Citation: XIE Xing-Kun, ZHANG Xiao-Feng, LIU Hai-Xiong, WANG Yang, CHEN Chang-Neng, HUANG De-Guang. Synthesis of a Hexagonal Molecular Nickel-wheel[J]. Chinese Journal of Structural Chemistry, ;2015, 34(11): 1689-1696. doi: 10.14102/j.cnki.0254-5861.2011-0725 shu

Synthesis of a Hexagonal Molecular Nickel-wheel

a.
a. College of Chemistry, Fuzhou University, Fuzhou 350002, China;
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b. State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, China

Corresponding author: HUANG De-Guang,
Received Date: 23 March 2015
Available Online: 20 April 2015
Fund Project: This investigation was granted by the National Natural Science Foundation of China (No. 21371171). (No. 21371171)

The macrocyclic ligand ⊂-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)(⊂-pyN₂-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 MoKα radiation diffractometer (λ=0.71073 Å): the crystal of 3 was grown in space group P2₁2₁2₁ with a=12.079(5), b=15.099(6), c=17.299(8) Å, V=3160(2) Å³, Z=4, D_c=1.369 g/cm³, F(000)=1384, C₃₃H₄₄N₄NiO₆, M_r=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) Å, β=106.195(2)°, V=8681.5(14) Å³, Z=2, Dc=1.352 g/cm³, F(000)=3704, C₁₇₀H₁₉₀N₂₂Ni₆O₄₀, M_r=3533.70, μ=719 cm^-1, R=0.0841 and wR=0.2339 for 9371 observed reflections with I>2σ(I).
- macrocyclic ligand,
- hydroxide,
- hexagonal,
- nickel-wheel
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