Synthesis, structure and solid state NMR analysis of a new templated titanium(III/IV) fluorophosphate

Synthesis of Titanium Fluorophosphates and Fluorosulfates from Hexafluorotitanic Acid

“…In LiTiPO 4 F the fluoride ion acts as a bridging unit between two central titanium metal atoms, as also observed in the 3D framework reported herein (structure II). [12,13,15,22] The inorganic chains in [DABCO-H][Ti(SO 4 ) 2 (SO 3 (OH,F))] are isostructural with those found in ferrinatrite, Na 3 Fe(SO 4 ) 3 · 3H 2 O and with a similar hexagonal spatial distribution. [17] The higher charge on titanium (4+) compared with Fe 3+ in ferrinatrite is compensated for by the lower level of the larger, monovalent DABCO.…”

“…[1][2][3][4][5]14,15] In the work reported herein we have employed hexafluorotitanic acid, H 2 TiF 6 , instead of titanium fluorides as a reactant to maintain high fluoride ion concentrations in the reaction medium.…”

“…[15,16] In this work we have employed these large templating species in combination with hexafluorotitanic acid and oxo-fluoro-tetrahedral species (e.g. PO 4 3-, PO 3 F 2-, SO 3 F -, SO 4 2-) to generate four new phases that were structurally characterized using single-crystal X-ray diffraction.…”

Frequency-swept pulse sequences for 19F heteronuclear spin decoupling in solid-state NMR

“…Consequently, a large number of examples may be found in the literature where a rare spin has been observed under 19 F decoupling . Whereas in many cases, only CW decoupling has been used [42][43][44][45][46][47][48][49][50][51][52][53], there is also evidence of application of multi-pulse techniques. In analogy to the results obtained for 1 H, it was attempted to improve spectral resolution by decoupling 19 F using TPPM [54][55][56][57][58], SPINAL [59,60] and also XiX [61,62].…”