Table 2.
Crystal Data for N-heterocyclic isoxazole esters 2c-e. Crystals 2c-e were mono-clinic, experiments were carried out at 100 K. The BA was triclinic and run at 293 K.
| Compound | m-Pyr 2c | p-Pyr 2d | 8-Quin 2e |
|---|---|---|---|
| Crystal Data | |||
| Empirical Formula | C26H20N2O3 | C26H20N2O3 | C30H22N2O3 |
| Formula Weight | 408.44 | 408.44 | 458.49 |
| Space group | P21/c | C2/c | P21/c |
| a/Å | 8.2571 (7) | 30.3595 (6) | 11.1995(12) |
| b/Å | 11.5857 (9) | 7.2167 (1) | 14.4696(16) |
| c/Å | 20.9084 (17) | 22.2409 (5) | 14.3170(16) |
| α/° | 90 | 90 | 90 |
| β/° | 90.242 (3) | 125.2256 (9) | 101.662(4) |
| γ/° | 90 | 90 | 90 |
| Volume/Å3 | 2000.2 (3) | 3980.59 (14) | 2272.2(4) |
| Z | 4 | 8 | 4 |
| Dx mg/m3 | 1.356 | 1.363 | 1.340 |
| μ/mm1 | 0.72 | 0.09 | 0.087 |
| F(000) | 856 | 1712 | 960.0 |
| Crystal appearance | Yellow Cube | Yellow Prism | Colorless Prism |
| Crystal size/mm3 | 0.4 × 0.25 × 0.2 | 0.49 × 0.24 × 0.16 | 0.24 × 0.16 × 0.08 |
| Data Collection | |||
| Radiation (λ) | Cu Kα (1.54178) | Mo Kα (0.71073) | Mo Kα (0.71073) |
| Θ /° | 4.2–72.3 | 2.7–28.7 | 2.9 – 28.7 |
| Index ranges | −10 ≤ h ≤ 10 | −40 ≤ h ≤ 40 | −15 ≤ h ≤ 15 |
| −14 ≤ k ≤ 13 | −9 ≤ k ≤ 9 | −19 ≤ k ≤ 19 | |
| −24 ≤ l ≤ 25 | −30 ≤ l ≤ 29 | −19 ≤ l ≤ 19 | |
| Measured Reflections | 36,456 | 25,023 | 105,583 |
| Independent reflections | 3955 | 5141 | 5905 |
| Reflections with I > 2σ(I) | 3627 | 3707 | 4752 |
| Refinement | |||
| Parameters | 282 | 282 | 318 |
| Goodness-of-fit on F2 | 1.08 | 1.02 | 1.031 |
| R[F2 > 2σ(F2)] | 0.040 | 0.043 | 0.047 |
| wR(F2) | 0.105 | 0.106 | 0.1200 |
| Largest diff. peak/hole / e Å−3 | 0.31/−0.30 | 0.31/−0.21 | 0.47/−0.19 |
| Calculated features | |||
| Isoxazole/Anthracene dihedral/° | 77.25 | 68.09 | 73.74 |
| Anthracene/N-heterocycle dihedral/° | 79.21 | 74.46 | 72.05 |
| Isoxazole/N-heterocycle angle/° | 25.28 | 6.81 | 4.76 |