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The variable coordination behavior of 2-[(2-hydroxy-3-methoxybenzyl)imino]methyl-6-methoxyphenol (H2L) and its hydrolyzed congener towards NiCl2·6H2O and LnIII nitrate salts provides a family of coordination aggregates containing an [Ni5Ln3] octanuclear core structure. Room temperature reactions in MeOH-CHCl3 medium and in the presence of NEt3 yielded isostructural [Ni5Ln3(L)4(μ-OH)2(μ3-OH)6(o-val)2(H2O)6]NO3·7H2O (Ln = Dy3+ (1), Tb3+ (2), and Ho3+ (3); o-val = o-vanillin) heterometallic complexes. All the three complexes hold an octan
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