Experiments were carried out with Mo Kα radiation using a Rigaku Xcalibur Sapphire3 diffractometer. Absorption was corrected for by multi-scan methods (CrysAlis PRO; Rigaku OD, 2020 ▸).
| I | III | IV | |
|---|---|---|---|
| Crystal data | |||
| Chemical formula | C4H4O2 | C4H5O2+·AsF6− | C6H8O4 |
| M r | 84.07 | 274.00 | 144.12 |
| Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Triclinic, P
|
| temperature (K) | 111 | 111 | 112 |
| a, b, c (Å) | 3.8409 (5), 15.593 (2), 7.6149 (10) | 6.9609 (5), 8.9319 (7), 13.7189 (9) | 3.8726 (11), 5.6546 (10), 8.3778 (18) |
| α, β, γ (°) | 90, 99.910 (12), 90 | 90, 91.664 (7), 90 | 100.642 (16), 100.42 (2), 105.73 (2) |
| V (Å3) | 449.27 (10) | 852.60 (11) | 168.30 (7) |
| Z | 4 | 4 | 1 |
| μ (mm−1) | 0.10 | 4.06 | 0.12 |
| Crystal size (mm) | 1.00 × 0.56 × 0.31 | 0.90 × 0.21 × 0.15 | 0.52 × 0.46 × 0.35 |
| Data collection | |||
| Tmin, Tmax | 0.457, 1.000 | 0.582, 1.000 | 0.579, 1.000 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 3885, 1060, 891 | 4205, 2303, 1900 | 1403, 825, 703 |
| R int | 0.023 | 0.029 | 0.015 |
| θmax (°) | 27.9 | 29.1 | 28.3 |
| (sin θ/λ)max (Å−1) | 0.658 | 0.685 | 0.667 |
| Refinement | |||
| R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.099, 1.05 | 0.039, 0.099, 1.05 | 0.048, 0.144, 1.04 |
| No. of reflections | 1060 | 2303 | 825 |
| No. of parameters | 71 | 123 | 51 |
| No. of restraints | 0 | 0 | 0 |
| H-atom treatment | All H-atom parameters refined | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
| Δρmax, Δρmin (e Å−3) | 0.18, −0.15 | 0.87, −0.92 | 0.52, −0.24 |
