Hydrothermal Synthesis and Crystal Structure of a Copper Complex

The title compound [Cu(IB)2]n·n(H2O) 1 was synthesized via the hydrothermal reaction of CuSO4·5H2O and NaOH with 4-(1H-Imidazol-1-yl)benzoic acid(HIB),and character-rized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in monoclinic,space group C2/c with a = 14.349(7),b = 5.977(3),c = 21.368(9) ,β = 104.956(9)o,V = 1770.5(2)3,Z = 4,C20H16CuN4O5,Mr = 455.92,Dc = 1.710 g/cm3,F(000) = 932 and μ(MoKα) = 1.279 mm-1.The final R = 0.0337 and wR = 0.0888 for 1972 observed reflections with Ⅰ 2σ(Ⅰ) and R = 0.0369 and wR = 0.0926 for all data.X-ray diffraction reveals that the IB ligand links the Cu(Ⅱ) atoms into a double stranded chain.The extensive supramolecular interactions lead to the formation of an infinite 2D structure.     

Hydrothermal Synthesis,Crystal Structure and Magnetic Behavior of a Novel 3D Supramolecular Complex [Cu（HDPPZC）（SO4）（H2 O）]2

In the title coordination compound,[Cu(HDPPZC)(SO4)(H2O)]2 (1,HDPPZC=dipyrido[3,2-a:2,3-c]-phenazine-2-carboxylic acid),has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction,elemental analysis and magnetic susceptibility measurement.It crystallizes in triclinic,space group P1 with a=0.69485(6),b=0.76878(4),c=1.76638(13)nm,α=99.437(6),β=94.690(6),γ=95.735(6)o,V=0.92151(12) nm 3,Z=1,Cu2C38 H24 N 8S2O14,Mr=1007.85,Dc= 1.816 g·cm-3,F(000)=510,GOOF=0.988,the final R=0.0580 and wR=0.0689.The structural analyses reveal that complex 1 shows discrete dinuclear clusters,which are further linked by hydrogen bonding and π·π stacking interactions to form a three-dimensional supramolecular compound.Magnetic measurement shows ferromagnetic and antiferromagnetic exchange interactions in the sample.     

Synthesis,Crystal Structure and Biological Activity of a Novel Complex： Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-Triazole-yl）-6-chloro-pyridazine）

The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018（3）, b = 9.832（5）, c = 9.921（5）A, a = 78.270（8）, β = 74.550（8）, γ = 83.807（8）°, V = 553.1（5）A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F（000） = 281,μ（MoKα） = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ（I）. The Co（II） ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt（II） complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.     

二苯乙醇酸铜配合物的合成、晶体结构、电化学和荧光性质

以二苯乙醇酸为配体合成了1个新的化合物[Cu(2,2′-bipy)(BAA)][Cu(2,2′-bipy)(BAA)(H2O)]2.(H2O)3(BAA=二苯乙醇酸阴离子,2,2′-bipy=2,2′-联吡啶)。该化合物晶体属三斜晶系,空间群P1,晶胞参数:a=1.121 7(5)nm,b=1.360 2(6)nm,c=2.335 2(10)nm,α=99.260(6)°,β=101.223(8)°,γ=94.805(8)°,V=3.425(3)nm3,Dc=1.385 g.cm-3,Z=6,μ(Mo Kα)=0.992 mm-1,F(000)=1 474,最终偏离因子R1=0.0561,wR2=0.1128。在标题化合物的不对称单元中有3个单核铜(Ⅱ)配合物,且3个中心铜(Ⅱ)离子的配位数不完全相同,如Cu(1)离子的配位数是4,而Cu(2)和Cu(3)离子的配位数都是5。本文还测定了标题化合物的电化学性能和荧光性能,结果表明:在电化学过程中配合物的电子转移是准可逆的,电子转移数为2个;配合物在478 nm的光激发下可发射荧光。     

双环[2.2.2]辛-7-烯-2，3，5，6-四羧酸铜配合物的合成和晶体结构研究

以双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸(H4L)为配体,采用水热法合成了个铜配合物[Cu2L2(H2O)2](2),并得到单晶,同时在水热条件下得到了化合物H4L.2H2O(1)的晶体。分别对化合物1和2进行了元素分析、红外光谱等分析,并用X-射线单晶衍射测定了化合物的单晶结构。化合物1属于三斜晶系,P1空间群,化合物1的晶体学数据为:a=0.88554(15)nm,b=0.95566(16)nm,c=1.043 88(17)nm,α=110.863(3)°,β=91.127(3)°,γ=91.429(3)°,V=0.824 9(2)nm3,Z=2,Mr=366.32,Dc=1.475 g.cm-3,F(000)=388,μ=0.129,R1=0.067 0,wR2=0.189 3;配合物2属于正交晶系,Pnnm空间群,配合物2的晶体学数据为:a=2.766 8(6)nm,b=0.638 75(14)nm,c=0.737 32(16)nm,V=1.303 1(5)nm3,Z=4,Mr=442.31,Dc=2.254 g.cm-3,F(000)=884,μ=3.324,R1=0.059 4和wR2=0.191 7。化合物1通过氢键形成三维网状结构,配合物2中的中心离子有3种配位方式,通过不同的配位方式也形成三维结构。     

Synthesis,Crystal Structure and Antitumor Activity in Vitro of a New Benzoate Binuclear Cupper（ Ⅱ） Complex

The title compound, [Cu2（C7H5O2）4（C2H6O）2], was synthesized by the reaction of benzoic acid, copper acetate and ethanol in an aqueous solution. Trypan blue dye exclusion method was used in experiment. X-ray single-crystal analysis has revealed that compound 1 （C32H32Cu2O10） crystallizes in the monoclinic system, space group C2/c, Mr = 703.66, a = 47.340（5）, b = 6.6613（4）, c = 22.028（2）A,β = 113.284（4）°, V = 6380.6（10） A^3, Z = 8, Dc= 1.465 g/cm^3, F（000） = 2896,μ = 1.388 mm^-11, the final R = 0.0515 and wR = 0.1172 for 5712 observed reflections with I 〉 2σ（I）. X-ray crystal structure analysis suggests that compound [CH2（C7H5O2）4（C2H6O）2] has a binuclear structure with two Cu（II） atoms coordinated by four benzoate groups and two ethanol molecules. The crystal packing is stabilized by intermolecular O-H...O hydrogen bonds. The compound inhibits the proliferation of K562 cells （chronic myeloid leukemic cells） significantly and dose-dependently in 48 h, and IC50 of K562 is 17.3μg/mL by trypan blue dye exclusion method.     

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,Structure and Luminescent Properties of [Zn(btzb)2Cl2]·2H2O[btzb=1,2-Bis(5-tetrazolyl)benzene]

The title compound[Zn(btzb)2Cl2]·2H2O(1·2H2O,btzb=1,2-bis(5-tetrazolyl)benzene)was synthesized in situ by the[2 3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions.1·2H2O crystallizes in the monoclinic system,space group P21/c with a=9.0119(18),b=7.5566(15),c=18.076(5)(A),β=114.67(2)°,V=1118.6(4)(A)3,Z=2,Dc=1.784 g/cm3 T=223(2)K,C16H16N16O2Cl2Zn,Mr=600.74,F(000)=608,μ(MoKα)=1.393 mm-1,S=1.081,R=0.0306 and wR=0.0669 for 1896 observed reflections with Ⅰ ＞2σ(Ⅰ).The Zn2 ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms,forming a distorted octahedral coordination geometry.A number of intermolecular hydrogen bonding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure.The luminescent property of 1·2H2O was also investigated.     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

A 2-D Copper Coordination Polymer [Cu(4,4''''-bpy)(H_2O)_4](C_4H_2O_4)(H_2O)_4 Integrated by Hydrogen Bonds and VDW Interactions

1 INTRODUCTION A great deal of interest in transition metal com- plex assembly has recently been devoted to the development of rational synthetic routes to novel one-, two- and three-dimensional crystal frameworks, due to their potential applications in…     

Synthesis and Crystal Structure of Picrates of 3,5-Diamino-1,2,4-triazole

The title compound C2N5H6+C6N3O7H2-was synthesized by the reaction of 3,5-diamino-1,2,4-triazole and picric acid in the mixture of ethanol and water solution.Single crystals suitable for X-ray measurement were obtained at room temperature.The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis.Crystallographic data:C8N8H8O7,Mr = 328.22,monoclinic,space group C2/c with a = 22.815(2),b = 4.8086(5),c = 22.564(2),β = 93.976(2)°,V = 2469.6(4)3,Dc = 1.766 g/cm3,Z = 8,μ = 0.156 mm-1,F(000) = 1344,the final R= 0.0309,wR= 0.0864.     

A Three-dimensional Neodymium（Ⅲ）- potassium（Ⅰ） Coordination Polymer

The title compound [NdK（btec）（H2O）2]n 1 was synthesized via the hydrothermal reaction of Zn（OAc）E·H2O, Nd（NO3）3 and KOH with 1,2,4,5-benzenetetra-carboxylic acid （H4btec）, and characterized by elemental analysis and infrared spectra. The crystal of 1 crystallizes in monoclinic, space group P21/c with a = 8.9023（3）, b = 7.8954（1）, c = 17.6249（5）A,β= 91.857（1）°, V= 1238.16（6）A^3, Z = 4, C10H6KNdO10, Mr= 469.49, Dc = 2.519 g/cm^3, F（000） = 900 andμ（MoKa） = 4.585 mm^-1. The final R = 0.0404 and wR = 0.0832 for 2197 observed reflections with I 〉 2σ（I） and R = 0.0431 and wR = 0.0854 for all data. X-ray diffraction reveals that the btec ligand serves as a μ16-bridging ligand to link the Nd（Ⅲ） and K（Ⅰ） atoms into a three-dimensional coordination polymer. Photoluminescent investigation shows that the title compound displays strong emission in the blue region, which may be attributed to an intraligand emission state.     

A Three-dimensional Neodymium(III)-potassium(I) Coordination Polymer

The title compound [NdK(btec)(H2O)2]n 1 was synthesized via the hydrothermal reaction of Zn(OAc)2·H2O, Nd(NO3)3 and KOH with 1,2,4,5-benzenetetra-carboxylic acid (H4btec), and characterized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in monoclinic, space group P21/c with a = 8.9023(3), b = 7.8954(1), c = 17.6249(5)A, β = 91.857(1)o, V = 1238.16(6) -3, Z = 4, C10H6KNdO10, Mr = 469.49, Dc = 2.519 g/cm3, F(000) = 900 and μ(MoKα) = 4.585 mm-1.The final R = 0.0404 and wR = 0.0832 for 2197 observed reflections with I > 2σ(I) and R = 0.0431 and wR = 0.0854 for all data.X-ray diffraction reveals that the btec ligand serves as a (16-bridging ligand to link the Nd(III) and K(I) atoms into a three-dimensional coordination polymer.Photoluminescent investigation shows that the title compound displays strong emission in the blue region, which may be attributed to an intraligand emission state.     

A Novel Hybrid Solid Constructed from Tetramolybdate and Copper Complexes with Mixed Ligands: [{(Cu·phen)_2(tp)}{(Cu·phen·H_2O)_2(tp)}{Mo_4O_(14)}]

A novel copper molybdate with mixed ligands, [{(Cu·phen)2(tp)}{(Cu·phen·H2O)2(tp)}{Mo4O14}] (phen = 1,10-phenanthroline, tp = terephthalate) 1, has been hydrothermally synthesized and structurally characterized. The crystal belongs to monoclinic system, space group P21/c with a = 13.1711(7), b = 19.6132(10), c = 13.6910(7) , β = 117.6870(10)°, V = 3131.8(3) 3, Z = 2, C64H44Cu4Mo4N8O24, Mr = 1946.99, Dc = 2.065 g/cm3, F(000) = 1920, μ(MoKα) = 2.198 mm-1, R = 0.0810 and wR = 0.2012 for 4233 observed reflections (I > 2σ(I)). The structural analysis indicates that the title compound contains a discrete tetramolybdate cluster decorated with copper complex fragments and tp ligands bridging the clusters into a wave-like layer. The hydrogen bond- ing between adjacent layers further extends the compound into a 3-D framework.     

Synthesis and Crystal Structur of (4,4''-H2bipy)[CdBr4]·H2O

The title compound (4,4'-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoelinic,space group P21/c with a=8.260(3), b=23.926(7), c=9.774(2) (A), β=106.777(9)°,C10H12Br4CdN2O, Mr=608.26, V=1849.4(9)(A)3, Z=4, Dc=2.185 g/cm3, S=1.005, μ(MoKα)=9.814 mm-1, F(000)=1128, R=0.0646 and wR=0.0989. The crystal structure analysis of 1reveals that the title compound features an isolated structure, based on discrete 4,4'-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetrahedral cadmium atoms terminally coordinated by four bromine atoms.     

Synthesis and Supramolecular Structure of Chloro（1,10-phenanthroline ）copper（I） Hexahydrate

1INTRODUCTION Atom transfer radical addition is an efficient me-thod for carbon-carbon bond formation in organic synthesis[1,2].In some of these reactions,a transi-tion-metal catalyst acts as a carrier of the halogen atom in a reversible redox process.The transition-metal-catalyzed has been successfully used to con-trol radical polymerization[3].In the process,the transition-metal species initially abstracts halogen atom X from organic halide to form oxidized species and carbon-centered r…     

Synthesis, Crystal Structure, and Biological Activity of Naphthalen-2-y1-4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-y1-4-methy1-1,2,3-thiadiazole-5-carboxylate(C14H10N2O2S,Mr = 270.31)was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a = 23.475(5),b = 9.6640(19),c = 10.814(2)(A°),β = 90.00°,Z= 8,V= 2453.2(9)(A°)3,Mr = 270.30,Dc = 1.464 g/cm3,μ= 0.262 mm-1,F(000)= 1120,R = 0.0444 and wR = 0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while,the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6)-H(6)…O(1)and C(14)-H(14)…O(1)were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.     

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

A new Cu(Ⅱ) complex [Cu(4-cba)(l,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 P1, a = 7.8420(2), b = 9.1070(2), c = 15.1140(6) A,α=76.889(9), β = 81.332( 11 ), γ = 74.844(11 )°, V = 1009.89(5) A3, Z = 2, Dc = 1.605 g/cm3, F(000)=498,μ=1.134 mm-1,the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with I ＞ 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.     

Synthesis and Crystal Structure of a One-dimensional Silver(Ⅰ) Coordination Polymer with 4,4'-Bipyridine

The title compound,{[Ag2(bipy)2(H2O2]·pydc·2H2O}n(bipy=4,4'-bipyridine,pydc=pyridine-3,5-dicarboxylate),has been synthesized by the reaction of Ag2O with pydc and bipy in CH3OH solution.It crystallizes in the monoclinic system,space group C2/c with a=21.419(8),b=7.515(3),c=18.070(7)(A),β=108.273(6)°,Mr=765.27,V=2761.9(17)(A)3,Z=4,Dc=1.840 g/cm3,F(000)=1528,μ=1.478 mm-1,the final R=0.0307 and wR=0.0681.The structure determined demonstrated that the Ag(Ⅰ)is three-coordinated by two nitrogen atoms from bipy and one water molecule,forming a one-dimensional coordination polymer[Ag2(bipy)2(H2O)2]n2n ,which is further linked to generate a two-dimensional layer structure via Ag…Ag attractions.     

Synthesis and Crystal Structure of [Cu3（dmpzm）4（μ-1, 3-dca）2（dca）4]·2H2O （dmpzm = 1,1＇-Methylenebis- （3,5-dimethyl-1H-pyrazole）, dca = dicyanamide）

The title compound, [Cu3（dmpzm）4（μ-1,3-dca）2（dca）4]·2H2O （dmpzm = 1,1＇-methylenebis（3,5-dimethyl-lH-pyrazole）, dca = dicyanamide） 1·2H2O, was synthesized via the reaction of CuCl2·2H2O with dmpzm and Na（dca）, and characterized by elemental analysis and IR spectra. 1·2H2O crystallizes in the monoclinic system, space group C2/m with a = 13.578（3）, b = 16.769（3）, c = 14.769（3） A, β = 104.10（3）° V = 3261.4（11） A^3, Z = 2, Dc = 1.466 g/cm^3, T = 153（2） K, C56H68N34O2Cu3, Mr = 1440.09, F（000） = 1490,μ（MoKa） = 1.040 mm^-1, S = 1.150, R = 0.0553 and wR = 0.1123 for 2744 observed reflections with I 〉 2σ（I）. The central copper atom is chelated by two dmpzm ligands and coordinated by two bridging dca anions, forming a slightly distorted octahedral geometry. The two external copper atoms adopt a square-pyramidal coordination geometry, coordinated by one chelating dmpzm ligand and one bridging and two terminal dca anions. Two intermolecular hydrogen bonding interactions result in the formation of a 2D （4,4） hydrogen-bonded network.