Table 2.
Crystallographic data of compounds (1) and (2).
| Compound (1) | Compound (2) | |
|---|---|---|
| Empirical formula | C22H30N6O4S | C28H40N6O12S |
| Formula weight | 474.58 | 684.72 |
| Wavelength (Å) | 0.71073 | 0.71073 |
| Crystal system | Monoclinic | Orthorhombic |
| Space group | P21/c | Pbca |
| a (Å) | 17.3380(15) | 24.0800(16) |
| b (Å) | 16.9739(11) | 11.0160(7) |
| c (Å) | 7.9847(6) | 24.5877(17) |
| α (°) | 90.00 | 90.00 |
| β (°) | 99.824(4) | 90.00 |
| γ (°) | 90.00 | 90.00 |
| Volume (Å3) | 2315.4(3) | 6522.3(8) |
| Z | 4 | 8 |
| Density (calculated) (g cm−3) | 1.362 | 1.395 |
| Absorption coefficient (mm−1) | 0.182 | 0.170 |
| F(0 0 0) | 1012 | 2896 |
| Crystal size (mm3) | 0.34 × 0.22 × 0.20 | 74.00 × 0.617 × 0.00 |
| θ range for data collection (°) | 1.19–25.16 | 1.66–22.50 |
| Index ranges | −20 ⩽ h ⩽ 18, −20 ⩽ k ⩽ 20, −9 ⩽ l ⩽ 9 | −25 ⩽ h ⩽ 25, −11 ⩽ k ⩽ 11, −26 ⩽ l ⩽ 26 |
| Reflections collected | 10868 | 53226 |
| Independent reflections | 4065 [Rint = 0.0325] | 4252 [Rint = 0.0775] |
| Completeness to θ = 22.50° | 97.6% | 100.0% |
| Absorption correction | None | None |
| Max and min transmission | 0.964 and 0.953 | 0.998 and 0.882 |
| Refinement method | Full-matrix least-squares on F2 | Full-matrix least-squares on F2 |
| Data/restraints/parameters | 4167/0/298 | 4252/0/425 |
| Goodness-of-fit on F2 | 1.077 | 1.124 |
| Final R indices [I > 2σ(I)] | R1 = 0.0448, wR2 = 0.1296 | R1 = 0.0757, wR2 = 0.1805 |
| R indices (all data) | R1 = 0.0643, wR2 = 0.1500 | R1 = 0.0889, wR2 = 0.1892 |
| Largest diff. peak and hole (e Å−3) | 0.608 and −0.758 | 0.598 and −0.461 |