Table 1. Experimental details.
For all structures: Z = 4. Experiments were carried out at 150 K using a Bruker AXS D8 Quest diffractometer with a PhotonII charge-integrating pixel array detector (CPAD). Absorption was corrected for by multi-scan methods (SADABS; Krause et al., 2015 ▸).
| 1a | 1b | 2 | |
|---|---|---|---|
| Crystal data | |||
| Chemical formula | [Fe(C14H32N4)Cl2][FeCl4] | [Fe(C14H32N4)Cl2]Cl·CH4O | [Fe(C14H32N4)Cl2]Cl |
| M r | 580.83 | 450.68 | 418.63 |
| Crystal system, space group | Monoclinic, C2/c | Monoclinic, P21/c | Orthorhombic, P b c n |
| a, b, c (Å) | 20.3512 (13), 6.4815 (4), 18.049 (1) | 8.1632 (4), 20.8470 (12), 12.1387 (7) | 9.2912 (12), 11.9579 (19), 17.267 (3) |
| α, β, γ (°) | 90, 100.452 (3), 90 | 90, 95.024 (2), 90 | 90, 90, 90 |
| V (Å3) | 2341.3 (2) | 2057.8 (2) | 1918.4 (5) |
| Radiation type | Mo Kα | Mo Kα | Cu Kα |
| μ (mm−1) | 1.93 | 1.13 | 10.15 |
| Crystal size (mm) | 0.20 × 0.20 × 0.20 | 0.34 × 0.10 × 0.09 | 0.12 × 0.08 × 0.05 |
| Data collection | |||
| T min, T max | 0.656, 0.747 | 0.679, 0.747 | 0.526, 0.754 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 71685, 4483, 3561 | 125711, 7859, 6505 | 14150, 2055, 1324 |
| R int | 0.074 | 0.049 | 0.082 |
| (sin θ/λ)max (Å−1) | 0.771 | 0.770 | 0.638 |
| Refinement | |||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.027, 0.067, 1.02 | 0.024, 0.061, 1.04 | 0.066, 0.196, 1.08 |
| No. of reflections | 4483 | 7859 | 2055 |
| No. of parameters | 148 | 235 | 196 |
| No. of restraints | 15 | 0 | 273 |
| H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.43, −0.48 | 0.70, −0.58 | 0.58, −0.95 |