Aminoguanidinium(1+) pentafluorozirconate: multiple redetermination and comparisons

The structure of CN(4)H(7)ZrF(5) reported by Bukvetskii et al. [Koord. Khim. (1992). 18, 576-579] has been independently redetermined on the basis of measurements on three different crystals. Assuming all four resulting structures are drawn from a normal distribution, normal probability analysis of the atomic coordinates taken in pairs reveals joint standard uncertainties that are underestimated by factors as large as 16.5 for the x(Zr) coordinate. Unit-cell parameters in the four crystals similarly have joint uncertainties, under the same assumption, that are underestimated by factors as large as 83.0 for the b axis. The variations in axial lengths from crystal to crystal and the declines in standard reflection intensities by 13-15% in at least two of the crystals measured are consistent with the inference that the distribution is not normal. Rather, the differences observed may be assumed to be caused by small but highly significant radiation-induced structural changes. The large underestimations hence reflect physical differences among the four irradiated crystals. The determinations show that the CN(4)H(7)(+1) cation is exactly planar except for the two H atoms bonded to the terminal N atom; the plane of this NH(2) group is normal to that of the cation. The average length of the three independent C-N bonds is 1.318 (11) A; the N-N bond length is 1.397 (3) A. Distorted ZrF(7) pentagonal bipyramids share edges, forming chains linked by N-H...F bonds to the CN(4)H(7)(+1) ions.