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Coarsely crystalline [C(NH 2 ) 3 ] 3 (PO 2 NH) 3  · H 2 O (1) and [C(NH 2 ) 3 ] 4 (PO 2 NH) 4  · 4 H 2 O (2) have been obtained by addition of [C(NH 2 ) 3 ] 2 CO 3  to a freshly prepared solution of H 3 (PO 2 NH) 3  or to a suspension of H 4 (PO 2 NH) 4  · 2 H 2 O , respectively, followed by diffusion controlled addition of acetone. The crystal structures of 1 and 2 have been determined by single crystal X-ray methods ([C(NH,) 3 ] 3 (PO,NH) 3  · H 2 O: Pbca; a = 1565.6(2), b = 1068.31(6), c = 2091.8(2) pm, Z = 8; [C(NH 2 ) 3 ] 4 (PO 2 NH) 4  · 4 H 2 O: Pbcn; a = 1739.64(10), b = 1084.19(6), c = 1334.96(11) pm, Z = 4). The P 3 N 3  and P 4 N 4  rings of the anions exhibit the chair conformation. In 1 two cyclic anions are interconnected into pairs via hydrogen bonds. In 2 columns along [001] are formed by hydrogen bonds between the anions. Hydrogen bonding through water molecules and C(NH 2 ) 3  +  ions results in a three-dimensional network in 2. Complete dehydration is achieved below 160 or 180 °C for 1 or 2, respectively. Heating to 700 °C causes condensation reactions with evolution of NH 3  and H 2 O yielding X-ray amorphous products

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Synthese, Kristallstruktur und Eigenschaften von Triguanidinium-tri--imidocyclotriphosphat-Monohydrat und Tetraguanidinium-tetra-/i-imidocyclotetraphosphat-Tetrahydrat, [C(NH 2 ) 3 ] 3 (PO 2 NH) 3  · H 2 O und [C(NH 2 ) 3 ] 4 (PO 2 NH) 4  · 4 H 2 O / Synthesis, Crystal Structure, and Properties of Triguanidinium Tri-/i-imidocyclotriphosphate Monohydrate and Tetraguanidinium Tetra-/i-imidocyclotetraphosphate Tetrahydrate, [C(NH 2 ) 3 ] 3 (PO 2 NH) 3  · H 2 O and [C(NH 2 ) 3 ] 4 (PO*  NH) 4  · 4 H 2 O