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 ℃.

Synthesis,Crystal Structure and Antitumor Activity of Mixed Ligand Coordination Compound of Copper with Norfloxacin and 1,10-Phen,[Cu(NFLX)(phen)(H2O)]NO3·3H2O

The mixed ligand coordination compound of copper with norfloxacin (NFLX) and 1, 10-phen has been synthesized and characterized by means of X-ray single crystal diffraction. The structure features of the coordination compound are described. Antibacterial activities of the coordination compound have been tested against different microorganisms. The antitumor activities of the coordination compound on leukemia HL-60 cell line and liver cancer BEL-7402 cell line have been measured, respectively. The results indicated that the coordination compound has strong inhibitory effect on HL-60 and BEL-7402 cell lines.

Synthesis,Crystal Structure and Thermal Stability Properties of a Binuclear Copper(Ⅱ) Coordination Polymer {[Cu_2(4,4'-bipy)_2(o-ABA)_4(H_2O)_2][(H_2O)_2]}_n

One-dimensional chain copper（Ⅱ） coordination polymer has been synthesized and characterized in the solvent mixture of water and alcohol with o-acetamidobenzoic acid,4,4＇-bipyridine and copper perchlorate.It is of tetragonal,space group P41212 with a=1.57756（10）,b= 1.57756（10）,c=2.1438（3）nm,V=5.3352（8） nm^3,Dc=1.524 g/cm^3,Z=4,F（000）=2536,R= 0.0479 and wR=0.0979.The crystal structure shows two coordination modes.The copper（1） is coordinated with two nitrogen atoms of one 4,4＇-bipyridine molecule and two oxygen atoms from two o-acetamidobenzoic acid molecules,forming a distorted tetrahedral coordination geometry; the copper（2） is coordinated with two nitrogen atoms of one 4,4＇-bipyridine molecule,four oxygen atoms from two o-acetamidobenzoic acid molecules and two water molecules,generating a distorted octahedral coordination geometry.The result of TG analysis shows that the title complex is stable below 180.0 ℃.

Synthesis and Crystal Structure of Bis[O,O'-di(2-phenylethyl)dithiophosphato](α,α'-bipyridine)copper(Ⅱ)

A ternary adduct Cu[S2P（OCH2CH2Ph）2]2·bipy（bipy=α,α＇-bipyridine） was syn-thesized and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a=10.2320（2）,b=11.5249（3）,c=18.0916（3）,α=98.95（1）,β =103.601（1）,γ=91.272（2）°,V=2044.49（7）3,Z=2,Dc=1.453 g/cm3,T=153（2） K,C42H44CuN2O4P2S4,Mr=894.51,λ（MoKα）=0.71073,μ=0.86 mm-1,S=0.999,（△/σ）max=0.002,the final R=0.0243 and wR=0.0704.A total of 9221 unique reflections were collected,of which 8573 with Ⅰ 〉2σ（Ⅰ） were observed.The Cu（Ⅱ） atom is five-coordinated in a rather distorted trigonal bipyramidal geometry（τ value=0.537）.The Cu-S distances range from 2.3491（4） to 2.4829（4） ,and the Cu-N distances are 1.9987（12） and 2.0584（11） ,respectively.An interesting feature of this adduct resides in its two-dimensional（2D） open framework constructing through hydrogen bonding and π-π interactions.

A Copper(Ⅱ)Complex Based on N-(4-hydroxybenzyl)-L-serine:Synthesis,Crystal Structure and Inhibitory Activity on PTP1B and TCPTP

A novel copper（II） complex with the reduced Schiff base, [Cu（L）2]·H2O （I, HL = N-（4-hydroxybenzyl）-L-serine）, was prepared in aqueous solution and characterized by elemental analysis, FT-IR, electrospray ionization mass spectrometry and single-crystal X-ray diffraction. Complex I crystallizes in the orthorhombic system, space group P212121, with a = 8.9040（18）, b = 9.1530（18）, c = 24.891（5）A^°, V = 2028.6（7） A^°3, Z = 4, C20H26CuN2O9, Mr = 501.97, Dc = 1.644g·cm^3, μ = 1.135 mm^-1, F（000） = 1044, GOOF = 1.194, the final R = 0.0484 and wR = 0.1420 for 6186 observed reflections （I 〉 2σ（I））. In I, two L^- anions are coordinated to the copper ion in tridentate and bidentate chelating modes, respectively, resulting in the coordinated geometry of copper ion to be a distorted square pyramid. The intermolecular hydrogen bonds between the complexes, complexes and lattice water molecules lead to a 2D supramolecular network. The bioactivity of the complex as a potential PTPs inhibitory agent in vitro was investigated, displaying potent inhibition against PTP1B （IC50, 0.27 μM） and TCPTP （IC50, 0.57 μM） with a moderate selectivity.

Hydrothermal Synthesis and Crystal Structure of One Novel 1-D Copper(Ⅱ)-organic Framework:{[Cu_2(PP)_2(CBPC)]_2·7H_2O}_n

One novel 1-D copper（Ⅱ）-organic compound,namely {[Cu2（PP）2（CBPC）]2·7H2O}n（1,H2CBPC=1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP=3-（2-pyridyl）pyrazole）,was synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that the two Cu（Ⅱ） ions in the distorted dimer [Cu2（PP）2] of 1 are linked by the carboxylate oxygen atoms on the phenyl and imidazole rings,respectively,forming one interesting snake-like chain.Single-crystal X-ray analyses reveal that it crystallizes in monoclinic,space group C2/c with a=30.656（8）,b=12.715（3）,c=22.405（5）,β=122.758（3）°,V=7344（3）3,Z=4,Mr=1681.65,Dc=1.521 g/cm3,F（000）=3464,μ=1.221 mm-1,the final R=0.0453 and wR=0.1023 for 4617 observed reflections with Ⅰ 〉2σ（Ⅰ）.

Synthesis and Crystal Structures of the α and β Forms of Bis(salicylaldoxime)copper(Ⅱ) Complexes

Modified α and β bis(salicylaldoxime)copper(Ⅱ) have been obtained by recrystallization from ethyl acetate(CCDC Nos. 212157 & 212158). The X-ray analysis reveals that the two modificated forms have the same structure with different geometric parameters. The α form crystallizes in the P2(1)/c space group and the β form in the P1 space group. Both the crystal structures consist of centrosymmetric monomeric molecules of Cu(OC_6H_4CNOH)_2. The IR spectra are in agreement with the structural data.

Synthesis and Crystal Structure of Copper(Ⅱ) Compound with Didentate Schiff-base Ligand

The title complex [Cu(L)2] (HL=4-salicylideneamino-3,5-dimethanol-1,2,4-triazole) was synthesized by the reaction of Cu(CH3COO)22H2O with 4-salicylideneamino-3,5-dimethanol- 1,2,4-triazole in the methanol. The single-crystal X-ray study reveals that the compound crystallizes in monoclinic, space group P21/n with a = 11.746(5), b = 8.145(3), c = 12.786(5) ? b = 106.64(1), V = 1172(1) ?, Z = 2, Dc = 1.581 g/cm3, m = 0.989 mm-1, F(000) = 574, C22H22Cu- N8O6, Mr = 558.02, T = 293(2) K, R = 0.0394 and Rw = 0.0835 for 2376 observed reflections with I > 2s(I). The complex comprises a four-coordinated copper(II) center, with an N2O2 planar coordi- nation environment. The molecules are connected by hydrogen bonds to form one-dimensional chains which are further linked to form a two-dimensional plane.

Synthesis,Crystal Structure and DNA-binding Properties of a New Copper(Ⅱ) Schiff Base Complex

A new asymmetric bidentate copper（Ⅱ） complex,CuL 2（HL=2-（（E）-（4-bromophenylimino）methyl）-6-bromo-4-chlorophenol）,has been synthesized and characterized by elemental analyses and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic space group P2 1 /c with a=11.218（3）,b=9.355（3）,c=13.449（4）,β=108.722（4）°,V=1336.8（6）3,Z=2,Dc=2.008 g/cm 3,μ（MoKα）=7.024 mm-1,F（000）=806,S=0.999,the final R=0.0342 and wR=0.0641for2611observed reflections （I〉2σ（I））.The central copper（Ⅱ） is four-coordinate and bonds to two nitrogen and two oxygen atoms from two Schiff base ligands.The complex is linked into a two-dimensional supramolecular structure by weak intermolecular interactions.In addition,DNA-binding properties of the metal complex were investigated using spectrometric titrations and viscosity measurements.The results show that the complex binds with calf-thymus DNA（CT-DNA）,presumably via a partial intercalative mode.The intrinsic binding constant of the Cu（Ⅱ） complex with DNA is 7.335×10 3 M-1.

Synthesis and Crystal Structure of 1-D Chain Copper(Ⅱ) Complex: [Cu(L)Cl_2]_n (L=2,5-Di-2-pyridyl-1,3,4-oxodiazole)

The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.

Synthesis,Crystal Structure and Catalytic Performance of the Trifluoro-substituted Mono(β-diiminato)Copper(Ⅱ)Complex

Two novel copper complexes with methyl or trifluoro-substituted mono-β-diiminato ligands and one acetoxyl anion were synthesized and characterized by IR spectroscopy and elemental analysis for the first time. The structure of complex 2 bearing trifluoro substituents was further confirmed by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.377（4）, b = 11.727（6）, c = 12.913（7） ？, α = 116.569（6）, β = 98.829（7）, γ = 96.520（6）°, V = 966.2（8） ？3, Z = 2, Mr = 479.86, Dc = 1.649 g/cm3, F（000） = 482, μ = 1.205 mm-1, the final R = 0.0370 and w R = 0.0903 for 3430 observed reflections with I 〉 2σ（I）. These mono-β-diiminato copper complexes can effectively catalyze methacrylate（MA） polymerization when activated by MMAO. The introduction of fluoro groups into the N-aryl ring of β-diiminato ligands can greatly increase the catalytic activity of copper complexes as well as the molecular weight of PMA.

Syntheses,Crystal Structures and Fluorescence Properties of Two Mononuclear Copper(Ⅱ) Compounds

Two new compounds,1（[Cu（IDB_）2]Cl_2·2CH_3CH_2OH·2H_2O（IDB = N,N-di（2-benzimidazolylmethyl）imine]） and 2（[Cu（EDTB）]·2[C_6H_4（OH）COO]·6H_2O（EDTB = N,N,N＇,N＇-tetrakis-[（2-benzimidazolyl）methyl]-1,2-ethanediamine]）,have been synthesized and their crystal structures were determined by single-crystal X-ray diffraction. Crystal 1 belongs to the triclinic system,space group P1 with a = 9.565（2）,b = 9.863（2）,c = 10.252（3） ？,α = 81.915,β = 88.330,γ = 87.347°,V = 956.28（40） ？3,Z = 1,F（000） = 427,D_c = 1.419 g/cm3,Mr = 817.27 and μ（MoKα） = 0.764 mm^（-1）. The final R indices（I 〉 2σ（I））： R = 0.0505,wR = 0.1417; R indices（all data）： R = 0.0591,wR = 0.1525. Crystal 2 is of triclinic system,space group P1 with a = 11.487（3）,b = 13.396（4）,c = 17.977（5） ？,α = 73.899（5）,β = 86.629（5）,γ = 65.018（4）°,V = 2403.8（12） ？3,Z = 2,F（000） = 1072,D3c = 1.417 g/cm,Mr = 1025.54,μ（MoKα） = 0.528 mm^（-1）. The final R indices（I 〉 2σ（I））： R = 0.0769,w R = 0.163 2; R indices（all data）： R = 0.0769,wR = 0.1632. The two compounds exhibit mononuclear structures. The copper（Ⅱ） atom of crystal 1 is six-coordinated by four nitrogen atoms of benzimidazole groups and two amine nitrogen atoms from the ligand IDB to adopt a distorted octahedral coordination geometry. The copper（Ⅱ） atom of crystal 2 is six-coordinated by four nitrogen atoms of benzimidazole groups and two amine nitrogen atoms from the ligand EDTB to show a distorted octahedral coordination geometry. Particularly,the two compounds exhibit fluorescent properties at room temperature in ethanol.

Synthesis,Crystal Structure and Redox Property of a Copper(Ⅱ)Complex Based on 1,1-Bis(1H-benzoimidazol-2-ylmethyl)cyclohexane

A novel mononuclear copper（Ⅱ） complex [Cu（bbmc）Cl_2]·DMF,where bbmc is 1,1-bis（1H-benzoimidazol-2-ylmethyl）cyclohexane,was synthesized and characterized by X-ray single-crystal structure analysis.The complex crystallizes in triclinic,space group P1 with a = 9.1088（5）,b = 11.0075（4）,c = 14.2326（6）A,α = 97.188（3）,β = 96.394（4）,γ = 111.430（4）°,V = 1298.73（10） A^3,Z = 2,D_c = 1.409 g/cm^3,μ（Mo Kα） = 1.074 mm^-1,F（000） = 572,S = 1.078,R = 0.0381 and w R = 0.0876 for 5593 observed reflections with I 〉 2σ（I）.The central Cu（Ⅱ） ion adopts a distorted tetrahedral geometry coordinated by two nitrogen atoms of the ligand and two chloride ions.The complex showed its thermal decomposition temperature up to 226 ℃ and exhibited an irreversible one-electron transfer process involving Cu^Ⅱ/Cu^I couple.

Hydrothermal Synthesis and Crystal Structure of Binuclear Copper(Ⅱ) Complex Bridged by 1,2,4,5- Benzenetetracarboxylato Trivalent Anion

The title complex [(phen) 2Cu(Htcb)Cu(phen) 2]H 3tcb(tcb=1,2,4,5-benzenetetracarboxylato tetravalent anion; phen=1,10-phenanthroline) was synthesized by the hydrothermal synthesis method. The crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic system with space group P1, a=1.04174(8) nm, b=1.07119(8) nm, c=1.26360(10) nm, α=98.169(2)°, β=99.679(10)°, γ=93.658(10)°, V=1.37031(18) nm3, Z=1. The two copper(Ⅱ) cations are bridged by Htcb in the monodentate fashion, and have the same five-coordinated environment completed by the four N atoms from the two phen molecules and one O atom from the carboxylic group of Htcb respectively, which can be best described as distorted trigonal-bipyramid geometry. Moreover, the three dimensional network is formed by H-bonding interactions [O…O distance from 0.2506(10) nm to 0.3176(11) nm] and π-π stacking interactions between the phen rings of adjacent binuclear entities with a face-to-face separation of ca. 0.354 nm.

Synthesis and Crystal Structure of 2,4-Diiodo-6-[(2-morpholin-4-yl-ethylimino)-methyl]-phenol-copper(Ⅱ)

2,4-Diiodo-6-[（2-morpholin-4-yl-ethylimino）-methyl]-phenol-copper（Ⅱ） has been designed and synthesized.The structure was determined by UV,IR and single-crystal X-ray study.The title complex crystallizes in the triclinic system,space group P1 with a=6.6090（13）,b=10.377（2）,c=12.550（3）A,α=113.29（3）,β=93.84（3）,γ=98.31（3）°,V=774.9（3）A^3,Dc=2.215g/cm^3,C26H30CuO4N4I4,Mr=1033.68,F（000）=487,μ=4.726 mm^-1,Z=1,the final R=0.0563 and wR=0.1475 for 2101 observed reflections（I〉2σ（I））.The central copper（Ⅱ） is four-coordinated by two nitrogen atoms and two oxygen atoms from two 3,5-diiodosalicylaldehyde-2-morpholinoethylamine Schiff bases.The complex is linked into a column by π-π stacking interaction.The complex was 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 MTT method.Fortunately,the title complex shows potent antibacterial activity against these six bacterial strains.

Synthesis and Crystal Structure of a Dinuclear Complex:Bis[aqua(phen)(4-aba)copper(Ⅱ)nitrate(4-abaH)dihydrate]

The title complex has been obtained by the reaction of copper nitrate trihydrate with 4-abaH （4-abaH = 4-aminobenzonic acid） and phenanthroline in ethanol solution, and its structure was determined by X-ray crystallography with the following data： monoclinic, space group C2/c, M, = 1266.13, Cu2C52H54N10O20, a = 25.884（5）, b = 10.205（2）, c = 20.849（4） A, β= 106.34（3）°, Z= 4, V= 5284.7（18） A^3, F（000） = 2616, Dc = 1.591 g/cm^3, μ = 0.896 mm ^-1, the final R = 0.0441 and wR = 0.1148 for 4200 observed reflections （Ⅰ 〉 2σ（Ⅰ））. In the molecule of the title complex, the asymmetric unit contains one half molecule, The Cu（Ⅱ） atom is five-coordinated by a tenninal water molecule, a bidentate phcnanthroline and two monodentate 4-ammobenzoate ligands forming a square pyramidal coordination environment. The two bridging 4-aminobenzoate ligands result in a dinuclear copper（Ⅱ） cluster with a short Cu-Cu distance （3.048 A） and a π-π rstacking between the adjacent phenanthroline rings （2.96 A）.

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.

Synthesis and Crystal Structure of Bis(barbiturato)triwater Complex of Copper(Ⅱ)

The crystal structure of the bis(barbiturato)triwater copper(Ⅱ) complex formulated as Cu(barb)2(HO2)3 (barb = barbiturato) has been determined by single-crystal X-ray diffraction. The analysis was carried out by direct and Fourier methods and the structure was refined by full-matrix least-square computations. The title compound crystallizes in orthorhombic, space group Fdd2 with a = 11.691(1), b = 30.200(4), c = 7.1901(9) , V = 2538.7(5) 3, Z = 8, C8H12CuN4O9, Mr = 371.76, Dc = 1.945 g/cm3, m(MoKa) = 1.781 mm-1, F(000) = 1512, the final R = 0.0347 and wR = 0.0766 for 827 observed reflections (I > 2s(I)). The copper atom is square- pyramidally bonded to the exocyclic oxygen atoms of the barbital anions (CuO, 1.976(3)) and the water molecules (CuO, 1.926(4) and 2.164(7) ?. The molecules are held together to form an extensive three-dimensional network via OH贩稯 and NH贩稯 hydrogen-bonded contacts.

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.