Synthesis and Crystal Structure of an Acetate Radical Bridged Dinuclear Copper(Ⅱ) Complex

A new acetate radical bridged dinuclear copper(Ⅱ ) complex (C8H9NO2)2-Cu2(CH3COO)4 has been synthesized by the reaction of Cu(OAc)2 with pyridine-3-ethyl formate and further characterized by X-ray single-crystal diffraction. Crystal data for the title compound: triclinic system,space group P1,with a=8.1654(14),b=9.7010(16),c=9.9005(17) ,α= 83.266(2),β=78.887(2),γ=72.881(2)o,V=733.9(2) 3,Mr=665.58,Z=1,Dc=1.506 g/cm3,F(000)=342,μ=1.510 mm-1,the final R=0.0392 and wR=0.1005. According to the structural determination,each unit of the title compound is composed of two Cu(Ⅱ) atoms,two pyridine-3-ethyl formate molecules and four acetate ions. Each Cu(Ⅱ) coordinates to oxygen atoms of acetate and nitrogen atoms of pyridine-3-ethyl formate ligand to give a six-coordinate distorted octahedral geometry. It is worth mentioning that strong Cu–Cu bond can be observed in the title compound.     

A New Dinuclear Cu(Ⅱ) Complex of a Ligand with Benzimidazole Group─Synthesis and Crystal Structure

A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2 (C18H22Cl4Cu2N6), has been synthe- sized and characterized by X-ray structure determination. It crystallizes in the triclinic P1 space group with a = 7.526(3), b = 9.473(4), c = 9.535(3) , α = 117.214(10), β = 108.251(9), γ = 91.560(6)o, V = 562.3(4) 3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm3, μ(MoKα) = 2.385 mm-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(II) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(II)-Cu(II) binuclear entity with the distance between two copper(II) atoms of 3.398 .     

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 MgCl_2(CH_3COOC_2H_5)_2

The crystal of the title compound was prepared and its structure determined by X-ray diffraction method.1672 independent reflections were collected. The crystal is orthogonal with space group P2_12_12, and a=7.353(3),b=25.111(10), c=8.631(2), Z=8. The structure was solved by using Patterson method and modified with LSM program.The final R= 0.0795. The structural features of the title compound are:Mg(Ⅱ) is octahedral and ethyl acetate is located on trans-position.Mg atoms are connected by double chloro-bridge and form polychains.     

Synthesis and Crystal Structure of N-(Biphenyl-2-thiocarbamoyl)-4-(1,3-dichlorophenyl) Carboxamide

The synthesis of the title molecule was achieved by the reaction of 2,4-dichlorobenzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13 C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) , β = 105.723(4)°, V = 1868.5(5) 3 and Z = 4.     

Synthesis,Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)-carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro- penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) , α = 75.311(4), β = 82.695(4), γ = 77.143(4)o, Z = 2, V = 847.9(3) 3, Dc = 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 ). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders. Keywords: α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopropenyl, preparation, crystal structure, DNA binding     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C_(13)H_9N_2O)Cl]_2·(CH_3CN)_2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2), has been synthesized and characterized by X-ray structure determination. It crystallizes in the tricli- nic system, space group P1, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) , α = 81.338(3), β = 88.173(4), γ = 66.199(3)o, V = 718.9(2) 3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3, μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions, and one chlorine atom). Two copper(II) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(II)–Cu(II) binuclear entity, and the distance between two copper(II) atoms is 3.0144(15) .     

Synthesis and Structure Characterization of a Tetranuclear Manganese(Ⅲ) Complex:[Mn_4O_2(O_2CMe)_6(MeOH)_2(dbm)_2]·2MeCOOH·2CH_2Cl_2

The title compound, [Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2 (Hdbm = dibenzoylmethane), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1, with a = 10.729(3), b = 12.269(3), c = 13.085(4) , α = 106.367(3), β = 107.643(2), γ = 94.771(2)o, V = 1547.9(7) 3, Z = 1, C50H64Cl4Mn4O24, Mr = 1410.57, Dc = 1.513 g/cm3, F(000) = 724, Rint = 0.0147, T = 293(2) K and μ = 1.046 mm–1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with I > 2σ(I). The structure of the complex consists of one [Mn4(μ3-O)2]8+ core with four coplanar Mn atoms disposed in an extended “butterfly-like” arrangement and two O atoms triply bridging each “wing”, and the peripheral ligation is provided by six μ2-MeCO2– , two terminal μ2-dbm– groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms. Intermolecular O…H–O hydrogen bonding interactions are found within the structure of the compound.     

Synthesis, Crystal Structure and Catalytic Behavior of 1-Ethyl-3-benyl-imidazolyl Tetranuclear N-Heterocyclic Carbene Silver Bromide

The title complex [Ag(carbene)2]2[Ag2Br4] has been synthesized by the reaction of Ag2O with 1-ethyl-3-benyl-imidazolium bromide in DMSO at room temperature, and characterized by elemental analysis, 1H NMR and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P with a = 10.1597(10), b =11.0646(11), c = 13.0245(14) , α = 102.230(2), β = 90.606, γ = 113.9250(10)o, V = 1300.3(2) 3, Mr = 748.06, Z = 2, Dc = 1.911 g/cm3, μ(MoKα) = 4.60 mm-1 and F(000) = 728. The structure was refined to R = 0.0316 and wR = 0.0835 for 3744 observed reflections with I > 2σ(I). The title compound crystallizes as a centrosymmetric tetranuclear compound. One half of the molecule comprises the asymmetric unit of the structure. The Ag(1) atom is nearly linear or T-shaped when the Ag(1)-Ag(2) interaction is taken into consideration, which is bi-coordinated by two carbene carbon atoms. The Ag(2) atom adopts tetrahedral geometry. The catalytic behavior of the title complex has been investigated, and the results indicate it has a highly catalytic activation for L-lactide polymerization.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

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-diphenylhydantoin, 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) , β = 98.762(2)o, V = 8098.8(16) 3, Dc = 1.429 Mg/m3, Z = 4, F(000) = 3640, μ = 1.107 mm-1, R = 0.0560 and wR = 0.1276(I 2(I)). 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 {Cu2O2} 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.     

A New Dinuclear Cu(Ⅱ) Complex of a Ligand with Benzimidazole Group - Synthesis and Crystal Structure

A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2(C18H22Cl4Cu2N6), has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic P-1 space group with a = 7.526(3), b = 9.473(4), c = 9.535(3)(A), α = 117.214(10), β = 108.251(9), γ = 91.560(6)°, V = 562.3(4)(A)3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm3, μ(MoKα) = 2.385 mm-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (Ⅰ＞ 2σ(Ⅰ)). In the title complex, each copper(Ⅱ) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(Ⅱ) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(Ⅱ)-Cu(Ⅱ) binuclear entity with the distance between two copper(Ⅱ) atoms of 3.398 (A).     

A Dinuclear Cu(Ⅱ)-based Coordination Framework with Two-fold Interpenetrated 3D pcu Topology Displaying Catalytic Activity

A new Cu(Ⅱ) coordination polymer, [Cu2(mip)2(bmix)]n(bmix = 1,4-bis(2-methylimidazole-1-ylmethyl)benzene, H2 mip = 5-methylisophthalic acid), has been hydrothermally synthesized and characterized by elemental analyses, IR, TGA and single-crystal X-ray diffraction. The title compound belongs to the triclinic system, space group P1 with a = 9.435(5), b = 12.241(6), c = 13.666(6), β = 94.396(8)o, V = 1565.5(13) 3, Z = 2, C34H30Cu2N4O8, Mr = 749.70, Dc = 1.590 g/cm3, μ = 1.419 mm-1 and F(000) = 768. The title metal-organic coordination polymer exhibits the first two-fold interpenetrated pcu topological structure assembled by two types of dinuclear copper(Ⅱ) clusters and a flexible bis(imidazole)-based ligand. In addition, the fluorescence and catalytic performances of the complex for the degradation of Congo red azo dye in Fenton-like process were presented.     

Synthesis and Crystal Structure of a 1D Coordination Polymer: {[Cu(HSSA)(py) 3]·H2O}n (H3SSA=5-Sulfosalicylic Acid, py=Pyridine)

The title compound [Cu(HSSA)(py)3H2O]n (H3SSA = 5-sulfosalicylic acid,py = pyridine) Ⅰ has been synthesized and structurally determined by single-crystal X-ray diffraction. Ⅰ was further characterized by elemental analyses,thermogravimetric analyses,IR and UV-visible spectroscopy. The crystal belongs to the monoclinic system,space group P21/c with a = 9.4564(10),b = 18.2679(19),c = 15.7284(12) ,β = 126.045(4)o,V = 2196.9(4) 3,Z = 4,Dc = 1.618 g/cm3,Mr = 535.02,μ = 1.141 mm-1,F(000) = 1100,λ(MoKα) = 0.71073 ,the final R = 0.0429 and wR = 0.1044 for all observed reflections. In the structure,every two Cu(Ⅱ) atoms are bridged by a bivalent 5-sulfosalicylic anion to form a 1D chain-like coordination polymer. Lattice waters between chains link them to form 2D layers which are further linked by C-H···O hydrogen bonds to form a three-dimensional supramolecular network.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.     

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 4-Oxo-1,2,4-triazino[4,5-a]benzimidazole

The title compound 4-oxo-1,2,4-triazino[4,5-a]benzimidazole(C9H6N4O,Mr = 186.18) has been synthesized and structurally characterized by IR,NMR and single-crystal X-ray diffraction. The crystal belongs to monoclinic,space group P21/c,with a = 9.1530(18) ,b = 7.2260(14),c = 12.604(3) ,β = 106.92(3) ,V = 797.5(3) 3,Z = 4,Dc = 1.551 g/cm3,λ(MoKa) = 0.71073,F(000) = 384,μ(MoKa) = 0.109 mm-1,the final R = 0.0632 and wR = 0.1095. A total of 1444 unique reflections were collected,of which 767 with I > 2σ(I) were observed. The structure of the title compound is planar. In packing,the molecules are intersected to each other to form chains along three dimensions,together by intermolecular N-H…O and C-H…N hydrogen bonds. The whole structure is further stabilized by π…π interaction between two adjacent tricyclic ring systems,with the centroid-to-centroid distance of 3.369(4) .     

Synthesis,Crystal and Electronic Structure of Ba_3ZnSb_2O_9 with the 6H-perovskite-type Structure

Crystals of Ba3ZnSb2O9 have been grown by a high-temperature solid-state reaction and characterized by single-crystal X-ray diffraction.Ba3ZnSb2O9 crystallizes in the hexagonal P63/mmc space group with a = 5.8663(4),c = 14.478(2) ,V = 431.49(8) 3,Z = 2 and R(all data) = 0.0167.The structure of Ba3ZnSb2O9 consists of pairs of face-sharing Sb2O9 bi-octahedra connected via corners with two single layers of mutually isolated ZnO6 octahedra.Each Ba2+ ion is bonded to 12 oxygen atoms.The UV-vis absorption spectrum of the compound has been investigated.Additionally,the calculations of band structure and density of states have also been performed with density functional theory method.The obtained results tend to support the experimental data of the absorption spectrum.     

Urothermal Synthesis and Crystal Structure of a Zn（Ⅱ） Coordination Polymer with a 3-D Supramolecular Structure

A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I >2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).     

Synthesis and Structural Characterization of Co( Ⅱ ) Coordination Polymer [Co(μ-phth)(imi)2]n

A new cobalt( Ⅱ ) complex [Co(μ-phth)(imi)2]n (phth = o-phthalato, imi = imidazole)has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group Pn with a = 8.405(1), b = 9.995(1), c = 9.996(2) (A),β= 104.479(2),V= 813.0(2) (A)3, Dc= 1.467 g/cm3, C14H12N4O4Co, Mr= 359.21, F(000) = 366,μ = 1.079 mm-1, Z = 2, R = 0.0483 and wR = 0.1209 for 1583 observed reflections (Ⅰ＞ 2σ(Ⅰ)). In the title complex, the Co(Ⅱ) ions are bridged by o-phthalate ligands in a bidentate mode, producing a zigzag infinite chain structure. Each four-coordinated cobalt( Ⅱ ) center was coordinated by two oxygen atoms and two nitrogen atoms to give a distorted tetrahedral geometry. The chains are linked by hydrogen bonds between oxygen atoms belonging to carboxylate groups and hydrogen atoms of imidazole molecules, forming an unusual two-dimensional coordination polymer.