The K 2 NiF 4 phases La 1+x Sr 1-x Co 0.5 Cr 0.5 O 4±δ (x = 0, 0.15) and La 1+x Sr 1-x Co 0.5 Mn 0.5 O 4±δ (x = 0, 0.2) have been synthesised and examined by X-ray powder diffraction, thermal analysis, neutron powder diffraction and magnetic susceptibility measurements. Mn 3+ /Co 3+ and Cr 3+ /Co 3+ states predominate in the oxidised forms. Structural stability and crystal symmetry are retained under reducing conditions which cause reduction of Co 3+ into Co 2+ and the creation of oxide ion