Synthesis, Structure, and Physicochemical Studies of Hexakis (5-Chloro-2,4-dimethoxyanilinium)cyclohexaphosphate Tetrahydrate

• Published in: Phosphorus, sulfur, and silicon and the related elements sulfur, and silicon and the related elements, 2010-03, Vol.185 (3), p.595-601
• Main Authors: Salah, R. Bel Haj, Khedhiri, L., Nasr, C. Ben, Rzaigui, M., Lefebvre, F.
• Format: Article
• Language: English
• Subjects: Crystal structure; cyclohexaphosphate; IR spectroscopy; NMR; Nuclear magnetic resonance; Spectrum analysis; thermal analysis; X-ray diffraction
• ISSN: 1042-6507; 1563-5325
• DOI: 10.1080/10426500902870579

The physicochemical properties of a new organic cyclohexaphosphate, [5-Cl-2,4-(OCH 3 ) 2 C 6 H 2- NH 3 ] 6 P 6 O 18 ·4H 2 O, are discussed on the basis of an X-ray crystal structure investigation. This compound crystallizes in the monoclinic space group C2/c, with cell parameters a = 37.987(7) Å, b = 13.125(4) Å, c = 14.331(5) Å, β = 98.21(3)°, Z = 4, V = 7072(3) Å 3 . Its crystal structure is determined and refined to a final R = 0.058 for 5223 independent reflections. The atomic arrangement can be described as a layer organization built up by P 6 O 18 ring anions and water molecules. Between these layers, the organic groups are located that form hydrogen bonds with oxygen atoms of P 6 O 18 rings and water molecules. Intermolecular π-π stacking interactions between two neighboring organic cation rings help to establish the crystal packing. Solid 31 P MAS-NMR spectroscopy is in agreement with X-ray structure. Ab initio calculations allow the attribution of the three phosphorus signals to the independent crystallographic sites. This compound is also characterized by thermal analysis and IR spectroscopy. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.