The macrocyclic ligand c-H2pyN2-O3ane （2） was readily prepared in a diluted condition in THF. The mixture of 2 and Ni（OTf）2 in DMF using Et4NOH as the base source gave a mononuclear square planar complex （Et4N）...The macrocyclic ligand c-H2pyN2-O3ane （2） was readily prepared in a diluted condition in THF. The mixture of 2 and Ni（OTf）2 in DMF using Et4NOH as the base source gave a mononuclear square planar complex （Et4N）[Ni（OH）（c-pyNE-O3ane）] （3）. Addition of Fe（OTf）2 into the solution of 3 in DMF instantly generated a hexagonal molecular nickel-wheel 4 in 72% yield. Both 3 and 4 were characterized by X-ray crystallography on a MoKa radiation diffractometer （λ= 0.71073 A）： the crystal of 3 was grown in space group P212121 with a = 12.079（5）, b=15.099（6）, c = 17.299（8） A, V = 3160（2） A3, Z = 4, Dc = 1.369 g/cm3, F（000） = 1384, C33H44N4NiO6, Mr = 651.43, μ= 0.665 cm-1, R = 0.0353, wR = 0.0668 for 4548 observed reflections with I〉 2σ（I）; 4 is in space group P21/n with a = 17.7416（17）, b = 17.5490（17）, c = 29.036（3）A,β = 106.195（2）°, V= 8681.5（14） As, Z = 2, Dc = 1.352 g/cm3, F（000） = 3704, C170H190N22Ni6O40, Mr = 3533.70,μ = 719 cm-1, R = 0.0841 and wR = 0.2339 for 9371 observed reflections with I〉 2σ（I）.展开更多
A new metal-organic coordination polymer, [Ag（L）（NO3）]H （1, L = β-amino-β- （pyrid-2-yl）acrylonitrile）, has been synthesized by solvent method at ambient temperature and characterized through single-crystal d...A new metal-organic coordination polymer, [Ag（L）（NO3）]H （1, L = β-amino-β- （pyrid-2-yl）acrylonitrile）, has been synthesized by solvent method at ambient temperature and characterized through single-crystal diffraction, Fourier transformed infrared spectrum （FTIR）, elemental analysis, thermogravimetry analysis （TGA） and fluorescent measurements. 1 crystallizes in the triclinic system, space group Pi with a = 7.3600（3）, b = 8.5095（17）, c = 9.2936（14） A, α= 66.65（6）, β = 70.56（7）, γ= 71.59（6）°, V = 492.4（4） A3, μ = 2.043 mm-1, Dc = 2.104 Mg/m3, Z = 2, Mr = 312.01, F（000） = 302, the final R = 0.0347 and wR = 0.0987 for 3924 observed reflections with I 〉 2σ（I）.展开更多
基金granted by the National Natural Science Foundation of China(No.21371171)
文摘The macrocyclic ligand c-H2pyN2-O3ane （2） was readily prepared in a diluted condition in THF. The mixture of 2 and Ni（OTf）2 in DMF using Et4NOH as the base source gave a mononuclear square planar complex （Et4N）[Ni（OH）（c-pyNE-O3ane）] （3）. Addition of Fe（OTf）2 into the solution of 3 in DMF instantly generated a hexagonal molecular nickel-wheel 4 in 72% yield. Both 3 and 4 were characterized by X-ray crystallography on a MoKa radiation diffractometer （λ= 0.71073 A）： the crystal of 3 was grown in space group P212121 with a = 12.079（5）, b=15.099（6）, c = 17.299（8） A, V = 3160（2） A3, Z = 4, Dc = 1.369 g/cm3, F（000） = 1384, C33H44N4NiO6, Mr = 651.43, μ= 0.665 cm-1, R = 0.0353, wR = 0.0668 for 4548 observed reflections with I〉 2σ（I）; 4 is in space group P21/n with a = 17.7416（17）, b = 17.5490（17）, c = 29.036（3）A,β = 106.195（2）°, V= 8681.5（14） As, Z = 2, Dc = 1.352 g/cm3, F（000） = 3704, C170H190N22Ni6O40, Mr = 3533.70,μ = 719 cm-1, R = 0.0841 and wR = 0.2339 for 9371 observed reflections with I〉 2σ（I）.
基金supported by the Natural Science Foundation of Fujian Province(2012J06006,2006L2005)
文摘A new metal-organic coordination polymer, [Ag（L）（NO3）]H （1, L = β-amino-β- （pyrid-2-yl）acrylonitrile）, has been synthesized by solvent method at ambient temperature and characterized through single-crystal diffraction, Fourier transformed infrared spectrum （FTIR）, elemental analysis, thermogravimetry analysis （TGA） and fluorescent measurements. 1 crystallizes in the triclinic system, space group Pi with a = 7.3600（3）, b = 8.5095（17）, c = 9.2936（14） A, α= 66.65（6）, β = 70.56（7）, γ= 71.59（6）°, V = 492.4（4） A3, μ = 2.043 mm-1, Dc = 2.104 Mg/m3, Z = 2, Mr = 312.01, F（000） = 302, the final R = 0.0347 and wR = 0.0987 for 3924 observed reflections with I 〉 2σ（I）.
