Table 1.
Crystallographic and structure refinement data for complexes 1, 2, and 3.
| Complex | 1 | 2 | 3 |
|---|---|---|---|
| Empirical formula | C30H29N3O5Ni | C33H27N3O4Ni | C95H101N9O20Ni3 |
| Formula weight | 570.27 | 588.28 | 1864.98 |
| Wavelength (Å) | 0.71073 | 0.71073 | 0.71073 |
| Crystal system | Monoclinic | Triclinic | Triclinic |
| Space group | C2/c | P-1 | P-1 |
| a (Å) | 26.741(3) | 10.8240(8) | 12.7068(10) |
| b (Å) | 18.1651(17) | 11.9041(9) | 13.5015(14) |
| c (Å) | 11.8350(9) | 13.0879(11) | 29.9214(17) |
| α (°) | 90 | 67.226(10) | 83.667(2) |
| β (°) | 108.528(2) | 73.566(2) | 82.7470(10) |
| γ (°) | 90 | 64.094(10) | 63.9790(10) |
| v (Å3) | 5450.9(8) | 1385.43(19) | 4567.4(6) |
| Z | 8 | 2 | 2 |
| D calc (Mg·m−3) | 1.390 | 1.410 | 1.356 |
| F(000) | 2384 | 612 | 1956 |
| Absorption coefficient (mm−1) | 0.756 | 0.744 | 0.687 |
| Crystal size (mm) | 0.43 × 0.38 × 0.35 | 0.23 × 0.20 × 0.12 | 0.25 × 0.21 × 0.18 |
| θ range | 2.66 to 25.02 | 2.19 to 25.01 | 2.57 to 25.02 |
| Index ranges | –25 ≤ h ≤ 31 | –12 ≤ h ≤ 12 | –15 ≤ h ≤ 10 |
| –21 ≤ k ≤ 21 | –14 ≤ k ≤ 11 | –16 ≤ k ≤ 16 | |
| –13 ≤ l ≤ 14 | –15 ≤ l ≤ 13 | –35 ≤ l ≤ 35 | |
| Reflections collected | 13562 | 7109 | 29803 |
| Unique reflections | 4816 | 4791 | 16112 |
| R int | 0.0432 | 0.0335 | 0.1085 |
| Max/min transmission | 0.7777, 0.7368 | 0.9160, 0.8475 | 0.8863, 0.8470 |
| Data, restraint, parameters | 4816, 3, 366 | 4791, 0, 363 | 16112, 2613, 1155 |
| Goodness-of-fit on F 2 | 1.094 | 0.952 | 1.010 |
| Final R indices (I > 2σ (I)) | R 1 = 0.0432, wR 2 = 0.0946 | R 1 = 0.0566, wR 2 = 0.1350 | R 1 = 0.0867, wR 2 = 0.1790 |
| R indices (all data) | R 1 = 0.0930, wR 2 = 0.1248 | R 1 = 0.0820, wR 2 = 0.1456 | R 1 = 0.1954, wR 2 = 0.2540 |
| Largest diff. peak and hole (e·Å−3) | 0.392, −0.287 | 1.099, −0.500 | 0.788, −0.500 |