水杨醛缩乙醇胺及8-羟基喹啉氧钒三元配合物的合成、晶体结构及热分解研究(英)

A new oxovanadium(Ⅴ) ternary complex, VO(L)(hq) [H₂L: N-salicylidene-N′-aminoethanol; hq: 8-hydroxy quinoline], was synthesized by the reaction of salicyaldehyde, aminoethanol and 8-hydroxy quinoline with vanadyl sulfate. It was characterized by elemental analysis, IR and X-ray diffraction analysis. The crystal of the title complex (C₁₈H₁₅N₂O₄V, M_r=374.26) belongs to monoclinic, space group P2₁/n with the following crystallographic parameters: a=1.5435(5) nm, b=0.662 0(2) nm, c=1.648 9(6) nm, β=105.043(7)°, V=1.627 3(10) nm³, Z=4, D_c=1.528 g·cm^-3, μ(MoKα)=0.636 mm^-1, F(000)=768, and final R₁=0.056 8, wR₂=0.106 7 for observed reflections 957 (I>2σ(I)). The complex is six-coordinate in distorted octahedral geometry. The thermal decomposition for the complex was studied by TG-DTG curves and the apparent activation energy was obtained by the Kissinger formula. CCDC: 218497.     

钴配合物的合成、晶体结构与抗微生物活性

The title complex [Co(pht)₂(bipy)](Hpht: 5,5-diphenylhydantoin, i.e. phenytoin;bipy: 2,2-dipyridine) was synthesized by hydrothermal methods and characterized by elemental analysis, IR and X-ray single-crystal structure determination. The compound crystallizes in the monoclinic system, space group C2/c with a=2.697 7(3) nm, b=0.868 40(10) nm, c=1.622 8(2) nm, β=119.66(2)°, V=3.303 6(6) nm³, D_c=1.443 mg·m^-3, Z=4, F(000)=1 484, μ=0.572 mm^-1, R=0.039 5, wR=0.082 7[I>2σ(I)], GOF=1.045. The complex was valued for its antimicrobial activity by diffu-sion test in vitro. It was found to be active against the three test bacterial organisms. CCDC: 669594.     

二苄基锡双(吗啉荒酸酯)的合成、表征及晶体结构

Dibenzyltin bis(dithiomorpholinocarbamate) was synthesized by the reaction of dibenzyltin dichloride with dithiomorpholinocarbamate. The compound was characterized by elemental analysis, IR, ¹H NMR and MS. and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to orthorhombic with space group Pca2₁, a=1.8327(3)nm, b= 0.65678(12)nm, c=2.2583(4)nm, Z=4, V=2.718 (9)nm³, D_x=1.528g·cm^-3,μ=1.271mm^-1, F(000)=1272, R₁=0.0434, wR₂=0.1152. In the crystals, the structures consist of discrete molecules containing six-coordinate tin atoms in a distorted octahedron configuration.     

配合物[Zn(tren)(H-SSA)]的合成、晶体结构及表征

A new mixed complex [Zn(tren) (H-SSA)] was synthesized based on the reaction of ZnO,5-sulfosalicylic acid and tren in water-methanol mixed solvents where tren was tris(2-aminoethyl)amine for the first time. The structure of the mixed complex was characterized by elemental analysis, IR, ¹H NMR and thermal analysis. The crystal structure of the complex was also determined by X-ray single crystal diffraction. Its crystal belongs to trigonal system with space group P3₁, a=1.109 67(18) nm, b=1.109 67(18) nm, c=1.236 8(4) nm, V=1.318 9(5) nm³; D_c=1.616 g·cm^-3; Z=3; F(000)=666; μ=1.553 mm^-1. CCDC: 253908.     

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.     

阶梯状配位聚合物[Cu(μ3-I)INH]n的合成、晶体结构及其热稳定性研究

The complex [Cu(μ₃-I)INH]_n has been synthesized in DMF solution with INH, CuI, where INH=isoniazid. The crystal structure of the complex has been determined by X-ray diffraction single crystal structure analysis. The crystal belong to monoclinic system, space group P2₁/c. The cell parameters are: a=1.009 48(10) nm, b=0.467 51(5) nm, c=1.992 62(19) nm, β=101.413 0(10)°, and V= 0.921 81(16) nm³, Z=4, μ(Mo Kα)=5.674 mm^-1, F(000)=616.0, R₁=0.031 6, wR₂=0.082 5 [I>2σ(I)]. The copper(Ⅰ) atom locates in a distorted coordination tetrahedron. The copper(Ⅰ) atoms bridged by μ₃-I to form a band stair-like chain, and INH occupying the remaining coordination site of the approximately tetrahedral. The stair-like chains extend along b axis. The results of TG analysis show the title complex was stable under 200℃. CCDC: 705346.     

钾的N-酰化牛磺酸配合物的合成、表征及其晶体结构

The title complex(K(C₉H₁₃NO₅S₂)(H2O)) was synthesized by the reaction of p-tolysulfonyl chloride, taurine and potassium hydrate in water-methanol-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 336.44. The crystal structure of the title complex belongs to orthorhombic space group Pbca and cell parameters: a=0.853 31(12) nm, b=0.820 42(12) nm, c=3.989 4(6) nm. V=2.792 8(7) nm³, Z=8, D_c=1.600 g·cm^-3, μ=0.699 mm^-1, F(000)=1 400. The compound is an one-dimension chain complex of infinite length which are connected with hydrogen bond and bridging coordination water. The difference and same of the complexes were discussed. CCDC: 244938.     

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.     

一个新的钴磷酸盐配合物Co(μ3-O3P)·H2O的合成与晶体结构

A new layered cobalt phosphate complex, Co( μ₃-O₃P)·H₂O, was prepared by the hydrothermal reaction. The crystal structure of the complex was determined by single-crystal X-ray diffraction. The results indicate that it contains two different infinite PO₃chains linked by CoO₆ octahedra with infinite 1-D tunnels. It crystallizes in the orthorhombic space group Pbcm with a=0.790 12(16) nm, b=0.900 25(18) nm, c=1.016 1(2) nm, β=90°, V=1.245 3nm³, Z=4. Refinement gave R₁=0.068 5, wR₂=0.175 1 for 2 133 unique observed reflections (I>2σ(I)). The title complex was also characterized by IR, TG-DTA and chemical analysis. CSD: 413934.     

一维双核锌配合物[Zn2(SHSH)2(2-Me-py)2]的合成、晶体结构及理论研究

The crystal of one-dimensional binuclear zinc complex [Zn₂(SHSH)₂(2-Me-py)₂] was obtained in DMF and 2-methylpyridine, where SHSH is salicylaldehyde salicylhydrazone. It has been characterized by IR, UV, element analysis and X-ray diffraction analysis. The crystallographic data were as follows: monoclinic system, space group P2₁/c, a=1.144 49 nm, b=1.206 69 nm, c=1.379 39 nm, β=97.039°, Z=2, V=1.890 6 nm³, M_r=825.47, D_c=1.450 g·cm^-3, μ=1.324 mm-1, F(000)=848 and the final R=0.033 6 and wR=0.094 7 for 3 752 observed reflections with I≥2σ(I). The theoretical investigation of title complex as a structure unit was carried out at B3LYP/6-31G and HF/6-31G levels with Guassian 03W program, and the atomic charges, natural bond orbital analysis and bond energies were also discussed. CCDC: 260920.     

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.     

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.     

[Cu(PTA)(Phen)2](p-MBA)(H6O)配合物的合成、晶体结构及电化学分析

The crystal structure of the title complex with the stoichiometric formula [Cu(PTA)(Phen)₂](p-MBA)(H₆O) (Phen=1,10-phenanthroline, PTA=terephthalic acid, p-MBA=p-toluic acid) has been determined by single-crystal X-ray diffraction. The crystal (C₄₈H₄₀CuN₄O₁₀, M_r=896.38) belongs to the monoclinic space group C2/c, with the following crystallographic parameters: a=1.778 6(3) nm, b=1.912 5(3) nm, c=1.389 9(2) nm, β=114.686(2)°, V=4.295 7(12) nm³, D_c=1.386 g·cm^-3, Z=4, μ(Mo Kα)=0.574 mm^-1, F(000)=1 860, final GooF=1.019, R=0.054 0, wR=0.148 3 for 2 644 observed reflections (I>2σ(I)). The crystal structure shows that the copper(Ⅱ) ion is coordinated with two oxygen atoms from one terephthalic acid molecule and four nitrogen atoms from two 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 298809.     

一种新方法合成荧光β-二酮铜(Ⅰ)配合物(英)

At room temperature, the reducing reaction between the bis(diphenylphosphino)butane (dppb) ligand and the compound [Cu(tfac)₂] (tfac=2-thenoyltrifluoroacetone) gave luminescent copper(Ⅰ) complex [Cu(dppb)(tfac)]₂. They have been characterized by physicochemical and spectroscopic methods. Crystal structure of the title complex shows that 2-thenoyltrifluoroacetone behaves as chelating ligand and dppb coordinates as bridging bidentate ligand to Cu(Ⅰ) atoms in the newly prepared copper(Ⅰ) complex. The crystal is monoclinic, space group P2₁/n, with cell parameters a= 1.031 0(2) nm, b= 1.8730(4) nm, c= 1.7630(4) nm, β = 95.10(3)°, Z = 4, V= 3.391 0(12) nm³, R= 0.060 3, wR= 0.1434. CCDC: 228393.     

锌与邻菲咯啉和α-萘乙酸配合物的合成、结构和抗菌活性

The complex with the molecular formula of Zn(Phen)(NAA)₂ was synthesized by the reaction of ZnSO₄, naphthylacetic acid and phenanthroline in ethanol-water solution at about pH≈7. It was characterized by elemental analysis, IR spectrum and X-ray single crystal diffraction. The antibacterial activity on E. Coli, S. Aureus and B. Subtilis were also been studied. The crystal of the complex belongs to triclinic system with space group P1, a=1.300 2 nm, b=1.306 4 nm, c=1.714 4 nm, α=89.41°, β=77.06°, γ=86.70°, V=2.833 5(2) nm³, Z=4, D_c=1.444 g·cm^-3, M_r=615.96, μ(Mo Kα)=0.912 mm^-1, the final R=0.039 8 and wR=0.103 4 [I>2σ(I)], F(000)=1 272. An asymmetry unit is composed of two independent molecules of Zn(Phen)(NAA)₂ with different bond length and bond angles. There exist two kinds of face to face π-π stacking interactions . The complex has a good effect against E. Coli. CCDC: 619222.     

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.     

具有S…S、S…Cl作用的一维链状有机锡化合物氯代二苄基锡哌啶荒酸酯的合成、表征及晶体结构

The chlorodibenzyltin dithiopiperidylcarbamate was synthesized by the reaction of dibenzyltin dichloride with dithiopiperidylcarbamate and was characterized by elemental analysis， IR and ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystallographic data are as follows： monoclinic， space group P2₁， a=0.63464(13)nm， b=1.9110(4)nm， c=0.87367(17)nm， β=97.67(3)°， Z=2， V=1.0501(4)nm³，D_c=1.571g·cm^-3， μ=1.546mm^-1， F(000)=500， R=0.0209， wR=0.0381 [I≥ 2σ(I)]. The str- uctures consist of discrete molecules containing five-coordinate tin atoms in a seriously distorted trigonal bipyramidal configuration. The molecules are packed in the unit cell in one-dimensional chain complex through a weak inter-action between the chlorine atom， the sulfur atom and one of the other sulfurs of an adjacent molecule. CCDC： 180034.     

N-苯基亚氨基二乙酸镍二维网状配合物的合成及结构表征(英)

A new nickel(Ⅱ) coordination compound [Ni(L^2-)(2,2′-bipy)(H₂O)]·2H₂O (H₂L=phenyliminodiacetic acid) was obtained by self-assembly of phenyliminodiacetic acid, 2,2′-bipy, and NiCl₂·6H₂O in the mixed solvent of water and ethanol (V∶V=1∶1). The complex was characterized by elemental analysis, IR spectra, and X-ray crystallography analysis. The crystal is monoclinic, space group P2₁ /c with a=0.867 4(2) nm, b=0.907 3(1) nm, c=2.643 5(5) nm, β=91.01(1)°, V=2.080 2(4) nm³, Z=4, F(000)=992, D_c=1.520 Mg·m^-3, R₁=0.027 0 and wR₂=0.067 5. In the complex, nickel (Ⅱ) atom is coordinated with a distorted octahedral geometry and extensive hydrogen bonds link the complexes into a 2D network structure. CCDC: 244926.     

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.     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to monoclinic system with space group P2₁/c, a=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.