Synthesis and characterization of a new cyclohexaphosphate, (C6H7ClN)6P6O18·0.5(H2O)

• A new cyclohexaphosphate (C6H7ClN)6P6O18·0.5(H2O) was synthesized.
• The structure involves a network of inorganic parallel layers built up by P6O186− ring anions, NH3 groups and water molecules.
• The crystal packing is also stabilized hydrogen bonds.
• The 13C, 15N and 31P CP-MAS NMR spectra are in agreement with the X-ray structure.

A new cyclohexaphosphate with the composition (C6H7ClN)6P6O18·0.5(H2O) has been synthesized at room temperature in the presence of 4-chloroaniline as organic template and investigated by various physicochemical techniques. Its unit cell is triclinic P-1 with parameters a = 9.0054(8), b = 10.1053(9), c = 16.4454(14) Å, α = 100.476(7), β = 93.485(7), γ = 115.407(9) °, Z = 2 and V = 1313.0(2)Å3. The structure involves a network of inorganic parallel layers built up by P6O186− ring anions, NH3 groups and water molecules. Charge balance is achieved by the protonated amine which is trapped in the interlayer space and interacts with the organic framework through strong hydrogen bonding. The 13C, 15N and 31P CP-MAS NMR spectra are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks.