Table 1. Experimental details.
Experiments were carried out with Mo Kα radiation using a Bruker SMART APEX diffractometer. Absorption was corrected for by multi-scan methods (APEX2; Bruker, 2012 ▸).
| T = 100 K | T = 200 K | T = 300 K | T = 520 K | |
|---|---|---|---|---|
| Crystal data | ||||
| Chemical formula | Ag3.06Sc2(PO4)3 † | Ag3.03Sc2(PO4)3 † | Ag3.05Sc2(PO4)3 † | Ag3.02Sc2(PO4)3 † |
| M r | 704.90 | 701.67 | 703.49 | 700.59 |
| Crystal system, space group | Monoclinic, C2/c | Monoclinic, C2/c | Trigonal, R
c:H
|
Trigonal, R
c:H
|
| Temperature (K) | 100 | 200 | 295 | 520 |
| a, b, c (Å) | 15.467 (3), 8.9627 (14), 9.1186 (15) | 15.5374 (2), 8.9703 (1), 22.5718 (3) | 8.9756 (4), 8.9756 (4), 22.6248 (10) | 8.9671 (8), 8.9671 (8), 22.7622 (19) |
| α, β, γ (°) | 90, 124.1439 (15), 90 | 90, 89.9984 (4), 90 | 90, 90, 120 | 90, 90, 120 |
| V (Å3) | 1046.2 (3) | 3145.95 (7) | 1578.49 (16) | 1585.1 (3) |
| Z | 4 | 12 | 6 | 6 |
| μ (mm−1) | 7.38 | 7.15 | 7.31 | 7.24 |
| Crystal size (mm) | 0.14 × 0.14 × 0.09 | 0.14 × 0.14 × 0.09 | 0.14 × 0.14 × 0.09 | 0.12 × 0.12 × 0.08 |
| Data collection | ||||
| T min, T max | 0.38, 0.52 | 0.51, 0.65 | 0.38, 0.52 | 0.417, 0.581 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 5927, 1407, 1355 | 50538, 6307, 2271 | 7548, 496, 472 | 4628, 924, 700 |
| R int | 0.032 | 0.038 | 0.027 | 0.038 |
| (sin θ/λ)max (Å−1) | 0.706 | 0.769 | 0.701 | 0.873 |
| Refinement | ||||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.035, 0.087, 1.22 | 0.032, 0.107, 1.04 | 0.018, 0.044, 1.11 | 0.033, 0.071, 1.07 |
| No. of reflections | 1407 | 6307 | 496 | 924 |
| No. of parameters | 140 | 380 | 60 | 60 |
| No. of restraints | 12 | 42 | 0 | 0 |
| Δρmax, Δρmin (e Å−3) | 1.16, −1.19 | 1.08, −0.92 | 0.39, −0.36 | 0.78, −0.64 |
Computer programs: APEX2 (Bruker, 2012 ▸), APEX3 (Bruker, 2015 ▸), SHELXL2014 (Sheldrick, 2015b ▸), SHELXT (Sheldrick, 2015a ▸), ORTEP for Windows (Farrugia, 2012 ▸) and WinGX (Farrugia, 2012 ▸).
†
Unconstrained refinements were used so the different Ag content results in uncertainity in determining the Ag content from the single crystal data. Over the whole T-range it is in between 3.02 and 3.06 atoms per formula unit.