abstract
Organically templated titanium phosphate, (C(2)H(5)NH(3))[Ti(H(1.5)PO(4))(PO(4))](2)center dot H(2)O, has been prepared by hydrothermal synthesis from titanium(IV) chloride, phosphoric acid, and ethylamine. The structure of this material has been characterized by synchrotron X-ray powder diffraction, (1)H, (13)C, (15)N, and (31)P (including (1)H{FS-LG}-(1)H HOMCOR, (1)H{FS-LG}-(31)P HETCOR, (1)H-(1)H DQ-SQ, (13)C {(31)P} REDOR) MAS NMR, and FTIR spectroscopies and thermal analyses (TG and DSQ. Its triclinic structure was solved in the space group PI (No. 1) with the following final unit cell parameters: a = 5.1126(1), b = 6.3189(2), c = 12.0396(5) angstrom, alpha = 100.931(2), beta = 97.211(2), gamma = 90.683(3)degrees, and V = 378.62(2) angstrom(3) (Z = 1). This pseudo-three-dimensional compound is built up of anionic titanium phosphate layers, similar to those present in the gamma-type titanium phosphate, and ethylammoniurn cations residing in the interlayer one-dimensional channels. On the basis of empirical (particularly NMR and powder XRD) and theoretical (DFT calculations using plane waves basis set) data, the (1)H NMR spectrum has been assigned, and evidence was found for a very strong interlayer P-O center dot center dot center dot H center dot center dot center dot O-P interaction.
keywords
SOLID-STATE NMR; RAY-POWDER DIFFRACTION; N-ALKYLAMINES; PHASE; SPECTROSCOPY; PROTEINS; ACIDS; C-13
subject category
Chemistry; Materials Science
authors
Mafra, L; Rocha, J; Fernandez, C; Castro, GR; Garcia-Granda, S; Espina, A; Khainakov, SA; Garcia, JR
our authors
João Rocha
Full Professor