Table 6. Experimental details.
For all structures: Z = 2. Experiments were carried out at 100 K with Mo Kα radiation using a Bruker Kappa APEXII area-detector diffractometer. Absorption was corrected for by multi-scan methods (SADABS; Bruker, 2008 ▸).
| (I) | (II) | (III) | |
|---|---|---|---|
| Crystal data | |||
| Chemical formula | C4H9NO·C4H10NO+·Br3 − | C4H9NO·C4H10NO+·Br2I− | C4H9NO·C4H10NO+·Cl2I− |
| M r | 414.98 | 461.97 | 373.05 |
| Crystal system, space group | Monoclinic, P21/n | Triclinic, P
|
Monoclinic, C2/m |
| a, b, c (Å) | 7.9009 (4), 10.3466 (6), 9.4948 (5) | 7.2943 (3), 7.9544 (4), 13.6097 (7) | 10.5264 (3), 6.7261 (2), 10.8124 (3) |
| α, β, γ (°) | 90, 107.703 (2), 90 | 90.645 (2), 103.651 (2), 93.656 (2) | 90, 105.950 (1), 90 |
| V (Å3) | 739.42 (7) | 765.51 (6) | 736.06 (4) |
| μ (mm−1) | 8.17 | 7.30 | 2.53 |
| Crystal size (mm) | 0.24 × 0.20 × 0.14 | 0.14 × 0.08 × 0.06 | 0.20 × 0.18 × 0.14 |
| Data collection | |||
| T min, T max | 0.315, 0.394 | 0.515, 0.669 | 0.630, 0.719 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 11995, 3239, 2402 | 30601, 6766, 5446 | 13071, 1745, 1745 |
| R int | 0.026 | 0.021 | 0.014 |
| (sin θ/λ)max (Å−1) | 0.807 | 0.811 | 0.811 |
| Refinement | |||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.025, 0.056, 1.01 | 0.019, 0.038, 1.03 | 0.008, 0.022, 1.06 |
| No. of reflections | 3239 | 6766 | 1745 |
| No. of parameters | 73 | 149 | 52 |
| H-atom treatment | H-atom parameters constrained | 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) | 0.43, −0.78 | 0.52, −0.62 | 0.46, −0.26 |