AbstractThe crystals of bis‐dimethyl glyoximino‐diammine cobalt(III) nitrate are Monoclinic with Space‐group P21/cand the cell‐dimensions are a = 9.80 ± 0.03 Å, b = 6.32 ±. 02 Å, c = 12.47 ±. 04 Å, β = 97°. The crystal data indicates either a free rotation or a statistical distribution in two different orientations of the oxygen atoms round nitrogen of the nitrate ion.The crystals of the chloride complex are Tetragonal with Space‐group P42and the cell dimensions are a = 6.50 +. 02 Å