Hydrothermal Synthesis,Crystal Structure and Antimicrobial Activity of a New Ni(Ⅱ) Complex

The title complex [NiL]·H2O(C20H24N2NiO5,L = paeonol-ehylenediamine) was synthesized by the hydrothermal method and characterized by IR,cyclic voltammetry and X-ray single-crystal diffraction.The complex belongs to the monoclinic system,space group P21/c with a=13.4361(13),b=7.3290(10),c=20.981(2),β=109.244°,V=1950.6(4)3,Z=4,F(000)=904,Dc=1.468 g/cm3,μ(MoKα)=1.029 mm-1,the final R=0.0588 and wR=0.1577.The complex exhibits antimicrobial activities(antimicrobial activities against Staphylococcus aureus and Escherichia codi) by agar diffusion measurement.     

Synthesis, Crystal Structure and Antimicrobial Activity of a Novel Ni(Ⅱ) Complex

A new nickel(Ⅱ) complex, C34H38N8NiO4, has been prepared and charac-terized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/c with a = 11.715(5), b = 12.328(5), c =11.113(5) A, β= 92.589(5)°, Z = 2, Dc = 1.411 g/cm3, μ = 0.658 mm-1, the final R = 0.0427 and wR = 0.1099 for 2229 observed reflections with Ⅰ> 2σ(Ⅰ). The complex is a centrosymmetric plane in which nickel(Ⅱ) is coordinated in a regular octahedron to the ligand phenytoin through the nitrogen atoms of ethylenediamine, imine and amine. The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method, and found to be active against the four test bacterial organisms. Preliminary screening for antimicrobial activities showed that the title complex is quite active against standard strains of Salmonella species, Staphylococcus aureus, Bacillus pumilus and Eschierichia coli.     

Synthesis,Crystal Structure and Antitumor Activity of a New Zn(Ⅱ) Complex Based on N-Acetyl-L-phenylalanine and 1,10-Phenanthroline

A new Zn(Ⅱ) complex, [Zn(L)_2(phen)(H_2O)](1, HL = N-acetyl-L-phenylalanine, phen = 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction analysis. The Zn(Ⅱ) complex belongs to monoclinic, space group P21 with a = 12.6749(13), b = 5.5965(6), c = 22.985(2) ?, β = 104.296(2)°, V = 1580.0(3) ?~3, Z = 2, M_r = 676.02, D_c = 1.421 μg·m~(-3), μ = 0.833 mm~(-1), F(000) = 704, and the final R = 0.0460, wR = 0.0899 for 4422 observed reflections with I 2σ(I). The molecules form a 1D chained structure by hydrogen bonds. The antitumor activities of Zn(Ⅱ) complex against human hepatoma SMMC-7721 cells, human lung adenocarcinoma A549 cells and human colon carcinoma WiDr cells have also been investigated.     

Synthesis and Crystal Structure of a New Zn(Ⅱ) Complex Exhibiting Strong Luminescence

The title complex,[Zn(ip)2(H2O)2][ZnCl4]·H2O·2DMF 1(ip=imidazo[4,5-f][1,10] phenanthroline),has been synthesized via the slow evaporation of concentrated reaction solution at room temperature.It was characterized by single-crystal X-ray diffraction.Crystal data for C32H36Cl4N10O5Zn2:white prism,0.17mm×0.15mm×0.10mm,monoclinic,space group P2/c,a=11.928(8),b=9.868(6),c=16.520(11),β=104.879(12)°,V=1879(2)3,Z=2,Mr=913.25,Dc=1.614 g/cm3,F(000)=932,μ=1.616 mm-1,λ(MoKα)=0.71073,GOOF=1.045,R=0.0710 and wR=0.1755 for 3055 observed reflections with Ⅰ2σ(Ⅰ).X-ray diffraction study reveals that the title complex has an interesting 3D architecture via hydrogen bonding interactions and π-π interactions.The IR,TGA,XRD and luminescent properties of complex 1 were also studied.     

Synthesis, Crystal Structure and Antimicrobial Activity of a Novel Ni(II) Complex

A new nickel(II) complex, C34H38N8NiO4, has been prepared and charac- terized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/c with a = 11.715(5), b = 12.328(5), c =11.113(5) , β = 92.589(5)°, Z = 2, Dc = 1.411 g/cm3, μ = 0.658 mm-1, the final R = 0.0427 and wR = 0.1099 for 2229 observed reflections with I > 2σ(I). The complex is a centrosymmetric plane in which nickel(II) is coordinated in a regular octahedron to the ligand phenytoin through the nitrogen atoms of ethylenediamine, imine and amine. The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method, and found to be active against the four test bacterial organisms. Preliminary screening for antimicrobial activities showed that the title complex is quite active against standard strains of Salmonella species, Staphylococcus aureus, Bacillus pumilus and Eschierichia coli.     

Synthesis, Crystal Structure and Magnetic Properties of a New Zn(Ⅱ)-Nitronyl Nitroxide Complex

A new complex [Zn(NIT-1'-MeBzIm)Cl2(H2O)] (NIT-1'-MeBzIm = 2-{2'-[(1'-methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method. Crystal data: monoclinic, space group P21/n, Z = 4, C15H21Cl2N4O3Zn, Mr = 441.63, a = 7.2225(10), b = 30.849(4), c = 8.8758(13) (A), β= 103.904(2)°, V = 1919.6(5) A3, Dc = 1.528 g/cm3, μ(MoKα) = 1.579 mm-1, F(000) = 908, R = 0.0436 and wR = 0.1029 for 2456 observed reflections with Ⅰ> 2σ(Ⅰ). X-ray analysis reveals that the Zn(Ⅱ) ion is four-coordinated with a distorted tetrahedron. There also exist H-bonds, π-π piling interactions and weak intermolecular contacts between the NO groups which form a mutual stagger 3-D network configuration. Magnetic investigation reveals that there exists intermolecular antiferro- and ferromagnetic interactions in the title complex.     

Synthesis and Crystal Structure of a New Mononuclear Copper Complex

<正>A new kind of Cu (II) complex [Cu(tpmb)2Cl2]·CH3OH·H2O (tpmb = 1,3,5-tri(2-pyrimidinyl)sulfanylmethyl-2,4,6-trimethylbenzene) was synthesized, and its structure has been determined by X-ray single-crystal diffraction. It crystallizes in the triclinic, space group P 1 with a = 8.8397(2), b = 13.327(3), c = 13.926(3) A, α = 63.27(3), β = 86.96(3), r = 80.68(3)°, V = 1445.6(5) A3, C49H51Cl2CuN12O2S6, Mr= 1166.82,Z=1, F(000) = 604, Dc = 1.340 g/cm3, μ = 0.735 mm-1, R = 0.0545 and wR = 0.1575 for 4521 observed reflections (I > 2σ(I)). X-ray analysis reveals that the Cu (II) ion is coordinated by two Cl- anions and two nitrogen atoms from different pyrimidine groups, forming a square structure.     

Synthesis,Crystal Structure and Antimicrobial Activity of a Novel Ni（Ⅱ） Complex

A new nickel（Ⅱ） complex, C34H38N8NiO4, has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/c with a = 11.715（5）, b = 12.328（5）, c =11.113（5）A, β= 92.589（5）°, Z = 2, Dc = 1.411 g/cm^3,μ = 0.658 mml, the final R = 0.0427 and wR = 0.1099 for 2229 observed reflections with I 〉 2σ（I）. The complex is a centrosymmetric plane in which nickel（Ⅱ） is coordinated in a regular octahedron to the ligand phenytoin through the nitrogen atoms of ethylenediamine, imine and amine. The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method, and found to be active against the four test bacterial organisms. Preliminary screening for antimicrobial activities showed that the title complex is quite active against standard strains of Salmonella species, Staphylococcus aureus, Bacillus pumilus and Eschierichia coli.     

Synthesis and Crystal Structure of a New Copper(Ⅱ) Complex with 4-Cyanobenzoic Acid

A new Cu(Ⅱ) complex [Cu(4-cba)(l,10-phen)(H2O)2](NO3) (4-Hcba = 4-cyanobenzoic acid) has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data: C20H16CuN4O7, Mr= 487.91, triclinic, space group P1, a = 7.8420(2), b = 9.1070(2), c = 15.1140(6) A,α=76.889(9), β = 81.332( 11 ), γ = 74.844(11 )°, V = 1009.89(5) A3, Z = 2, Dc = 1.605 g/cm3, F(000)=498,μ=1.134 mm-1,the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with I ＞ 2σ(Ⅰ).The Cu(Ⅱ) atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.     

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 diethyle-netriamine,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.O(5)(A)3,Z=4,C15H20ClCuN3O2,Mr=373.33,Dc=1.551 g/cm3,μ=1.543mm-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 Novel Terpyridine-based Cd(Ⅱ) Complex

A novel terpyridine-based complex CdL'S2 (L'= oxide of L; L = 10-hexyl-3-(2,6-di(pyridine-2-yl)pyridine-4-yl)-10H-phenothiazine) has been solvothermally synthesized and characterized by FT-IR spectroscopy, elemental analysis, 1 H NMR and X-ray crystallography. The sulfur of phenothiazine moiety was oxidized when the crystal is formed. The complex C36H37CdN5O2S3 crystallizes in triclinic, space group P1 with a = 9.4452(9), b = 13.0181(14), c = 14.6721(18), α = 73.872(1), β = 81.531(1), γ = 87.547(2)°, V = 1714.2(3)3 , Mr = 780.29, Dc = 1.512 g·cm-3 , μ = 0.861 mm-1 , F(000) = 800, Z = 2, the final R = 0.0456 and wR = 0.1059 for Ⅰ > 2σ(Ⅰ). The Cd(Ⅱ) is coordinated by two terminal sulfur ions and three pyridyl nitrogen atoms in a distorted trigonal bipyramidal geometry. Universal hydrogen bonds between the neighboring molecules have generated a supramolecular arrangement which contributes to the stability of the title complex. Fluorescence property and thermogravimetry of the complex have also been investigated and discussed.     

Synthesis, Crystal Structure and Characterization of a New Manganese(Ⅱ)Tetracarboxylate

By hydrothermal synthesis,a manganese(Ⅱ)tetracarboxylate [Mn(2,2'-bipyridi-ne)btec)o.5(H2O)]2n(H4btec=1,2,4,5-benzenetetracarboxylic acid)was obtained and characteri-zed by single-crystal X-ray diffraction,IR,elemental analysis and thermogravimetrie analysis.It crystallizes in triclinic,space group P(1),with a=7.721(4),b=8.905(5),c=10.712(6)(A),α=80.899(8),β=70.371(8),γ=78.201(8)°,z=2,V=675.8(7)(A)3,Mr=354.20,Dc=1.741 g/cm3,μ=1.007mm-1,F(000)=360,S=0.956,(△/σ)max=0.000,the final R=0.0490 and wR=0.1262.This compound presents an infinite 1D polymer featuring a double-chain structure.The Mn(Ⅱ)ion is five-coordinated.The four carboxylate groups of btec4- are all deprotonated and coordinated to four Mn atoms in a monodentate fashion,forming a 1D double chain structure with a cavity.Such chains are interconnected by π-π stacking interactions into 2D layers which are further interlinked into a supramolecular structure by hydrogen bonds.     

Synthesis, Crystal Structure and Characterization of a New Mononuclear Zn(Ⅱ) Complex from Schiff-base Ligand

A new mononuclear [Zn(H-1L)2] (L = 1H-indole-3-ethylene-salicylaldimine) was synthesized through the reaction of Zn(Ac)2, salicylaldehyde and tryptamine in hot ethanol solution and characterized by X-ray crystal structure analysis. The crystal belongs to monoclinic, space group P21/n with a = 15.014(2), b = 10.857(1), c = 17.489(1) , β = 95.49(1)°, V = 2837.8(5) 3, Z = 4, Dc = 1.386 g/cm3, μ = 0.904 mm-1, F(000) = 1232, the final R = 0.0463 and wR = 0.0890 for 4990 independent reflections. In the complex, the Zn2+ ion presents a distorted N2O2 tetrahedral coordination involving two H-1L ligands.     

Synthesis,Crystal Structure and Antimicrobial Activity of a New Ternary Copper(Ⅱ) Complex with p-Chlorophenoxyacetic Acid and 2-Amino Benzothiazole

A novel ternary complex of Cu(pcpa)2(aben)2 (pcpa=p-chlorophenoxyacetic acid anion,aben=2-amino benzothiazole) was synthesized by the reaction of copper acetate,2-amino benzothiazole and p-chlorophenoxyacetic acid.Elemental analysis,IR,UV and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure.The crystal crystalli-zes in the monoclinic system,space group C2/c with a=25.795(4),b=7.384(3),c =17.741(6),β=107.47(2)°,C30H24Cl2CuN4O6S2,Mr=735.09,V=3223.2(18) 3,Z=4,Dc=1.515 Mg/m3,λ(MoKα)=0.71073 ,μ=1.022 mm-1,F(000)=1500,the final R=0.0464 and wR=0.1244.A total of 3218 unique reflections were collected,of which 2228 with I 2σ(I) were observed.The Cu(II) atom is four-coordinated with two carboxylate oxygen atoms of the two pcpa ligands and two nitrogen atoms in thiazole rings of two aben ligands.The analysis of crystal structure shows intermolecular and intramolecular hydrogen bonds between amino-nitrogen atoms of the two aben ligands and carboxylate oxygen atoms of the two pcpa ligands.The antimicrobial properties of the title complex and its two free ligands were tested against representative bacterial and fungal strains.Results show that the antibacterial activity of the complex is less than or equal to that of 2-amino benzothiazole,but for yeasts and moulds,it exhibits excellent inhibitory effect better than that of its two free ligands.     

Synthesis and Crystal Structure of a New Lanthanum(Ⅲ) 4-Cyanobenzoate Complex

A new dinuclear La(Ⅲ) complex [La2(4-cba)4[H(4-cba)2]2(phen)2(H2O)4] (4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline) 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single- crystal X-ray diffraction. Crystallographic data: C88H58La2N12O20, Mr = 1881.28, triclinic P(1), a = 7.518(3), b = 17.033(6), c = 17.551(6)(A), α = 115.333(4), β = 92.9910(10), γ = 99.366(5)°, V = 1985.3(12) (A)3, Z = 1, Dc = 1.574 g/cm3, F(000) = 944 μ = 1.145 mm-1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with Ⅰ ＞2σ(Ⅰ). In 1, two nine-coordinated La(Ⅲ) ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La(Ⅲ) ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-πstacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Synthesis,Crystal Structure and Antitumor Activity in Vitro of a New Benzoate Binuclear Cupper（ Ⅱ） Complex

The title compound, [Cu2（C7H5O2）4（C2H6O）2], was synthesized by the reaction of benzoic acid, copper acetate and ethanol in an aqueous solution. Trypan blue dye exclusion method was used in experiment. X-ray single-crystal analysis has revealed that compound 1 （C32H32Cu2O10） crystallizes in the monoclinic system, space group C2/c, Mr = 703.66, a = 47.340（5）, b = 6.6613（4）, c = 22.028（2）A,β = 113.284（4）°, V = 6380.6（10） A^3, Z = 8, Dc= 1.465 g/cm^3, F（000） = 2896,μ = 1.388 mm^-11, the final R = 0.0515 and wR = 0.1172 for 5712 observed reflections with I 〉 2σ（I）. X-ray crystal structure analysis suggests that compound [CH2（C7H5O2）4（C2H6O）2] has a binuclear structure with two Cu（II） atoms coordinated by four benzoate groups and two ethanol molecules. The crystal packing is stabilized by intermolecular O-H...O hydrogen bonds. The compound inhibits the proliferation of K562 cells （chronic myeloid leukemic cells） significantly and dose-dependently in 48 h, and IC50 of K562 is 17.3μg/mL by trypan blue dye exclusion method.     

Synthesis and Crystal Structure of a New Lanthanum(III) 4-Cyanobenzoate Complex

A new dinuclear La(III) complex [La2(4-cba)4[H(4-cba)2]2(phen)2(H2O)4] (4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline) 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single- crystal X-ray diffraction. Crystallographic data: C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518(3), b = 17.033(6), c = 17.551(6), α = 115.333(4), β = 92.9910(10), γ = 99.366(5)°, V = 1985.3(12)3, Z = 1, Dc = 1.574 g/cm3, F(000) = 944 μ = 1.145 mm–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with I > 2σ(I). In 1, two nine-coordinated La(III) ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La(III) ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Synthesis and Crystal Structure of a New Dinuclear Manganese(Ⅱ) Manganese(Ⅲ) Complex of a Macrocyclic Ligand

A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.