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Herein a series of chiral BTI radical anions bearing different chiral substituents were efficiently prepared by chemical reduction. X‐ray crystallography revealed finely‐tuned packing and helix assemblies of the radicals by the size of chiral substituents in crystalline state. In accordance with the crystalline‐state packing, the powder ESR spectra indicate that 4 a−⋅CoCp2+ and 4 c−⋅CoCp2+ π‐dimers...
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