Synthesis, Crystal Structure and Properties of a Copper Complex with the Bicycle[2.2.1]-2-heptene-5,6-dicarboxylic Acid

A new copper complex 2{Cu（C10H8N2）[C8H11O2（COO）]（H2O）3}·（H2O）5 with bicycle[2.2.1]hept-2-en-5,6-dicarboxylic acid（H2L） [C7H8（COOH）2], basic copper carbonate and 2,2＇-bipyridine has been synthesized in the mixed solvents of methanol and water. It crystallizes in the triclinic system, space group P1, with a = 7.4626（5）, b = 11.9779（8）, c = 12.9841（8）A, α = 109.7040（10）, β = 98.7550（10）, γ = 90.6240（10）°, V = 1077.50（12）A3, Dc = 1.538 g/cm^3, Z = 1, F（000） = 520, GOOF = 1.065, R = 0.0360 and wR = 0.0950. The copper ion is coordinated with four oxygen atoms from one H2 L molecule and three water molecules together with two nitrogen atoms from the 2,2＇-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stability and electrochemical properties were also studied.

Synthesis,Crystal Structure and Biological Activity of a Planar Copper Complex Derived from S-benzyldithiocarbazate

A planar transition metal complex Cu（L）2 （L = （E）-benzyl-2-（4-nitrobenzylidene）-hydrazinecarbodithioate） has been prepared and determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system,space group P21/c with a = 6.7101（11）,b = 16.952（3）,c = 13.962（3） ,β = 92.458（4）°,V = 1586.7（5） 3,Z = 4,Mr = 724.33,Dc = 1.516 g·m-3,μ = 0.998 mm-1,F（000） = 742,S = 1.021,R = 0.0634 and wR = 0.1077 for 813 observed reflections with Ⅰ〉 2σ（Ⅰ） and 205 parameters. In the molecular structure of the title complex,the copper atom exhibits a slightly distorted square-planar geometry in which the basal plane is defined by two N and two S atoms from two bidentate ligands. The complex was evaluated for its antitumor activity against two kinds of cell lines （MKN45 and HepG2） by MTT method. The preliminary bioassay indicates that the complex exhibits weak antitumor activity.

Synthesis and Crystal Structure of the Copper Complex {[Cu(CH_3COO)_2(bbtz)](H_2O)_2}_n

The new copper complex { [Cu（CH3COO）2（bbtz）]（H2O）2 }, 1 （bbtz = 1,4-bis（ 1,2,4- triazol-1-ylmethyl）benzene） was synthesized and the structure was determined by single-crystal X-ray diffraction. Crystal data： C16H22CuN6O6, monoclinic, space group P21/n, a = 12.589（5）, b = 6.455（2）, c = 12.677（5） A, β= 98.748（9）°, V= 1018.2（7） A^3, Mr = 457.95, Z = 2, Dc= 1.494 g/cm^3, F（000） = 474, μ = 1.118 mm^-1, R = 0.0463 and wR = 0.0939 for 1971 observed reflections with I 〉 2σ（I）. The crystal structure of 1 is a one-dimensional chain via the bridging flexible ligand bbtz.

Synthesis, Crystal Structure and Property of a Binuclear Copper Complex [Cu_2L_2(pht)_2]_2·H_2O

A new binuclear copper complex, [Cu2L2（pht）2]2·H2O （Hpht = 5,5-diphenylhy- dantoin, i.e. phenytoin; L = 2-diethylaminoethanol）, has been synthesized by the solvothermal method, and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 31.918（3）, b = 12.9222（15）, c = 19.868（2） A,β = 98.762（2）°, V= 8098.8（16） A3, Dc = 1.429 Mg/m3, Z= 4, F（000） = 3640, p = 1.107 mm-1, R = 0.0560 and wR = 0.1276 （1 〉 20（/））. Each copper（Ⅱ） in a molecule is coordinated with N and O atoms from ligand L and N atom from ligand Hpht in a tetradentate manner. Moreover, two copper（Ⅱ） centers are bridged by two O atoms of hydroxyl groups from two L ligands to form a slightly distorted binuclear {Cu202} diamond configuration. In addition, the interaction of this complex with calf thymus DNA （CT-DNA） was investigated by UV-vis spectrum and viscometry, and the complex may bind to DNA through intercalation.

Synthesis, Crystal Structure and Catechol Oxidase Mimic Activity of a Dinuclear Copper Complex

A dinuclear copper complex [Cu2LCl2]（ClO4）2 （L = 2,2＇-（piperazine-1,4-diyl）bis- （N,N-bis（pyridine-2-ylmethyl）ethan-1-amine）） has been synthesized and structurally characterized. It crystallizes in triclinic, space group Pī with α = 8.5707（9）, b = 10.5083（12）, c = 11.4878（13） A, α = 76.197（2）, β = 88.271（2）, γ = 87.855（2）o, V = 1003.81（19） A3, Z = 1, F（000） = 478, Dc = 1.544 Mg/m3, Mr = 933.60, μ = 1.383 mm^-1, the final R = 0.0669 and wR = 0.1486 for 3675 observed reflections with I 〉 2σ（I）. Its catechol oxidase mimic activity was studied spectroscopically by using 3,5-di-tert-butylcatechol （3,5-DTBC） as the substrate. The results showed that the kinetics of catechol catalyzed by the complex accorded with the Michaelis-Mentent equation, and the catechol oxidase catalytic activity of the complex increased with increasing the pH values.

Synthesis,Crystal Structure and Antibacterial Activity of a New Ternary Copper(Ⅱ) Complex with 2,6-Pyridinedicarboxylic Acid and 1,10-Phenanthroline

A new ternary copper（Ⅱ） complex, [C43H27Cu2N7O5][C14H6CuN2O8]＇6.5H2O, has been synthesized by the reaction of copper sulfate, 2,6-pyridinedicarboxylic acid and 1,10- phenanthroline （phen）, and characterized by elemental analysis, IR, UV and X-ray single-crystal diffraction. It crystallizes in triclinic, space group P1, with a = 14.379（5）, b = 15.510（5）, c = 15.835（6） A, a = 78.567（6）, β = 63.594（6）, y = 81.287（6）°, V= 3092.1（19） A3, C57H46Cn3N9O19.5, Mr = 1359.54, Z = 2, Dc = 1.446 Mg/m3, λ（MoKa） = 0.71073 A,μ = 1.101 mm^-1, F（000） = 1362, S = 1.071, the final R = 0.0718 and wR = 0.11960 for 10705 observer reflections （I 〉 2σ（I））. The structure unit of the title complex consisfs of a mononuclear part and a di-nuclear part, and the three copper ions show three coordination modes. Each 6-coordinated geometry of the Cu atom is a distorted octahedral coordination geometry. The 3D supramolecular system is formed by the hydrogen bond O-H-O and π-π stacking interaction between neighboring single cells. The antibacterial activity of the title complex is also studied.

Syntheses and Crystal Structures of Copper(Ⅱ) and Nickel Complexes with 1,2,3-Triazole-carboxylic Acid

Three novel complexes [Cu（L1）2（H2O）2] （1）, [Ni（L1）2（H2O）2]·（H2O）4（2,HL1=5-methyl-1-（4-methylphenyl）-1,2,3-triazole-4-carboxylic acid） and [Ni2 （HL2）2（CH3OH）6]·（CH3OH）2（3,H3L2=1,2,3-triazole-4,5-dicarboxylic acid） were synthesized and characterized by elemental analysis, IR and X-ray diffraction. Complexes 1 and 2 are mononuclear structures, and are assembled into a two-dimensional sheet by C（7） H（7）···O（3） weak interactions or hydrogen-bonding interaction. Complex 3 is a centrosymmetric dinuclear structure, and is assembled into a three-dimensional supramolecular structure by hydrogen-bonding interaction.

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

A new Cu（Ⅱ） complex [Cu（4-cba）（1,10-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 PI, a = 7.8420（2）, b = 9.1070（2）, c = 15.1140（6） A, a = 76.889（9）, β = 81.332（11）, γ = 74.844（ 11）°, V = 1009.89（5） A^3, Z = 2, Dc = 1.605 g/cm^3, F（000） = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 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.

Syntheses,Crystal Structures and Antibacterial Activities of 5-Chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic Acid and Its Copper(Ⅱ) Compound

The title compounds 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic acid（C11H9Cl N2O2, HL）（1） and [Cu（L）2（H2O）]（2） were prepared and structurally characterized by elemental analysis, IR and single-crystal X-ray diffraction. Compound 1（C11H9Cl N2O2） crystallizes in the monoclinic system, space group P21/n with a = 7.249（3）, b = 20.515（10）, c = 7.249（3）,β= 96.30°, V = 1071.6（9） ？3, Z = 4, Mr = 236.65, Dc = 1.467 g/cm3, F（000） = 488, GOOF = 1.029, μ= 0.341 mm-1, the final R = 0.0736 and w R = 0.1966 for 1500 observed reflections with I 〉 2σ（I）. Compound 2（C22H18Cl2Cu N4O5） crystallizes in the monoclinic system, space group P21/c with a = 7.2931（6）, b = 24.548（2）, c = 13.2726（11）, β= 99.4040（10）°, V = 2344.2（3） ？3, Z = 4, Mr = 552.84, Dc = 1.566 g/cm3, F（000） = 1124, GOOF = 1.050, μ= 1.201 mm-1, the final R = 0.0376 and w R = 0.1000 for 3626 observed reflections with I 〉 2σ（I）. 1 and 2 are connected through hydrogen bonding interactions to generate 2D and 3D supramolecular structures, respectively. Moreover, the preliminary antibacterial activities of 1 and 2 against the gram positive bacteria（S. aureus, C. albicans and B. subtilis） and gram negative bacteria（E. coli and P. aeruginosa） have been tested by using the microdilution method, and the results indicate that 2 is more active than 1 against the tested bacteria.

Synthesis and Crystal Structure of a Copper(II) Complex with Benzilic Acid and 1,10-Phenanthroline

A new complex [Cu（phen）3][（C6H4）2C（OH）COO]2·6H2O was prepared by selfassembly of benzilic acid, 1,10-phenanthroline （phen）, and copper perchlorate. It crystallizes in triclinic, space group P1-, with a = 1.14661（17）, b = 1.6455（2）, c = 1.6457（2） nm, α= 74.779（2）, β = 74.904（3）, γ = 84.424（3）°, V = 2.8914（7） nm^3, Dc = 1.340 g/cm^3, Z = 2, F（000） = 1218, GOOF = 1.018, the final R = 0.0643 and wR= 0.1633. The crystal structure shows that the copper ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry.

A Novel Palladium(Ⅱ)Complex Self-assembled from Anthracene-9-carboxylic Acid:Synthesis,Crystal Structure and Spectroscopic Properties

A novel palladium（II） complex [（TMEDA）Pd（anca）2].2DMSO （1, TMEDA = N,N,N＇,N＇-tetramethylethylethylenediamine, anca = anthracene-9-carboxylic acid） was synthesized and characterized by single-crystal X-ray diffraction, 1H NMR, UV-Vis and fluorescence spectroscopy. The cell belongs to orthorhombic Aba2 space group with a = 19.698（7）, b = 21.045（7） c = 9.062（3） A, Z = 4, V= 3757（2） A3, C40H46N206PdS2, Mr = 821.31, D, = 1.452 g/cm3, F（000） = 1704, the final R = 0.0272, wR = 0.0667 and GOOF = 0.999. Complex 1 exhibits an interesting distorted clip-shaped molecular configuration which is stabilized by intramolecular C-H...O hydrogen bonds. The cells are packed into a 3D supramolecular structure based on the intermolecular C-H...zr interactions which further construct the tubular channels serving as guest molecular channels to include the DMSO solvent molecules inside. Furthermore, the spectroscopic properties of 1 were also investigated.

Synthesis and Crystal Structure of a Copper(II) Complex with α-Hydroxylated Acid, [Cu(C_(14)H_8O_3)(C_5H_(13)NO)(H_2O)].0.5H_2O

The complex monoaqua[(9-hydroxy-fluorene-9-carboxylato)(N,N-Dimethylisopro- panolamine)]copper(II) semihydrate, Cu(C14H8O3)(C5H13NO)(H2O)]0.5H2O (Mr = 417.93), crystallizes in triclinic system, space group P with a = 9.846(2), b =12.419(3), c =16.781(3)? =75.55(3), b = 75.00(3), g = 84.58(3), V =1918.5(7)?, Z = 4, F(000) =872, Dc=1.45g/cm3 and m= 1.17mm-1. The final R and wR are 0.0481 and 0.1427 for 7099 observed reflections, respectively. The coordination polyhedron around the copper atom is a distorted square pyramid, the basal plane consisting of one carboxyl oxygen atom and one -hydroxylated oxygen atom from a 9-hydroxy-fluorene-9-carboxylato ligand, one nitrogen atom and one oxygen atom from the N,N-dimethylisopropanolamine ligand; while the axial coordination site is occupied by a water oxygen atom with a Cu-O bond length of 2.428(3)?

Two New Copper(Ⅱ) Complexes with p-Cyanobenzoic Acid: Synthesis, Crystal Structures and Properties

The complexes of [Cu（bpy）（H2O）（CBA）2]n 1 and [Cu（phen）（H2O）（CBA）2]·H2O 2 based on p-cyanobenzoic acid （HCBA） have been synthesized in aqueous ethanolic solution at room temperature. The single-crystal X-ray diffraction studies demonstrated that complex 1 crystallizes in orthorhombic and complex 2 is of triclinic system. The results indicate the complex 1 shows a 1D chain structure bridged bytwo carboxylic oxygen atoms from CBA–, and complex 2 is a mononuclear structure. Through intermolecular hydrogen bonding and π···π stacking interactions, the complexes are assembled into supramolecular structures.Complex 1 has been characterized by magnetic measurements. Themagnetic measurement indicates that weak ferromagnetic interaction （zJ＇ = 0.038（5）） between the Cu^2＋ ions is dominant in the structure. The IR spectrum and results of thermal and elemental analyses are also presented.

Crystal Structure of a Ternary Copper(Ⅱ) Complex of N,N'-(p-Xylylene)dialanine Acid and 1,10-Phenanthroline

The compound [Cu2（bpy）2（PDIAla）（H2O）2]（ClO4）2·H2O（H2PDIAla = N,N＇-（p-xylylene）dialanine,bipy = 2,2＇-bipyridine） 1 has been synthesized and structurally determined by single-crystal X-ray diffraction,elemental analyses and IR spectroscopy.The crystal belongs to the monoclinic system,space group P21 with a = 10.9772（6）,b = 18.5464（9）,c = 11.0790（6） ,β = 116.3110o,V = 2021.87（18） 3,Z = 2,Dc = 1.594 Mg/m3,Mr = 970.70,μ = 1.260 mm-1,F（000） = 996,λ（MoKα） = 0.71073 ,the final R = 0.0400 and wR = 0.1050 for all observed reflections.In the structure,the O（5）-H（52）…O（4） hydrogen bonding between aqua ligand and carbonyl oxygen of the H2PDIAla ligand along the c axis produce hydrogen-bonded helices which are assembled along the b axis through O（61）-H（61）…O（2） and N（6）-H（6N）…O（2） interactions to form 2-D layers that are further linked by π···π interactions between bpy ligands to yield a three-dimensional supramolecular network.

Crystal Structure and Molecular Structure of Binuclear Copper(Ⅱ) Complex, [Cu (C_5H_5NO) (C_6H_5COO)_2]_2

At room temperature, dibenzoyl peroxide and pyridine N-oxide reacted with metallic copper powder in a mixed solvent(dichloromethane, trichloromethane and tetrahydrofuran), resulting in a binuclear copper(Ⅱ) complex. [Cu (C_5H_5NO)-(C_6H_5COO)_2]_2. The structure of the complex was characterized by elemental analyses.IR spectra and X-ray single crystal analysis. The crystal is triclinic, space group P1,with cell parameters . a= 9. 262(4) ,b= 10. 697(2) , c=10. 881 (3 )A , a=59. 60( 2 ),β= 74. 83 ( 3 ) .Y = 72. 80 ( 2 )°. V= 880. 0 A￣3 . D_c = 1 . 5 20 g/cm￣3 . Z = 1 . μ= 1 2. 7 cm-1, R=0. 044 ,R_w=0. 048 for 3477 reflections with I>3σ(I), M_r=805. 78. Each copper(Ⅱ) atom is coordinated by four bridging bidentate benzoate ligands and one pyridine M-oxide.

THE CRYSTAL STRUCTURE OF RARE EARTH COMPLEX WITH AMINO ACIDS Ⅱ The Crystal Structure of Gtutamate Comptex of Erbium Perchtorate

The crystat structure of {[Er;（L—Glu）;（H;O）;]（ClO;）;·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987（3） , b=16.505（3） , c=11.040（2） , β=104.69（1）;, V=3538（1） , Z=2, Dc=2.29 g. cm;, μ=53.2 cm;, F（000）=2384. The asymmetric unit contains two complex motecules and four centre ions. Each erbium （Ⅲ） is coordinated by five oxygen donors from four different glutamates and four oxygen donors from the aqua ligand to form a nine coordination potyhedron. The mean distances of Er—0 （carboxylate） and Er—Ow are 2.439 and 2.41 respectivety. The finat R and Rw are 0.043 and 0. 058, respectivety.

Synthesis, Crystal Structure and DNA-Binding Property of a Mn(Ⅱ) Complex Based on 5-(Tri-fluoromethyl)pyridine-2-carboxylic Acid

A new complex Mn(Htpc)2(H2O)2(1, Htpc = 5-(trifluoromethyl)pyridine-2-carboxylic acid) has been synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. 1 belongs to triclinic system, space group P■ with a = 5.0885(10), b = 6.5574(13), c = 14.016(3) ?, β = 90.67(3)o, V = 436.34(17) ?3, Z = 1, Dc = 1.793 g·cm-3, μ = 0.855 mm-1, Mr = 471.18, F(000) = 235, the final R = 0.0454 and wR = 0.1134 for 1998 observed reflections with I > 2σ(I). The Mn(Ⅱ) ion is coordinated by two N and two O atoms from two Htpc as well as two O atoms from two coordinated water molecules, forming a 0D motif with distorted octahedral coordinate geometry. The adjacent 0D units are linked into 1D chains through hydrogen bond O(1W)–H(1 WB)···O(2), and via the O(1 W)–H(1 WA)···O(1) hydrogen bond the neighboring 1D chains are connected into a 2D supramolecular layer. Moreover, the interactions between the ligand and its complex with CT-DNA were studied by EtBr fluorescence probe, which suggested that these compounds bind to CT-DNA through an intercalation mode. The binding constants were 0.41 and 0.64 for Htpc and complex 1, respectively. It indicates that the interaction between complex 1 and CT-DNA is stronger than Htpc.

Thiocyanate-controlled Copper(Ⅱ)-L-arginine Complex:Synthesis,Crystal Structure and Characterization

A novel thiocyanate-controlled copper（Ⅱ）-L-arginine complex with the formula of Cu（Arg）（SCN）2（1,Arg：L-arginine） has been obtained from aqueous solution and structurally characterized by single-crystal X-ray diffraction method.Crystal data：orthorhombic,space group P212121,a = 6.0156（5）,b = 12.1905（11）,c = 18.4203（16） A°,V = 1350.8（2） A°3,Z = 4,μ = 1.933mm^（-1）,F（000） = 724,S = 1.084,the final R = 0.0410,wR = 0.0754 for 1893 observed reflections with I 〉 2σ（I）,and R = 0.0559,wR = 0.0820 for all reflections.In addition,elemental analysis,IR,TG-DTG and magnetism characterization are presented.

Structure Studies on New Types of Macrocyclic Compounds Part Ⅵ. Crystal Structure of Copper(Ⅱ) Complex of 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-N', N'-diaceticacid

The crystal structure of copper(Ⅱ) complex with a new 14-membered tetraazamacrocyclic ligand 5,5,7,12,12,14-hexamethy1-1,4,8,11-tetraazacyclotetradecane-N'N'-diacetic acid,[CuC16N4H34(CH2COO)(CH2COOH)]·ClO4·0. 5HCIO4·1. 5H2O was determined. Crystallographic data: Mr = 639.22,orthorhombic, space group Pcnb with a=11.743(4),b=16.446(2),c=29.611 (4) A,Z=8,V=5726(3) A3, Dc=1.482 g·cm-3, F(000)=1344,μ=9. 64 cm-1,R=0.063,and Rw=0.067 for 2386 reflections with I≥3σ(I). The structure shows an unusual configuration in which two carboxyl groups were bonded to two neighboring nitrogen atoms of the macrocycle, N1 and N4, and six methyl substituents occur on one side of the macrocycle, while two carboxyl groups on the other side, and central copper(Ⅱ) ion forms a five-coordinated geometry.

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Binuclear Copper(Ⅱ) Complex with 3-(Pyridin-2-yl)-1,2,4-triazole

One novel binuclear copper（Ⅱ） complex [Cu 2 （Hpt） 2 （CO 3） 2 （H 2 O） 2 ]·H 2 O with copper carbonate and 3-（pyridin-2-yl）-1,2,4-triazole （Hpt） was hydrothermally synthesized and characterized by IR and X-ray diffraction analysis.The complex crystallizes in triclinic,space group P2 1 /n with a=0.6862（1）,b=0.7805（1）,c=1.1983（2） nm,α=72.03（2）,β=107.72（3）,γ=75.28（2）o,V=0.5884 nm 3,D c=2.105 g/cm 3,Z=1,F（000）=357,GOOF=1.041,the final R=0.01859 and wR=0.04348.The whole molecule is composed of two cooper ions,two Hpt molecules,two carbonate and three water molecules,forming a binuclear structure.The crystal structure shows that the cooper ion is coordinated with three nitrogen atoms from two Hpt molecules,two oxygen atoms from one carbonic acid and one water molecule,forming a distorted square pyramidal geometry.The TG analysis result shows that the title complex is stable under 131.0 ℃.