In a one-pot reaction, the tetranuclear iron chelate complex [Fe 4 (L 4 ) 4 ] 6 was generated from benzene-1,3,5-tricarboxylic acid trichloride (4), bis-tert-butyl malonate (5 a), methyllithium, and iron(ii) dichloride under aerobic conditions. Alternatively, hexanuclear iron chelate complex [Fe 6 (L 5 ) 6 ] 7 was formed starting from bis-para-tolyl malonate (5 b) by employing identical reaction conditions to those applied for the synthesis of 6. The clusters 6 and 7 are present as racemic mixtures of homoconfigurational (D