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The structure of the title cation, I+-hyponitrito-bisrpenta-amminecobalt(lll)], has been determined as a mixed bromide-nitrate salt from single-crystal three-dimensional X-ray photographic data, the stoicheiometry of the crystals used being [ C O ( N H ~) ~N O ] ~B ~~-, ( N O ~) ~+ , . ~H , O , where x = ca. 0.5. The structure was solved by Patterson and Fourier methods, and refined by least-squares techniques to R 0.1 3 for 1264 independent reflections. The complex cation is binuclear with the two metal atoms bridged by a hyponitrito-group in a cis-asymmetric manner via a nitrogen atom and the oxygen atom bonded to the other nitrogen atom of the hyponitrite group. The unit cell is monoclinic with Z = 4, a = 13.72(3), b = 7.00(2), c = 23.65(4) 8, p = 100.4(2)", space group A2/m.THERE has been much controversy about the nature of the red and black isomers of the nitrosylpenta-amminecobalt (111) ion since their initial preparation.1 This has been due largely to misleading conclusions drawn from the magnetic data of impure samples of the black isomer, conflicting iiiterpretations of the different chemical reactivities exhibited by the two isomeric forms, and the disputed assignments of the NO stretching frequencies in the i.r. spectra.