Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of a New Dinuclear Copper Complex [C2H6ON]2[Cu2Cl2(μ-CH2COO)4]

The hydrothermal reaction of copper chloride dihydrate and 5,5-dimethyl-imi-dazolidine-2,4-dione with a mole ratio of 1:1 in acetonitrile resulted in the formation of a new acetate-bridged dinuelear copper complex, [C2H6ON]2[Cu2Cl2(μCH3COO)4]. Protonated aeetamide in enolic form and acetic acid were yielded by the hydrolysis of aeetonitrile under hydrothermal condition. The title complex (C12H24Cl2Cu2N2O10) was charactetized by X-ray single-crystal diffraction, IR spectrum, elemental and electrochemical analysis. It crystallizes in the monoclinie system, space group P21/c with a = 8.2980(14), b = 14.358(2), c = 12.0010(2) A,β= 130.620(3)°, V= 1085.3(2)A3, Dc = 1.696 g/am3, Mr = 554.31, Z = 2, F(000) = 564 and μ= 2.254 mm-1. The crystal structure consists of a tetraacetate-bridging dinulcear copper complex anion [Cu2Cl2(μ-CH3COO)4]2-, with the chlorine anions in the axial positions, and two protonated acetamide cations [C2H6ON]+, which were connected through hydrogen bonds to form a three-dimensional infinite network.     

Synthesis and Crystal Structure of a Novel Binuclear Copper（Ⅱ） Complex, [Cu（paba）Cl]

A novel binuclear Cu（Ⅱ） complex [Cu（paba）Cl] （pabaH = 2-（2-pyridylmethylimine）benzenesulfonic acid） has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of the title complex crystallizes in a monoclinic system, space group P21/n, with a = 6.8165（7）, b = 15.3073（16）, c = 12.3795（13） A^°, β= 95.0160（10）°, V= 1286.8（2） A^°^3, Mr = 360.26, Dc= 1.860 g/cm^3,μ = 2.074 mm^-1, F（000） = 724, Z = 4, the final R = 0.0252 and wR = 0.0675 for 2395 observed reflections with I 〉 20（I）. The title complex is centrosymmetric and a pair of chlorides act as μ2-bridges to link two Cu（Ⅱ） ions forming a binuclear complex. Every Cu（Ⅱ） ion is five-coordinated by pyridyl N, imine N and sulfonate O atoms of the tridentate paba ligand as well as two bridging Cl^-, constructing the distorted square-pyramidal geometry. In the structure extensive hydrogen bonds and weak π-π stacking stabilize the solid structures, through which the complex builds its 3-dimensional supramolecular structure.     

Dinuclear Copper（Ⅱ） Complex with a New Polycarboxylate Ligand：Syntheses,Characterization and Crystal Structure

A dinuclear copper(Ⅱ) complex,[Cu2(HL)2(H2O)6] 1(H3L = 2,4,6-tri(3-carboxy-phenylthio)-1,3,5-triazine),was synthesized hydrothermally and characterized by single-crystal X-ray diffraction,IR and thermal analysis.Single-crystal X-ray diffraction reveals that complex 1 is a dinuclear copper(Ⅱ) complex,which is further extended to a 3D network by weak interactions such as O…H-O hydrogen bonds and noncovalent S...S interactions.The crystal of compound 1 belongs to monoclinic,space group C2/c,with a = 50.15(2),b = 6.789(3),c =15.667(8) ,β = 90.588(9)o,V = 5334(4) 3,Z = 4,C48H38Cu2N6O18S6,Mr = 1306.28,Dc = 1.627 g/cm3,F(000) = 2664,Rint = 0.0631,T = 293(2) K,μ = 1.112 mm-1,the final R = 0.0661 and wR = 0.1850 for 3782 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of Dinuclear Copper Complex[Cu（CH2O（C6H4）N=C（C6H4）O）（Py]2

1 INTRODUCTION Synthesis of transition metal complexes with Schiff-base has been a subject of considerable importance [1,2]. They are not only good complexing agents for Schiff-base, but also good bactericide and antitumour agent [3,4]. At present, there is a spectacular growth in this field. Recently, some bridged binuclear complexes have received much attention on account of their biological relevance and condensed-phase magnetic properties[5,6]. Especially, the complexes containin…     

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 P1^- 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/cm^3, 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）.     

Hydrothermal Synthesis, Crystal Structure and Thermal Analysis of a Dinuclear Complex Cd2（3,5-Dinitrobenzoate）4（pyridine）4

A dinuclear complex Cd2(dnba)4(pyridine)4 (dnba = 3,5-dinitrobenzoate) has been synthesized by hydrothermal method and characterized by X-ray single-crystal diffraction, elemen- tal analysis, FT-IR spectroscopy, DSC and TG-DTG techniques. The complex with empirical formula C48H32Cd2N12O24 (Mr = 692.83) crystallizes in monoclinic, space group P21/n with a = 12.0344(14), b = 10.5752(13), c = 21.578(3) (A), β = 104.150(2)o, V = 2662.8(6) (A)3, Z = 2, Dc = 1.728 g/cm3, μ(MoKα) = 0.897 mm-1, F(000) = 1384, S = 1.016 and (Δ/σ)max = 0.001. R = 0.0638 and wR = 0.0737 for all data; the final R = 0.0337 and wR = 0.0644. In this complex, four carboxylates are bidentate- or chelate-coordinated with the Cd(Ⅱ) centers to give the dinuclear structure. The other coordination positions of Cd(Ⅱ) are occupied by the lone pair electrons from N of four pyridines. Thermal analyses DSC and TG-DTG have been used to determine the thermal decomposition mechanism of the title complex.     

Synthesis,Crystal Structure and Photoluminescent Properties of a New Dinuclear Copper（Ⅰ） Complex [Cu2（μ2-dppm）2（MeCN）2（μ2-MeCN）]（ClO4）2·MeCN

The title compound [Cu2（μ2-dppm）2（MeCN）2（μ2-MeCN）]（ClO4）2·MeCN （dppm = bis（diphenylphosphino）methane） has been prepared and characterized. It crystallizes in the monoclinic system,space group P21/n,with a = 11.904（6）,b = 20.755（11）,c = 24.744（13）A,β = 98.226（12）°,C58H56Cl2Cu2N4O8P4,Mr = 1258.93,V = 6051（5） A^3,Z = 4,Dc = 1.382 g/cm^3,μ = 9.52 mm^-1,F（000） = 2592,R = 0.0533 and wR = 0.1295 for 6175 observed reflections with I 〉 2σ（I）. Each Cu（I） center is tetrahedrally coordinated by two phosphine atoms from two bridging dppm ligands,one nitrogen atom from a terminally coordinated acetonitrile molecule,and another nitrogen atom from a μ2-acetonitrile molecule. The two Cu（I） centers are bridged by two dppm ligands as well as a unique acetonitrile molecule. The full molecule exhibits a ＇chair-like＇ configuration. This dinuclear complex exhibits intense or middle photoluminescence at room temperature in the solid state or actonitrile solution at 486 nm.     

Hydrothermal Synthesis and Crystal Structure of a Novel Hexanuclear Copper（Ⅱ） Complex：[Cu_6（DPPZ）_4（btc）_4（H_2O）_8]·5H_2O

A new hexanuclear copper(Ⅱ) complex,[Cu 6 (DPPZ) 4 (btc) 4 (H 2 O) 8 ]·5H 2 O (1,DPPZ=dipyrido[3,2-a:2,3-c]phenazine,H 3 btc=1,3,5-benzenetricarboxylic acid),has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analyses,IR,and thermogravimetric analysis.Its crystal structure is of triclinic system,space group P1 with a=12.489(4),b=14.234(5),c=14.484(5),α=82.848(4),β=79.399(4),γ=73.646(4)°,V=2421.2(13) 3,Z=1,Cu 6 C 108 H 78 N 16 O 37,M r=2573.17,D c=1.752 g/cm 3,μ=1.398 mm-1,F(000)=1308,GOOF=1.011,the final R=0.0495 and wR=0.1030 for 5420 observed reflections with I > 2σ(Ⅰ).In 1,four btc 3ligands act as bridges between six neighboring Cu atoms to form an unusual hexanuclear copper cluster.The clusters are further connected by two types of O-H···O and O-H···N hydrogen bonds,generating a three-dimensional supramolecular structure.In addition,intermolecular and intramolecular π-π stacking interactions further consolidate the three-dimensional supramolecular framework of 1.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Copper（Ⅱ） Complex

A metal-organic coordination polymer [Cu(cbba)2(bix)]n(Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid,bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis,IR,TG,UV and single-crystal X-ray diffraction.Blue crystals crystallize in the monoclinic system,space group C2/c with a = 26.127(3),b = 10.6143(14),c = 14.5676(19) ,β = 111.289(2),V = 3764.3(8) 3,C42H30Cl2CuN4O6,Mr = 821.14,Dc = 1.449 g/cm3,F(000) = 1684,Z = 4,μ(MoKα) = 0.777 mm 1,the final R = 0.0528 and wR = 0.1200 for 2241 observed reflections(I > 2(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

Hydrothermal Synthesis and Crystal Structure of a Polyoxometalate- based Complex [Cu^I（phen）2]4（SiW12O40）

A new hybrid polyoxometalate-based complex, [Cu^I（phen）214（SiW12O40） （phen = 1,10-phenanthroline）, has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallography analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data： a = 18.3574（14）, b = 21.1952（16）, c = 27.992（2）A, Mr = 4570.08, V = 10891.4（14）A^3, Z = 4, Dc = 2.787 g/cm^3,μ = 13.478 mm^-1, R = 0.0364, wR = 0.0638 （I 〉 2σ（I）） and F（000） = 8360. The complex consists of one α-Keggin anion [SIW12O40]^4- and four discrete [Cu^I（phen）2]^＋ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the ＋1 oxidation state.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Zn（phen）（m-CBA）2（H2O）

A novel complex Zn(phen)(m-CBA)2(H2O) with m-chlorobenzoic acid (m-CBA), 1,10-phenanthroline (phen) and zinc chloride has been hydrothermally synthesized and characterized. Crystal data for this complex: triclinic, space group P1, a = 0.8361(5), b = 1.2455(7), c = 1.3107(7) nm, α = 115.637(8), β = 91.014(9), γ = 104.857(8)o, V = 1.1763(11) nm3, Dc = 1.623 g/cm3, Z = 2, F(000) = 584, GOOF = 1.078, the final R = 0.0453 and wR = 0.1192. Structure analysis shows that the zinc ion coordinates with two nitrogen atoms of one 1,10-phenanthroline molecule, three oxygen atoms from two m-chlorobenzoic acid molecules and one water molecule, giving a distorted square-pyramidal coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

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.     

Synthesis and Crystal Structure of a New Diamine Complex CuC14（H2tn）

In an attempt to synthesize a new pyrimidine complex of copper(H) in a solution reaction of CuBr2 with 2,2‘-bis(hexahydropydmidine) and hydro-chloric acid, we unexpectedly obtained a bright yellow chip-like crystal of CuCl4(H2tn) [H2tn=(H3NCH2CH2CH2NH3)^2 ]. Its structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system, space group Pnma, with cell parameters: a=0.7216(2)nm, b=1.8308(6)nm, c=0.7553(3)nm, V=0.9953(6)nm^3, Z=4, F(000)=564, Mr=281.49, Dc=1.879 g/cm^3. u(Mo Ka)=3.204 mm^-1, R1=0.0248, wR2=0.0575. The analysis of the crystal structure indicates that the complex has a three-dimensional network structure, which is formed by hydrogen bonds and electrostatic interaction.     

Synthesis and Crystal Structure of a Dinuclear Complex of Cu（II） with Tetra（3,5-diphenyl pyrazole）

A Cu(II) complex of tetra(3,5-diphenyl pyrazole) [Cu(C15H12N2)2Cl2]2 (1) was synthesized, and its structure was determined by single-crystal X-ray diffraction and further characterized by elemental analysis, NMR and IR. 1 belongs to the monoclinic system, space group P21/c with a = 13.3780(5), b = 15.1392(6), c = 15.5923(6) , β = 124.522(2)°, Z = 2 and V = 2601.86(17) 3. In 1, each Cu2+ ion is coordinated with two N atoms from two tetra(3,5-diphenyl pyrazole) ligands and three Cl- anions to give a distorted square-pyramidal geometry, which is further linked through edge-sharing bridging by Cl- anions to form a centrosymmetric dinuclear structure.     

Synthesis and Crystal Structure of a Cu^2＋ Supramolecular Complex [Na2Cu（BTA）2（H2O）8]·H2O with a Three-dimensional Network Structure

A three-dimensional Cu^2＋ supramolecular complex [Na2Cu（BTA）2（H2O）8]·H2O 1 （H2BTA = bistetrazolylamine） was synthesized by reacting the aqueous solution of CuSO4·5H2O and H2BTA under stirring. The crystal structure of 1 was determined by single-crystal X-ray diffraction. The result indicates that 1 crystallizes in triclinic, space group P1, with a = 7.0518（2）, b = 12.2692（2）, c = 13.8583（3） A, α = 115.7260（10）,β = 93.2440（10）, γ = 98.3610（10）°, Mr = 573.90, V= 1059.01（4） A^3, Z = 2, De= 1.800 g·cm^-3,μ（MoKα） = 1.155 mm^-l, F（000） = 586.0, S = 1.074, the final R = 0.0273 and wR = 0.0744 for 4334 observed reflections with I 〉 2σ（I）. The Cu^2＋ ion is five-coordinated with a N4O1 donor set with r = 0.153 according to the method of Addison et al. And the Na^＋ ions form an infinite main chain through bridging O atoms from coordinated water molecules. In 1, a three-dimensional supratnolecular network is formed by O-H….O, O-H…N, N-H…O and N-H…N hydrogen bonds.     

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.     

Synthesis and Crystal Structure of a Dinuclear Compound Cu2[（O=PPh2）2N]2（μ-O2PPh2）2

1 INTRODUCTION Transition-metal complexes supported by poly-dentate phosphine ligands have been widely studieddue to the unique photophysical properties andpotential applications as industrial catalysts, mole-cular sensors and drugs[1~3]. As known, oxidation ofphosphine ligands could happen in the synthesisreaction to result in novel complex with unexpectedstructure[4, 5]. For example, the structure of complexFe((OPPh2)2N)3[6] is an octahedral tris-chelate arrange-ment of the oxidized a…     

Synthesis and Crystal Structure of the Copper（Ⅱ） Complex [Cu2Cl2（HEMDP）2]·THF

One dinuclear complex [Cu2Cl2(HEMDP) 2]·THF 1(H2EMDP = 2-[(2-hydroxyethylimino)-methyl]-4,6-diiodo-phenol,THF = tetrahydrofuran) has been designed and synthesized by H2EMDP with CuCl2·2H2O in THF solvent. Complex 1 was characterized by UV,IR,ESI-MS,and elemental analyses. 1 was characterized by X-ray crystallography. The crystal belongs to the monoclinic system,space group C2/c with a = 27.886(3) ,b = 8.6890(12) ,c = 26.698(2) ,β = 105.521(2) o,V = 6233.1(12) 3,Z = 8,Mr = 1102.01,μ = 5.533 mm-1,Dc = 2.349 Mg/m3,F(000) = 4112,the final R = 0.0486 and wR = 0.1175(I > 2σ(I)) . In addition,further investigation revealed that the central copper(Ⅱ) atom in the complex is five-coordinated by one nitrogen atom and two oxygen atoms from H2EMDP and two chlorine atoms from chlorid. The 3,5-diiodosalicylaldehyde Schiff base acts as a tridentate ligand. H2EMDP and 1 were assayed for antibacterial(B. subtilis,S. aureus,S. faecalis,P. aeruginosa,E. coli and E. cloacae) activities by MTT(3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl trtrazolium bromide) method. 1 showed the most favorable antimicrobial activity with MICs of 3.125,6.25,6.25,12.5,3.125 and 6.25 μg/mL against B. subtilis,S. aureus,S. faecalis,P. aeruginosa,E. coli and E.cloacae,respectively.     

Hydrothermal Synthesis and Crystal Structure of a Three-dimensional Cadmium（II） Complex

A metal-organic coordination polymer [Cd2(PDC)2(bix)(H2O)2]n ·nH2O(H2PDC=2,4-pyridinedicarboxylic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Brown crystals crystallize in the orthorhombic system, space group P2 12 12 1 with a=11.741(3), b=14.190(4), c=18.963(5) , V=3159.4(14) 3 , C28H26Cd2N6O11, Mr=847.35, Dc=1.781 g/cm3 , F(000)=1680, Z=4, μ(MoKα)=1.415 mm 1 , the final R=0.0381 and wR=0.0882 for 5472 observed reflections (I >2σ(I)). The structure of 1 exhibits a threedimensional network structure.