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Thermal spin crossover (SCO) was induced in a high‐spin FeIII complex by alkylation of the polyamino ligand backbone. The SCO profile was responsive to chain length with partial crossover observed with C6 alkylation and full transition upon lengthening to C12. No crossover was observed when the backbone was unfunctionalised, and all three complexes were obtained as unsolvated tetrafluoroborate salts.
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