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The asymmetric assembly and spontaneous resolution of chiral heterometal-organic frameworks from achiral precursors remain a great challenge.Herein,we report the formation and spontaneous resolution of three-dimensional(3D)chiral 3d-4f hetero-metal-organic frameworks from achiral ligands in the presence of lactic acid enantiomers as chiral inducers.In the absence of a chiral inducer,the reactants randomly generated both enantiopure crystals in equal measure.However,enantiopure lactic acid induced asymmetric resolution to achieve single chiral crystallization.DFT theoretical calculations showed that the absolute chiral resolution of the enantiomers is due to the difference in the interactions between the two enantiomeric Λ/Δ-[FeL3]3-units and the chiral inducer.