Table 2.
Crystal data, data collection, and structure refinement for compounds 3, 4b, 5
| Compound | 3 | 4b | 5 |
|---|---|---|---|
| Formula | C27H33N5O5 | C20H29N5O2 | C24H39N5O2 |
| Mr | 507.58 | 371.48 | 429.60 |
| Crystal system | Triclinic | Monoclinic | Monoclinic |
| Space group | P | P21/c | P21/n |
| Unit cell dimensions | |||
| a (Å) | 6.5352(2) | 9.2224(2) | 13.5941(6) |
| b (Å) | 11.5286(4) | 12.0168(3) | 12.2011(5) |
| c (Å) | 18.2987(7) | 18.8805(4) | 14.7166(6) |
| β (°) | 94.5953(10) | 97.7864(6) | 102.9960(10) |
| Volume, Å3 | 1325.39(8) | 2073.12(8) | 2378.42(17) |
| Z | 2 | 4 | 4 |
| Calcd. density (g/cm3) | 1.272 | 1.190 | 1.200 |
| µ (mm−1) | 0.089 | 0.079 | 0.078 |
| F(000) | 540 | 800 | 936 |
| Crystal size (mm) | 0.19 × 0.03 × 0.02 | 0.48 × 0.43 × 0.24 | 0.47 × 0.38 × 0.25 |
| Θ range (°) | 2.255 to 34.986 | 2.760 to 35.008 | 2.192 to 33.176 |
| Complentess to Θmax | 0.997 | 0.998 | 0.985 |
| Index ranges |
− 10 < = h < = 10 − 18 < = k < = 18 − 29 < = l < = 29 |
− 14 < = h < = 13 − 19 < = k < = 19 − 30 < = l < = 30 |
− 20 < = h < = 20 − 18 < = k < = 18 − 22 < = l < = 22 |
| Reflections | |||
| Measured | 64,206 | 68,972 | 60,463 |
| Independent [Rint] | 11,655 [0.0960] | 9131 [0.0337] | 8943 [0.0807] |
| Observed [I > 2σ(I)] | 5283 | 7517 | 6136 |
| Parameters, restraints | 483, 70 | 261, 0 | 304, 0 |
| R1, wR2 [I > 2σ(I)] |
0.0732, 0.1572 |
0.0453, 0.1180 |
0.0592, 0.1335 |
| R1, wR2 (all data) |
0.1793, 0.2028 |
0.0577, 0.1281 |
0.0984, 0.1566 |
| GooF on F2 | 1.008 | 1.023 | 1.033 |
| Δρmax, Δρmin (e Å−3) | 0.345, − 0.389 | 0.469, − 0.296 | 0.523, − 0.287 |
| CCDC number | 2024440 | 2077346 | 2098491 |