For compound 4, the Fourier transform EXAFS (Figure ) shows a notable increase in scattering intensity at long distances compared to 3, with strong features evident up to 5 Å (not phase-shift corrected). Despite the structural similarity of 3 and 4, the EXAFS behavior indicates slight changes in bond distances and angles between Co and the tBu PNNP ligand system that result in significant multiple scattering contributions from the rings. The features from 1-2.5 Å in the Fourier transform spectra were fitted by The geometrical features of complexes 1 and 2 were also probed using EXAFS, and the geometrical parameters for both these complexes match those determined by scXRD (Figure ) well (see SI for detailed discussion).