TABLE 3.
Crystal data and refinement statistics for X-ray crystal structures of compounds 3b and 3ca
| Parameter | 3b (SD) | 3c (SD) |
|---|---|---|
| Unit cell | ||
| a (Å) | 8.9531 (9) | 4.7893 (4) |
| b (Å) | 23.374 (2) | 10.8709 (10) |
| c (Å) | 8.862 (9) | 30.040 (3) |
| α (°) | 90 | 90 |
| β (°) | 112.271 (2) | 92.474 (2) |
| γ (°) | 90 | 90 |
| Space group | P21/c | P21/c |
| Unit cell vol (Å3) | 1,717.4 (3) | 1,562.5 (2) |
| Z | 4 | 4 |
| θ range for data collection (°) | 1.74 to 24.99 | 1.36 to 28.27 |
| Limiting indices | −11 ≤ h ≤11 | −6 ≤ h ≤ 6 |
| −17 ≤ k ≤ 31 | −8 ≤ k ≤ 14 | |
| −11 ≤ l ≤ 11 | −39 ≤ l ≤ 37 | |
| Reflections collected | 8,167 | 8,744 |
| Independent reflections (Rint) | 2,990 (0.0676) | 3,507 (0.0486) |
| Data/restraints/parameters | 2,990/0/194 | 3,507/0/183 |
| Goodness of fit on F2 | 1.029 | 1.095 |
| Final R indices [I>2ς(I)] | R1, 0.0578; wR2, 0.0856 | R1, 0.0666; wR2, 0.1384 |
| R indices (all data) | R1, 0.1207; wR2, 0.1028 | R1, 0.1114; wR2, 0.1569 |
| Absorption coefficient (mm−1) | 0.310 | 0.338 |
| Max, min transmission | 0.4894, 0.4456 | 0.8356, 0.6542 |
| Extinction coefficient | 0.0023 (6) | 0.0004 (11) |
| Largest difference peaks (eÅ−3)b | 0.227, −0.204 | 0.279, −0.211 |
a
Data were collected at 22°C (λ = 0.71073 Å), refined by using full-matrix least-squares refinement on F2, and corrected for absorption by using semiempirical psi-scan data. Rint = Σ|Fo2 − <Fo2|/Σ|Fo2|, F1 = Σ‖Fo| − |Fc‖/Σ|Fo|. R1 = Σ‖Fo| − |Fc‖/Σ|Fo|. wR3 = {Σ[w(Fo2 − Fc2)2]/Σ[w(Fo2)2]}1/2. GooF = S = {Σ[w(Fo2 − FFc2)2]/(n − p)}1/2, where n is reflections and p is parameters.
b
eÅ, −3, electrons/Å3.