Structural characterization of layered γ-titanium phosphate (C6H13NH3)[Ti(HPO4)(PO4)]•H2O

An organically templated titanium phosphate, (C6H13NH3)[Ti(HPO4)(PO4)](H2O)-H-., has been prepared by hydrothermal synthesis from titanium(IV) chloride, phosphoric acid, and n-hexylamine. The structure of this material has been characterized by powder X-ray diffraction (XRD), H-1 [including H-1{FS-Lee-Goldburg (LG)}-H-1 homonuclear correlation (HOMCOR), H-1 double quantum (DQ), and H-1{FS-LG}-P-31 cross-polarization (CP) heteronuclear correlation (HETCOR)], C-13, and P-31 magic-angle spinning (MAS) NMR, Fourier transform infrared (FTIR) spectroscopy, and thermal analyses [thermogravimetry (TG) and differential scanning calorimetry (DSC)]. Based on the empirical evidence, particularly solid-state NMR, modeling studies, and powder XRD, a crystal structure has been proposed, having unit cell parameters a = 5.089(2) angstrom, b = 6.335(2) angstrom, c = 22.792(5) angstrom,beta 102.48(2)degrees, space group P2(1), and Z 2. This compound is built up of anionic titanium phosphate layers, similar to those present in the gamma-type titanium phosphate, with n-hexylammonium cations intercalated in the interlayer space.