Synthesis and Crystal Structure of a New Three-dimensional Supramolecule of Copper(Ⅱ) Schiff Base Complex

A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu（naphdien）]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490（15）, b = 7.0847（16）, c = 30.845（3）A, β= 95.33（3）°, V = 1599.0（5）A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F（000） = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones （I 〉2σ（I））. In the crystal structure, mononuclear units [Cu（naphdien）]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.

Synthesis and Crystal Structure of a New 2D O-bridged Copper(Ⅱ) Coordination Polymer Constructed from Sulfonate-derived Schiff Base

A new chain-like coordination polymer, namely, [CuL]n （1, Na2L = 2-[（2-hydroxy- benzylidene）-amino]-benzenesulfonic acid sodium salt）, has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy and elemental analysis. Complex 1 crystallizes in monoclinic system, space group P21/c with a = 9.2296（16）, b = 10.4754（18）, c = 12.200（2） A, β = 102.392（2）°, V = 1152.0（3）A3, CI3H9CuNOaN, Mr = 338.83, Dc = 1.953 g/cm3, Z = 4, F（000） = 684, p = 2.089 mm-1, the final R = 0.0376 and wR = 0.0956. X-ray diffraction analyses indicate that 1 displays a square-pyramidal metal center with NO4 donor sets. The sulfonate-derived Schiff base serves as a common N,O,O＇-tridentate and a unique O-bridged ligand connecting the metals. Dinuclear copper complexes serve as secondary building blocks （SBUs） to construct an unusual 2D coordination network. In the crystal, the components form a stable 3D supramolecular architecture by C-H...O interactions and to-stacking

Synthesis and Crystal Structure of a Novel Dinuclear Copper(Ⅱ) Complex Containing Benzimidazole Schiff Base Ligand

A novel dinuclear copper（Ⅱ） complex [CuL（NO3）]2·2MeOH was obtained by the coordination reaction of Cu（NO3）2·3H2O with ligand HL （HL=N-（methyl-2-benzimidazol- methylidene）-2-hydroxyaniline）. The single-crystal X-ray analysis has revealed that the complex crystallizes in triclinic, space group P with a=9.535（3）, b=10.009（3）, c=10.666（4） , α=104.303（4）, β=100.105（4）, γ=115.917（4）o, V=839.0（5） 3, C16H16CuN4O5, Mr=407.87, Z=2, Dc=1.614 g/cm3, F（000）=418, μ=1.338 mm-1, R=0.0543 and wR=0.0980. The basic dinuclear copper（Ⅱ） complex units [CuL（NO3）]2 are formed by NO3- as co-bridging ligands and L as NNO tridentate chelate coordinating to the copper ions. The ladder-like one-dimensional chain motifs are formed by O…H-O and O…H-N hydrogen bonds from methanol molecules connecting the dinuclear copper（Ⅱ） units.

Antifungal Evaluation of Copper(Ⅱ) Complex from a Schiff Base Derivative of Pyrazine on Schizosaccharomyces pombe

A new copper(Ⅱ) complex of CuLCl_2, where L = N^1-(1-pyrazin-2-yl-ethylidene)-ethane-1,2-diamine, a tridentate Schiff base derived from 2-acetylpyrazine has been prepared. The complex has been characterized by FT-IR, elemental analysis and single-crystal X-ray diffraction studies. Structural studies reveal that CuLCl_2 is a mononuclear copper(Ⅱ) complex with distorted square pyramidal geometry. Antifungal activity of CuLCl_2 was investigated by use of microcalorimetric measurement system and evaluated against S. pombe. It has high antifungal activity with IC_(50) = 213 μg/mL.

Synthesis and Characterization of Dipeptide Schiff Base Complexes of Copper(Ⅱ), Zinc(Ⅱ), Nickel(Ⅱ) and Cobalt(Ⅱ)

A new Schiff base (LK) obtained from 2, 4, -dihydroxybenzaldehyde and glycly-DL- phenylalanine reacted with Cu(II), Zn(II), Ni(II) and Co(II) to yield new complexes. The complexes were characterized by elemental analyses, molar conductance, 1H NMR DTA, TG, IR and UV spectroscopy. In these complexes the ligand is coordinated to the metal through its phenolic oxygen, carboxyl oxygen, imino nitrogen and amide nitrogen. All complexes are non-electrolytes and four coordinated with 1:1(metal; ligand) stoichiometry. The probable structure of the complexes is suggested

Syntheses and Crystal Structures of Two Copper(II) Complexes Derived from Bidentate Schiff Bases

Two new Cu（Ⅱ） complexes have been synthesized with two different bidentate N2O2 donor Schiffbase ligands HL1 （2-（（E）-（4-chlorophenylimino）methyl）-6-bromo-4-chlorophenol） and HL2 （2-（（E）-（2-chlorophenylimino）methyl）-6-bromo-4-chlorophenol）, respectively. Both complexes 1 and 2 have been characterized by elemental analysis and single-crystal X-ray diffraction studies. Structural studies reveal that in both complexes the metal centers are four-coordinated with N202 donor set of Schiff base ligands. Complex 1 belongs to the tetragonal system, space group P4（3）2（1）2 with a = 10.2379（2）, b = 10.2379（2）, c = 24.9623（90） A, V = 2616.41（12） A^3, Z = 4, Dc = 1.908 g/cm^3,μ（MoKa） = 4.3327 mm^-1, F（000） = 1468, S = 0.999, the final R = 0.0345 and wR = 0.0835 for 3506 unique reflections （Rint= 0.0428） with 3249 observed ones （I 〉 2σ（I））. Complex 2 is of monoclinic system, space group P21/c with a = 11.064（3）, b = 9.437（2）, c = 13.277（4） A, fl = 108.997（3）°, V = 1310.8（6） A^3, Z = 2, Dc= 1.904 g/cm^3,μ（MoKa） = 4.319 mm^-1, F（000） = 734, S = 0.997, the final R = 0.0282 and wR = 0.0619 for 3491 unique reflections （Rint = 0.0428） with 2777 observed ones （I 〉 20（I））. The units of the complex are linked via weak interactions, such as C-H…Br hydrogen bonds together with Cl…C1 and Cu…Cl interactions, leading to the formation of one-dimensional chain and two-dimensional network and stabilizing the crystal structure.

基于Schiff Base配体及吡啶环的铜(Ⅱ)、镍(Ⅱ)配合物构筑、表征与热稳定性(英文)

用缓慢挥发法和水热法分别合成了镍配合物NiLPy(L=5-溴-2-羟基苯基苯基酮-4-甲氧基苯甲酰腙,Py=吡啶)(1)及铜配合物Cu(babh)2(Py)(Hbabh=查尔酮苯甲酰腙,Py=吡啶)(2),并用元素分析、红外、热重及X-射线单晶衍射对其进行了表征。晶体结构表明:1属三斜晶系,P1空间群;2属单斜晶系,Pc空间群。化合物1和2分别通过分子间弱的C-H…π与C-H…N作用堆积形成二维片状超分子层。热重分析表明配合物1和2分别处于225和170℃以下温度时很稳定。

Synthesis and Crystal Structure of a Novel Binuclear Cu(Ⅱ) Complex with Tetradentate Schiff-base Ligand

A novel binuclear complex （[Cu^2（μ2-shed）（hshed）].（CIO4）,H2O, h2shed = N-salicylidene-N＇-（2-hydroxyethyl）ethylenediamine） has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 12.511（10）, b = 15.750（12）, c = 14.281 （12） A, β = 100.564（14）°, C22H31CIN4O9Cu2, Mr = 658.04, V = 2766（4） A^3, Z = 4, Dc = 1.580 g/cm^3,μ（MoKα = 1.689 mm^-1, F（000） = 1352, the final R = 0.0528 and wR = 0.1433 for 4880 independent reflections with Rint = 0.0577. The complex is a binuclear copper compound, and two Cu（Ⅱ） ions in the binuclear cation are in different coordination environments. The Cu（1） ion adopts a distorted square pyramidal geometry （x = 0.22） with four donor atoms （N2O2） of the ligand in the basal plane, and one hydroxyl oxygen atom with protonated form occupying the apical position. The Cu（2） ion assumes the geometry of a distorted square plane with four donor atoms （N2O2） of the ligand. The Cu...Cu separation is 3.103 A,. In addition, N-H…O and C-H…O intermolecular hydrogen bonding interactions link these binuclear cations into a quasi one-dimensional chain along the a axis.

Two 3-D Neutral Zn(Ⅱ)-MOFs Generated from the Asymmetric Schiff-base Ligand

Two new Zn（Ⅱ）-MOFs were synthesized based on an asymmetric Schiff-base ligand LH, which is obtained by the condensation of 5-formyl-8-hydroxyquinoline and 3-pyridinecar- boxylic acid hydrazide. In different mixed solvents, we get two new isomorphism compounds, [Zn（L）2]＇CaHsO2-2MeOH （1） and [Zn（L）2]＇CH2CIz＇2MeOH （2）. Compounds 1 and 2 have been characterized by single-crystal X-ray diffraction, elemental analysis and IR. Compound 1 crystallizes in monoclinic, space group P2/c, with a - 13.856（4）, b = 14.156（4）, c = 9.620（3）А, β = 110.167（5）°, V = 1771.3（9） /k3, Dc = 1.500 g/cm3, C3sH3sNsOsZn, Mr = 800.13, F（000） = 832, p（MoKa） = 0.761 mm-1, Z = 2, the final R = 0.0596 and wR = 0.1221 for 2112 observed reflections （I 〉 2σ（0）. Compound 2 belongs to monoclinic, space group P21/c, with a = 13.575（3）, b = 14.130（3）, c = 9.485（2） A, β = 107.908（3）°, V= 1731.2（6） A3, Dc = 1.529 g/cm3, CasH32C12NsO6Zn, Mr = 796.96, F（000） = 820, g（MoKa） = 0.926 mm-1, Z = 2, the final R -- 0.0527 and wR = 0.1395 for 2501 observed reflections （I 〉 2σ-（/））. The Zn（II） centers in both 1 and 2 display a distorted octahedral coordination geometry. The octahedral Zn（lI） nodes and L linkages build up 2-D nets consisting of parallelogram-like grids in the ab plane. The neighboring nets stack through hydrogen bonds to generate 3-D rhombic channels. In 1, the 1,4-dioxane and MeOH guests alternatively arrange in the channels and effectively take up the free space; while in 2, the CH2CI/guests are arranged in the channels. In addition, the encapsulated MeOH molecules are bonded to the framework by hydrogen bonds.

Novel Isatin-Schiff Base Cu (II) and Ni(II) Complexes. X-ray Crystal Structure of Bis[3-(4-hexylphenylimino)-1H-indol-2(3H)-one]-dichlorocopper(II) Complex

Schiff base ligand （HL） derived from 4-hexylaniline with isatin （1H-indole-2,3-dione） and its complexes with Cu（Ⅱ）, Ni（Ⅱ） were prepared and characterized by analytical, spectroscopic （IR, UV-Vis, Mass） techniques, electrical conductivity, magnetic and thermal measurements. The crystal and molecular structure of [Cu（HL）2Cl2] was determined by a single-crystal X-ray diffraction study. The molecular structure of the title compound has an inversion center on the Cu atom.

Synthesis and Crystal Structure of a Bimetallic Cyanide-bridged Complex Derived from Manganese(Ⅲ) Schiff-base Complex and Pentacyanidonitrosylferrate(Ⅱ) Building Blocks

A new cyanide-bridged bimetallic assembly [Mn（3-meosalpn）（H2O）]2[Fe（CN）5NO]（1） was obtained by the reaction of [Fe（CN）5NO]2-with [Mn（3-meosalpn）]＋,and characterized by elemental analysis,IR and single-crystal X-ray structure analysis.The complex crystallizes in the monoclinic system,space group P21/c with a = 12.992（5）,b = 13.274（6）,c = 14.644（6） ,β = 115.198（4）o,V = 2285.2（16）3,Z = 2,C43H44FeMn2N10O11,Mr = 1042.61,Dc = 1.515 g/cm3,F（000） = 1072,μ = 0.928 mm-1,S = 1.052,the final R = 0.0347 and wR = 0.0957 for 17377 observed reflections（Ⅰ 〉 2σ（Ⅰ））.X-ray single-crystal diffraction analysis reveals that 1 has a trinuclear molecular structure,in which the two [Mn（3-meosalpn）（H2O）]＋ cations are linked by the central [Fe（CN）5NO]2-anion via two trans CN-groups.Furthermore,the two [Mn（3-meo-salpn）（H2O）]＋ cations and [Fe（CN）5NO]2-anion are connected into a one-dimensional zigzag chain through hydrogen bonding interactions.

Synthesis,Crystal Structure and Cytotoxic Activity of a Zinc(Ⅱ) Complex of the Schiff Base Derived from S-benzyldithiocarbazate

A novel zinc（Ⅱ） complex of empirical formula,ZnL2（L=anionic forms of S-benzyl-β-N-（2,4-dichlorobenzylidene） hydrazine carbodithioate）,has been synthesized and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P with a = 9.3168（9）,b = 13.0353（13）,c = 14.7702（15） ,α = 71.2860（10）,= 87.5140（10）,γ = 79.4480（10）o,V = 1670.0（3） 3,Z = 2,Mr = 773.93,Dc = 1.539 g/cm3,μ = 1.334 mm-1,F（000） = 784,the final R = 0.0403 and wR = 0.0800 for 4060 observed reflections with I〉2（I）.In the crystal structure,the zinc（Ⅱ） complex has a distorted tetrahedral geometry in which the zinc ion is coordinated by the nitrogen and sulfur atoms from two Schiff base ligands,respectively.The preliminary bioassay indicates that the Schiff base and its zinc complex exhibit inhibitory activity against the human gastric cancer cell lines（MKN45） and hepatoma cell lines（HepG2）.

A Diphenoxo-bridged Ferromagnetic Copper(Ⅱ) Dimer Based on N-(2-Hydroxybenzyl)salicylaldimine

A new dinuclear copper（Ⅱ） complex, [Cu（L）（py）]2 1 （H2L = N-（2-hydroxybenzyl）- salicylaldimine, py = pyridine）, has been synthesized and characterized by elemental analysis, IR and UV spectra. 1 crystallizes in space group P2 1/n with a = 8.2106, b = 10.715, c = 17.864A, β = 99.365°, V = 1550.7A3, Z = 4, C19H16CuN2O2, Mr = 367.88, Dc = 1.576 g/cm3,μ（MoKα） = 1.422 mm-1, F（000） = 756, the final R = 0.0280 and wR = 0.0746. Complex 1 is a centrosymmetric dimer with two copper（H） centers, two py ligands and two L2- ligands. Each L2- ligand donates its azomethine nitrogen and one of the phenolate groups to one copper（Ⅱ） ion and shares the other phenolate group between the two copper（H） ions, affording a Cu2O2 plane. Each copper（Ⅱ） center has a slightly distorted square pyramidal geometry with a bridging phenolate group at the apex. Magnetic studies suggest the presence of a weak ferromagnetic interaction Via two phenoxo bridges. The magnetic susceptibility data （2-300 K） of complex 1 were analyzed by means of H = -2JS1S2 -DSz. The least-squares fitting of the data to the theoretical equation leads to J = 10.3 cm-1, g = 2.03, D = 0.67 cm-1 and R = ∑（Xobsd -Xcalcd）2/∑Xobsd2= 2.76 × 10^-3.

Coordination and Photoisomerization of Azobenzene-Amino Acid Schiff Base Copper(II) Complexes to Lysozyme

In this study, we exhibited an amino acid (arginine and threonine) derivative Schiff base copper(II) complexes incorporating an azobenzene moiety as a photoresponsive site and conjugated it to egg white lysozyme, a well-known protein, to change ligand conformation under binding to lysozyme. Among several spectroscopic investigations, ESR clearly showed that the nitrogen atom of the amino acid residue of lysozyme was bound to the paramagnetic copper(II) ion of the complex, and UV light irradiation confirmed photoisomerization of the azobenzene moiety of the ligand to cis-form. The binding mode was considered by means of spectroscopic as well as computational methods, whereas complete crystallographic verification was still a preliminary stage.

The Uptake of Copper(II) Ions by Chelating Schiff Base Derived from 4-Aminoantipyrine and 2-Methoxybenzaldehyde

The Schiff base, 4-[(2-methoxybenzylidene)amino]-1,5-dimethyl-2-phenyl-1H-pyrizol-3(2H)-one (SB), was used for the first time to adsorb copper(II) ions in aqueous solution. Various parameters such as initial pH, agitation period and different initial concentration of copper(II) ions which influenced the adsorption capacity were investigated. The equilibrium adsorption data for copper(II) ions were fitted to Langmuir, Freundlich and Dubinin-Radushkevish isotherm models. The maximum monolayer adsorption capacity of SB as obtained from Langmuir isotherm was 5.64 mg/g. Kinetic data correlated well with the pseudo second-order kinetic model indicating that chemical adsorption was the rate limiting step.

Synthesis, Spectroscopic, Structural Characterization, Conductivity and Electrochemical Studies of a Schiff Base Ligand and Its Copper Complexes

Schiff base ligand (L) derived from glyoxal and 4-aminoantipyrine was synthesized. The ligand (L) has been characterized by IR, NMR, electronic spectral studies and electrochemical studies. Cu(II) complexes of a Schiff base ligand (L) from 4-aminoantpyrine and glyoxal having the composition [CuL1]X2 where X = Cl¯?or NO3¯? have been prepared and characterized by elemental analysis, electrical conductivity in non-aqueous solvent, infrared and electronic, as well as cyclic voltammetric studies. L acts as a neutral tetradentate ligand coordinating through both the carbonyl oxygen and azomethine nitrogen. On both the complexes both the anions are not coordinated. A square planar geometry is assigned for complexes. The electrochemical studies of ligand show a typical cyclic voltammogram for an irreversible process. While copper(II) complexes show the typical cyclic voltammograms for quasi reversible process.

Asymmetric Cyclopropanation Catalyzed by Four Stereoisomers of a Copper-(Schiff-base) Complex with Double Chiral Centers

Four stereoisomers of a copper-(Schiff-base) complex with double chiral centers were applied to catalyze the asymmetric cyclopropanation. Two of the stereoisomers were also efficient catalysts affording high enantiomeric excess of up to 91.8%. A mechanism that predicts the observed results accurately was proposed.

Syntheses, Crystal Structures and Antibacterial Activities of Cobalt(Ⅱ) and Manganese(Ⅱ) Complexes with Schiff Base Ligand Derived from Tryptamine

Two new mononuclear complexes, namely [Co（L）2]（1） and [Mn（L）2]（2）（HL = N-（3-methylsalicylidene）tryptamine）, have been synthesized by the reactions of the ligand with cobalt acetate or manganese acetate in anhydrous ethanol. The crystal structures of the complexes were characterized by IR spectrum, elemental analysis, PXRD and single-crystal X-ray diffraction analysis. Complex 1 crystallizes in monoclinic, space group C2/c, with a = 23.146（2）, b = 9.4864（10）, c = 13.9261（15）A, β = 102.898（2）°, V = 2980.6（5） ？3, Z = 4, Dc = 1.367 g/cm3, F（000） = 1284 and μ = 0.616 mm^-1. Complex 2 crystallizes in monoclinic, space group P21/n, with a = 14.807（11）, b = 13.118（10）, c = 16.663（13） A, β = 111.237（14）°, V = 3017（4） A^3, Z = 4, Dc = 1.342 g/cm^3, F（000） = 1276 and μ = 0.477 mm-1. The units of complex 1 are linked by intermolecular N–H…π hydrogen bonds into infinite 1D chains, which are further extended into a 3D supramolecular structure by a series of π···π stacking interactions. The units of complex 2 are linked by intermolecular N–H…π hydrogen bonds and C–H…π hydrogen bonds into an infinite 3D supramolecular structure. Meanwhile, the antibacterial activities of the ligand and its complexes have been tested against four kinds of bacteria. The results show that the three compounds all have excellent antibacterial activities and that 1 and 2 possess stronger inhibiting effects against the bacteria than the Schiff base.

Synthesis, Structure Characterization, Antibacterial Activity and Fluorescence Studies of a Ni(Ⅱ) Compound with Schiff-base Ligand

We synthesized one novel Schiff-base ligand by modifying the aromatic aldehyde： H2L^1（H2L^1 = N,N？-bis（2-oxy-acetate-3-methoxyl）benzylpropylene（1,3-propane）diamine）. [Ni（C（23）H（24）N2O8）]·6H2O]（1） was prepared by the reaction between H2L^1 and NiCl2·6H2O in C2H5 OH. Compound 1 was structurally characterized by elemental analysis, IR, H NMR and single-crystal X-ray diffraction. 1 crystallizes in monoclinic system, space group P21/n with a = 1.3952（4）, b = 1.3746（9）, c = 1.6121（0） nm, β = 112.66（3）°, V = 2.8533（4） nm^3, Z = 4, Mr = 623.25 and Dc = 1.451 g·cm^（-3）. The Ni（Ⅱ） atom is hexa-coordinated to furnish a slightly distorted octahedral geometry. Lattice water molecules are found in 1, and the H-bonding intersections formed novel water clusters. The IR, antibacterial activity and luminescence of 1 are studied.