A new chain-like coordination polymer, namely, [CuL]n (1, Na2L = 2-[(2-hydroxy- benzylidene)-amino]-benzenesulfonic acid sodium salt), has been synthesized and characterized by single-crystal X-ray diffraction, IR...A new chain-like coordination polymer, namely, [CuL]n (1, Na2L = 2-[(2-hydroxy- benzylidene)-amino]-benzenesulfonic acid sodium salt), has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy and elemental analysis. Complex 1 crystallizes in monoclinic system, space group P21/c with a = 9.2296(16), b = 10.4754(18), c = 12.200(2) A, β = 102.392(2)°, V = 1152.0(3)A3, CI3H9CuNOaN, Mr = 338.83, Dc = 1.953 g/cm3, Z = 4, F(000) = 684, p = 2.089 mm-1, the final R = 0.0376 and wR = 0.0956. X-ray diffraction analyses indicate that 1 displays a square-pyramidal metal center with NO4 donor sets. The sulfonate-derived Schiff base serves as a common N,O,O'-tridentate and a unique O-bridged ligand connecting the metals. Dinuclear copper complexes serve as secondary building blocks (SBUs) to construct an unusual 2D coordination network. In the crystal, the components form a stable 3D supramolecular architecture by C-H...O interactions and to-stacking展开更多
A copper(Ⅱ) complex [LCu2Cl4]n was synthesized by a new bis-Schiff base ligand containing quinoline unit, 1,4-bis[2-(4-fluorophenyl)iminomethyl-8-quinolinoxy]butane(L). X-ray crystal structure shows that it is ...A copper(Ⅱ) complex [LCu2Cl4]n was synthesized by a new bis-Schiff base ligand containing quinoline unit, 1,4-bis[2-(4-fluorophenyl)iminomethyl-8-quinolinoxy]butane(L). X-ray crystal structure shows that it is a binuclear complex, and the crystal belongs to the triclinic system, space group P1, with a = 9.387(2), b = 9.968(2), c = 10.291(2) ?, α = 87.532(3), β = 63.762(2), γ = 86.628(3)o, V = 862.1(3) ?^3, Z = 1, Dc = 1.640 Mg/m^3, F(000) = 428, R = 0.0416 and wR = 0.1141. Each Cu(Ⅱ) metal ion coordinates with a quinoline N atom, an imine N atom, an ether oxygen atom and three chlorides, forming a distorted six-coordinated octahedronal structure. Each copper(Ⅱ) complexation unit links with one of the adjacent ligand copper complexation units through the chlorido bridging groups, thus generating an infinite one-dimensional chain structure. Such 1D chains further construct a 2D network structure by π-π stacking interactions.展开更多
The title compound [Cu(bix)2(NO3)z·H2P]n 1 (bix = 1,4-bis(imidazole-1-ylme-thyl) benzene) has been synthesized by hydrothermal method. Its crystal structure is of monoclinic, space group P1^- with a = 8.3...The title compound [Cu(bix)2(NO3)z·H2P]n 1 (bix = 1,4-bis(imidazole-1-ylme-thyl) benzene) has been synthesized by hydrothermal method. Its crystal structure is of monoclinic, space group P1^- with a = 8.3075(13), b = 9.4725(13), c = 10.0192(13) A, α = 91.088(4), β = 104.063(6), γ = 101.88(1), V = 746.5(3) A^3, Z = 1, C28H30N10O7Cu1, Mr = 682.16, Dc = 1.518 g/cm^3, μ = 0.796 mm^-1, F(000) = 353, the final R = 0.0535 and wR = 0.0996 for 2921 observed reflections with I 〉 2σ(I). Each bix ligand binds two Cu(Ⅱ) ions to form a 2-D(4,4) square grid layer, which is connected by hydrogen bonds showing large channels occupied by solvated water molecules and nitrate anions.展开更多
The title compound, [Cu(C6H4N2O4F)2(H2O)4].4(H2O) I, has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in monoclinic, space group P21/c w...The title compound, [Cu(C6H4N2O4F)2(H2O)4].4(H2O) I, has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in monoclinic, space group P21/c with a = 8.3041(17), b = 12.045(2), c = 11.077(2) A, β = 92.567(3)°, V= 1106.8(4) A^3, Mr = 581.89, Z= 2, Dc = 1.746 g/cm^3, F(000) = 598,μ(MoKa) = 1.090 mm^-1, the final R = 0.0296 and wR = 0.0806 for 3195 observed reflections with Ⅰ 〉 2σ(Ⅰ). In the centrosymmetric compound I, each Cu(Ⅱ) ion is coordinated by six O atoms from two 5-fluorouracil-1-acetate anions and four water molecules, forming a six-coordinated octahedral environment. N-H…O and O-H…O hydrogen-bonding interactions are observed in the structure, leading to the formation of a three-dimensional network.展开更多
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 characteriz...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.展开更多
A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and d...A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3)A, β= 95.33(3)°, V = 1599.0(5)A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I 〉2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.展开更多
A novel supramolecular adduct 3(C 42H 42N 28O 14) 2·H 2O (1) was synthesized by mixing 2- and cucurbit uril in solution of hydrochloric acid. The crystal structure was determined by single crys...A novel supramolecular adduct 3(C 42H 42N 28O 14) 2·H 2O (1) was synthesized by mixing 2- and cucurbit uril in solution of hydrochloric acid. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system and space group F dd2 with cell dimensions: a=4.705 33 (5) nm, b=7.153 80 (6) nm, c= 1.894 61 (2) nm, Z=16, V=63.7744 (11) nm3, D c= 1.534 g/cm3, μ=3.007 mm -1, F(000)=29 120, R 1= 0.070 7, wR 2=0.169 2. In crystal, the cucurb uril molecules form two zig-zag chains.展开更多
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...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.展开更多
A new copper(Ⅱ) complex with formula CuL(py), where L^2- is the dianion of 2,4-dihydroxybenzylidene benzoylhydrazone, has been synthesized and characterized by IR spectra and single-crystal X-ray diffraction meth...A new copper(Ⅱ) complex with formula CuL(py), where L^2- is the dianion of 2,4-dihydroxybenzylidene benzoylhydrazone, has been synthesized and characterized by IR spectra and single-crystal X-ray diffraction method. The crystal belongs to monoclinic, space group P2 1/c with a=0.9630(4), b=1.4808(6), c=1.2320(5) nm, β=104.969(6)°, V=1.6973(Ⅱ) nm^3, Z=4, Dc=1.553 g/cm^3,μ(MoKa)=1.311 mm^-1, F(000)=812, R=0.0694 and wR=0.1727 for 1511 observed reflections (I〉2σ(I)). The crystal structure analysis indicates that the copper(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom from the tridentate acylhydrazone Schiff base ligand L^2- and one nitrogen atom from the pyridine ligand. Two adjacent molecules are connected via weak Cu…O bonding interactions to form dimers, which are further linked to generate a two-dimensional layer structure via interdimeric hydrogen bonds.展开更多
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 ana...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).展开更多
The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H1...The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?展开更多
To obtain advanced quality pure copper, the microstructure of solidified copper was optimized by imposing electric pulse on liquid copper in this study. Experiments were performed to determine the effect of electric p...To obtain advanced quality pure copper, the microstructure of solidified copper was optimized by imposing electric pulse on liquid copper in this study. Experiments were performed to determine the effect of electric pulse voltage, arrangement mode of electrodes, and energy input on the microstructure of solidified copper. The results show that, when the energy input of electric pulse is bigger than 28.95 kJ per ton copper, the percent of fine grains increases noticeably with the increase of energy input; but when the energy input of electric pulse is smaller than 28.95 kJ per ton copper, the percent of fine grains decreases with the increase of energy input. The influence order of above factors on grain refinement is electric pulse voltage 〉 arrangement mode of electrodes 〉 energy input. According to the above experimental results, the optimum process conditions are chosen as the voltage being 400 V and the energy input greater than 28.95 kJ per ton copper. Meanwhile, the best arrangement mode of electrodes should be that, one electrode is immerged in the middle of liquid copper in the crystallizer, and the other is connected to the inner wall of the crystallizer, which is divided into two electrode poles for the symmetrical electric field distribution.展开更多
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...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.展开更多
A new coordination polymer [Cu2(OH)(nbta)(tib)(H2 O)2]n(1, H3 nbta = 5-nitro-1,2,3-benzenetricarboxylic acid, tib = 1-(4 H-1,2,4-triazol-4-yl)-4-(imidazol-1-yl)benzene) constructed from dimeric Cu(Ⅱ) units has been s...A new coordination polymer [Cu2(OH)(nbta)(tib)(H2 O)2]n(1, H3 nbta = 5-nitro-1,2,3-benzenetricarboxylic acid, tib = 1-(4 H-1,2,4-triazol-4-yl)-4-(imidazol-1-yl)benzene) constructed from dimeric Cu(Ⅱ) units has been synthesized under hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction analysis. The compound crystallizes in monoclinic system, space group I2/c, with a = 17.8474(9), b = 11.7588(6), c = 21.9221(11) ?, β = 104.419(5)°, V = 4455.7(4) ?3 and Z = 8. Compound 1 is a three-dimensional structure constructed from dimeric Cu(Ⅱ) units and presents a 2-nodal(3,5)-connected net. Moreover, the thermal stability and solid UV-Vis absorption spectra have been investigated.展开更多
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 stru...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.展开更多
The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ) complex [Cu(L)(py)]2 2 (L = C10H11O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine) with mixed ligand have been s...The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ) complex [Cu(L)(py)]2 2 (L = C10H11O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine) with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1: orthorhombic, space group Pbca with a = 11.921(4), b = 15.816(6), c = 17.076(6) A, V= 3219.7(19) A^3, C15H17CuN3O5S, Z = 8, Mr = 414.92, De = 1.712 g/cm^3,μ(MoKα) = 1.520 mm^-1, F(000) = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I 〉 2σ(I); and crystal data for 2: monoclinic, space group P21/c with a = 7.929(3), b = 17.038(5), c = 11.734(4) A, β = 98.162(6)°, V = 1569.1(9) A^3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm^3, F(000) = 820,μ(MoKα) = 1.554 mm^-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections (I 〉 2σ(I)). The molecular structure of complex 1 consists of one tetra-coordinated Cu(Ⅱ) atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper(Ⅱ) structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.展开更多
A novel hexanuclear copper-indium thiolate complex, [(InCl)2(OMe)(μ-OMe)2(μ- OMe)(μ-SPrn)2(CuPPh3)]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu(Me- CN)a][PF6] in the presence of Ph3...A novel hexanuclear copper-indium thiolate complex, [(InCl)2(OMe)(μ-OMe)2(μ- OMe)(μ-SPrn)2(CuPPh3)]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu(Me- CN)a][PF6] in the presence of Ph3P and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P211n with a = 11.3533(8), b = 15.4939(11), c = 20.5189(14) A, β = 98.577(2)°, V = 3569.0(4) A3, Z = 2, C56H82Cl4Cu2In4O8P2S4, Mr = 1801.56, Dc = 1.676 g/cm3,μ(MoKa) = 2.213 mm^-1, F(000) = 1796, S = 0.985, the final R = 0.0559 and wR = 0.1099 for 8878 observed reflections with I 〉 2σ(I) and 367 variables. Complex 1 consists of two CuPPh3 fragments which symmetrically side-attach to the tetranuclear core of [InaCl4(OMe)2(μ-OMe)a(μ- OMe)2(μ-SPrn)4] by coordinating with sulfur atoms of propane-thio moieties. The average In-Ot (terminal), In-μ-O and In-μ3-O bond distances are 2.305(4), 2.144(4) and 2.294(4) A, respectively.展开更多
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 ...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).展开更多
A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n(1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characteriz...A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n(1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [Cu N3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data: monoclinic, space group C2/c, a = 17.8599(15), b = 8.2889(5), c = 14.8076(14) A, β = 113.2580(10)o, V = 2014.0(3) A3, Z = 8, S = 1.025, the final R = 0.0303, w R = 0.0825 for 1460 observed reflections with I 2σ(I) and R = 0.0386, wR = 0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.展开更多
A binuclear complex including ferrocenyl, Cu2{Fe(C5H5)[C5H4CH2N(CH3)2]}2 (CH3COO)4, was synthesized and characterized by X-ray diffraction. The title complex crystallizes in triclinic, space group P with a = 8.2779(8...A binuclear complex including ferrocenyl, Cu2{Fe(C5H5)[C5H4CH2N(CH3)2]}2 (CH3COO)4, was synthesized and characterized by X-ray diffraction. The title complex crystallizes in triclinic, space group P with a = 8.2779(8), b = 9.4830(8), c = 12.262(1) ? = 81.079(5), b = 80.620(4), g = 78.960(4), V = 924.4(1) 3, Z = 1, C34H46Cu2Fe2N2O8, Mr = 849.51, Dc = 1.526 g/cm3, l(MoK) = 0.71073 ? ?= 1.954 mm-1, F(000) = 438, R = 0.0297 and wR = 0.0901. Both cyclopentadienyl rings in each dmaf (dmaf = (dimethylaminomethyl)ferrocene, Fe(C5H5)- [C5H4CH2N(CH3)2]) have an eclipsed conformation. The binuclear molecule has a crystallographic centrosymmetry; four acetates and two Cu atoms form a cage structure with the distance between two neighboring Cu atoms of 2.655(1) .展开更多
基金Supported by Guangxi Provincial Department of Education(No.YB2014333)the Scientific research and technological development project of Guilin(No.20110330)+2 种基金the Project of Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources(Guangxi Normal University)Ministry of Education of China(CMEMR2011-13)Key Subjects of Universities in Guangxi Province Applied Chemistry(2007<20>)
文摘A new chain-like coordination polymer, namely, [CuL]n (1, Na2L = 2-[(2-hydroxy- benzylidene)-amino]-benzenesulfonic acid sodium salt), has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy and elemental analysis. Complex 1 crystallizes in monoclinic system, space group P21/c with a = 9.2296(16), b = 10.4754(18), c = 12.200(2) A, β = 102.392(2)°, V = 1152.0(3)A3, CI3H9CuNOaN, Mr = 338.83, Dc = 1.953 g/cm3, Z = 4, F(000) = 684, p = 2.089 mm-1, the final R = 0.0376 and wR = 0.0956. X-ray diffraction analyses indicate that 1 displays a square-pyramidal metal center with NO4 donor sets. The sulfonate-derived Schiff base serves as a common N,O,O'-tridentate and a unique O-bridged ligand connecting the metals. Dinuclear copper complexes serve as secondary building blocks (SBUs) to construct an unusual 2D coordination network. In the crystal, the components form a stable 3D supramolecular architecture by C-H...O interactions and to-stacking
文摘A copper(Ⅱ) complex [LCu2Cl4]n was synthesized by a new bis-Schiff base ligand containing quinoline unit, 1,4-bis[2-(4-fluorophenyl)iminomethyl-8-quinolinoxy]butane(L). X-ray crystal structure shows that it is a binuclear complex, and the crystal belongs to the triclinic system, space group P1, with a = 9.387(2), b = 9.968(2), c = 10.291(2) ?, α = 87.532(3), β = 63.762(2), γ = 86.628(3)o, V = 862.1(3) ?^3, Z = 1, Dc = 1.640 Mg/m^3, F(000) = 428, R = 0.0416 and wR = 0.1141. Each Cu(Ⅱ) metal ion coordinates with a quinoline N atom, an imine N atom, an ether oxygen atom and three chlorides, forming a distorted six-coordinated octahedronal structure. Each copper(Ⅱ) complexation unit links with one of the adjacent ligand copper complexation units through the chlorido bridging groups, thus generating an infinite one-dimensional chain structure. Such 1D chains further construct a 2D network structure by π-π stacking interactions.
文摘The title compound [Cu(bix)2(NO3)z·H2P]n 1 (bix = 1,4-bis(imidazole-1-ylme-thyl) benzene) has been synthesized by hydrothermal method. Its crystal structure is of monoclinic, space group P1^- with a = 8.3075(13), b = 9.4725(13), c = 10.0192(13) A, α = 91.088(4), β = 104.063(6), γ = 101.88(1), V = 746.5(3) A^3, Z = 1, C28H30N10O7Cu1, Mr = 682.16, Dc = 1.518 g/cm^3, μ = 0.796 mm^-1, F(000) = 353, the final R = 0.0535 and wR = 0.0996 for 2921 observed reflections with I 〉 2σ(I). Each bix ligand binds two Cu(Ⅱ) ions to form a 2-D(4,4) square grid layer, which is connected by hydrogen bonds showing large channels occupied by solvated water molecules and nitrate anions.
基金This work was supported by the National Natural Science Foundation of China (No. 20571057)
文摘The title compound, [Cu(C6H4N2O4F)2(H2O)4].4(H2O) I, has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in monoclinic, space group P21/c with a = 8.3041(17), b = 12.045(2), c = 11.077(2) A, β = 92.567(3)°, V= 1106.8(4) A^3, Mr = 581.89, Z= 2, Dc = 1.746 g/cm^3, F(000) = 598,μ(MoKa) = 1.090 mm^-1, the final R = 0.0296 and wR = 0.0806 for 3195 observed reflections with Ⅰ 〉 2σ(Ⅰ). In the centrosymmetric compound I, each Cu(Ⅱ) ion is coordinated by six O atoms from two 5-fluorouracil-1-acetate anions and four water molecules, forming a six-coordinated octahedral environment. N-H…O and O-H…O hydrogen-bonding interactions are observed in the structure, leading to the formation of a three-dimensional network.
基金This work was supported by the NSF for Distinguished Young Scientist of China (20425104) and the NSF of Fujian Province (A0420002, 2005I017)
文摘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.
基金This work was supported by the National Natural Science Foundation of China (Nos. 20671011, 20331010, 90406002 and 90406024)the 111 Project (B07012) and Key Laboratory of Structural Chemistry Foundation (No. 060017)
文摘A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3)A, β= 95.33(3)°, V = 1599.0(5)A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I 〉2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.
文摘A novel supramolecular adduct 3(C 42H 42N 28O 14) 2·H 2O (1) was synthesized by mixing 2- and cucurbit uril in solution of hydrochloric acid. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system and space group F dd2 with cell dimensions: a=4.705 33 (5) nm, b=7.153 80 (6) nm, c= 1.894 61 (2) nm, Z=16, V=63.7744 (11) nm3, D c= 1.534 g/cm3, μ=3.007 mm -1, F(000)=29 120, R 1= 0.070 7, wR 2=0.169 2. In crystal, the cucurb uril molecules form two zig-zag chains.
基金supported by the Education Committee of Sichuan Province (No.09ZA057)Department of Science and Technology of Sichuan Province (No. 2009JY0071 and 2010GZ0130)+1 种基金Science and Technology Office of Zigong City (No. 08X01)Key Laboratory of Material Corrosion and Protection of Sichuan Colleges and Universities (No. 2008CL04)
文摘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.
文摘A new copper(Ⅱ) complex with formula CuL(py), where L^2- is the dianion of 2,4-dihydroxybenzylidene benzoylhydrazone, has been synthesized and characterized by IR spectra and single-crystal X-ray diffraction method. The crystal belongs to monoclinic, space group P2 1/c with a=0.9630(4), b=1.4808(6), c=1.2320(5) nm, β=104.969(6)°, V=1.6973(Ⅱ) nm^3, Z=4, Dc=1.553 g/cm^3,μ(MoKa)=1.311 mm^-1, F(000)=812, R=0.0694 and wR=0.1727 for 1511 observed reflections (I〉2σ(I)). The crystal structure analysis indicates that the copper(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom from the tridentate acylhydrazone Schiff base ligand L^2- and one nitrogen atom from the pyridine ligand. Two adjacent molecules are connected via weak Cu…O bonding interactions to form dimers, which are further linked to generate a two-dimensional layer structure via interdimeric hydrogen bonds.
基金supported by grants from the 973 Program (2007CB815301)the National Science Foundation of China (21073192,20733003, 20871114 and 20801055)+1 种基金the Science Foundation of CAS (KJCX2-YW-H20)Fujian Province (2009HZ0006-1,2006L2005)
文摘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).
基金This work was supported by the foundation of Natural Science Research of Jiangsu Education Department (02KJB150007)
文摘The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?
文摘To obtain advanced quality pure copper, the microstructure of solidified copper was optimized by imposing electric pulse on liquid copper in this study. Experiments were performed to determine the effect of electric pulse voltage, arrangement mode of electrodes, and energy input on the microstructure of solidified copper. The results show that, when the energy input of electric pulse is bigger than 28.95 kJ per ton copper, the percent of fine grains increases noticeably with the increase of energy input; but when the energy input of electric pulse is smaller than 28.95 kJ per ton copper, the percent of fine grains decreases with the increase of energy input. The influence order of above factors on grain refinement is electric pulse voltage 〉 arrangement mode of electrodes 〉 energy input. According to the above experimental results, the optimum process conditions are chosen as the voltage being 400 V and the energy input greater than 28.95 kJ per ton copper. Meanwhile, the best arrangement mode of electrodes should be that, one electrode is immerged in the middle of liquid copper in the crystallizer, and the other is connected to the inner wall of the crystallizer, which is divided into two electrode poles for the symmetrical electric field distribution.
基金This work was supported by the Natural Science Foundation of Universities of Jiangsu Province (No. 03KJB150118) ② Corresponding author. Fax: +86-512-65224783, E-mail: blli1965@pub.sz.jsinfo.net
文摘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.
基金supported by the National Natural Science Foundation of China(21401097)
文摘A new coordination polymer [Cu2(OH)(nbta)(tib)(H2 O)2]n(1, H3 nbta = 5-nitro-1,2,3-benzenetricarboxylic acid, tib = 1-(4 H-1,2,4-triazol-4-yl)-4-(imidazol-1-yl)benzene) constructed from dimeric Cu(Ⅱ) units has been synthesized under hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction analysis. The compound crystallizes in monoclinic system, space group I2/c, with a = 17.8474(9), b = 11.7588(6), c = 21.9221(11) ?, β = 104.419(5)°, V = 4455.7(4) ?3 and Z = 8. Compound 1 is a three-dimensional structure constructed from dimeric Cu(Ⅱ) units and presents a 2-nodal(3,5)-connected net. Moreover, the thermal stability and solid UV-Vis absorption spectra have been investigated.
文摘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.
基金This work was supported by the Scientific Research Common Program of Beijing Municipal Commission of Education (KM20051028005)
文摘The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ) complex [Cu(L)(py)]2 2 (L = C10H11O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine) with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1: orthorhombic, space group Pbca with a = 11.921(4), b = 15.816(6), c = 17.076(6) A, V= 3219.7(19) A^3, C15H17CuN3O5S, Z = 8, Mr = 414.92, De = 1.712 g/cm^3,μ(MoKα) = 1.520 mm^-1, F(000) = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I 〉 2σ(I); and crystal data for 2: monoclinic, space group P21/c with a = 7.929(3), b = 17.038(5), c = 11.734(4) A, β = 98.162(6)°, V = 1569.1(9) A^3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm^3, F(000) = 820,μ(MoKα) = 1.554 mm^-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections (I 〉 2σ(I)). The molecular structure of complex 1 consists of one tetra-coordinated Cu(Ⅱ) atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper(Ⅱ) structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.
基金supported by the National Natural Science Foundation of Chinathe Program for New Century Excellent Talents in University (20871002 and NCET-06-0556)
文摘A novel hexanuclear copper-indium thiolate complex, [(InCl)2(OMe)(μ-OMe)2(μ- OMe)(μ-SPrn)2(CuPPh3)]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu(Me- CN)a][PF6] in the presence of Ph3P and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P211n with a = 11.3533(8), b = 15.4939(11), c = 20.5189(14) A, β = 98.577(2)°, V = 3569.0(4) A3, Z = 2, C56H82Cl4Cu2In4O8P2S4, Mr = 1801.56, Dc = 1.676 g/cm3,μ(MoKa) = 2.213 mm^-1, F(000) = 1796, S = 0.985, the final R = 0.0559 and wR = 0.1099 for 8878 observed reflections with I 〉 2σ(I) and 367 variables. Complex 1 consists of two CuPPh3 fragments which symmetrically side-attach to the tetranuclear core of [InaCl4(OMe)2(μ-OMe)a(μ- OMe)2(μ-SPrn)4] by coordinating with sulfur atoms of propane-thio moieties. The average In-Ot (terminal), In-μ-O and In-μ3-O bond distances are 2.305(4), 2.144(4) and 2.294(4) A, respectively.
基金supported by the Chinese Academy of Sciences (KJCX2-YW-M05,KJCX2-YW-319)the Natural Science Foundation of Fujian Province (2007HZ0001-1,2009HZ0004-1)
文摘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).
基金Supported by the National Natural Science Foundation of China(No.21203160)Education Department Foundation of Shaanxi Province(No.12JK0631)+1 种基金Natural Science Foundation of Shaanxi Province(No.2013JM2013)Special Research Fund of Xianyang Normal University(No.11XSYK204,11XSYK205,12XSYK023)
文摘A novel cuprous azide complex with the formula of [Cu2(dmpz)(N3)2]n(1, dmpz: 2,6-dimethylpyrazine) has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [Cu N3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data: monoclinic, space group C2/c, a = 17.8599(15), b = 8.2889(5), c = 14.8076(14) A, β = 113.2580(10)o, V = 2014.0(3) A3, Z = 8, S = 1.025, the final R = 0.0303, w R = 0.0825 for 1460 observed reflections with I 2σ(I) and R = 0.0386, wR = 0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.
基金The work was supported by the Provincial Education Foundation of Fujian (JA99135) the Test Foundation of Fuzhou University and the foundation of the Department of Chemistry Fuzhou University
文摘A binuclear complex including ferrocenyl, Cu2{Fe(C5H5)[C5H4CH2N(CH3)2]}2 (CH3COO)4, was synthesized and characterized by X-ray diffraction. The title complex crystallizes in triclinic, space group P with a = 8.2779(8), b = 9.4830(8), c = 12.262(1) ? = 81.079(5), b = 80.620(4), g = 78.960(4), V = 924.4(1) 3, Z = 1, C34H46Cu2Fe2N2O8, Mr = 849.51, Dc = 1.526 g/cm3, l(MoK) = 0.71073 ? ?= 1.954 mm-1, F(000) = 438, R = 0.0297 and wR = 0.0901. Both cyclopentadienyl rings in each dmaf (dmaf = (dimethylaminomethyl)ferrocene, Fe(C5H5)- [C5H4CH2N(CH3)2]) have an eclipsed conformation. The binuclear molecule has a crystallographic centrosymmetry; four acetates and two Cu atoms form a cage structure with the distance between two neighboring Cu atoms of 2.655(1) .