Table 3.
Crystallographic and structure refinement data for complexes 1, 2, and 3.
| Complex | 1 | 2 | 3 |
|---|---|---|---|
| Empirical formula | C31H26N4NiO4 | C34H36N4NiO7 | C35H28N4NiO4 |
| Formula weight | 577.27 | 671.38 | 627.32 |
| Temperature (K) | 298 (2) | 298 (2) | 298 (2) |
| Wavelength (Å) | 0.71073 | 0.71073 | 0.71073 |
| Crystal system | Monoclinic | Monoclinic | Monoclinic |
| Space group | C 2 | P 21/c | P 21 |
| a (Å) | 16.9956 (14) | 12.9281 (12) | 12.5532 (11) |
| b (Å) | 16.7323 (13) | 11.9960 (11) | 19.1631 (16) |
| c (Å) | 12.4490 (9) | 22.131 (2) | 14.850 (4) |
| α = γ (°) | 90 | 90 | 90 |
| β (°) | 130.648 (3) | 104.568 (2) | 111.483 (3) |
| V (Å3) | 2686.0 (4) | 3321.8 (5) | 3324.2 (10) |
| Z | 4 | 4 | 4 |
| D calc (Mg·m−3) | 1.427 | 1.342 | 1.257 |
| F (000) | 1200 | 1408 | 1310 |
| Absorption coefficient (mm−1) | 0.767 | 0.637 | 0.626 |
| Crystal size (mm) | 0.22 × 0.21 × 0.15 | 0.36 × 0.20 × 0.11 | 0.43 × 0.36 × 0.25 |
| θ Range (°) | 2.434 to 25.016 | 2.549 to 25.020 | 2.587 to 25.020 |
| Limiting indices | –20≤ h ≤ 15; –19≤ k ≤ 19; | –10≤ h ≤ 15; –12≤ k ≤ 14; | –14≤ h ≤ 11; –22≤ k ≤ 21; |
| –14l ≤ 14 | –26l ≤ 16 | –17l ≤ 17 | |
| Reflections collected | 6750 | 15812 | 16814 |
| Unique reflections | 4497 | 5824 | 10297 |
| R int | 0.0243 | 0.0988 | 0.0467 |
| Data, restraints, parameters | 4497, 1, 363 | 5824, 0, 421 | 10297, 1649, 795 |
| Goodness–of–fit on F2 | 0.961 | 1.089 | 0.964 |
| Absolute structure parameter | −0.009 (11) | 0.000 (15) | |
| Final R indices [I > 2σ (I)] | R 1 = 0.0381, wR2 = 0.0787 | R 1 = 0.0949, wR2 = 0.2006 | R 1 = 0.0502, wR2 = 0.1044 |
| R Indices (all data) | R 1 = 0.0560, wR2 = 0.0868 | R 1 = 0.1568, wR2 = 0.2242 | R 1 = 0.1001, wR2 = 0.1233 |
| Largest diff. Peak and hole (e·Å−3) | 0.437 and -0.196 | 0.904, and -0.853 | 0.295, and -0.281 |