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
A series of new NIR dyes bearing 4-(4-morpholinyl) phenyl and substituted phenyl, were synthesized. The maximum absorption wavelengths of these dyes range from 928 nm to 990 nm.
A novel nickel（II）-complex Ni[L]Cl2-CH3CN（1） containing the tridentate ligand 2,6-bis[1-（2,4,6- trimethylphenylimino）ethyl]pyridine（L） has been synthesized. The crystal structure of complex 1 was determined by...A novel nickel（II）-complex Ni[L]Cl2-CH3CN（1） containing the tridentate ligand 2,6-bis[1-（2,4,6- trimethylphenylimino）ethyl]pyridine（L） has been synthesized. The crystal structure of complex 1 was determined by single crystal X-ray diffraction analysis. The catalytic activity of complex 1 for the polymerization of ethylene was studied under activation with methylaluminoxane（MAO）.展开更多
A new 3-D nickel（Ⅱ） metal-organic framework（MOFs） with formula [Ni（bib）_2（SO_4）]_n（1）, where bib = 1,4-bis（imidazol-1-yl）benzene, has been synthesized and characterized by single-crystal X-ray diffraction...A new 3-D nickel（Ⅱ） metal-organic framework（MOFs） with formula [Ni（bib）_2（SO_4）]_n（1）, where bib = 1,4-bis（imidazol-1-yl）benzene, has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and surface photovoltage spectroscopy（SPS）. Complex 1 crystallizes in monoclinic system, space group C2/c with a = 19.5988（6）, b = 9.7531（3）, c = 11.8146（4） ？, β = 96.185（3）°, V = 2245.20（12） ？~3, C_（24）H_（20）N_8NiO_4S, M_r = 575.25, D_c = 1.702 g/cm^3, Z = 4, F（000） = 1184, μ = 1.011 mm-1, the final R = 0.0293 and w R = 0.0702. X-ray diffraction analyses indicated that the center Ni^（2＋） ion is six-coordinated with an O_2N_4 donor set of two μ_2-SO_4^（2–） and four bib ligands, resulting in an ideal octahedral geometry. Topological analysis on complex 1 considers each Ni^（2＋） as a 6-connected node, while bib and sulfate ion as linkers, giving an α-Po topology with short Schl？fli symbol 412·63. In the crystal packing, the components interact with pairs of intermolecular C–H×××O hydrogen bonds. The SPS of 1 indicates that there are positive response bands in the range of 300~600 nm showing photo-electric conversion properties.展开更多
The N,N -(phenyl-2-pyridinylmethylene)-3,3 ,5,5 -tetramethylbenzidine and its dimeric Co(Ⅱ)and Ni(Ⅱ) complexes were synthesized.The organic compound was characterized by elemental analyses,IR and NMR spectra,while t...The N,N -(phenyl-2-pyridinylmethylene)-3,3 ,5,5 -tetramethylbenzidine and its dimeric Co(Ⅱ)and Ni(Ⅱ) complexes were synthesized.The organic compound was characterized by elemental analyses,IR and NMR spectra,while the bimetal complexes were determined by elemental analyses,IR spectra as well as the single-crystal X-ray diffraction.The nickel complex showed high activity for ethylene polymerization and its cobalt analogue showed negligible active in ethylene activation.展开更多
A Ni（Ⅱ） complex [Ni（bdpm）2（OAc）]2（N3）2.5H20 （bdpm = bis（3,5-dimethylpyrazol-1-yl）-methane） was synthesized and characterized by elemental analysis, 1R and single-crystal X-ray diffraction. It crystallizes...A Ni（Ⅱ） complex [Ni（bdpm）2（OAc）]2（N3）2.5H20 （bdpm = bis（3,5-dimethylpyrazol-1-yl）-methane） was synthesized and characterized by elemental analysis, 1R and single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 18.630（2）, b = 16.6624（19）, c = 19.821（2） A, fl = 90.146（2）°, V = 6152.9（12） A3, Z = 4, C48H80N22Ni2O9, Mr = 1226.76, Dc = 1.324 g/cm^3, F（000） = 2600 and μ = 0.680 mm^-1. The structure was refined to the final R = 0.0578 and wR = 0.1337 for 10848 independent reflections （Rint = 0.0311） and 6915 observed reflections （1 〉 2σ（I））. The complex contains two asymmetric molecules in the cell with small difference in bond distances and bond angles. Each Ni（Ⅱ） ion is bound by four nitrogen atoms of two chelating bdpm groups in a six-membered boat conformation and two oxygen atoms from one chelating bidentate acetate group to form a distorted octahedral geometry. The complex also contains azide anion outside acting as counteranion and two crystalline water molecules to link two discrete mononuclear cations though hydrogen bonds.展开更多
A new complex with binuclear nickel(Ⅱ) complex [Ni2(bbimp)(CH3CH2OH)2Cl2]Cl· 4H2O (bbimp=2,6 bis[bis(2 benzimidazolylmethyl)]aminomethyl 4 methylpheno)(o)had been synthesized and characterized by elementary anal...A new complex with binuclear nickel(Ⅱ) complex [Ni2(bbimp)(CH3CH2OH)2Cl2]Cl· 4H2O (bbimp=2,6 bis[bis(2 benzimidazolylmethyl)]aminomethyl 4 methylpheno)(o)had been synthesized and characterized by elementary analysis, IR and UV. The molecular structure of the title complex was determined by X ray single crystal diffraction method. The crystal is monoclinic, space group P21/n with a=20.803(2)? , b=30.708(3)? , c=20.959(2)? , β =105.776(2)° , Z=8, V=12885(2)? 3, Dx=1.132Mg· m- 3, μ =0.755mm- 1, F(000)=4592, R1=0.1267, S=1.376. It was showed that the nickel? cation is the central ion of a distorted octahedral coordination with two N belonging to benzimidazole, a bridging phenolate O, a N of tertiary amine, a Cl anion, and an O of an ethanol molecule. Two nickel? cations in a molecular structure had the same coordinated environment. CCDC: 197601.展开更多
The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the t...The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR spectrum of the nickel complex shows three broadening signals at g1=2.097, g2=2.042, g3=2.022. Magnetic susceptibility data for [Bu4N][Ni(CgH6S4)2] reveal enhanced anti-ferromagnetic interaction.展开更多
Two novel metal-organic coordination compounds, [Co2(OH)(chdc)1.5(bibp)]n(1) and [Ni(chdc)(bib)]n·2nH2O(2, H2chdc=1,4-cyclohexanedicarboxylic acid, bibp=4,4’-bis(1-imidazolyl)biphenyl, bib=1,4-bis(1-imidazolyl)b...Two novel metal-organic coordination compounds, [Co2(OH)(chdc)1.5(bibp)]n(1) and [Ni(chdc)(bib)]n·2nH2O(2, H2chdc=1,4-cyclohexanedicarboxylic acid, bibp=4,4’-bis(1-imidazolyl)biphenyl, bib=1,4-bis(1-imidazolyl)benzene), were synthesized and characterized. Compound 1 crystallizes in monoclinic system, space group PI with a=10.591(3), b=11.146(3), c=12.264(3) ?, α=89.009(6), β=88.397(4), γ=87.823(3)°, V=1446.0(6) ?3, Dc=1.554 g/cm3, C30H30Co2N4O7, Mr=676.44, F(000)=696, μ(MoKα)=1.202 mm-1, Z=2, R=0.0278 and wR=0.0718. In 1, it contains an interesting tetranuclear Co(Ⅱ) cluster. The neighboring {Co4} clusters are linked by chdc2-ligands to generate a 2D network. The bibp ligands connect adjacent layers to form an open 3 D metal-organic framework. Compound 2 crystallizes in monoclinic system, space group P21/n with a=8.8110(1), b=19.369(1), c=12.7379(4) ?, β=102.952(5)o, V=2118.5(2) ?3, Dc=1.490 g/cm3, C20H24N4NiO6, Mr=475.14, F(000)=992, μ(MoKα)=0.961 mm-1, Z=4, R=0.0306 and wR=0.0738. In 2, each deprotonated chdc 2-ligand links two Ni(Ⅱ) atoms to generate a 1 D chain along the a axis. The adjacent chains are further connected by bib ligands to build up an interesting two-dimensional network. Compound 1 shows antiferromagnetic property.展开更多
Tridentate bis(oxazolinylpyridine)(1) reacted with nickel chloride or ferrous chloride in anhydrous ethanol to form bis(oxazolinylpyridine) Nickel? and Iron? complexes. The stable solid complexes were characterized wi...Tridentate bis(oxazolinylpyridine)(1) reacted with nickel chloride or ferrous chloride in anhydrous ethanol to form bis(oxazolinylpyridine) Nickel? and Iron? complexes. The stable solid complexes were characterized with IR, UV, MS, XPS and elemental analysis. No stable complexes were formed with bidentate bis(oxazoline)(2) ins tead of bis(oxazolinylpyridine).展开更多
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A series of new NIR dyes bearing 4-(4-morpholinyl) phenyl and substituted phenyl, were synthesized. The maximum absorption wavelengths of these dyes range from 928 nm to 990 nm.
基金National Natural Science Foundation of China(Nos.20771030 and 20671025)Development Program for Outstanding Young Teachers in Harbin Institute of Technology(No.HITQNJS.2006.029)+1 种基金Science Innovation Special Founda-tion of Harbin City in China(No.2006RFQXG037)Young Foundation of Heilongjiang Province, China(No.QC06C029)
文摘A novel nickel（II）-complex Ni[L]Cl2-CH3CN（1） containing the tridentate ligand 2,6-bis[1-（2,4,6- trimethylphenylimino）ethyl]pyridine（L） has been synthesized. The crystal structure of complex 1 was determined by single crystal X-ray diffraction analysis. The catalytic activity of complex 1 for the polymerization of ethylene was studied under activation with methylaluminoxane（MAO）.
基金supported by the Guangxi Provincial Department of Education(No.KY2015ZD130,YB2014414)the Natural Science Foundation of Guangxi Province(No.2014GXNSFBA118040)+2 种基金The supports of the National Natural Science Foundation of China(No.51402158)are gratefully acknowledgedthe financial support by the Opening Project of Guangxi Colleges and Universities Key Laboratory of Beibu Gulf Oil and Natural Gas Resource Effective Utilization(No.2015KLOG09)the financial support from the Natural Science Foundation of Qinzhou University(No.2014PY-GJ05)
文摘A new 3-D nickel（Ⅱ） metal-organic framework（MOFs） with formula [Ni（bib）_2（SO_4）]_n（1）, where bib = 1,4-bis（imidazol-1-yl）benzene, has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and surface photovoltage spectroscopy（SPS）. Complex 1 crystallizes in monoclinic system, space group C2/c with a = 19.5988（6）, b = 9.7531（3）, c = 11.8146（4） ？, β = 96.185（3）°, V = 2245.20（12） ？~3, C_（24）H_（20）N_8NiO_4S, M_r = 575.25, D_c = 1.702 g/cm^3, Z = 4, F（000） = 1184, μ = 1.011 mm-1, the final R = 0.0293 and w R = 0.0702. X-ray diffraction analyses indicated that the center Ni^（2＋） ion is six-coordinated with an O_2N_4 donor set of two μ_2-SO_4^（2–） and four bib ligands, resulting in an ideal octahedral geometry. Topological analysis on complex 1 considers each Ni^（2＋） as a 6-connected node, while bib and sulfate ion as linkers, giving an α-Po topology with short Schl？fli symbol 412·63. In the crystal packing, the components interact with pairs of intermolecular C–H×××O hydrogen bonds. The SPS of 1 indicates that there are positive response bands in the range of 300~600 nm showing photo-electric conversion properties.
文摘The N,N -(phenyl-2-pyridinylmethylene)-3,3 ,5,5 -tetramethylbenzidine and its dimeric Co(Ⅱ)and Ni(Ⅱ) complexes were synthesized.The organic compound was characterized by elemental analyses,IR and NMR spectra,while the bimetal complexes were determined by elemental analyses,IR spectra as well as the single-crystal X-ray diffraction.The nickel complex showed high activity for ethylene polymerization and its cobalt analogue showed negligible active in ethylene activation.
基金This work was supported by the Natural Science Foundation of South China University of Technology (20501008) and Guangdong Provincial Laboratory for Green Chemical Technology
文摘A Ni（Ⅱ） complex [Ni（bdpm）2（OAc）]2（N3）2.5H20 （bdpm = bis（3,5-dimethylpyrazol-1-yl）-methane） was synthesized and characterized by elemental analysis, 1R and single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 18.630（2）, b = 16.6624（19）, c = 19.821（2） A, fl = 90.146（2）°, V = 6152.9（12） A3, Z = 4, C48H80N22Ni2O9, Mr = 1226.76, Dc = 1.324 g/cm^3, F（000） = 2600 and μ = 0.680 mm^-1. The structure was refined to the final R = 0.0578 and wR = 0.1337 for 10848 independent reflections （Rint = 0.0311） and 6915 observed reflections （1 〉 2σ（I））. The complex contains two asymmetric molecules in the cell with small difference in bond distances and bond angles. Each Ni（Ⅱ） ion is bound by four nitrogen atoms of two chelating bdpm groups in a six-membered boat conformation and two oxygen atoms from one chelating bidentate acetate group to form a distorted octahedral geometry. The complex also contains azide anion outside acting as counteranion and two crystalline water molecules to link two discrete mononuclear cations though hydrogen bonds.
文摘A new complex with binuclear nickel(Ⅱ) complex [Ni2(bbimp)(CH3CH2OH)2Cl2]Cl· 4H2O (bbimp=2,6 bis[bis(2 benzimidazolylmethyl)]aminomethyl 4 methylpheno)(o)had been synthesized and characterized by elementary analysis, IR and UV. The molecular structure of the title complex was determined by X ray single crystal diffraction method. The crystal is monoclinic, space group P21/n with a=20.803(2)? , b=30.708(3)? , c=20.959(2)? , β =105.776(2)° , Z=8, V=12885(2)? 3, Dx=1.132Mg· m- 3, μ =0.755mm- 1, F(000)=4592, R1=0.1267, S=1.376. It was showed that the nickel? cation is the central ion of a distorted octahedral coordination with two N belonging to benzimidazole, a bridging phenolate O, a N of tertiary amine, a Cl anion, and an O of an ethanol molecule. Two nickel? cations in a molecular structure had the same coordinated environment. CCDC: 197601.
基金Project supported by grants for key research project in climbing program from the State Science and Technology Commission,and the National Nature Science Foundation of China.
文摘The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR spectrum of the nickel complex shows three broadening signals at g1=2.097, g2=2.042, g3=2.022. Magnetic susceptibility data for [Bu4N][Ni(CgH6S4)2] reveal enhanced anti-ferromagnetic interaction.
基金This work was financially supported by the National Natural Science Foundation of China(21571034)。
文摘Two novel metal-organic coordination compounds, [Co2(OH)(chdc)1.5(bibp)]n(1) and [Ni(chdc)(bib)]n·2nH2O(2, H2chdc=1,4-cyclohexanedicarboxylic acid, bibp=4,4’-bis(1-imidazolyl)biphenyl, bib=1,4-bis(1-imidazolyl)benzene), were synthesized and characterized. Compound 1 crystallizes in monoclinic system, space group PI with a=10.591(3), b=11.146(3), c=12.264(3) ?, α=89.009(6), β=88.397(4), γ=87.823(3)°, V=1446.0(6) ?3, Dc=1.554 g/cm3, C30H30Co2N4O7, Mr=676.44, F(000)=696, μ(MoKα)=1.202 mm-1, Z=2, R=0.0278 and wR=0.0718. In 1, it contains an interesting tetranuclear Co(Ⅱ) cluster. The neighboring {Co4} clusters are linked by chdc2-ligands to generate a 2D network. The bibp ligands connect adjacent layers to form an open 3 D metal-organic framework. Compound 2 crystallizes in monoclinic system, space group P21/n with a=8.8110(1), b=19.369(1), c=12.7379(4) ?, β=102.952(5)o, V=2118.5(2) ?3, Dc=1.490 g/cm3, C20H24N4NiO6, Mr=475.14, F(000)=992, μ(MoKα)=0.961 mm-1, Z=4, R=0.0306 and wR=0.0738. In 2, each deprotonated chdc 2-ligand links two Ni(Ⅱ) atoms to generate a 1 D chain along the a axis. The adjacent chains are further connected by bib ligands to build up an interesting two-dimensional network. Compound 1 shows antiferromagnetic property.
文摘Tridentate bis(oxazolinylpyridine)(1) reacted with nickel chloride or ferrous chloride in anhydrous ethanol to form bis(oxazolinylpyridine) Nickel? and Iron? complexes. The stable solid complexes were characterized with IR, UV, MS, XPS and elemental analysis. No stable complexes were formed with bidentate bis(oxazoline)(2) ins tead of bis(oxazolinylpyridine).
