A new pentadentate N-isobutyrylsalicylhydrazidate ligand (H(3)ibushz, C11H14N2O3) and a self-assembly synthesis of the first 24-azametallacrown-8, [Fe-8(C11H11N2O3)(8)(CH3OH)(8)].0.5CH(2)Cl(2).7.5CH(3)OH.3.5H(2)O, have been reported. Eight Fe(III) ions and eight deprotonated ibushz(3-) ligands construct a planar 24-membered ring based on the M-N-N-M linkage. The chiralities of the iron atoms on the 24-azametallacrown-8 ring alternate between the A and A forms. The title octanuclear azametallacrown has no crystallographic centrosymmetry, while all the known metallacrowns and azametallacrowns with an even nuclear number have crystallographic centrosymmetry. The study of H-1 NMR spectra suggests that the title compound retains its metallacrown structure in solution at room temperature over a period of at least three months. There exists a strong antiferromagnetic exchange interaction between the iron paramagnetic centers.