zn(CF3COO)2(C7H6NS)2]的合成、晶体结构及表征

A mixed complex [Zn(CF₃COO)₂(C₇H₆NS)₂] was synthesized based on the reaction of Zn(CF₃COO)₂ and 2-aminobenzothiazol (C₇H₆NS) in methanol. The structure of the complex was characterized by elemental analysis, IR, ¹H NMR and thermal analysis. The crystal structure of the complex was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group C2/c, a=3.174 3(9) nm, b=1.010 0(3) nm, c=1.723 1(5) nm, β=118.841(4)°, V=4.839(2) nm³; D_c=1.625 g·cm^-3; Z=8; F(000)=2 368; μ=1.266 mm^-1. CCDC: 600233.     

对氟苯甲醛水杨酰腙镍(II)配合物的合成、表征及其晶体结构

A nickel(II) complex Ni(C₁₄H₁₀N₂O₂F)₂ was synthesized from p-fluorobenzaldehyde salicylhydrazone and Ni(CH₃COO)₂·4H₂O and crystallized by diffusion, the structure of which was characterized by IR spectrum, ¹H NMR, and X-ray single-crystal diffraction. The complex crystallizes in monoclinic space group C2/c with a=2.460 6(2) nm, b=0.774 1(1) nm, c=1.534 9(1) nm, β=122.300(1)°, and V=2.471 1(4), Z=8, D_c=1.541 g·cm^-3. We reported the IR, ¹H NMR, crystal structure. CCDC: 638652.     

镉(Ⅱ)与对乙酰氨基苯甲酸、4，4′-联吡啶配位聚合物的合成、晶体结构及荧光性质

The complex {[Cd₂(C₉H₈O₃N)₂(CH₃COO)₂(4,4′-bipy)₂]·(4,4′-bipy)·(H₂O)₄}_n with 4-acetamidobenzoic acid and 4,4′-bipyridine has been synthesized with liquid diffusion method and characterized. It crystallizes in the monoclinic space group C2/c. The crystal structure shows that two neighboring cadmium(Ⅱ) ions are linked together by two bridging acetic acid radicals, forming a binuclear structure. Adjacent binnuclear structure is linked together by two bridging 4,4′-bipy molecules and the complex molecule forms an one-dimensional double-chain structure. The luminescent properties of the complex were studied. CCDC: 734878.     

具有N…Cu作用的一维链状配合物Cu(C8H9N2O2)2的合成和晶体结构

The title complex Cu(L)₂ (HL=o-vanillin hydrazone) was synthesized by the reaction of Cu(CH₃COO)₂·H₂O with o-vanillin hydrazone in the ethanol. It was characterized by elemental analysis, IR and X-ray single crystal structure analysis. The crystal of the title complex [Cu(C₈H₉N₂O₂)₂] belongs to triclinic, space group P1 with a=0.457 57(8) nm, b=1.333 2(2) nm, c=1.386 0(3) nm, α=108.955(2)°, β=90.868(2)°, γ=95.859(2)°, V=0.794 4(2) nm³, Z=2, D_c=1.647 Mg·m^-3, μ=1.406 mm^-1, F(000)=406, and final R₁=0.035 1, wR₂=0.096 3. The complex comprises a four-coordinated copper(Ⅱ) center, with an N₂O₂ planar coordination environment. The molecules are packed in one-dimensional chain polymer though the N…Cu interaction from adjacent molecules, respectively. CCDC: 634854.     

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.     

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.     

N，N′-二苄基-苯并咪唑四氯合铜(Ⅱ)化合物的合成、结构和性能研究(英)

A novel N，N′-dibenzyl-benzimidazolium tetrachlorocuprate(Ⅱ) complex, [C₂₁H₁₉N₂]₂[CuCl₄], was synthesized and its crystal structure was determined by X-ray diffraction. It crystallizes in monoclinic system, space group P2/c, a=1.203 9(2) nm, b=0.975 0(2) nm, c=1.878 2(6) nm, β=114.12(2)°, V=2.012 2(8) nm³. Its structure was identified by EA, IR and UV spectra and characterized by electrochemistry, thermal and magnetic property. The Cu(Ⅱ) atom of [CuCl₄]^2- has distorted tetrahedral coordination geometry. In the crystal structure, there are strong extensive C-H…Cl hydrogen bonds and π-π stacking interactions, which stabilized the crystal structure. CCDC: 221570.     

双核铜(Ⅱ)-氟喹诺酮-邻菲咯啉混配配合物的合成、晶体结构和抗肿瘤活性

A new binuclear copper (Ⅱ) complex with 1,10-phen and fluoroquinolone ligands, [Cu₂(cfc)₂(phen)₂(pip)](NO₃)₂(CO)₂,was synthesized and its crystal structure was solved.The formula of the complex is C₂₈H₂₄ClCuFN₅O₇, and the crystallography data are as follows, triclinic, space group P1, a=0.80372(6)nm, b=0.94712 (7)nm, c=1.67826(13)nm, α=88.5650(10)°, β=80.9920(10)°, γ=70.2780(10)°, V=1.18722(6)nm³, Z=2, D=1.848g· cm^-3, F(000)=676. R₁=0.0627 and wR₂=0.1684 (I>2σ(I)). The copper atom is five- coordinate with square-based pyramidal geometry and involves two nitrogen atoms from phen, two oxygen atoms from cfc and one nitrogen atom from pip anion. The stacking effect between cfc and phen ligands from two neighboring molecules was observed. FT-IR spectrum of the complex was also discussed. Both ligand and complex were assayed against gram-positive and gram-negative bacteria by doubling dilutions method； the complex shows the same mini-mal inhibitory concentration (MIC) as the corresponding ligand against S. Aureus, E. Coli and M. Lutens bac-teria. The inhibitory effect of the ligand and complex on leukemia HL-60 cell line and liver cancer BEL-7402 cell line have been measured by using MTT (Methyl-Thiazol- Tetrozolium) and SRB (Sulphurhodamin B) assay meth-ods, respectively. The results indicated that the complex has strong inhibitory effect on HL-60 and BEL-7402 cell line. CCDC: 203964.     

9-羟基-芴-9-羧酸双核铜配合物[Cu(C14H8O3)(C9H7N)(C2H5OH)]2的合成、晶体结构及热稳定性研究

A novel binuclear copper complex of [Cu(C₁₄H₈O₃)(C₉H₇N)(C₂H₅OH)]₂ was synthesized and characterized by elemental analysis, IR, thermal analysis and X-ray single crystal diffraction. The title complex crystallizes in monoclinic system, space group P2₁/c with a=1.381 7(3) nm, b=1.184 3(2) nm, c=1.332 5(3) nm, β=104.77(3)°. Each copper(II) atom is five-coordinated by three oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, one quinoline nitrogen atom and one ethanol oxygen atom, forming a distorted square-pyramidal coordination geometry. Two copper(II) atoms are linked by two 9-hydroxy-fluorene-9-carboxylate ligands into a dimmer structure with the Cu…Cu separation being 0.298 39(8) nm. The dinuclear motifs are further linked into a two-dimensional supramolecular layer via hydrogen bonds interactions. CCDC: 272850.     

二聚体配合物[(n-Bu)2Sn(C10H8N2O3)(C2H5OH)]2的合成和晶体结构

The novel seven-coordinate complex [(n-Bu)₂Sn(C₁₀H₈N₂O₃)(C₂H₅OH)]₂ (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionic acid benzoyl hydrazone) was synthesized by the reaction of (n-Bu)₂SnO with 2-oxo-propionic acid benzoyl hydrazone in 1∶1 molar ratio in benzene-ethanol (V/V, 3/1), and its structure was characterized by X-ray single crystal diffraction. The crystal belongs to a tetragonal system with space group I4₁/a, a=2.4890(2)nm, b=2.4890(2)nm, c=1.5170(3)nm, V=9.398(2)nm³, Z=8, F(000)=3968, D_c=1.366g·cm^-3, and the structure was refined to final R₁=0.0530, wR₂=0.0971. The structure of the title complex is described as a dimer through weak interactions of Sn…O bonding and hydrogen bond. The tin atoms rendered sev-en-coordination in a distorted pentagonal bipyramid geometry structure, four oxygen atoms [O1, O2, O2^#1 and O4] and one nitrogen atom N2 formed the equatorial plane and C11-Sn1-C15 is the axis. CCDC: 212696.     

含硫镍金属镍配合物[Ni(C13H7Br2NOS)2(DMF)]·(C3H7O)的合成与晶体结构

The complex, Ni[(C₁₃H₇Br₂NOS)₂(DMF)]·(C₃H₇O) (DMF=N,N′-dimethylformamide), was synthesized and characterized by the element analysis, IR and X-ray diffraction single crystal structure determination. The title complex crystallizes in monoclinic system, space group P2₁/n, with a=8.297 6(15) nm, b=12.866(2) nm, c=31.889(3) nm, β=95.024(2)°, and V=3 391.3(9) nm³, Z=4, R=0.075 2, wR=0.176 8. The nickel iron is six-coordinated by three O atoms, two N atoms, one S from the Schiff base and one O atom from DMF ligand, forming a octahedron coordination geometry. Schiff bases are bridged by the two S atoms. The molecules in the crystal are linked through intermolecular Br…Br, C-H…O, S…Br interactions. Its electrochemical property is reported. CCDC: 675768.     

牛磺酸合铜螯合物的合成及晶体结构

The new chelate complex formulated [Cu(NC₂H₆SO₃)(phen)(CH₃CO₂)]·2H₂O (phen is o-phenanthroline) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to triclinic system with space group and unite cell parameters： a=7.298(1)?， b=11.573(2)?， c=11.942(3)?;α=69.77(1)°， β=80.05(1)°， γ=76.39(1)°， V=915.2(3)?³， Z=2， F(000)=478. D_c=1.680g·cm^-3， μ=1.354mm^-1， S=1.045. In the crystal structure Cu(Ⅱ) ion is five-coordinated to form a distorted tragonal cone. CCDC： 193112.     

2D氢键网状Mg(Ⅱ)配合物的合成和晶体结构

The title complex [Mg(H₂O)₆]·(L)·(H₂O) [L=2-formyl-benzenesulfonate-hydrazine] was synthesized by the reaction of magnesium chloride hexahydrate with 2-formyl-benzenesulfonic acid sodium-hydrazine in the CH₃CH₂OH/H₂O. It was characterized by elemental analysis, IR and X-ray single crystal structure analysis. The crystal of the title complex [Mg(H₂O)₆]·(C₁₄H₁₂N₂O₇S₂)·(H₂O) belongs to triclinic, space group P1 with a=0.781 09(12) nm, b=0.781 27(13) nm, c=0.995 68(19) nm, α=102.054(2)°, β=92.331 0(10)°, γ=105.500(2)°, V=0.569 59(17) nm³, Z=1, D_c=1.559 Mg·m^-3, μ=0.334 mm^-1, F(000)=280, and final R₁=0.033 9, wR₂=0.091 6. The complex comprises a six-coordinated magnesium(Ⅱ) center, with a O₆ distorted octahedron coordination environment. The molecules are connected by hydrogen bonds to form two dimensional network structures. CCDC: 716601.     

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.     

水杨醛缩乙醇胺双氧钒席夫碱配合物的合成、晶体结构及热分解研究(英)

A new complex bis[(N-salicylidene-N′-aminoethanol)dioxovandium(Ⅴ)], [V(Ⅴ)O₂(SALAE)]₂, was synthesized by the reaction of salicylaldehyde and aminoethanol with vanadyl sulfate. It was characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The crystal of the title complex (C₁₈H₂₀N₂O₈V₂, M_r = 494.24) belongs to monoclinic, space group P2₁/c with the following crystallographic parameters: a= 1.7966(6) nm, b= 0.7587(3) nm, c= 2.1539(7) nm, β = 92.551 (6) °, V= 2.9329 (17) nm³, Z= 6, D_c= 1.679 g·cm^-3, μ(MoKα) = 1.006 mm^-1, F(000) =1512, and final R₁ = 0.0563, wR₂= 0.1243 for observed reflections 2861(I> 2σ(I)). The complex is a bis(μ-oxo)-bridged V(Ⅴ) schiff base dimer formed by two dioxovandium units, V(Ⅴ) is six-coordinated and forms a distorted octahedral structure. The thermal decomposition for the complex was studied by TG-DTG curves and the apparent activation energy was obtained by the Kissinger formula. CCDC: 211147.     

[Na(DB18C6)(CH3CN)]2Mo6O19的合成、晶体结构及谱学表征

A novel super-molecular complex, [Na(DB18C6)(CH₃CN)]₂Mo₆O₁₉, was obtained by solvothermal reaction and characterized by elementary analysis, IR, ¹H NMR, gumbc spectrum and X-Ray diffraction experiment. The compound crystallizes in monoclinic space group P2₁/n with a=1.187 1(3) nm, b=2.096 3(6) nm, c=1.415 8(4) nm, β=110.854(5)° and Z=4. The complex contains four basic units: Na⁺, CH₃CN, DB₁₈C₆和Mo₆O₁₉^2-. Sodium ions located in the cavity of dibenzo-18-crown-6 with 6 Na-O bonds and the crown ether-sodium ion complex is supported on the terminal oxygen atoms of the typical Lindqvist isopolyanion Mo₆O₁₉^2- via the coordinative interactions. Mo₆O₁₉^2- located between two DB₁₈C₆ and led to the formation of the “hamburger” structure. The crystal is stabilized by van der waals force and interaction of π-π system. CCDC: 272936.     

配合物Cu(C14H10N2O2)(C5H5N)的合成和晶体结构

The novel copper(Ⅱ) complex with salicylaldehyde benzoylhydrazone and pyridine ligands， Cu(C₁₄H₁₀N₂O₂)(C₅H₅N)， has been synthesized and characterized by elemental analysis， IR and thermal analysis. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group P2₁/c. The cell parameters are： a=1.6362(9)nm， b=1.7140(9)nm， c=1.2255(7)nm， β=105.168(9)°， V=3.317(3)nm³， Z=8， D_c=1.525g·cm^-3， μ(MoKα)=1.334mm^-1， F(000)=1560. The structure was refined to final R₁=0.0376， wR₂=0.0909. The copper(Ⅱ) ion lies in a dis-torted 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. CCDC： 193111.