Table 2.
Crystallographic data.
| Piv-Pro-Ac3c-Val-NHMe | Piv-Pro-Ac5c-Val-NHMe | Boc-Gly-Val-NHMe | Ac-Ac3c-Val-NHMe | Piv-Ac5c-Val-NHMe | |
|---|---|---|---|---|---|
| 2ba | 3b | 4a | 5c | 6b | |
| Crystallization solvent | Et2O/CH2Cl2 | iPr2O/CH2Cl2 | iPr2O/CHCl3 | Et2O/CH2Cl2 | Et2O/CH2Cl2 |
| Crystal system | monoclinic | orthorhombic | orthorhombic | orthorhombic | orthorhombic |
| Space group | C2 | P212121 | P212121 | P212121 | P212121 |
| Unit cell dimensions a (Å) | 28.576(3) | 10.0590(6) | 9.0788(4) | 8.5773(2) | 9.4086(7) |
| b (Å) | 9.443(2) | 11.1909(5) | 9.4696(4) | 9.5980(3) | 11.0310(12) |
| c (Å) | 10.241(2) | 20.7908(9) | 18.1496(9) | 17.7198(4) | 18.4029(15) |
| β (deg.) | 106.566(17) | 90 | 90 | 90 | 90 |
| Z | 4 | 4 | 4 | 4 | 4 |
| Calculated density (g·cm-3) | 1.226 | 1.199 | 1.223 | 1.163 | 1.132 |
| Reflections collected / unique | 5386 / 3782 | 27691 / 4346 | 28118 / 2896 | 29374 / 2724 | 6929 / 3075 |
| (Rint = 0.061) | (Rint = 0.093) | (Rint = 0.055) | (Rint = 0.083) | (Rint = 0.064) | |
| Residual factors [I > 2σ(I)] R1 | 0.060 | 0.037 | 0.030 | 0.034 | 0.042 |
| wR2 | 0.065 | 0.066 | 0.060 | 0.067 | 0.070 |
| Residual factors [all data] R1 | 0.163 | 0.102 | 0.047 | 0.105 | 0.133 |
| wR2 | 0.079 | 0.076 | 0.062 | 0.077 | 0.081 |
| Largest diff. peak / hole (e· Å-3) | 0.15 / -0.17 | 0.22 / -0.12 | 0.15 / -0.14 | 0.10 / -0.09 | 0.14 / -0.18 |
a
Monohydrate, dichloromethane solvate.