Antitumor Metallothiosemicarbazonate:Synthesis,Crystal Structure,Spectra and Antitumor Studies of Co(Ⅲ) Complex with Thiosemicarbazone Derivative of 2-Benzoylpyridine

The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P21/n, with a=10.227(3), b=17.363(4), c=17.459(4), β=100.408(4)o, V=3049.2(13)3, Z=4, Mr=677.08, Dc=1.475 g/cm3, μ(MoKα)=0.834 mm-1, F(000)=1400, the final R=0.0747 and wR=0.0896 for 1663 observed reflections with I > 2σ(I). The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different com-ponents to stabilize the crystal structure. The antitumor activity of the title complex was tested against A549 lung cancer cell line. Complex I exhibits antitumor activity.     

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.     

Solvothermal Synthesis,Crystal Structure and Antimicrobial Activity of a Novel Imide Nickel Complex [Ni（CH_3CONCOCH_3）_2·2（H_2O）]

A novel imide nickel complex [Ni(CH3CONCOCH3)2·2(H2O)] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl imide in enol form during the formation process of the title complex.The complex was characterized by elemental analysis,IR spectrum and X-ray single-crystal diffraction analysis.It crystallizes in the orthorhombic system,space group Pbca with a = 7.4503(7),b = 13.1089(12),c = 14.1303(14),V = 1380.0(2)3,Dc = 1.420 g/cm3,Mr = 294.94,Z = 4,F(000) = 616,μ = 1.422 mm-1,the final R = 0.0487 and wR = 0.1482.The four-coordinated nickel(II) center is surrounded by 4O atoms from two imide ligands and has a distorted square planar geometry.The complex is connected to form a supramolecule with an infinite three-dimensional network through intramolecular and intermolecular hydrogen bonds.Antimicrobial activity was investigated by agar diffusion method,and the result showed that the complex was active against coli bacillus,staphylococcus aureus and bacillus subtilis.The thermal stability of the title complex was also studied by TG-DTA method.     

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 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.     

Crystal Structure and Properties of a Copper(Ⅱ) Complex Containing p-Toluenesulfonate and Imidazole Ligands

A novel supramolecular mixed ligand complex of formula [Cu(PTS)2(Him)2(H2O)2] (C20H26CuN4O8S2,PTS=p-toluenesulfonate,Him=imidazole) has been synthesized in aqueous solution and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The compound crystallizes in the monoclinic system,space group P21/n,Z=2,a=5.650(2),b=14.671(3),c=14.638(3),β=100.10(3)°,V=1194.60(4)3,Dc=1.607 g/cm3,μ(MoKα)=1.143 mm-1,F(000)=598,R=0.0615 and wR=0.1503 for 1752 observed reflections with I 2σ(I).The copper(II) ion in the complex adopts a slightly distorted octahedral coordination geometry and is six-coordinated with N2O4 donor set consisting of two nitrogen atoms and four oxygen atoms provided by the ligands of two imidazole molecules,two water molecules and two p-toluenesulfonate ions.The sulfonate group of the PTS ligand remains weak-coordinated and forms a number of hydrogen bonds with water molecules and imidazole ligands.X-ray structural analysis reveals that the coordination molecules are connected to form a 3-D supramolecular framework by electrostatic interaction,weak van der Waals forces,hydrogen bonding and π-π interaction.The thermal behaviour of the title complex was investigated by using DSC and TG-DTG techniques.     

Structure Elucidation and Biological Screening of Bis(4-{[(E)-(2-Hydroxybenzylidene)amino]methyl}-cyclohexane-carboxylato-O)-triaqua-cadmium

Using a bidentate ligand, a Schiff base 4-({[(Z)-(2-hydroxyphenyl)methyldene]amino}methyl)cyclohexanecarboxylic acid, complex I(ML2, where M = Cd(Ⅱ)) was synthesized and characterized by IR spectroscopy and X-ray crystallography. It crystallizes in monoclinic system, space group C2/c, M_r = 685.04, 0.34 mm × 0.26 mm × 0.14 mm, a = 54.050(3), b = 6.1220(3), c = 9.5081(5) ?, β = 90.229(2)°, Z = 4, C_(30) H_(40) CdN_2 O_9 and V = 3146.2(3) ?~3. Complex I was screened for its bactericidal activity against four bacterial strains Chromohalobactersalexigens, Chromohalobacterisraelensis, Halomonashalofila and Halomonassalina and fungicidal activity against Aspergillusnigerand Aspergillusflavus. Antimicrobial activity results showed that the synthesized complex displayed good anti-fungal activity against two fungal strains. It was found to be inactive against four different bacterial strains analyzed and was negative for bactericidal effect.     

Synthesis and Crystal Structure of a New [Mn_2Ni_2] Cubane Complex

A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction,FT IR spectra and elemental analysis.The title compound [MnIII2NiII2(hmp)4(N3)4(O2CR)2](hmp-is the anion of 2-pyridinemethanol and O2CR-is α-na-phthaleneacetate)crystallizes in the monoclinic system,space group P21/c with a = 10.519(5),b = 22.109(10),c = 23.235(9),β = 106.096(17)o,C48H42Mn2N16Ni2O8,Mr = 1198.28,V = 5192(4)3,Dc = 1.533 g/cm3,F(000)= 2448,μ = 1.258 cm1,Z = 4,the final R = 0.0875 and wR = 0.2020 for 3398 reflections with I > 2σ(I).X-ray diffraction analysis reveals that each Mn(III)center is octahedrally coordinated by two nitrogen atoms of azide anions and three oxygen atoms from three 2-pyridinemethanol anion ligands together with one oxygen atom from naphthaleneacetate.Each Ni(II)is octahedrally coordinated by two nitrogen atoms of 2-pyridinemethanol anion ligands as well as three oxygen atoms from three 2-pyridinemethanol anion ligands and one oxygen atom from naphthaleneacetate.     

Syntheses,Crystal Structures and Antibacterial Activities of Schiff Base Ligand and Its Nickel(Ⅱ) Complex

A complex [NiL2] was synthesized, in which L, or to be exact, a Schiff base ligand(HL), was derived from the condensation of 1-phenyl-3-methyl-4-phenylacetyl-5-pyrazolone(PMPAP) with L-phenylalanine methyl ester. They were characterized by IR and single-crystal X-ray diffraction. Green block crystals of both ligand and its complex were grown at room temperature. The ligand, which consists of two individual fragments, crystalizes in the P1 space group(a = 5.6268(5), b = 10.6892(11) and c = 19.4869(18) ). The complex crystalizes in the P21 space group(a = 21.4076(18), b = 9.4792(8) and c = 25.287(2) ), which consists of a nickel six-coordinated compound. Every fragment is a distorted octahedron with four oxygen and two nitrogen atoms. The Schiff base ligand(HL) and its complex have been tested in vitro to evaluate their antibacterial activity against bacteria Escherichia Coli and Bacillus subtilis. It is found that the complex has higher activity than the corresponding free Schiff base ligand(HL) against the same bacterial.     

Synthesis,Crystal Structure and Antibacterial Activity of Dibenzyl Dithiocarbamate Bismuth Complex

A new complex, {Bi(Ⅲ)[S2CN(CH2C6H5)2]3}2·2CH3CN, was synthesized and characterized by elemental analysis, IR, TG, 1H NMR and X-ray single-crystal diffraction. The complex crystallizes in the triclinic system, space group P1, with a = 12.705(6), b = 13.430(6), c = 15.489(12) , α = 102.135(12), β = 99.649(12), γ = 111.521(9)°, Z = 1, V = 2315(2) A3, Dc = 1.531 g·cm-3, F(000) = 1068, μ = 4.116 mm-1, the final R = 0.0559, w R = 0.1069 and S =1.056. The coordinated geometry of Bi(Ⅲ) with six sulfur atoms from three ligands is a distorted pentagonal pyramidal configuration, and the structural system is formed by weak interactions of Bi···S between two molecules. The complex was valued for its antibacterial activity by agar-streak method. It was found that the complex is weakly active against three of the five tested bacterial organisms.     

Crystal Structure and Inhibitory Activity against Xanthine Oxidase of Bis(μ_2-chloro)-chloro-(μ-N,N'-(2-pyridylmethylene) Furanmethanoamine Copper(II) Complex

A chloro-bridged dinuclear copper(II) complex with ligand 2-pyridylme-thylene-furfurylamine has been synthesized and characterized by single-crystal X-ray diffraction, and its inhibitory activity on xanthine oxidase (XO) was also evaluated. It crystallizes in the triclinic system, space group P1 with a=8.0441(16), b=8.5663(17), c=10.060(2), α=77.52(3), β= 72.04(3), γ=70.12(3)°, V=615.3(2)3, Z=1, Dc=1.731 g/cm3, F(000)=322, the final R= 0.0401 and wR=0.0934 for 1971 observed reflections with I > 2σ(I). X-ray analysis reveals that the Cu(II) cation is five-coordinated by two N atoms of Schiff base and three Cl anions. The C-H…Cl intermolecular and intramolecular hydrogen bonds connect the molecules to form a three-dimensional network. This copper(II) complex shows more potent inhibitory activity against XO with IC50=3.48 μM than the standard inhibitor allopurinol.     

Syntheses and Crystal Structures of 3,5-Diiodo-salicylalidehyde and 3,5-Diiodo-salicylalidene-4-nitroaniline

The title compounds, C7H4I2O2 1 and C13H7I2N2O3 2, have been synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 9.802（2）, b = 13.867（3）, c = 7.364（2） A, β = 109.74（3）°, V= 942.1（3） A^3, Dc= 2.636 g/cm^3, C7H4I2O2, Mr= 373.90, F（000） = 672, μ = 6.627 mm^-1, Z = 4, R = 0.0459 and wR = 0.1018 for 1805 observed reflections （I 〉 2 σ（I））. Compound 2 belongs to the monoclinic system, space group P21/n with a = 9.015（2）, b = 12.024（2）, c = 14.072（3） A, β = 103.91（3）°, V = 1480.6（5） A^3, Dc= 2.216 g/cm^3, C13H7I2N2O3, Mr= 494.01, F（000） = 920, p = 4.255 mm^-1, Z = 4, R = 0.0777 and wR = 0.1757 for 2896 observed reflections （I 〉 2σ（I））. Compounds 1 and 2 were assayed for antibacterial activities against three Gram positive bacterial strains （B. subtilis, S. aureus and S. faecalis） and three Gram negative bacterial strains （E. coli, P. aeruginosa and E. cloacae） by MTr method. Fortunately, compound 2 is found to show potent antibacterial activity against these six bacterial strains.     

Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce(III)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline), was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912(2), b = 11.962(3), c = 12.474(3) , α = 104.889(3), β = 93.523(3), γ = 113.332(3)o, C66H46Ce2N4O12, Mr = 1366.90, V = 1420.2(6) 3, Z = 1, Dc = 1.598 g/cm3, μ = 1.652 mm-1, S = 1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I > 2σ(I). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units, forming a binuclear molecule. Each Ce(III) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

Synthesis,Crystal Structure and Luminescent Property of a New Copper(Ⅰ) Iodide Complex Based on 3,5-Dimethyl-4-amino-triazole

The title compound,[Cu4I4(C4H8N4)4],has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in monoclinic,space group Pbca,with a=18.1851(10),b=9.3697(5),c=19.8034(10),V=3374.3(3)3,C16H32Cu4I4N16,Mr=1210.34,Z=4,Dc=2.383 g/cm3,μ=6.183 mm-1,F(000)=2272,S=1.032,the final R=0.0309 and wR=0.1180 for 3854 observer reflections(I2σ(I)).The structure of the title compound consists of tetranuclear copper cluster units bridged by the halogen atoms with the 3,5-dimethyl-4-aminotriazole ligands coordinated to the metal ions through the triazole nitrogen atoms.The luminescent property of 1 was also studied.     

Synthesis and Structure of a Novel Tetranuclear Erbium(Ⅲ) Complex with L-Proline(HPro) [Er4(HPro)4(Pro)2·(μ3-OH)4(H2O)7](ClO4)6·6H2O

The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-ray diffraction. The crystal is rhombohedral, space group R3 with a=1.947 0(3) nm, b=1.947 0(3) nm, c=1.768 3(3) nm, α=90°, β=90°, γ=120°, V=5.805(2) nm3, Z=3, the final R value is 0.051 2. The complex contains a novel tetranuclear cation with four Er3+ ions connected by four μ3-OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ3-OH, three carboxylic oxygen atoms from three L-proline, and two or one oxygen atoms from water molecules.     

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 Thermal Stability of a Saturated Dimeric Ce(Ⅲ)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline),was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P(1) with a =10.912(2), b = 11.962(3), c = 12.474(3)(A), a = 104.889(3), β = 93.523(3), γ = 113.332(3)°,C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2(6) (A)3, Z = 1, Dc = 1.598 g/cm3,μ = 1.652 mm-1, S =1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I ＞ 2σ(1). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units,forming a binuclear molecule. Each Ce(Ⅲ) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

Synthesis and Structure of a NovelTetranuclear Erbium( Ⅲ) Complex with α-Alanine [Er4(Hala)6·(μ3-OH)4(H2O)8](ClO4)8·3H2O

The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-ray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a=1.306 3(2) nm, b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β=93.998(11)°, γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R1=0.065 4, wR2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er3+ ions connected by four μ3-OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ3-OH, three carboxylic oxygen atoms from three α-alanine and two oxygen atoms from water molecules, forming a square-antiprismatic coordination polyhedron.     

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,Crystal Structure and Antibacterial Activities of 4-Methyl-2-(4-methylphenyl)-5-(2-thiazolinyl)-1,3-thiazole

4-Methyl-2-(4-methylphenyl)-5-(2-thiazolinyl)-1,3-thiazole, a novel compound, was synthesized by the annulation of 5-hydroxyethylcarbamoyl-4-methyl-2-(4- methylphenyl)-1,3-thiazole with P_2S_5. 5-Hydroxyethylcarbamoyl-4-methyl-2-(4-methylphenyl)-1,3-thiazole was prepared from the starting material of p-tolunitrile. The newly synthesized compounds were characterized by elemental analysis, IR, NMR(~1H, ~(13)C) and MS spectra. Hence, the crystal of the title compound was obtained, and its structure was determined by X-ray diffraction analysis. The crystal belongs to the triclinic system, space group P1 with a = 7.354(4), b = 8.383(4), c = 11.543(6) ?, α = 76.688(6), β = 72.299(6), γ = 88.157(6)°, V = 659.2(6) ?~3, Z = 2, M_r = 274.39, D_c = 1.382 g/cm~3, μ = 0.386 mm~(-1), F(000) = 288, R = 0.0586 and w R = 0.1808 for 2984 unique reflections with 2213 observed ones(I 2σ(I)). The title compound was also screened for its antibacterial activities against Bacillus subtilis and Escherichia coli. The result indicates that the target compound presents potential antimicrobial activities, and that the minimum inhibitory concentration(MIC) values of the title compound against the two tested strains are both 62.5 μg/mL.