The complex Cu(phon)(NO3)2(CH3CN) (phon = 1,10-phenanthroline-5,6-dione) has been synthesized and characterized by elemental analysis, infrared and UV-Vis spectra. X-ray diffraction analysis at room temperature indica...The complex Cu(phon)(NO3)2(CH3CN) (phon = 1,10-phenanthroline-5,6-dione) has been synthesized and characterized by elemental analysis, infrared and UV-Vis spectra. X-ray diffraction analysis at room temperature indicates that the complex crystallizes in orthorhombic system, space group P212121 with a = 8.353(1), b = 11.299(2), c = 17.764(2)(A), V = 1676.5(4) (A)3, Z = 4, C14H9CuN5O8, Mr = 438.8, Dc = 1.739 g/cm3, F(000) = 884 and ((MoK() = 1.361 mm-1. The final R and wR factors for the observed reflections with I > 2((I) are 0.0353 and 0.0855, respectively. R = 0.0432 and wR = 0.0899 for all data. The structure of the title complex consists of a neutral mononuclear entity. The central Cu (Ⅱ) atom is five-coordinated by two nitrogen donors of one ligand, two unidentate NO3- ions and one CH3CN molecule. The coordination geometry of Cu (Ⅱ) can be considered as a distorted trigonal bipyramidal configuration. The complex ability of the NO3- ion has more effect than that of the ClO4- ion on the structure of the complex.展开更多
A new ternary complex of nickel(II) with L-aspartate (L-Asp) and 1, 10-phenan- throline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4?4.75H2O, has been synthesized in a mixed sol- vent of H2OC2H5OH at the pH value of 3. I...A new ternary complex of nickel(II) with L-aspartate (L-Asp) and 1, 10-phenan- throline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4?4.75H2O, has been synthesized in a mixed sol- vent of H2OC2H5OH at the pH value of 3. It crystallizes in triclinic, space group P1 with a = 11.861(2), b = 18.384(4), c = 19.746(3) ?, α = 107.68(1), β = 105.94(1), γ = 103.41(2)°, V = 3703.6(11) ?3, Mr = 1745.66, Z = 2, Dc =1.565 g/cm3, μ = 0.989 mm-1, F(000) = 1791, R = 0.0643 and wR = 0.1611. The complex contains two cations, binuclear [Ni2(L-Asp)(Phen)3(H2O)]2+ and mononu- clear [Ni(Phen)2(H2O)2]2+. All the nickel ions in the complex are six-coordinated with a distorted octahedral geometry, but the coordination environments for them are different. There exist hydrogen bonds and π-π stacking interactions in the complex.展开更多
The nickel complex {Ni(2,2-bipy)(H2O)3[C8H11O2(COO)]}(H2O)3 with bicycle-[2.2.1]-2-hepten-5,6-dicarboxylic acid [C7H8(COOH)2] and 2,2'-bipyridine (bipy) as ligands has been synthesized and characterized. ...The nickel complex {Ni(2,2-bipy)(H2O)3[C8H11O2(COO)]}(H2O)3 with bicycle-[2.2.1]-2-hepten-5,6-dicarboxylic acid [C7H8(COOH)2] and 2,2'-bipyridine (bipy) as ligands has been synthesized and characterized. It crystallizes in monoclinic, space group P , with a = 0.74975(3), b = 1.20309(4), c = 1.30593(4) nm, α = 109.861(2), β = 98.519(2), γ = 90.575(2)o, V = 1.09337(7) nm3, Dc = 1.552 g/cm3, Z = 2, F(000) = 524, the final GOOF = 1.064, R = 0.0397 and wR = 0.1171. The crystal structure shows that the nickel ion is coordinated with four oxygen atoms from one bicycle[2.2.1]-2-hepten-5,6-dicarboxylic acid molecule and three water molecules and two nitrogen atoms from the 2,2′-bipyridine molecule, forming a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex is stable under 200.0 ℃.展开更多
A new metal-organic coordination polymer [Ni[(2-pya)2(4,4′-bipy)]n·6nH2O (2-pya = 2-pyridinecarboxylic acid, 4,4′-bipy = 4,4′-pyridine) 1 has been hydrothermally synthesized and structurally characterize...A new metal-organic coordination polymer [Ni[(2-pya)2(4,4′-bipy)]n·6nH2O (2-pya = 2-pyridinecarboxylic acid, 4,4′-bipy = 4,4′-pyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I4 1/α with a = b = 22.5642(19), c = 10.7118(18) A, V = 5453.8(11) A^3, C22H28N4NiO10, Mr= 567.19, Dc = 1.382 g/cm^3, μ(MoKα) = 0.769 mm^-1, F(000) =2368, Z = 8, the final R = 0.0572 and wR = 0.1254 for 1401 observed reflections (I 〉 2σ(I)). It exhibits a one-dimensional chain-like structure by mixed ligands of 2-pyridinedicarboxylic acid and 4,4′-pyridine.展开更多
A series of new nickel(Ⅱ)complexes with 2-aminomethylpyridine ligands,(2-PyCH_2NHAr)_2NiBr_2(Ar=2,6- dimethylphenyl 2a;2,6-diisopropylphenyl 2b,2,6-difluorophenyl 2c),have been synthesized and used as catalyst precur...A series of new nickel(Ⅱ)complexes with 2-aminomethylpyridine ligands,(2-PyCH_2NHAr)_2NiBr_2(Ar=2,6- dimethylphenyl 2a;2,6-diisopropylphenyl 2b,2,6-difluorophenyl 2c),have been synthesized and used as catalyst precursors for ethylene polymerization in the presence of methylaluminoxane(MAO).The catalysts containing ortho-alkyl-substituents afford high molecular weight branched polyethylenes as well as a certain amount of oligomers.Enhancing the steric bulk of the alkyl substituent of the catalyst resulted in...展开更多
A new trinuclear nickel complex,[Ni3(pdc)3(2,2'-bipy)3(H2O)2]·2H2O(H2pdc = pyridine 2,6-dicarboxylic acid,2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and characterized by IR,elemen...A new trinuclear nickel complex,[Ni3(pdc)3(2,2'-bipy)3(H2O)2]·2H2O(H2pdc = pyridine 2,6-dicarboxylic acid,2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and characterized by IR,elemental analysis and X-ray diffraction methods.Crystal data for this complex:monoclinic,space group P21/n,a = 21.206(4),b = 10.002(2),c = 28.066(6),β = 108.18(3)°,C51H41N9Ni3O16,Mr = 1212.06,V = 5.656(2) nm3,Dc = 1.423 g·cm-3,μ(MoKα) = 1.062 mm-1,Z = 4,F(000) = 2488,GOOF = 1.034,the final R = 0.0543 and wR = 0.1237 for 6149 observed reflections with Ⅰ 〉 2σ(Ⅰ).In the complex,three nickel(Ⅱ) ions are bridged by the pyridine 2,6-dicarboxylic acid groups,and all nickel(Ⅱ) ions are seven-coordinated by nitrogen atoms of 2,2'-bipyridine and pyridine 2,6-dicarboxylic acid and oxygen atoms from pyridine 2,6-dicarboxylic and water to adopt a severely distorted pentagonal bipyramidal geometry.The emission and excitation peaks of the complex in ethanol solutions are located at 336 and 316 nm,respectively.展开更多
A new binuclear nickel(Ⅱ) complex [Ni_2(C_7 N_4 H_5)_3(C_9 H_9 O_2)]n has been hydrothermally synthesized with nickel sulfate, 3-(pyridin-2-yl)-1H-1,2,4-triazole and 3,5-dimethylbenzoic acid(3,5-DMBA). It c...A new binuclear nickel(Ⅱ) complex [Ni_2(C_7 N_4 H_5)_3(C_9 H_9 O_2)]n has been hydrothermally synthesized with nickel sulfate, 3-(pyridin-2-yl)-1H-1,2,4-triazole and 3,5-dimethylbenzoic acid(3,5-DMBA). It crystallizes in the triclinic space group P1 with a = 11.5769(7), b = 12.3115(7), c = 12.6431(7) A, α = 81.4860(10)o, β = 64.2830(10)o, γ = 63.7130(10)o, V = 1453.45(15) A^3, D_c = 1.604 g/cm^3, Z = 2, F(000) = 720, the final GOOF = 1.048, R = 0.0285 and wR = 0.0628. The crystal structure shows that the whole molecule consists of two nickel ions bridged by three μ_2-η~1:η~0-3-(pyridin-2-yl)-1,2,4-triazole anions. The coordination environment of Ni(Ⅱ) ion is NiO_2 N_4 and NiN_5, giving a distorted octahedral geometry and square pyramidal geometry respectively. The luminescence and thermal properties of the complex were investigated.展开更多
The reactions of chiral four-coordinated nickel(Ⅱ) complex [Ni(RR-L)](ClO4)2/[Ni(SS- L)](ClO4)2 with β-dl-phenylalanine in acetonitrile/water gave a six-coordinated enantiomer of [Ni(RR-L)(β-d-HPhe)]...The reactions of chiral four-coordinated nickel(Ⅱ) complex [Ni(RR-L)](ClO4)2/[Ni(SS- L)](ClO4)2 with β-dl-phenylalanine in acetonitrile/water gave a six-coordinated enantiomer of [Ni(RR-L)(β-d-HPhe)](ClO4)2(1) and [Ni(SS-L)(β-l-HPhe)](ClO4)2(2), respectively(L = 5,5,7, 12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane, HPhe = phenylalanine). Single-crystal X-ray diffraction analyses revealed that the nickel(Ⅱ) atom displays a distorted octahedral coordination geometry by coordinating with four nitrogen atoms of L in a folded configuration, and two carboxylate oxygen atoms of β-d/l-HPhe in cis-position in both complexes. The monomers of [Ni(RR-L)(β-d-HPhe)]2+ and [Ni(SS-L)(β-l-HPhe)]2+ are connected through intermolecular hydrogen bonds to generate one-dimensional zigzag chains, respectively. The homochiral natures of 1 and 2 are confirmed by the results of CD spectroscopy.展开更多
Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR,...Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.展开更多
A new oxalato-bridged dinickel(Ⅱ) complex [Ni2(NIT-MeImz)4(C2O4)](Ac)2·8H2O has been synthesized and characterized structurally as well as magnetically.It crystallizes in monoclinic,space group C2/c with...A new oxalato-bridged dinickel(Ⅱ) complex [Ni2(NIT-MeImz)4(C2O4)](Ac)2·8H2O has been synthesized and characterized structurally as well as magnetically.It crystallizes in monoclinic,space group C2/c with a=24.608(4),b=21.399(3),c=17.992(3),β=131.680(2)°,V=7076(2)3,C50H86N16Ni2O24,Mr=1412.77,Z=4,Dc=1.326 g/cm3,μ(MoKα)=0.614 mm-1,F(000)=2984,R=0.0751 and wR=0.1791 for 2956 observed reflections with Ⅰ>2σ(Ⅰ).X-ray analysis reveals that the crystal structure consists of [Ni2(NIT-MeImz)4(C2O4)]2+ moiety and two Ac^- anions. Each nickel(H) ion is six-coordinated with a distorted octahedral geometry: two nitrogen atoms and two oxygen atoms from NIT-Melmz together with two other oxygen atoms from the oxalato ion. The 2-D net structure is formed and arranged through intermolecular H-bonding interactions. Magnetic measurements show antiferromagnetic interactions for this complex.展开更多
A novel ternary complex of [NiL1L2·2H2O]·NO3·H2O (L1 = 2-hydroxyl-1,10-phenanthroline (HOphen), L2 = 2-hydroxynicotinic acid (H2nicO)) was synthesized, and its crystal structure was determined by ...A novel ternary complex of [NiL1L2·2H2O]·NO3·H2O (L1 = 2-hydroxyl-1,10-phenanthroline (HOphen), L2 = 2-hydroxynicotinic acid (H2nicO)) was synthesized, and its crystal structure was determined by X-ray diffraction and further characterized by infrared and elementary analysis. The title complex (C18H18NiN4O10, Mr = 509.07) belongs to the triclinic system, space group P1^- with a = 712490(7), b = 11.0164(10), c = 13.3864(13)A, α = 91.6040(10),β= 98.8620(10), γ= 107.1140(10)°, V= 1006.43(17)A^3, Z = 2, Dc = 1.680 g/cm^3,μ= 1.032 mm^-1, F(000) = 524, the final R = 0.0461 and wR= 0.1238. In the complex, the Ni(H) ion is six-coordinated to assume a distorted octahedral geometry, and a 3D supramolecular network comes into being via weak intermolecular interactions of X-O--.H (X = N, O).展开更多
A new nickel(Ⅱ) complex Ni2(L)2(2,2'-bipy)2·5.5H2O with methy-bicycle[2.2.1]hept-5-ene-2,3-dicarboxylic acid(H2L) and 2,2?-bipyridine(2,2'-bipy) as ligands has been synthesized in the mixed solvent ...A new nickel(Ⅱ) complex Ni2(L)2(2,2'-bipy)2·5.5H2O with methy-bicycle[2.2.1]hept-5-ene-2,3-dicarboxylic acid(H2L) and 2,2?-bipyridine(2,2'-bipy) as ligands has been synthesized in the mixed solvent DMF and water(v:v = 5:2). It crystallizes in the triclinic space group P1 with a = 10.414(2), b = 12.884(3), c = 16.176(4) A, α = 70.715(5), β = 80.599(5), γ = 77.383(6)°, V = 1989.4(8) A^3, Dc = 1.531 g/cm^3, Z = 2, F(000) = 958, GOOF = 1.028, the final R = 0.0808 and w R = 0.2036. The crystal structure shows that the whole molecule consists of two independent dinuclear units, in which two nickel ions are bridged by two μ2-η1:η0 3-carboxylate groups of L2- anions. The coordination environment of Ni(Ⅱ) ion is Ni N2O3, giving a distorted square pyramidal geometry. The thermal stability and electrochemical properties of the complex were investigated.展开更多
Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4...Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4 )3· 5H2O (complex3) and [Ni3 (BZT ) (Nphen )6] (ClO4 )3 (complex 4 ) (BZT = 1, 3, 5-benzenetricarboxylato, Phen = 1, 10-phenthroline, Nphen = 5-nitro-1, 10-phenanthroline )have been synthesized. The complexes were characterized using elemental analysis,IR and electronic reflection spectra. These complexes are proposed to have extended 1, 3, 5-benzenetricarboxylato-bridged structure and to consist of three manganese (Ⅱ) or three nickel(Ⅱ). The X-band ESR spectra of the complex 1 and complex 2were recorded at room temperature. The variable-temperature magnetic susceptibilities of complex 1 and complex 3 were measured over 4. 2-300 K. According to experimental results of the variable-temperature magnetic susceptibility, the magnetic interaction between the paramagnetic centers is too weak to be detected using the usual magnetic susceptibility technique.展开更多
Two complexes with formulas [Ni L][(Ni L)(IPA)2]·8H2O(1) and [(Ni L)(H2O)2] [(Ni L)(PMA)]·4H2O(2)(L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,IPA2– = isophthalic anion,P...Two complexes with formulas [Ni L][(Ni L)(IPA)2]·8H2O(1) and [(Ni L)(H2O)2] [(Ni L)(PMA)]·4H2O(2)(L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,IPA2– = isophthalic anion,PMA4– = 1,2,4,5-benzenetetracarboxylic anion) were synthesized and characterized by elemental analyses and IR spectra.The crystal structures were determined by X-ray diffraction.In complex 1,the [Ni L]^2+ bridged IPA^2– to give [(Ni L)(IPA)2]^2– monomer,and the [Ni L]^2+ bridged PMA4– to form a one-dimensional chain [(Ni L)(PMA)]n^2n– in complex 2.The [Ni L]^2+ and [(Ni L)(IPA)2]^2–/[(Ni L)(PMA)]^2– are connected through intermolecular hydrogen bonding to generate three-dimensional supramolecular structures.展开更多
Reactions of NiCl2-6H2O with dmpzm and formic or acetic acid at PH = 7 produced the two title compounds, [Ni(dmpzm)2(HCO2)]Cl·2H2O 1 and [Ni(dmpzm)2(OAc)]C2·H2O 2 (dmpzm = 1,1 '-methylenebis(3,5-d...Reactions of NiCl2-6H2O with dmpzm and formic or acetic acid at PH = 7 produced the two title compounds, [Ni(dmpzm)2(HCO2)]Cl·2H2O 1 and [Ni(dmpzm)2(OAc)]C2·H2O 2 (dmpzm = 1,1 '-methylenebis(3,5-dimethyl-lH-pyrazole)). 1 and 2 were characterized by elemental analysis, IR spectra, and thermogravimetric analysis. 1 crystallizes in the orthorhombic system, space group Pcca with a = 18.700(2), b = 8.6843(9), c = 18.098(2)A, V= 2939.1(5)A^3, Z = 4, Dc = 1.319 g/cm^3, T = 193 K, C23H37CINsNiO4, Mr = 583.75, F(000) = 1232, p(MoKa) = 0.792 cm^-1, S = 1.079, R = 0.0772 and wR = 0.1958 for 2265 observed reflections with I〉 2σ(I). 2 crystallizes in the orthorhombic system, space group Pcca with a = 17.011(3), b = 18.630(4), c = 19.300(4)A, V = 6117(2)A^3, Z = 8, Dc = 1.337 g/cm^3, T= 193(2) K, C24H41C1N8NiO5, Mr = 615.79, F(000) = 2608, μ(MoKa) = 0.768 cm^-1, S = 1.059, R = 0.0518 and wR = 0.1109 for 5124 observed reflections with I 〉 2σ(I). The Ni atoms in 1 or 2 are chelated by two dmpzm ligands and one formate or acetate anion, forming slightly distorted octahedral geometries. In the crystals of 1 or 2, intermolecular hydrogen bonding interactions result in the formation of 2D hydrogen-bonded frameworks.展开更多
In the ethanol solvent, a nickel(Ⅱ) complex Ni(C12H10N2O2S)2 upon reaction of 2'-(2-thienylidene)-hydroxybenzoylhydrazide with nickel acetate was synthesized, and its structure was characterized by IR, UV, ele...In the ethanol solvent, a nickel(Ⅱ) complex Ni(C12H10N2O2S)2 upon reaction of 2'-(2-thienylidene)-hydroxybenzoylhydrazide with nickel acetate was synthesized, and its structure was characterized by IR, UV, elemental analysis and X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 22.052(3), b = 5.9681(6), c = 18.522(2)A , β = 110.679(4)°, V = 2280.6(4)A^3, Z = 4, Mr = 551.27, μ = 1.606 mm^-1, Dc = 1.075 g/cm^3, F(000) = 1136 and Rint = 0.0556. The nickel(Ⅱ ) atom in the compound is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The biological activities have been measured, show- ing the compound exhibits better anti-bacterial activity than the ligand.展开更多
Under given conditions, two complexes of [Ni(H20)2BEDA]·2H2O 1 and [Ni(Py)2- BEDA]·6H2O 2 (BEDA = bis(3-methoxy-2-pyridyl)ether-6,6′-dicarboxylic acid) have been synthesized and characterized by ele...Under given conditions, two complexes of [Ni(H20)2BEDA]·2H2O 1 and [Ni(Py)2- BEDA]·6H2O 2 (BEDA = bis(3-methoxy-2-pyridyl)ether-6,6′-dicarboxylic acid) have been synthesized and characterized by elemental analysis and X-ray single-crystal diffraction. Crystal data for 1: C14H18NiN2O11, monoelinic C2/c, a = 14.3844(17), b = 12.9900(15), c = 9.6309(11) A, β = 104.3350(10)°, V= 1743.5(4) A3, Z = 4, Dc= 1.711 g/cm^3, F(000) = 928, μ = 1.179 mm^-1, Mr= 449.01, the final R = 0.0228 and wR = 0.0625. Crystal data for 2: C24H32NiN4O13, triclinic P1, a = 9.423(2), b = 11.863(3), c = 13.089(3) A, α = 91.511(3), β = 92.465(3), γ = 100.696(2)°, V = 1435.6(6) A^3, Z = 2, Dc= 1.488 g/cm^3, F(000) = 672, μ = 0.748 mm^-1, Mr= 643.25, the final R = 0.0400 and wR = 0.0975. Interestingly, in the two complexes, lattice water molecules dominate its crystal structures. Therefore, extensive intermolecular hydrogen bonds assemble 1 and 2 into 2D extended sheets and a 3D open framework, respectively. Furthermore, water molecules present in 2 are associated to form water clusters.展开更多
Three new asymmetrical ruthenium (Ⅱ) complexes :[Ru(phen)2{phen-NHCO(CH2)4BR}](pf6)2,[rU(PHEN)2{PHEN-nhco(ch2)5br}](pf6)2 and [Ru(phen)2{phen-NHCO(CH2)10Br}](PF6)2 were synthesized ,which were confirmed byh the techn...Three new asymmetrical ruthenium (Ⅱ) complexes :[Ru(phen)2{phen-NHCO(CH2)4BR}](pf6)2,[rU(PHEN)2{PHEN-nhco(ch2)5br}](pf6)2 and [Ru(phen)2{phen-NHCO(CH2)10Br}](PF6)2 were synthesized ,which were confirmed byh the technique of FT-IR 1HNMR and ESI-MS ,The electrochemical and fluorescent properties of three Ru(Ⅱ)complexes were investigated with cyclic voltammetry and fluorometry.展开更多
基金This work was financially supported by the National Natural Science Foundation of China(No.29971019)
文摘The complex Cu(phon)(NO3)2(CH3CN) (phon = 1,10-phenanthroline-5,6-dione) has been synthesized and characterized by elemental analysis, infrared and UV-Vis spectra. X-ray diffraction analysis at room temperature indicates that the complex crystallizes in orthorhombic system, space group P212121 with a = 8.353(1), b = 11.299(2), c = 17.764(2)(A), V = 1676.5(4) (A)3, Z = 4, C14H9CuN5O8, Mr = 438.8, Dc = 1.739 g/cm3, F(000) = 884 and ((MoK() = 1.361 mm-1. The final R and wR factors for the observed reflections with I > 2((I) are 0.0353 and 0.0855, respectively. R = 0.0432 and wR = 0.0899 for all data. The structure of the title complex consists of a neutral mononuclear entity. The central Cu (Ⅱ) atom is five-coordinated by two nitrogen donors of one ligand, two unidentate NO3- ions and one CH3CN molecule. The coordination geometry of Cu (Ⅱ) can be considered as a distorted trigonal bipyramidal configuration. The complex ability of the NO3- ion has more effect than that of the ClO4- ion on the structure of the complex.
基金This work was supported by the Natural Science Foundation of Guangxi Province (No. 9912044)
文摘A new ternary complex of nickel(II) with L-aspartate (L-Asp) and 1, 10-phenan- throline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4?4.75H2O, has been synthesized in a mixed sol- vent of H2OC2H5OH at the pH value of 3. It crystallizes in triclinic, space group P1 with a = 11.861(2), b = 18.384(4), c = 19.746(3) ?, α = 107.68(1), β = 105.94(1), γ = 103.41(2)°, V = 3703.6(11) ?3, Mr = 1745.66, Z = 2, Dc =1.565 g/cm3, μ = 0.989 mm-1, F(000) = 1791, R = 0.0643 and wR = 0.1611. The complex contains two cations, binuclear [Ni2(L-Asp)(Phen)3(H2O)]2+ and mononu- clear [Ni(Phen)2(H2O)2]2+. All the nickel ions in the complex are six-coordinated with a distorted octahedral geometry, but the coordination environments for them are different. There exist hydrogen bonds and π-π stacking interactions in the complex.
基金Project supported by the Fund of Hunan Provincial Natural Science Foundation of China (No.11JJ9006)the Fund of Science and Technology Committee of Hunan Province (2009FJ3031)
文摘The nickel complex {Ni(2,2-bipy)(H2O)3[C8H11O2(COO)]}(H2O)3 with bicycle-[2.2.1]-2-hepten-5,6-dicarboxylic acid [C7H8(COOH)2] and 2,2'-bipyridine (bipy) as ligands has been synthesized and characterized. It crystallizes in monoclinic, space group P , with a = 0.74975(3), b = 1.20309(4), c = 1.30593(4) nm, α = 109.861(2), β = 98.519(2), γ = 90.575(2)o, V = 1.09337(7) nm3, Dc = 1.552 g/cm3, Z = 2, F(000) = 524, the final GOOF = 1.064, R = 0.0397 and wR = 0.1171. The crystal structure shows that the nickel ion is coordinated with four oxygen atoms from one bicycle[2.2.1]-2-hepten-5,6-dicarboxylic acid molecule and three water molecules and two nitrogen atoms from the 2,2′-bipyridine molecule, forming a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex is stable under 200.0 ℃.
基金Supported by the Science and Technology Research Projects of the Education Office of Jilin Province (No. 2007. 213)
文摘A new metal-organic coordination polymer [Ni[(2-pya)2(4,4′-bipy)]n·6nH2O (2-pya = 2-pyridinecarboxylic acid, 4,4′-bipy = 4,4′-pyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I4 1/α with a = b = 22.5642(19), c = 10.7118(18) A, V = 5453.8(11) A^3, C22H28N4NiO10, Mr= 567.19, Dc = 1.382 g/cm^3, μ(MoKα) = 0.769 mm^-1, F(000) =2368, Z = 8, the final R = 0.0572 and wR = 0.1254 for 1401 observed reflections (I 〉 2σ(I)). It exhibits a one-dimensional chain-like structure by mixed ligands of 2-pyridinedicarboxylic acid and 4,4′-pyridine.
基金the National Natural Science Foundation of China(Nos.20674097,20734004)the Ministry of Education of China(Foundation for Ph.D.Training).
文摘A series of new nickel(Ⅱ)complexes with 2-aminomethylpyridine ligands,(2-PyCH_2NHAr)_2NiBr_2(Ar=2,6- dimethylphenyl 2a;2,6-diisopropylphenyl 2b,2,6-difluorophenyl 2c),have been synthesized and used as catalyst precursors for ethylene polymerization in the presence of methylaluminoxane(MAO).The catalysts containing ortho-alkyl-substituents afford high molecular weight branched polyethylenes as well as a certain amount of oligomers.Enhancing the steric bulk of the alkyl substituent of the catalyst resulted in...
基金Supported by the Science and Technology Fund of Hengyang Science and Technology Bureau (No. 2008KS035)the Construct Program of the Key Discipline in Hunan Province
文摘A new trinuclear nickel complex,[Ni3(pdc)3(2,2'-bipy)3(H2O)2]·2H2O(H2pdc = pyridine 2,6-dicarboxylic acid,2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and characterized by IR,elemental analysis and X-ray diffraction methods.Crystal data for this complex:monoclinic,space group P21/n,a = 21.206(4),b = 10.002(2),c = 28.066(6),β = 108.18(3)°,C51H41N9Ni3O16,Mr = 1212.06,V = 5.656(2) nm3,Dc = 1.423 g·cm-3,μ(MoKα) = 1.062 mm-1,Z = 4,F(000) = 2488,GOOF = 1.034,the final R = 0.0543 and wR = 0.1237 for 6149 observed reflections with Ⅰ 〉 2σ(Ⅰ).In the complex,three nickel(Ⅱ) ions are bridged by the pyridine 2,6-dicarboxylic acid groups,and all nickel(Ⅱ) ions are seven-coordinated by nitrogen atoms of 2,2'-bipyridine and pyridine 2,6-dicarboxylic acid and oxygen atoms from pyridine 2,6-dicarboxylic and water to adopt a severely distorted pentagonal bipyramidal geometry.The emission and excitation peaks of the complex in ethanol solutions are located at 336 and 316 nm,respectively.
基金Supported by Scientific Research Found of Hunan Provincial Education Department of China(17A049,17C0226)Industry and Research Key Project of Hengyang City(2017KJ155,2017KJ193)Doctoral Scientific Research Foundation of Hengyang Normal University(17D01)
文摘A new binuclear nickel(Ⅱ) complex [Ni_2(C_7 N_4 H_5)_3(C_9 H_9 O_2)]n has been hydrothermally synthesized with nickel sulfate, 3-(pyridin-2-yl)-1H-1,2,4-triazole and 3,5-dimethylbenzoic acid(3,5-DMBA). It crystallizes in the triclinic space group P1 with a = 11.5769(7), b = 12.3115(7), c = 12.6431(7) A, α = 81.4860(10)o, β = 64.2830(10)o, γ = 63.7130(10)o, V = 1453.45(15) A^3, D_c = 1.604 g/cm^3, Z = 2, F(000) = 720, the final GOOF = 1.048, R = 0.0285 and wR = 0.0628. The crystal structure shows that the whole molecule consists of two nickel ions bridged by three μ_2-η~1:η~0-3-(pyridin-2-yl)-1,2,4-triazole anions. The coordination environment of Ni(Ⅱ) ion is NiO_2 N_4 and NiN_5, giving a distorted octahedral geometry and square pyramidal geometry respectively. The luminescence and thermal properties of the complex were investigated.
基金Supported by the Scientific Research Fund of Hunan Provincial Education Department(13B029,13A030,13CY029)the Program for Excellent Talents in Hunan University of Science and Engineering(2013)+2 种基金the Construct Program of the Key Discipline in Hunan Province(2011-76)the Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province(2012-318)NSF of Hunan(11JJ2009)
文摘The reactions of chiral four-coordinated nickel(Ⅱ) complex [Ni(RR-L)](ClO4)2/[Ni(SS- L)](ClO4)2 with β-dl-phenylalanine in acetonitrile/water gave a six-coordinated enantiomer of [Ni(RR-L)(β-d-HPhe)](ClO4)2(1) and [Ni(SS-L)(β-l-HPhe)](ClO4)2(2), respectively(L = 5,5,7, 12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane, HPhe = phenylalanine). Single-crystal X-ray diffraction analyses revealed that the nickel(Ⅱ) atom displays a distorted octahedral coordination geometry by coordinating with four nitrogen atoms of L in a folded configuration, and two carboxylate oxygen atoms of β-d/l-HPhe in cis-position in both complexes. The monomers of [Ni(RR-L)(β-d-HPhe)]2+ and [Ni(SS-L)(β-l-HPhe)]2+ are connected through intermolecular hydrogen bonds to generate one-dimensional zigzag chains, respectively. The homochiral natures of 1 and 2 are confirmed by the results of CD spectroscopy.
基金Supported by the Natural Science Foundation of Education Department of Henan Province (No. 2011B150025)
文摘Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.
基金supported by the National Natural Science Foundation of China (Nos 20471026 and 20771054)the Natural Science Foundation of Henan Province (No 0311021200)
文摘A new oxalato-bridged dinickel(Ⅱ) complex [Ni2(NIT-MeImz)4(C2O4)](Ac)2·8H2O has been synthesized and characterized structurally as well as magnetically.It crystallizes in monoclinic,space group C2/c with a=24.608(4),b=21.399(3),c=17.992(3),β=131.680(2)°,V=7076(2)3,C50H86N16Ni2O24,Mr=1412.77,Z=4,Dc=1.326 g/cm3,μ(MoKα)=0.614 mm-1,F(000)=2984,R=0.0751 and wR=0.1791 for 2956 observed reflections with Ⅰ>2σ(Ⅰ).X-ray analysis reveals that the crystal structure consists of [Ni2(NIT-MeImz)4(C2O4)]2+ moiety and two Ac^- anions. Each nickel(H) ion is six-coordinated with a distorted octahedral geometry: two nitrogen atoms and two oxygen atoms from NIT-Melmz together with two other oxygen atoms from the oxalato ion. The 2-D net structure is formed and arranged through intermolecular H-bonding interactions. Magnetic measurements show antiferromagnetic interactions for this complex.
文摘A novel ternary complex of [NiL1L2·2H2O]·NO3·H2O (L1 = 2-hydroxyl-1,10-phenanthroline (HOphen), L2 = 2-hydroxynicotinic acid (H2nicO)) was synthesized, and its crystal structure was determined by X-ray diffraction and further characterized by infrared and elementary analysis. The title complex (C18H18NiN4O10, Mr = 509.07) belongs to the triclinic system, space group P1^- with a = 712490(7), b = 11.0164(10), c = 13.3864(13)A, α = 91.6040(10),β= 98.8620(10), γ= 107.1140(10)°, V= 1006.43(17)A^3, Z = 2, Dc = 1.680 g/cm^3,μ= 1.032 mm^-1, F(000) = 524, the final R = 0.0461 and wR= 0.1238. In the complex, the Ni(H) ion is six-coordinated to assume a distorted octahedral geometry, and a 3D supramolecular network comes into being via weak intermolecular interactions of X-O--.H (X = N, O).
基金Supported by the Construct Program of the Key Discipline in Hunan ProvinceKey Project of Industrial Science and Technology Support of Hengyang City(2015KG23)
文摘A new nickel(Ⅱ) complex Ni2(L)2(2,2'-bipy)2·5.5H2O with methy-bicycle[2.2.1]hept-5-ene-2,3-dicarboxylic acid(H2L) and 2,2?-bipyridine(2,2'-bipy) as ligands has been synthesized in the mixed solvent DMF and water(v:v = 5:2). It crystallizes in the triclinic space group P1 with a = 10.414(2), b = 12.884(3), c = 16.176(4) A, α = 70.715(5), β = 80.599(5), γ = 77.383(6)°, V = 1989.4(8) A^3, Dc = 1.531 g/cm^3, Z = 2, F(000) = 958, GOOF = 1.028, the final R = 0.0808 and w R = 0.2036. The crystal structure shows that the whole molecule consists of two independent dinuclear units, in which two nickel ions are bridged by two μ2-η1:η0 3-carboxylate groups of L2- anions. The coordination environment of Ni(Ⅱ) ion is Ni N2O3, giving a distorted square pyramidal geometry. The thermal stability and electrochemical properties of the complex were investigated.
文摘Two new manganese(Ⅱ ) trinuclear complexes and two new nickel (Ⅱ) trinuclear compIexes, namely, [Mn3 (BZT ) (Phen )6] (ClO4 )3 (complex 1 ), [Mn (BZT)· (Nphen )6] (ClO4 )3 (complex 2), [Ni3 (BZT) (Phen)6] (ClO4 )3· 5H2O (complex3) and [Ni3 (BZT ) (Nphen )6] (ClO4 )3 (complex 4 ) (BZT = 1, 3, 5-benzenetricarboxylato, Phen = 1, 10-phenthroline, Nphen = 5-nitro-1, 10-phenanthroline )have been synthesized. The complexes were characterized using elemental analysis,IR and electronic reflection spectra. These complexes are proposed to have extended 1, 3, 5-benzenetricarboxylato-bridged structure and to consist of three manganese (Ⅱ) or three nickel(Ⅱ). The X-band ESR spectra of the complex 1 and complex 2were recorded at room temperature. The variable-temperature magnetic susceptibilities of complex 1 and complex 3 were measured over 4. 2-300 K. According to experimental results of the variable-temperature magnetic susceptibility, the magnetic interaction between the paramagnetic centers is too weak to be detected using the usual magnetic susceptibility technique.
基金supported by the Natural Science Foundation of Hunan Province(2015JJ2072)the Key Laboratory of Comprehensive Utilization of Advantage Plants Resources in Hunan South(XNZW14C08)+1 种基金the Construct Program of the Key Discipline in Hunan Province(2011-76)the Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province(2012-318)
文摘Two complexes with formulas [Ni L][(Ni L)(IPA)2]·8H2O(1) and [(Ni L)(H2O)2] [(Ni L)(PMA)]·4H2O(2)(L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,IPA2– = isophthalic anion,PMA4– = 1,2,4,5-benzenetetracarboxylic anion) were synthesized and characterized by elemental analyses and IR spectra.The crystal structures were determined by X-ray diffraction.In complex 1,the [Ni L]^2+ bridged IPA^2– to give [(Ni L)(IPA)2]^2– monomer,and the [Ni L]^2+ bridged PMA4– to form a one-dimensional chain [(Ni L)(PMA)]n^2n– in complex 2.The [Ni L]^2+ and [(Ni L)(IPA)2]^2–/[(Ni L)(PMA)]^2– are connected through intermolecular hydrogen bonding to generate three-dimensional supramolecular structures.
基金The project was supported by the NSF of Jiangsu Province (No. BK2004205)the Specialized Research Fund for the Doctoral Program of Higher Education (No. 20050285004)
文摘Reactions of NiCl2-6H2O with dmpzm and formic or acetic acid at PH = 7 produced the two title compounds, [Ni(dmpzm)2(HCO2)]Cl·2H2O 1 and [Ni(dmpzm)2(OAc)]C2·H2O 2 (dmpzm = 1,1 '-methylenebis(3,5-dimethyl-lH-pyrazole)). 1 and 2 were characterized by elemental analysis, IR spectra, and thermogravimetric analysis. 1 crystallizes in the orthorhombic system, space group Pcca with a = 18.700(2), b = 8.6843(9), c = 18.098(2)A, V= 2939.1(5)A^3, Z = 4, Dc = 1.319 g/cm^3, T = 193 K, C23H37CINsNiO4, Mr = 583.75, F(000) = 1232, p(MoKa) = 0.792 cm^-1, S = 1.079, R = 0.0772 and wR = 0.1958 for 2265 observed reflections with I〉 2σ(I). 2 crystallizes in the orthorhombic system, space group Pcca with a = 17.011(3), b = 18.630(4), c = 19.300(4)A, V = 6117(2)A^3, Z = 8, Dc = 1.337 g/cm^3, T= 193(2) K, C24H41C1N8NiO5, Mr = 615.79, F(000) = 2608, μ(MoKa) = 0.768 cm^-1, S = 1.059, R = 0.0518 and wR = 0.1109 for 5124 observed reflections with I 〉 2σ(I). The Ni atoms in 1 or 2 are chelated by two dmpzm ligands and one formate or acetate anion, forming slightly distorted octahedral geometries. In the crystals of 1 or 2, intermolecular hydrogen bonding interactions result in the formation of 2D hydrogen-bonded frameworks.
基金Supported by the Natural Science Foundation of Zhejiang Province (No. Y406049)Scientific Research Fund of Zhejiang Provincial Education Department (No. 20060079)
文摘In the ethanol solvent, a nickel(Ⅱ) complex Ni(C12H10N2O2S)2 upon reaction of 2'-(2-thienylidene)-hydroxybenzoylhydrazide with nickel acetate was synthesized, and its structure was characterized by IR, UV, elemental analysis and X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 22.052(3), b = 5.9681(6), c = 18.522(2)A , β = 110.679(4)°, V = 2280.6(4)A^3, Z = 4, Mr = 551.27, μ = 1.606 mm^-1, Dc = 1.075 g/cm^3, F(000) = 1136 and Rint = 0.0556. The nickel(Ⅱ ) atom in the compound is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The biological activities have been measured, show- ing the compound exhibits better anti-bacterial activity than the ligand.
基金supported by the Henan Innovation Project for University Prominent Research Talents (No. 2005KYCX021)Natural Science Foundation of Henan Province (No. 082300420040)
文摘Under given conditions, two complexes of [Ni(H20)2BEDA]·2H2O 1 and [Ni(Py)2- BEDA]·6H2O 2 (BEDA = bis(3-methoxy-2-pyridyl)ether-6,6′-dicarboxylic acid) have been synthesized and characterized by elemental analysis and X-ray single-crystal diffraction. Crystal data for 1: C14H18NiN2O11, monoelinic C2/c, a = 14.3844(17), b = 12.9900(15), c = 9.6309(11) A, β = 104.3350(10)°, V= 1743.5(4) A3, Z = 4, Dc= 1.711 g/cm^3, F(000) = 928, μ = 1.179 mm^-1, Mr= 449.01, the final R = 0.0228 and wR = 0.0625. Crystal data for 2: C24H32NiN4O13, triclinic P1, a = 9.423(2), b = 11.863(3), c = 13.089(3) A, α = 91.511(3), β = 92.465(3), γ = 100.696(2)°, V = 1435.6(6) A^3, Z = 2, Dc= 1.488 g/cm^3, F(000) = 672, μ = 0.748 mm^-1, Mr= 643.25, the final R = 0.0400 and wR = 0.0975. Interestingly, in the two complexes, lattice water molecules dominate its crystal structures. Therefore, extensive intermolecular hydrogen bonds assemble 1 and 2 into 2D extended sheets and a 3D open framework, respectively. Furthermore, water molecules present in 2 are associated to form water clusters.
文摘Three new asymmetrical ruthenium (Ⅱ) complexes :[Ru(phen)2{phen-NHCO(CH2)4BR}](pf6)2,[rU(PHEN)2{PHEN-nhco(ch2)5br}](pf6)2 and [Ru(phen)2{phen-NHCO(CH2)10Br}](PF6)2 were synthesized ,which were confirmed byh the technique of FT-IR 1HNMR and ESI-MS ,The electrochemical and fluorescent properties of three Ru(Ⅱ)complexes were investigated with cyclic voltammetry and fluorometry.