Table 1.
Crystal and experimental data of compounds 1a, 2a and 2b.
| Parameters | Compound 1a | Compound 2a | Compound 2b |
|---|---|---|---|
| Empirical formula | C8H5Cl2NO2 | C14H13Cl2N3O5·H2O | C14H13Cl2N3O5 |
| Formula weight | 218.03 | 391.02 | 374.17 |
| Temperature | 293(2) K | 293(2) K | 293(2) K |
| Wavelength (Mo Kα radiation, λ) | 0.71073 Å | 0.71073 Å | 0.71073 Å |
| Crystal system | monoclinic | trigonal | Monoclinic |
| Space group | P 21/c | R-3 | Cc |
| Unit cell dimensions | a = 3.8395 (1) Å, α = 90.00° b = 19.8653 (7) Å β = 90.6258 (10)° c = 11.9619 (4) Å, γ = 90.00° | a = 18.0177(7) Å, α = 90.00° b = 18.0177(7) Å, β = 90.00° c = 26.6558(9) Å, γ = 120.00° | a = 12.9432 (4) Å, α = 90.00° b = 9.3084 (4) Å, β = 101.3572 (16)° c = 13.4650 (5) Å, γ = 90.00° |
| Volume | 912.31 (5)Å3 | 7494.1(6) Å3 | 1590.51 (11) Å3 |
| Z | 4 | 6 | 4 |
| Density (calculated) | 1.587 Mg/m3 | 1.535 Mg/m3 | 1.563 Mg/m3 |
| Absorption coefficient | 0.67 mm−1 | 0.424 mm−1 | 0.439 mm−1 |
| F(000) | 440 | 3564 | 768 |
| Crystal size | 0.58 × 0.35 × 0.27 mm | 0.33 × 0.21 × 0.09 mm | 0.57 × 0.35 × 0.26 mm |
| Theta range for data collection | 2.7 to 30.5°. | 2.3 to 30.6°. | 2.7 to 30.6°. |
| Index ranges | −5 ≤ h ≤ 5, −28 ≤ k ≤ 28, −17 ≤ l ≤ 17 | −25 ≤h ≤ 25, −25 ≤ k ≤ 25, −38 ≤ l ≤ 38 | −18 ≤ h ≤ 18, −13 ≤ k ≤ 13, −19 ≤ l ≤ 19 |
| Reflections collected/ unique | 41303/2404 [R(int) = 0.042] | 107278/5130 [R(int) = 0.059] | 35961/4754 [R(int) = 0.024] |
| Completeness to theta = 30.57° | 99.8% | 99.6% | 99.6% |
| Absorption correction | multi-scan | multi-scan | multi-scan |
| Refinement | method Full-matrix least-squares on F2 | method Full-matrix least-squares on F2 | method Full-matrix least-squares on F2 |
| Goodness-of-fit on F2 | 1.04 | 1.03 | 1.27 |
| Largest diff. peak and hole | 0.28 and −0.22 e.Å−3 | 0.72 and −0.26 e.Å−3 | 0.22 and −0.25 e.Å−3 |