The reduction of cis-[CoIII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2]Cl into the neutral compound cis-[CoII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2] was observed during developmental studies of new antimalarial drugs. The crystal structure of cis-[CoII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2] was unveiled by powder X-ray diffraction studies (PXRD). PXRD details, unit cell parameters, and space group for cis-[CoII(κ2N,N′-1,10-phenanthroline-5,6-dione)2Cl2], C24H12Cl2CoN4O4, are reported [a = 41.4951 (13) Å, b = 8.2768 (2) Å, c = 12.4994 (3) Å, unit cell volume V = 4292.9 (2) Å3, Z = 8, and space group Fdd2]. Infrared spectroscopy features are also discussed.