Synthesis and Structural Characterization of a Novel Cyclotetraphosphate

The crystal structure of (2-NH2-5-ClC5H4N)4P4O12.6H2O was determined by X-ray diffraction on a single crystal. This compound crystallizes in an orthorhombic unit cell Pccn with the parameters a = 25,387(7) Å, b = 15,756(6) Å, c = 9,750(5) Å, V = 3900(2) Å3, Z = 4, and Dx = 1,605 g.cm-3. Crystal structure has been determined and refined to R = 0,036, using 7678 independent reflexions. This structure can be described as inorganic layers stacked along a-direction and held together through N-H… O hydrogen bonds, originating from the organic cations, giving rise to three-dimensional H-bonded assemblies. In addition, in this structure there is electrostatic, van der Waal forces and Cl… Cl interaction so as to increase the cohesion of 3D-network. Chemical preparation and characterization by RX diffraction, IR absorption, and thermal analysis are described.