Synthesis of a Hexagonal Molecular Nickel-wheel

摘要

The macrocyclic ligand -H2 py N2-O3ane(2) was readily prepared in a diluted condition in THF.The mixture of 2 and Ni(OTf)2 in DMF using Et4 NOH as the base source gave a mononuclear square planar complex(Et4N)[Ni(OH)(-py N2-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 Mo Kα radiation diffractometer(λ=0.71073 ?):the crystal of 3 was grown in space group P212121 with a=12.079(5),b=15.099(6),c=17.299(8) ?,V=3160(2) ?3,Z=4,Dc=1.369 g/cm3,F(000)=1384,C33H44N4 Ni O6,Mr=651.43,μ=0.665 cm-1,R=0.0353,w R=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) ?,β=106.195(2)°,V=8681.5(14) ?3,Z=2,Dc=1.352 g/cm3,F(000)=3704,C170H190N22Ni6O40,Mr=3533.70,μ=719 cm-1,R=0.0841 and w R=0.2339 for 9371 observed reflections with I > 2σ(I).