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The chemical, electrochemical, optical and electro-optical properties of titanium oxyfluoride, TiOF
2, have led to interest in this compound for a number of applications. Prior analyses have indicated that TiOF
2 possesses a simple cubic structure (space group
Pm
m) at room temperature. Three-dimensional nanostructured assemblies of polycrystalline TiOF
2 have recently been synthesized
via chemical conversion of intricate SiO
2 structures by metathetic reaction with TiF
4(g). Rietveld analysis has been used to evaluate the structure of the TiOF
2 product formed by such reaction at 623 K. Unlike prior reports, this TiOF
2 product possessed a hexagonal structure (space group
Rc) at room temperature. Upon heating through 333-338 K, the hexagonal TiOF
2 polymorph converted into cubic (
Pmm) TiOF
2. Differential scanning calorimetry and X-ray diffraction analyses have been used to evaluate this thermally induced phase transformation.
Supporting information
Titanium oxydifluoride
top
Crystal data top
| TiF2O | Z = 6 |
| Mr = 101.86 | Dx = 3.114 Mg m−3 |
| Hexagonal, R3c | Cu Kα1 radiation, λ = 1.54060 Å |
| a = 5.3325 (1) Å | T = 298 K |
| c = 13.2321 (4) Å | × × mm |
| V = 325.86 (1) Å3 | |
Data collection top
PANalytical Alpha1
diffractometer | k = ?→? |
| Johansson monochromator | l = ?→? |
| h = ?→? | |
Refinement top
| R[F2 > 2σ(F2)] = 9.70 | S = 1.64 |
| wR(F2) = 12.64 | |
Crystal data top
| TiF2O | V = 325.86 (1) Å3 |
| Mr = 101.86 | Z = 6 |
| Hexagonal, R3c | Cu Kα1 radiation |
| a = 5.3325 (1) Å | T = 298 K |
| c = 13.2321 (4) Å | × × mm |
Data collection top
PANalytical Alpha1
diffractometer | |
Refinement top
| R[F2 > 2σ(F2)] = 9.70 | S = 1.64 |
| wR(F2) = 12.64 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top| | x | y | z | Uiso*/Ueq | Occ. (<1) |
| Ti | 0.000000 | 0.000000 | 0.000000 | 0.010492* | |
| F | 0.5486 (5) | 0.000000 | 0.250000 | 0.000000* | 0.666667 |
| O | 0.5486 (5) | 0.000000 | 0.250000 | 0.000762* | 0.333333 |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Ti | 0.000000 | 0.000000 | 0.000000 | 0.000000 | 0.000000 | 0.000000 |
| F | 0.000000 | 0.000000 | 0.000000 | 0.000000 | 0.000000 | 0.000000 |
| O | 0.000000 | 0.000000 | 0.000000 | 0.000000 | 0.000000 | 0.000000 |
Geometric parameters (Å, º) top
| Ti—F | 1.9112 (3) | F—F | 2.702 (2) |
| Ti—F | 1.911 (2) | F—F | 2.702 (2) |
| Ti—F | 1.911 (2) | F—F | 2.704 (2) |
| Ti—F | 1.911 (2) | F—F | 2.704 (2) |
| Ti—F | 1.911 (2) | F—F | 2.704 (1) |
| Ti—F | 1.9112 (3) | F—F | 2.704 (1) |
| F—F | 2.702 (2) | F—F | 3.442 (2) |
| F—F | 2.702 (2) | F—F | 3.442 (2) |
| | | |
| F—Ti—F | 90.04 (6) | F—F—F | 140.4 (2) |
| F—Ti—F | 89.96 (7) | F—F—F | 50.43 (3) |
| F—Ti—F | 89.96 (6) | F—F—F | 93.02 (9) |
| F—Ti—F | 180.0 (2) | F—F—F | 137.9 (2) |
| F—Ti—F | 90.04 (7) | F—F—F | 50.48 (4) |
| F—Ti—F | 90.0 (1) | F—F—Ti | 45.02 (3) |
| F—Ti—F | 180.0 (4) | F—F—F | 127.1 (1) |
| F—Ti—F | 89.96 (6) | F—F—F | 169.0 (8) |
| F—Ti—F | 90.0 (1) | F—F—F | 60.05 (4) |
| F—Ti—F | 90.0 (1) | F—F—F | 59.98 (3) |
| F—Ti—F | 90.04 (7) | F—F—F | 90.00 (8) |
| F—Ti—F | 180.0 (1) | F—F—F | 124.6 (2) |
| F—Ti—F | 90.04 (6) | F—F—Ti | 94.31 (7) |
| F—Ti—F | 90.0 (1) | F—F—F | 94.62 (8) |
| F—Ti—F | 89.96 (7) | F—F—F | 140.4 (2) |
| F—F—Ti | 44.98 (3) | F—F—F | 84.55 (7) |
| F—F—F | 101.61 (8) | F—F—F | 101.61 (8) |
| F—F—F | 100.91 (7) | F—F—F | 137.9 (2) |
| F—F—F | 50.43 (3) | F—F—F | 93.02 (9) |
| F—F—Ti | 143.3 (1) | Ti—F—F | 145.9 (2) |
| F—F—F | 59.98 (3) | Ti—F—F | 124.1 (1) |
| F—F—F | 90.00 (7) | Ti—F—F | 45.02 (4) |
| F—F—F | 112.2 (1) | Ti—F—F | 44.98 (3) |
| F—F—F | 139.1 (1) | Ti—F—F | 44.98 (5) |
| F—F—F | 160.9 (4) | Ti—F—F | 122.3 (1) |
| F—F—F | 60.00 (4) | F—F—F | 60.05 (4) |
| Ti—F—F | 94.31 (7) | F—F—F | 169.0 (8) |
| Ti—F—F | 145.9 (2) | F—F—F | 100.91 (7) |
| Ti—F—F | 95.40 (8) | F—F—F | 124.6 (2) |
| Ti—F—Ti | 164.4 (1) | F—F—F | 90.00 (8) |
| Ti—F—F | 45.02 (3) | F—F—F | 114.4 (1) |
| Ti—F—F | 45.02 (4) | F—F—F | 112.2 (1) |
| Ti—F—F | 124.1 (1) | F—F—F | 79.09 (7) |
| Ti—F—F | 143.3 (1) | F—F—F | 59.98 (5) |
| Ti—F—F | 122.3 (1) | F—F—F | 90.00 (7) |
| Ti—F—F | 44.98 (5) | F—F—F | 59.98 (5) |
| F—F—F | 94.62 (8) | F—F—F | 79.09 (7) |
| F—F—F | 102.78 (9) | F—F—F | 60.00 (4) |
| F—F—Ti | 95.40 (8) | F—F—F | 160.9 (4) |
| F—F—F | 50.48 (4) | F—F—F | 100.9 (1) |
| F—F—F | 84.55 (7) | | |
Experimental details
| Crystal data |
| Chemical formula | TiF2O |
| Mr | 101.86 |
| Crystal system, space group | Hexagonal, R3c |
| Temperature (K) | 298 |
| a, c (Å) | 5.3325 (1), 13.2321 (4) |
| V (Å3) | 325.86 (1) |
| Z | 6 |
| Radiation type | Cu Kα1 |
| µ (mm−1) | ? |
| Crystal size (mm) | × × |
| |
| Data collection |
| Diffractometer | PANalytical Alpha1
diffractometer |
| Absorption correction | ? |
No. of measured, independent and
observed (?) reflections | ?, ?, 77 |
| Rint | ? |
| |
| Refinement |
| R[F2 > 2σ(F2)], wR(F2), S | 9.70, 12.64, 1.64 |
| No. of reflections | ? |
| No. of parameters | ? |
| No. of restraints | ? |
| Δρmax, Δρmin (e Å−3) | ?, ? |
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m) at room temperature. Three-dimensional nanostructured assemblies of polycrystalline TiOF2 have recently been synthesized via chemical conversion of intricate SiO2 structures by metathetic reaction with TiF4(g). Rietveld analysis has been used to evaluate the structure of the TiOF2 product formed by such reaction at 623 K. Unlike prior reports, this TiOF2 product possessed a hexagonal structure (space group R
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