Table 1. Experimental details and results of refinement of neutron diffraction data between 2.5 K and 400 K for the Czochralski-grown (CZ) LLZTO single crystal.
For all structures: M
r = 932.8, cubic, 
, Z = 8, crystal dimensions (mm): 2.35 × 2.15 × 1.95. Experiments were carried out with neutron radiation, λ = 0.793 Å, using a Huber Eulerian Cradle diffractometer. Refinement was on 32 parameters with two restraints (occupation of 16a site was fixed to full occupation, but Ta/Zr ratio was allowed to refine and in the final refinements, the total Li content was fixed to the value obtained at 2.5 K for all temperatures, but the distribution of Li+ over Li1 and Li2 sites was refined freely).
| CZ-LLZTO at 2.5 K | CZ-LLZTO at 200 K | CZ-LLZTO at 300 K | CZ-LLZTO at 400 K | |
|---|---|---|---|---|
| Crystal data | ||||
| Chemical formula | Li6La3O12TaZrO12 | Li6La3O12TaZrO12 | Li6La3O12TaZrO12 | Li6La3O12TaZrO12 |
| Temperature (K) | 2.5 | 200 | 300 | 400 |
| a (Å) | 12.8511 (2) | 12.8592 (2) | 12.8775 (2) | 12.9051 (2) |
| V (Å3) | 2122.37 (10) | 2126.39 (10) | 2135.48 (10) | 2149.24 (10) |
| μ (mm−1) | 0.04 | 0.03 | 0.03 | 0.03 |
| Data collection | ||||
| No. of measured, independent and observed [I > 2σ(I)] reflections | 624, 347, 289 | 676, 404, 289 | 674, 401, 291 | 645, 408, 267 |
| R int | 0.044 | 0.043 | 0.028 | 0.043 |
| (sin θ/λ)max (Å−1) | 0.811 | 0.810 | 0.809 | 0.811 |
| Refinement | ||||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.023, 0.038, 0.98 | 0.027, 0.041, 0.97 | 0.026, 0.033, 1.01 | 0.046, 0.065, 1.35 |
| No. of reflections | 347 | 404 | 401 | 408 |
| Δρmax, Δρmin (e Å−3) | 0.53, −0.40 | 0.59, −0.64 | 0.39, −0.49 | 0.99, −0.97 |