Acta Cryst. (2006). B62, 798-807 [ doi:10.1107/S0108768106025171 ]
Abstract: Reaction of cyanuric acid (C3H3N3O3; neutral form CYH3; anionic form CYH
; dianionic form CYH2-) with K2CO3 or KOH in aqueous solution gave three different crystalline products, according to the reaction stoichiometry used. The structures of two products were easily determined by single-crystal X-ray diffraction: [K(CYH2)(H2O)], (1), of which the crystal structure is already known [Marsh, R. E. et al. (2002). Acta Cryst. B58, 62-77], and [K2(CYH)], (2), a highly symmetrical and dense structure. Further stoichiometric variation produced another new complex, (3), and reaction of Rb2CO3 with CYH3 yielded a further product, (4), which was found to be isostructural with (3). Determination of the structures of (3) and (4) by X-ray diffraction gave a result that was chemically unreasonable owing to a charge imbalance, with the asymmetric unit apparently containing 2- against 1.5+ (partial charges as the result of crystallographic mirror symmetry). A single-crystal neutron diffraction analysis carried out on a fully deuterated sample of (3) revealed the presence of a supercell, with the c axis doubled compared with the X-ray result. Subsequent refinement of the structure with this supercell showed that it is the result of just two D atoms breaking crystallographically imposed mirror symmetry, which is otherwise essentially observed by the rest of the structure. This minor deviation from pseudo-symmetry could not be identified by X-ray diffraction. Thus, single-crystal neutron diffraction data revealed that the true chemical formula of the structure of (3) [and presumably also of the isostructural (4) with Rb instead of K and H instead of D], is [K3(C3D2N3O3)3(C3D3N3O3)(D2O)4], the deuterated form of [K3(CYH2)3(CYH3)(H2O)4].
Keywords: stoichiometry-dependent structures; potassium-cyanurate systems.
 |   Structure factor file (CIF format) (60.2 kbytes) |
| Structure factor file (CIF format) (25.9 kbytes) |
| Structure factor file (CIF format) (400.9 kbytes) |
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