Table 1. Structural Parameters for the Main Li4CuSbO5.5 Phase from a Combined Rietveld Refinement on Neutron and Synchrotron X-ray Diffraction Data.
| refinement parameters | ||||
|---|---|---|---|---|
| formula | Li8Cu2Sb2O11 | |||
| temperature (K) | 298 | |||
| pressure | atmospheric | |||
| source | neutron time-of-flight | synchrotron X-ray | ||
| data bank | ND, bank 1 | ND, bank 2 | ND, bank 3 | SXRD |
| angle (°)/wavelength (Å) | 168.657 | 90.248 | 29.930 | 0.82468(1) |
| d spacing range (Å) | 0.68–2.59 | 0.89–3.89 | 3.14–6.28 | 0.58–9.44 |
| TOF (μs)/2θ (°) range | 40000–125000 | 31000–135500 | 40000–80000 | 5–120 |
| TOF (μs)/2θ (°) step | 20.3307 | 48.7172 | 75.1060 | 0.004 |
| no. of reflections | 1459 | 1120 | 15 | 6082 |
| no. of refined parameters | 95 | |||
| Rp | 13.4 | 8.78 | 25.7 | 14.0 |
| Rwp | 11.9 | 6.89 | 17.2 | 16.7 |
| Rexp | 5.35 | 1.96 | 9.42 | 3.39 |
| χ2 | 4.92 | 12.4 | 3.34 | 24.3 |
| ρmin/max residuals (fm·Å–3/e–·Å–3) | [−0.004/+0.005] | [−0.003/+0.002] | [−0.0002/+0.0003] | [−0.9/+1.5] |
| Phases | Estimated Mass Fraction (%) | |||
| Li4CuSbO5.5, main | 79.3 | 66.2 | 94.0 | 76.5 |
| Li4CuSbO5.5, secondary | 20.0 | 32.3 | – | 22.1 |
| Li2CuO2 | 0.6 | 0.8 | 0.9 | 1.1 |
| Li7SbO6 | 0.1 | 0.7 | 5.1 | 0.3 |
| structure
parameters for Li4CuSbO5.5 | |||||||
|---|---|---|---|---|---|---|---|
| space group | Z | density (g·cm–3) | formula weight (g·mol–1) | ||||
| P1 | 1 | 4.459 | 602.13 | ||||
| a (Å) | b (Å) | c (Å) | α (°) | β (°) | γ (°) | volume (Å3) | |
| main | 5.207365(8) | 5.817536(8) | 7.888147(13) | 100.58195(11) | 96.93693(11) | 106.96091(9) | 220.7860(6) |
| secondary | 5.20263(3) | 5.82002(4) | 7.88000(6) | 100.4694(6) | 97.0145(5) | 107.0248(6) | 220.413(3) |
| atom | site | x | y | z | occupancy | Biso (Å2) |
|---|---|---|---|---|---|---|
| O1 | 2i | 0.4547(10) | 0.4047(9) | 0.1628(7) | 1 | 0.66(10) |
| O2 | 2i | 0.5547(9) | 0.0990(9) | 0.8389(6) | 1 | 0.59(10) |
| O3 | 2i | 0.0067(10) | 0.1693(9) | 0.6879(7) | 1 | 0.65(11) |
| O4 | 2i | 0.0050(10) | 0.3225(8) | 0.3134(6) | 1 | 0.35(9) |
| O5 | 2i | 0.4768(10) | 0.2336(9) | 0.4789(6) | 0.959(8) | 0.78(11) |
| O6 | 1g | 0 | 0 | 0 | 0.906(6) | 0.28(15) |
| vacancy | 1b | 0 | 0.5 | 0 | 0 | – |
| Sb8 | 2i | 0.23390(15) | 0.11964(15) | 0.24415(10) | 1 | 0.351(4) |
| Cu9/Li9 | 2i | 0.2395(4) | 0.6223(4) | 0.2526(3) | 0.633/0.367(2) | 0.35(3) |
| Cu10/Li10 | 2i | 0.7483(8) | 0.0411(7) | 0.4149(5) | 0.249/0.751(2) | 0.38(6) |
| Cu11/Li11 | 2i | 0.2691(19) | 0.8018(17) | 0.9062(13) | 0.061/0.939(2) | 0.76(19) |
| Li12 | 2i | 0.669(3) | 0.691(2) | 0.1043(19) | 1 | 2.1(3) |
| Li13 | 2i | 0.749(3) | 0.528(3) | 0.4070(19) | 1 | 1.3(3) |