Table 1.
Crystal data and structure refinement for ethers 3(R/S), 4 and 5.
| Identification Code | 3(R/S) | 4 | 5 |
|---|---|---|---|
| Empirical formula | C19H28O3 | C15H22O2 | C20H34O2Si |
| Formula weight | 304.41 | 234.32 | 334.56 |
| Crystal size/mm3 | 0.284 × 0.242 × 0.115 | 0.468 × 0.269 × 0.068 | 0.395 × 0.16 × 0.041 |
| Crystal system | monoclinic | monoclinic | monoclinic |
| Space group | I2/a | P21/n | P21/c |
| a/Å | 26.978 (6) | 12.960 (5) | 21.564 (9) |
| b/Å | 10.423 (2) | 5.626 (7) | 8.172 (5) |
| c/Å | 39.524 (2) | 18.066 (9) | 22.833 (4) |
| α/° | 90 | 90 | 90 |
| β/° | 142.58 (8) | 95.09 (3) | 95.33 (3) |
| γ/° | 90 | 90 | 90 |
| Volume/Å3 | 6752.3 (13) | 1312.3 (3) | 4006.6 (8) |
| Z | 16 | 4 | 8 |
| ρcalcg/cm3 | 1.198 | 1.186 | 1.109 |
| μ/mm−1 | 0.625 | 0.601 | 1.078 |
| 2Θ range for data collection/° | 6.662 to 152.732 | 8.066 to 152.906 | 7.778 to 149.008 |
| Reflections collected | 28329 | 25650 | 42438 |
| Independent reflections | 7073 [Rint = 0.0238, Rsigma = 0.0175] |
2745 [Rint = 0.0527, Rsigma = 0.0222] |
8196 [Rint = 0.0293, Rsigma = 0.0197] |
| Data/parameters/restraints | 7073/535/48 | 2745/160/0 | 8196/435/0 |
| Goodness-of-fit on F2 | 1.103 | 1.055 | 1.038 |
| Final R indexes [I > =2σ (I)] | R1 = 0.0473, wR2 = 0.1220 |
R1 = 0.0642, wR2 = 0.1775 |
R1 = 0.0487, wR2 = 0.1391 |
| Final R indexes [all data] | R1 = 0.0495, wR2 = 0.1238 |
R1 = 0.0697, wR2 = 0.1877 |
R1 = 0.0535, wR2 = 0.1474 |
| Largest diff. peak/hole /eÅ−3 | 0.26/−0.23 | 0.30/−0.42 | 1.42/−0.36 |