Abstract: | Synthesis and Structure Determination of Two Salts of the Trimetaphosphimic Acid, K3(PO2NH)3 and Rb3(PO2NH)3 The reaction between P3N5 and the corresponding alkalimetal hydroxide monohydrate under ammonothermal conditions (6 kbar, 450 °C after 10 d) in autoclaves leads to the salts of the trimetaphosphimic acid K3(PO2NH)3 resp. Rb3(PO2NH)3. The structure of K3(PO2NH)3 was solved by single crystals X-ray methods. The isotypic structure of Rb3(PO2NH)3 was solved by X-ray powder diffraction methods. K3(PO2NH)3: R3 (No. 148), a = 12.615(3) Å, c = 10.224(2) Å, Z = 6, R1/wR2 = 0.0276/0.0726, N(F > 2σ(F)) = 769, N(Var.) = 51.Rb3(PO2NH)3: R3 (No. 148), a = 12.9971(5) Å, c = 10.5485(5), Z = 6, RBragg(F) = 0.0626, 289 reflections. K3(PO2NH)3 and Rb3(PO2NH)3 contain six-membered rings P3N3 substituted by oxygen which are connected to double molecules by N–H … O bridge bonds. These twinmolecules are stacked in columns which form the motive of close packed rods. K+ resp. Rb+ are between these columns. They are coordinated by 6 O which belong to 5 different rings. |