Table 3. Experimental details.
| I | II | |
|---|---|---|
| Crystal data | ||
| Chemical formula | [Ni(C16H36N4)]2(ClO4)4·H2O | [Ni(C16H36N4)]Br2·3H2O |
| M r | 1102.21 | 557.06 |
| Crystal system, space group | Monoclinic, P21/c | Orthorhombic, F d d2 |
| Temperature (K) | 295 | 295 |
| a, b, c (Å) | 8.906 (4), 29.412 (11), 19.505 (9) | 60.3649 (18), 19.8364 (9), 7.9773 (3) |
| α, β, γ (°) | 90, 107.030 (19), 90 | 90, 90, 90 |
| V (Å3) | 4885 (4) | 9552.2 (6) |
| Z | 4 | 16 |
| Radiation type | Cu Kα | Mo Kα |
| μ (mm−1) | 3.60 | 4.17 |
| Colour | Orange | Yellow |
| Crystal size (mm) | 0.52 × 0.25 × 0.11 | 0.37 × 0.15 × 0.10 |
| Data collection | ||
| Diffractometer | Picker 4-circle | Enraf–Nonius KappaCCD |
| Radiation source | sealed X-ray tube | fine-focus sealed tube |
| Absorption correction | Gaussian (Busing & Levy, 1957 ▸) | Part of the refinement model (ΔF) (SCALEPACK; Otwinowski & Minor, 1997 ▸) |
| T min, T max | 0.454, 0.686 | 0.34, 0.67 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 7450, 6870, 4899 | 41142, 5382, 4897 |
| R int | 0.060 | 0.096 |
| θmax (°) | 58.4 | 27.5 |
| (sin θ/λ)max (Å−1) | 0.552 | 0.649 |
| Refinement | ||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.043, 0.109, 1.04 | 0.035, 0.085, 1.04 |
| No. of reflections | 6870 | 5382 |
| No. of parameters | 686 | 253 |
| No. of restraints | 184 | 4 |
| 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 |
| Δρmax, Δρmin (e Å−3) | 0.30, −0.31 | 0.88, −0.56 |
Data reduction followed procedures in Corfield et al. (1973 ▸). Structure solution was by the heavy-atom method with local programs. Computer programs: Corfield & Gainsford (1972 ▸), KappaCCD Server Software (Nonius, 1997 ▸), DENZO and SCALEPACK (Otwinowski & Minor, 1997 ▸), SHELXL2017 (Sheldrick, 2015 ▸), ORTEPIII (Burnett & Johnson, 1996 ▸), ORTEP-3 for Windows (Farrugia, 2012 ▸) and publCIF (Westrip, 2010 ▸).