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1.
The condensation reaction of cobalt(II) and nickel(II) complexes with 1-amino-8-hydroxynaphthalene-2,4-disulfonic acid and aromatic carbonyl compounds (benzoin and 2-hydroxy-1-naphthaldehyde) was carried out. Four new complexes (I–IV) were synthesized. The compounds were identified by elemental analysis, powder X-ray diffraction, thermogravimetry, magnetic susceptibility, IR and diffuse reflection spectroscopy, and EXAFS. The spatial arrangement of the donor centers of the ligands in the coordination units (tetrahedral for I, octahedral for II and III, and square planar for IV) was determined.  相似文献   

2.
The solution state and thermodynamic stability of complexes of the new antituberculosis agent 1,4-bis(amidomethylsulfinyl)butane (L) with iron(III), copper(II), cobalt(II), nickel(II), and manganese(II) in an aqueous solution in the presence and in the absence of the nonionic surfactant Brij 35 were studied by spectrophotometry, pH potentiometry, NMR relaxation technique (T = 25 °C; variable ionic strength), and mathematical simulation. The geometry optimization of all structures was carried out by the molecular mechanics method MM2 in order to obtain data on coordination modes. In addition, the structure of 1,4-bis(amidomethylsulfinyl)butane was refined by the DFT/B3LYP/6-311++G(d,p) quantum chemical method using the IEFPCM model to take into account solvent effects. In an aqueous solution (in the concentration range of 1.3?10–5—1?10–3 mol L–1) and in the presence of Brij 35, 1,4-bis(amidomethylsulfinyl)butane exists as a neutral monomer. The Beer—Lambert—Bouguer law is obeyed in a wide concentration range for compound L in an aqueous solution, as well as in the presence of the surfactant, which can be used for the quantification of compound L. Iron(III), cobalt(II), and nickel(II) were shown to form 1: 1 mononuclear complexes with L; and copper(II) forms, 1: 1 and 2: 2 complexes. The presence of Brij 35 in the Cu2+L system at a micellar concentration promotes the formation of a dinuclear complex.  相似文献   

3.
A new centrosymmetric mononuclear copper(II) complex [Cu(L)2](ClO4)2 (I) and a new centrosymmetric mononuclear nickel(II) complex [Ni(L)2(MeOH)2](ClO4)2 (II), where L is the zwitterionic ligand 2-bromo-4-chloro-6-[(2-methylammonioethylimino)methyl]phenolate, have been prepared from the Schiff base 2-bromo-4-chloro-6-[(2-methylaminoethylimino)methyl]phenol with copper perchlorate and nickel perchlorate, respectively. The complexes were characterized by elemental analysis, infrared spectra, and single-cyrstal X-ray diffraction (CIF files CCDC nos. 1408054 (I) and 1407973 (II)). Complex I crystallizes in the monoclinic space group P21/c with unit cell dimensions a = 7.7736(4), b = 21.608(1), c = 8.5194(4) Å, β = 93.907(2)°, V = 1427.7(1) Å3, Z = 2, R 1 = 0.0546, and wR 2 = 0.1531. Complex II crystallizes in the monoclinic space group P21/c with unit cell dimensions a = 21.324(3), b = 16.821(2), c = 9.425(1) Å, β = 90.114(2)°, V = 3380.5(7) Å3, Z = 4, R 1 = 0.0693, and wR 2 = 0.1627. The Cu atom in I is in square planar coordination, and the Ni atom in II is in octahedral coordination.  相似文献   

4.
The reactions of copper(II) nitrate with 3-oxapentane-1,5-diamine (Oda) were investigated under different molar ratio. In the case of a 1: 1 molar ratio of copper(II) nitrate and Oda, the mononuclear complex [Cu(Oda)(NO3)2] (I) was obtained. In contrast, the treatment of copper(II) nitrate with twice Oda afforded inorganic polymer {[Cu(μ-Oda)(Oda)] · (NO3)2} n (II). The molecular structures of the two new complexes were determined from the elemental analyses, IR spectra and single-crystal X-ray diffraction (CIF files CCDC nos. 828193 (I) and 828018 (II)). Two Cu(II) complexes were both five-coordinated and forming a distorted square-base pyramidal geometry. Two complexes are stabilized by the intermolecular hydrogenbond.  相似文献   

5.
A planar rectangular cluster Ni18 (I) was obtained from N-(2-pyridylmethyl)iminodipropionic acid (II). The crystal structure of complex I was determined by X-ray diffraction. Complex I is built from the octanuclear planar framework (III) of the nickel(II) hydroxo complex (Ni...Ni 2.976–3.092 Å), four nickel chelates with the corresponding acid (IV), which are coplanar with the framework and are on both its sides (Ni...Ni, 2.938–3.188 Å), four hydroxo complexes, and two mixed chloro chelates V), which are not coplanar with the framework (Ni...Ni, 3.141 and 3.181 Å). In the chelate parts of complex I, the organic ligand is hexadentate because of bridging bonds; the coordination polyhedroLn of the metal center is a distorted square bipyramid (4 + 2).  相似文献   

6.
In this research, we prepared a new series of the Cu(II) (1) and Ni(II) (2) metal complexes of a tridentate Schiff base ligand, (E)-2-(5-bromo-2-hydroxybenzylideneamino) phenol (H2L). These complexes were characterized by elemental analysis, FT-IR, UV–Vis, and 1H-NMR spectroscopy. The crystal structures of (1) and (2) were determined by X-ray diffraction studies. The single crystal X-ray diffraction analyses revealed that copper(II) cation is five-coordinated and the coordination polyhedron is a slightly distorted square pyramid. Nickel(II), on the other hand, is four-coordinated, and has a regular, square planar geometry. Further discussed were the electrochemical reduction of these complexes. We also analyzed the nature of the metal–ligand bond in the complexes through NBO and EDA analysis. Besides, vibrational sample magnetometer (VSM) revealed complex (1) was ferromagnetic.  相似文献   

7.
The syntheses of a mononuclear zinc(II) complex [ZnCl(L1)(Amp)] (I) and a mononuclear nickel(II) complex [Ni(L2)(HL2)](BF4) · 0.5H2O (II) (HL1 = 4-methyl-2-[(4-methylpyridin-2-ylimino) methyl]phenol, HL2 = 4-methyl-2-[(pyridin-2-ylmethylimino)methyl]phenol; Amp = 2-amino-4- methylpyridine) were prepared under microwave irradiation. The complexes were characterized by a combination of elemental analyses, and IR and electronic spectra. Their structures were further confirmed by single crystal X-ray crystallography (СIF files CCDC nos 1437737 (I), 1437738 (II)). The Zn atom in the monomeric complex I is in tetrahedral coordination. The Ni atoms in the dimeric complex II are in octahedral coordination. Crystals of the complexes are stabilized by hydrogen bonds. In order to evaluate the biological activity of the complexes, in vitro antibacterial against Staphylococcus aureus, Bacillus subtilis, Escherichia coli, and Pseudomonas aeruginosa was assayed. The complexes have strong activity against Bacillus subtilis.  相似文献   

8.
Chiral Schiff base complexes containing azo-groups, bis(N-R-1-cyclohexylethyl-4-phenyldiazenylsalicydenaminato) nickel(II), copper(II) and zinc(II) complexes, and without azo-groups, bis(N-R-1-cyclohexylethyl-3,5-dichlorosalicydenaminato) nickel(II), copper(II) and zinc(II) complexes, affording a distorted square planar trans-[MN2O2] coordination geometry were prepared. Organic/inorganic hybrid materials in polymethylmethacrylate (PMMA) spincoat films of the complexes (both the azobenzene (AZ) containing type and the latter complexes of the AZ separated type) were assembled for a comparison of polarized UV light induced molecular arrangement caused by the Weigert effect. Investigation of the parameters for the optical anisotropy of the metal complexes as well as AZ suggested that the degree of increasing optical anisotropy of the containing type was higher than that of the separated type based on π-π (of which a characteristic band appeared around 380 nm) and n-π bands of polarized absorption electronic spectra. In the AZ containing type, the rigid nickel(II) or zinc(II) complexes easily increase the optical anisotropy compared to the flexible copper(II) complexes. In the AZ separated type, interestingly, enhancement of some CD bands suggests the role of chiral dopants of some complexes without azo-groups for AZ.  相似文献   

9.
The reaction between coproporphyrin I tetraethyl ester and ruthenium(II) dodecacarbonyl in toluene is investigated. The formation of two different products, complexes 2 and 3 of ruthenium(II) with coproporphyrin I tetraethyl ester, studied by means of mass spectrometry, electronic absorption spectroscopy, NMR, X-ray diffraction, and thermogravimetric analysis, is revealed. Structures are proposed for the products, of which (2) is a monocarbonyl complex of ruthenium(II) porphyrin that exists as a coordination polymer formed owing to intermolecular axial bonding between the oxygen atoms of carboethoxyl groups and ruthenium(II). The structure proposed for second product (3) is in the form of the corresponding monomer of a monocarbonyl complex of ruthenium(II) porphyrin. It is established that polymeric complex 2 transforms into monomeric complex 3 when it is heating in pyridine.  相似文献   

10.
Two new cadmium(II) coordination polymers, {[Cd(L1)(tbta)]·H2O} n (1) and [Cd(L2)(tbta)] n (2) (L1 = 1,4-bis(5,6-dimethylbenzimidazol-1-ylmethyl)benzene, H2tbta = tetrabromoterephthalic acid and L2 = 1,4-bis(2-methylbenzimidazol-1-ylmethyl)benzene) are obtained under hydrothermal conditions and structurally characterized by single crystal X-ray diffraction methods, IR spectroscopy, TGA and elemental analysis. The L1 and L2 ligands differ by subtle variation of substituents at semi-rigid bis(benzimidazole) bakcbones. Complex 1 features a 3D threefold interpenetrating dia array with a 4-connected 66 topology. Complex 2 displays a 2D {44.62} sql/Shubnikov tetragonal plane network. Complexes 1 and 2 possess high thermal stabilities and promising fluorescence behavior in the solid state.  相似文献   

11.
An end-on azido-bridged dinuclear nickel(II) complex [Ni2(L1)21,1-N3)2] · CH3COOH (I) and an end-on azido-bridged polynuclear copper(II) complex [CuL21,1-N3)] n , where L1 is the deprotonated form of 2-[(2-ethylaminoethylimino)methyl]-4-fluorophenol and L2 is the deprotonated form of 2-[(2- dimethylaminoethylimino)methyl]-4-fluorophenol, were prepared and characterized by elemental analysis and FT-IR spectra. Crystal and molecular structures of the complexes were determined by single crystal X-ray diffraction method (CIF files CCDC nos. 942641 (I) and 942642 (II)). Single crystal X-ray structural studies indicate that the Schiff base ligands coordinate to the metal atoms through phenolate oxygen, imine nitrogen, and amine nitrogen. The Ni atoms in the nickel complex are in octahedral coordination, and the Cu atoms in the copper complex are in square pyramidal coordination. Crystals of the complexes are stabilized by hydrogen bonds. The Schiff bases and the complexes showed potent antibacterial activities.  相似文献   

12.
The structural and spectroscopic characterization of coordination compounds of four aromatic amines derived from benzimidazole, 2-aminobenzimidazole (L1), 1-(S-methylcarbodithioate)-2-aminobenzimidazole (L2), 2-(2-aminophenyl)-1H-benzimidazole (L3) and 6,6-dimethyl-5H-benzimidazolyl[1,2-c]quinazoline (L4) are reported. Cobalt(II) [Co(L1)2(CH3COO)2] (1) and nickel(II) [Ni(L1)2(CH3COO)2] (2) acetate coordination compounds of L1 are discussed. The synthesis and the X-ray crystal structure of the new 1-(S-methylcarbodithioate)-2-aminobenzimidazole (L2) is informed, together with its cobalt(II) [Co(L2)2Cl2] (3), [Co(L2)2Br2] (4) and zinc(II) [Co(L2)2Cl2] (5), [Zn(L2)2Br2] (6) coordination compounds. In these compounds the imidazolic nitrogen is coordinated to the metal center, while the ArNH2 and the S-methylcarbodithioate groups do not participate as coordination sites. A co-crystal of L1 and L2 is analyzed. Structural analyses of the coordination compounds of L3 showed that this ligand behaves as a bidentate ligand through the aniline and the imidazole groups forming six membered rings in the cobalt(II) [Co(L3)Cl2] (7) and zinc(II) [Zn(L3)Cl2] (8) compounds, as well as the nickel(II) nitrate [Ni(L3)2(H2O)2](NO3)2 (9). The quinazoline L4 was produced by insertion of one acetone molecule and water elimination in L3, its X-ray crystal diffraction analysis, as well as that of its zinc(II) coordination compound [Zn(L4)2Cl2] (10), are discussed.  相似文献   

13.
Coordination compounds [CoLCl2] (I), [CuLCl(NO3)] (II), CuL(NO3)2 (III), and CuLCl2 (IV) (where L is a chiral pyrazolylquinoline—a derivative of terpenoid (+)-3-carene) were synthesized. X-ray diffraction data showed that crystal structures I and II are built of mononuclear acentric molecules. In the molecule of complex I, the Co2+ ion coordinates two N atoms of bidentate cycle-forming ligand L and two Cl atoms. The coordination polyhedron of Cl2N2 is a distorted tetrahedron. For complex I, μeff = 4.50 μB, which corresponds to a high-spin configuration d 7. In the molecules of II(1), II(2) (which are diastereoisomers of complex II), each Cu2+ ion coordinates two N atoms of bidentate cycle-forming ligand L, the Cl atom, and two O atoms of bidentate cyclic NO 3 ? ion. The ClN2O2 coordination polyhedra are tetragonal pyramids with different degrees of distortion. The structure of complex II consists of supramolecular clusters, i.e., isolated chains incorporating the molecules of II(1) and II(2). The values of μeff for II–IV correspond to the d 9 configuration. The results of EPR and IR study suggest that complex III contains the O4N2 polyhedron, whereas complex IV contains the Cl2N2 polyhedron. Complexes I and IV were found to show a high catalytic activity in ethylene polymerization reaction.  相似文献   

14.
By self-assembly of delocalized organic ligands (L1 and L2) with Cd(SCN)2, ZnI2 and Zn(NCS)2, three luminescent complexes ZnI2(L1)2 (I), [Cd(L1)21,3-SCN)2] n (II) and Zn(NCS)2(L2)2 (III) were obtained (L1 = 2-{5,5-dimethyl-3-[2-(pyridine-4-yl)ethenyl]cyclohex-2-enylidene}propanedinitrile and L2 = 2-{5,5-dimethyl-3-[2-(pyridine-3-yl)ethenyl]cyclohex-2-enylidene}propanedinitrile). The structures of the complexes were determined by single crystal X-ray diffraction analysis (CIF files CCDC nos. 1406116 (I), 1406115 (II), and 1400360 (III)). In complex I, Zn(II) is coordinated by two functional organic ligands and two I ions, to form a I2N2 distorted tetrahedral geometry. In 1D coordination polymer II, the Cd(II) centers show six-coordinated geometries, two organic ligands and four SCN ions involve in coordination with each Cd(II) center. The thiocyanate groups show μ1,3-SCN bridging coordination modes and the adjacent Cd(II) ions are bridged by double μ1,3-SCN ions to form an infinite chain. In complex III, Zn(II) is coordinated by two functional organic ligands and two NCS groups, to form a N4 distorted tetrahedral geometry. Compared with the free ligands, the complexes show superior luminescent property with red-shift and enhancement of fluorescence intensity.  相似文献   

15.
Three coordination polymers based on the new ligand oxamide N,N-bis(4-phthalic acid), namely [Zn(L)0.5-(2,2′-bpy)] n (1), [Ni2(2,2′-bpy)4(µ 2-Ox)]L·3H2O (2) and [Cd(L)(1,10-phen)] (3) [L = oxamide N,N-bis(4-phthalic acid)], (2,2′-bpy = 2,2′-bipyridine), (1,10-phen = 1,10-phenanthroline), have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction: compound 1 is one-dimensional ladder-like coordination polymer, compound 2 exhibits a three-dimensional structure resulting in extensive hydrogen bonds built with the help of lattice water molecules, compound 3 also exhibits a three-dimensional supramolecular structure. All compounds were also characterized by elemental analysis, IR spectra and thermogravimetric analysis; furthermore, the magnetic measurements for 2 reveal antiferromagnetic coupling between the nickel(II) ions.  相似文献   

16.
In the present work, catecholase activity is presented. The complexes were prepared by condensation of the organic ligand pyrazolyl L 1 L 4 and copper(II) ion in situ. The pyrazolyl compounds L 1 L 4 used in this study are: L 1 is (3,5-dimethyl-pyrazol-1-ylmethyl)-(4-methyl-pyridin-2-yl)-pyrazol-1-ylmethyl-amine; L 2 is 1-{4-[(3,5-dimethyl-pyrazol-1-ylmethyl)-pyrazol-1-ylmethyl-amino]-phenyl}-ethanone; L 3 is 1-{4-[(3,5-dimethyl-pyrazol-1-ylmethyl)-[1,2,4]triazol-1-ylmethyl-amino]-phenyl}-ethanone, and L 4 is 2-[(3,5-dimethyl-pyrazol-1-ylmethyl)-[1,2,4]triazol-1-ylmethyl-amino]-6-methyl-pyrimidin-4-ol, and copper ions salts Cu(II) are (Cu(CH3COO)2, CuCl2, Cu(NO3)2 and CuSO4). In order to determine factors influencing the catecholase activity of these complexes, the effect of ligand nature, ligand concentration, nature of solvent and nature of counter anion has been studied. The best activity of catechol oxidation is given by the combination formed by one equivalent of ligand L 2 and one equivalent of Cu(CH3COO)2 in methanol solvent which is equal to 9.09 µmol L?1 min?1. The Michaelis–Menten model is applied for the best combination, to obtain the kinetic parameters, and we proposed the mechanism for oxidation reaction of catecholase.  相似文献   

17.
We report the preparation of bromo-aryl functionalized bis(diphenylphosphino)amine ligands of the type Ph2PNArPPh2 (1, Ar = p-BrC6H4; 2, Ar = p-BrC6H4–C6H4) and their coordination properties. Mono- and dinuclear complexes were formed with Cu(I), Au(I), Pd(II), Pt(II) and tetranuclear cobalt carbonyl clusters were obtained. The crystal structures of [PdCl2(1)] (3), [PdCl2(2)] (4), [(AuCl)(μ-1)] (6), [Co4(CO)5(μ-CO)3(μ-dppa)(μ-1)] (dppa = Ph2PNHPPh2) (8) and [Co4(CO)5(μ-CO)3(μ-dppm)(μ-1)] (dppm = Ph2PCH2PPh2) (9) have been determined by X-ray diffraction. Whereas the diphosphine ligands chelate the metal center in 3 and 4, and in the Pt(II) complex 5 which is analogous to 3, ligand 1 acts as a bridge in 6 where the separation between the two Au(I) centers is 3.0402(5) Å. In the tetranuclear clusters 8 and 9, and in the cluster 10 analogous to 9 with 2 as bridging ligand, two orthogonal Co–Co edges are bridged by a diphosphine ligand and each cobalt center is thus coordinated by one P donor. Complex 3 was shown to react with the Pd(0) complex [Pd(dba)2] (dba = dibenzylideneacetone) to afford a tetranuclear complex resulting from both the insertion of Pd(0) into the ligand C–Br bond and Pd(II)/Pd(0) comproportionation to form a doubly ligand-bridged Pd(I)–Pd(I) core.  相似文献   

18.
Two new Zn(II) and Co(II) compounds obtained by reactions of tetrafluoroborates of these metals with 1,3,5-benzenetricarboxylic (trimesic) acid (H3Btc) and 1,3-bis(pyridyl)propane (Bpp) as an additional ligand were studied by X-ray diffraction. The formation of coordination polymers of various dimensionality, {[Zn4(Bpp)4(HBtc)3((Me)Btc)]{(Me)2HBtc} · 2H2O} n (I), 1D, and {[Co43-OH)2(Btc)2(H2O)8] · 4(H2O)} n (II), 2D (CIF files CCDC no. 1552167 (I), 1552168 (II)) was demonstrated. Since H3Btc is partially methylated during the reaction, in I, this acid is stabilized in three forms: HBtc2–, (Me)Btc2–, and (Me)2HBtc. The tetrahedral Zn(II) coordination polyhedron is formed by the N2O2 set of donor atoms: the O atoms belong to two different carboxylate ligands, HBtc2– and (Me)Btc2–, while the N atoms belong to two Bpp ligands. In II, the Bpp ligand is not incorporated in the complex and H3Btc is coordinated to five metal atoms as a triply deprotonated ligand. Two carboxyl groups are coordinated to Co atoms as bidentate bridging ligands, while the third group is monodentate. The octahedral coordination polyhedra of Co(II) atoms in II are supplemented by terminal water molecules and μ3-bridging OH groups.  相似文献   

19.
The anodic dissolution of tin metal in absolute alcohols yields oxoalkoxides with the general formula Sn6O4(OR)4 (R = Me (1), Et (2), i-Pr (3)) and orthoalkoxides with the general formula Sn(OR)2 (R = n-Bu (4), C2H4OMe (5)). According to X-ray crystallographic data, the molecule of Sn6O4(OEt)4 (2) is an octahedral [Sn6] cluster with alternating oxo and OEt groups on its faces. The mass spectra of 1 and 2 indicate the presence of fragments of the hexanuclear oxoalkoxides.  相似文献   

20.
胡雁鸣  张学全 《高分子科学》2016,34(9):1060-1069
Cobalt and nickel complexes (1a-1d and 2a-2d, respectively) supported by 2-imidate-pyridine ligands were synthesized and used for 1,3-butadiene polymerization. The complexes were characterized by IR and element analysis, and complex 1a was further characterized by single-crystal X-ray diffraction. The solid state structure of complex 1a displayed a distorted tetrahedral geometry. Upon activation with ethylaluminum sesquichloride (EASC), all the complexes showed high activities toward 1,3-butadiene polymerization. The cobalt complexes produced polymers with high cis-1,4 contents and high molecular weights, while the nickel complexes displayed low cis-1,4 selectivity and the resulting polymers had low molecular weights. The catalytic activities of the complexes highly depended on the ligand structure. With the increment of polymerization temperature, the cis-1,4 content and the molecular weight of the resulting polymer decreased.  相似文献   

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