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
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).