Table 2.
XRD data and experimental details for compounds 2–5.
| 2 | 3 | 4 | 5 | |
|---|---|---|---|---|
| Empirical formula | C26H42O3 | C24H35O | C24H37ClO | C24H36Cl2 |
| Formula weight | 402.59 | 339.52 | 376.98 | 395.43 |
| Crystal system | Monoclinic | Monoclinic | Triclinic | Monoclinic |
| Space group | P21 | P21 | P1 | C2 |
| Unit cell dimensions a, b, c (Å) | 25.332(2), 7.6508(5), 25.543(2) | 7.5834(6), 20.548(2), 12.9331(9) | 6.3333(3), 7.4257(5), 11.8452(8) | 13.880(1), 6.3288(4), 24.409(2) |
| α, β, γ (°) | 90, 107.232(3), 90 | 90, 90.020(4), 90 | 89.026(2), 84.321(2), 69.960(2) | 90, 97.004(4), 90 |
| Volume (Å3) | 4728.1(6) | 2015.3(3) | 520.69(6) | 2128.1(3) |
| Z | 8 | 4 | 1 | 4 |
| Density (calcd.) (Mg.mm−3) | 1.131 | 1.119 | 1.202 | 1.234 |
| F(000) | 1776 | 748 | 206 | 856 |
| Absorption coefficient (mm−1) | 0.07 | 0.07 | 0.19 | 0.311 |
| Crystal size (mm3) | 1.00 × 0.08 × 0.05 | 1.00 × 0.45 × 0.01 | 1.00 × 0.72 × 0.20 | 1.00 × 0.30 × 0.02 |
| Tmin, Tmax | 0.832, 0.928 | 0.770, 0.928 | 0.764, 0.813 | 0.762, 0.801 |
| Θ range for data collection | 0.8–26.5 | 1.0–26.1 | 2.9–33.5 | 0.8–27.1 |
| Reflections collected | 101,280 | 19,801 | 14,660 | 35,210 |
| Independent reflections [Rint] | 19,379 [0.088] | 7303 [0.095] | 6349 [0.024] | 4471 [0.049] |
| Observed [I > 2 σ (I)] reflections | 11,585 | 4090 | 5142 | 4097 |
| Completeness to θ = 25° (%) |
99.9 | 99.7 | 99.9 | 98.8 |
| Data/restraints/parameters | 193,79/1/1073 | 7303/2/462 | 6349/3/240 | 4471/1/240 |
| Goodness-of-fit on F2 | 1.01 | 0.99 | 1.02 | 1.107 |
| Final R1, [I > 2σ(I)] | 0.061 | 0.064 | 0.046 | 0.041 |
| Final wR2 (all data) | 0.155 | 0.148 | 0.138 | 0.109 |
| Largest diff. peak/hole e.Å−3 | 0.20, −0.21 | 0.18, −0.17 | 0.36, −0.27 | 0.27, −0.201 |
| Absolute structure parameter | −0.1(5) | 0.5(10) | 0.039(17) | 0.029(17) |
| CCDC | 2,315,012 | 2,315,013 | 2,315,014 | 2,350,691 |