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A DEER (double electron–electron resonance) spin–echo technique was applied to measure the electron–electron dipolar spectrum of a frozen toluene solution of the biradical, 2,6‐bis[(((2,2,5, 5‐tetramethyl‐1‐oxypyrrolin‐3‐yl)carbonyl)oxy)]‐anthracene. Modulation of the DEER spin–echo envelope was observed and identified as originating from the dipolar coupling between the two nitroxide spins of the biradical. Fourier transformation of the modulated components of the echo envelope yielded a dipolar spectrum from which a spin–pair separation of 19.73±0.14 Å was calculated. Constraints on the relative orientation of the two nitroxide spin moieties were obtained by analysis of the effect of the microwave pulse orientational selectivity on the DEER modulation amplitudes. Molecular models of the studied compound exhibit structures that correspond well with the structural information deduced by DEER …