Anal. Calcd. for [Co(C2H8NZ)2C~O4]C1~Hz0: C, 22.48; H,5.66; N, 17.48. Found: C,22.70; H, 5.76; N, 17.69.
d-Oxalatobisethylenediamine-cobalt(II1)Iodide .-The dl-chloride, above, (12.84 9.) in water (80 ml., 65"), was shaken with silver acetate (6.4 g.) for 10 min. The silver chloride was removed and washed with hot water. To the filtrate a t 60' was added l-K[CoEDTA].2Hz0 (8.44 8.) and dissolved by shaking. Almost immediately the diastereoisomer d-[CoenzCz04]-Z-[Co(EDTA)]~ 3Hz0 commenced t o separate, and the mixture was allowed to cool slowly to room temperature. The pink-violet diastereoisomer was then collected, washed with ice-water and then ethanol and air-dried (yield, 10.7 g., [ a ]~ = +550°). Anal. Calcd. for [CO(C~H,NZ)Z(CZO~)] [CO(C~OHIZNZOS)]-3H20: C, 28.75; H, 5.13; N, 12.58. Found: C, 29.0; H , 4.91; N, 12.63.The diastereoisomer was ground up with water (50 ml.) containing potassium iodide (10 9.) and the insoluble d-iodide collected. The resolving agent was recovered from the iiltrate by adding alcohol (yield, 7.2 g., 85%). The d-iodide (7.0 g.) was recrystallized from a large volume of hot water. By standard methods using the appropriate silver salts, the chloride, bromide and sulfate were prepared. The specific rotations [ C Y ] D~ were: [CoenzC204]I, +72OO0; [CoenzCt04] Br.HZ0, $820 . [Coen2C?04] Cl.HzO, +930 ; [CoenzCz04] 2-Anal. Calcd. for [ C O ( C~H~N~)~( C~O~) ] I : C, 18.28; H, 4.09; N, 14.22. Found: C, 18.51; H , 4.16; N, 13.90. l-Oxalatobis-( ethylenediamine)-cobalt( 111) Bromide 1-Hydrate.-The filtrate from the separation of the diastereoisomer above was treated a t 60' with 50% aqueous ammonium bromide (20 ml.) and the crystalline I-bromide collected after cooling. It was recrystallized once from hot water (yield, 6.