Solid-state molecular structure for (a) (TrHBOX)NiI(py) (3) and (b) (TrHBOX)Ni(py) (4) with thermal ellipsoids at 50% probability level. Color scheme: Ni, pink; N, blue; C, gray; O, red; I, purple. H atoms (except for the ones on chiral centers and meso carbon) and solvent molecules omitted for clarity. (c) Frozen solution EPR spectrum of (TrHBOX)Ni(py) (4) collected at 77 K in toluene (Red). Blue line represents a fit of the data using the program EasySpin.55 Fitting parameters: S = ½, g1 = 2.43, g2 = 2.13, g3 = 2.07.