Abstract

The crystal structure of [(NH3)5CoO2Co(NH3)5] (SCN)4, originally determined by Vannerberg in 1965, has been reinvestigated. Our values of the unit-cell dimensions are a = 13.266 (2), b = 10.574 (2), c = 7.940 (2) A; the space group is Pnnm. We collected data on an automated diffractometer using Co Kα radiation, and least-squares refinement on 824 observed reflections yielded an R index of 0.042. The cobalt atoms and the peroxide linkage of the cation lie in a mirror plane. Two of the three crystallographically distinct thiocyanate groups are disordered about twofold axes. The O-O distance, 1.469 (6) A, is much shorter than that reported in Vannerberg's earlier investigation.

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