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We show here that the phenomenon of spontaneous resolution of enanti-omers occurs during the crystallization of the sodium and rubidium double salts of the transition metal complex tris-(oxalato)ferrate(III), namely sodium penta-rubidium bis-[tris-(oxalato)ferrate(III)], NaRb 5 [Fe(C 2 O 4 ) 3 ] 2 . One enanti-omer of the salt crystallizes in the cubic space group P 4 3 32 with Z = 4 and a Flack absolute structure parameter x = -0.01 (1) and its chiral counterpart in the space group P 4 1 32 with x = -0.00 (1). All metal ions are at crystallographic special positions: the iron(III) ion is on a threefold axis, coordinated by three oxalate dianions in a propeller-like conformation. One of the two independent rubidium ions is on a twofold axis in an eightfold coordination with neighbouring oxalate oxygen atoms, and the other one on a threefold axis in a sixfold RbO 6 coordination. The sodium ion is at a site of D  3 point group symmetry in a trigonal-anti-prismatic NaO 6 coordination.

Spontaneous enantiomorphism in poly-phased alkaline salts of tris(oxalato)ferrate(III): crystal structure of cubic NaRb5[Fe(C2O4)3]2