Table 8. Experimental details.
| 1 | 2 | 3 | |
|---|---|---|---|
| Crystal data | |||
| Chemical formula | C16H25NO5 | C22H30N2O4 | C20H33NO6 |
| M r | 311.37 | 386.48 | 383.47 |
| Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
| Temperature (K) | 100 | 100 | 100 |
| a, b, c (Å) | 22.3351 (18), 5.0467 (4), 14.2265 (10) | 11.5626 (8), 19.5328 (9), 9.5488 (7) | 24.6345 (18), 8.4646 (5), 10.0598 (7) |
| β (°) | 99.956 (7) | 109.369 (8) | 100.851 (2) |
| V (Å3) | 1579.4 (2) | 2034.5 (2) | 2060.2 (2) |
| Z | 4 | 4 | 4 |
| Radiation type | Mo Kα | Mo Kα | Cu Kα |
| μ (mm−1) | 0.10 | 0.09 | 0.74 |
| Crystal size (mm) | 0.15 × 0.02 × 0.01 | 0.25 × 0.08 × 0.02 | 0.80 × 0.05 × 0.02 |
| Data collection | |||
| Diffractometer | Rigaku AFC12 | Rigaku AFC12 | Rigaku Saturn944+ |
| Absorption correction | Multi-scan (CrysAlis PRO; Agilent, 2014 ▸) | Multi-scan (CrysAlis PRO; Agilent, 2014 ▸) | Multi-scan (CrystalClear-SM Expert; Rigaku, 2012 ▸) |
| T min, T max | 0.803, 1.000 | 0.384, 1.000 | 0.814, 1.000 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 19396, 3627, 2039 | 26057, 4655, 3869 | 18993, 3706, 3362 |
| R int | 0.123 | 0.040 | 0.037 |
| (sin θ/λ)max (Å−1) | 0.649 | 0.649 | 0.602 |
| Refinement | |||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.062, 0.133, 0.97 | 0.041, 0.105, 1.04 | 0.035, 0.095, 1.05 |
| No. of reflections | 3626 | 4652 | 3706 |
| No. of parameters | 210 | 264 | 253 |
| 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 atoms treated by a mixture of independent and constrained refinement |
| Δρmax, Δρmin (e Å−3) | 0.25, −0.33 | 0.32, −0.18 | 0.23, −0.28 |
Computer programs: CrystalClear-SM Expert (Rigaku, 2012 ▸), CrysAlis PRO (Agilent, 2014 ▸), SHELXT (Sheldrick, 2015a ▸), Flipper 25 (Oszlányi & Sütő, 2004 ▸), OLEX2 (Dolomanov et al., 2009 ▸), OSCAIL (McArdle et al., 2004 ▸), ShelXle (Hübschle et al., 2011 ▸), SHELXL2014 (Sheldrick, 2015b ▸), Mercury (Macrae et al., 2006 ▸) and PLATON (Spek, 2009 ▸).