Characterization of layered gamma-titanium phosphate (C(2)H(5)NH(3))[Ti(H(1.5)PO(4))(PO(4))](2)center dot H(2)O intercalate: A combined NMR, synchrotron XRD, and DFT calculations study

authors	Mafra, L; Rocha, J; Fernandez, C; Castro, GR; Garcia-Granda, S; Espina, A; Khainakov, SA; Garcia, JR
nationality	International
journal	CHEMISTRY OF MATERIALS
keywords	SOLID-STATE NMR; RAY-POWDER DIFFRACTION; N-ALKYLAMINES; PHASE; SPECTROSCOPY; PROTEINS; ACIDS; C-13
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.
publisher	AMER CHEMICAL SOC
issn	0897-4756
year published	2008
volume	20
issue	12
beginning page	3944
ending page	3953
digital object identifier (doi)	10.1021/cm800165p
web of science category	Chemistry, Physical; Materials Science, Multidisciplinary
subject category	Chemistry; Materials Science
unique article identifier	WOS:000256854800025