Crystals of the title compound, [N 3 P 3 (NMe 2 ) 6 H] 2 CoCl 4 , are orthorhombic, a = 34.623, b = 13.964, c = 10.486 Å, Z = 4, space group P2 1 2 1 2 1 . The structure was determined by Patterson and electron-density methods and refined by full-matrix least-squares procedures to R = 0.088 for 2178 observed reflexions. Both rings are slightly non-planar, with three distinct pairs of NP bonds: commencing at the protonated nitrogen atom, 1.68, 1.56, and 1.58 Å. The CoCl 4 2− ion is tetrahedral and is hydrogen bonded to both rings, N—H … Cl = 3.32, 3.36 Å.
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Macdonald et al. (1974) studied this question.