| Literature DB >> 22590253 |
Nazia Sattar, Hamid Latif Siddiqui, Matloob Ahmad, Muhammad Akram, Masood Parvez.
Abstract
In the title mol-ecule, C(22)Entities:
Year: 2012 PMID: 22590253 PMCID: PMC3344491 DOI: 10.1107/S160053681201481X
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| C22H15Cl2NO4S | |
| Monoclinic, | Mo |
| Hall symbol: -P 2ybc | Cell parameters from 8696 reflections |
| θ = 1.0–27.5° | |
| µ = 0.46 mm−1 | |
| β = 110.511 (2)° | Prism, yellow |
| 0.20 × 0.18 × 0.16 mm | |
| Nonius KappaCCD diffractometer | 4592 independent reflections |
| Radiation source: fine-focus sealed tube | 3598 reflections with |
| Graphite monochromator | |
| ω and φ scans | θmax = 27.6°, θmin = 2.7° |
| Absorption correction: multi-scan ( | |
| 16108 measured reflections |
| Refinement on | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| Hydrogen site location: inferred from neighbouring sites | |
| H-atom parameters constrained | |
| 4592 reflections | (Δ/σ)max = 0.001 |
| 272 parameters | Δρmax = 0.33 e Å−3 |
| 0 restraints | Δρmin = −0.44 e Å−3 |
| Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. |
| Refinement. Refinement of |
| Cl1 | 0.52481 (7) | −0.04749 (10) | 0.39033 (6) | 0.0658 (3) | |
| Cl2 | 0.50174 (9) | 0.57915 (12) | 0.37257 (7) | 0.0804 (3) | |
| S1 | 0.87675 (5) | 0.25684 (7) | 0.53887 (4) | 0.03478 (16) | |
| O1 | 0.98780 (15) | 0.2067 (2) | 0.56375 (12) | 0.0457 (5) | |
| O2 | 0.84712 (17) | 0.3467 (2) | 0.59407 (11) | 0.0465 (5) | |
| O3 | 0.79566 (17) | 0.0186 (2) | 0.31269 (11) | 0.0418 (5) | |
| H3O | 0.7866 | −0.0624 | 0.3235 | 0.050* | |
| O4 | 0.77251 (15) | −0.18006 (19) | 0.40080 (11) | 0.0408 (5) | |
| N1 | 0.79342 (17) | 0.1262 (2) | 0.52149 (12) | 0.0331 (5) | |
| C1 | 0.8421 (2) | 0.3280 (3) | 0.43643 (16) | 0.0339 (6) | |
| C2 | 0.8521 (2) | 0.4653 (3) | 0.42629 (18) | 0.0406 (6) | |
| H2 | 0.8739 | 0.5236 | 0.4744 | 0.049* | |
| C3 | 0.8297 (2) | 0.5165 (3) | 0.34482 (19) | 0.0465 (7) | |
| H3 | 0.8365 | 0.6104 | 0.3369 | 0.056* | |
| C4 | 0.7977 (3) | 0.4316 (3) | 0.27565 (18) | 0.0483 (7) | |
| H4 | 0.7830 | 0.4676 | 0.2201 | 0.058* | |
| C5 | 0.7866 (2) | 0.2949 (3) | 0.28534 (17) | 0.0421 (7) | |
| H5 | 0.7638 | 0.2378 | 0.2366 | 0.050* | |
| C6 | 0.8089 (2) | 0.2404 (3) | 0.36662 (15) | 0.0318 (5) | |
| C7 | 0.7989 (2) | 0.0952 (3) | 0.37903 (15) | 0.0326 (6) | |
| C8 | 0.7978 (2) | 0.0396 (3) | 0.45361 (14) | 0.0307 (5) | |
| C9 | 0.7971 (2) | −0.1051 (3) | 0.46462 (16) | 0.0334 (6) | |
| C10 | 0.8276 (2) | −0.1656 (3) | 0.55114 (16) | 0.0357 (6) | |
| C11 | 0.9160 (2) | −0.1140 (3) | 0.61913 (17) | 0.0403 (6) | |
| H11 | 0.9531 | −0.0345 | 0.6119 | 0.048* | |
| C12 | 0.9498 (2) | −0.1792 (3) | 0.69745 (18) | 0.0463 (7) | |
| H12 | 1.0107 | −0.1448 | 0.7438 | 0.056* | |
| C13 | 0.8954 (3) | −0.2934 (3) | 0.70810 (19) | 0.0498 (8) | |
| H13 | 0.9190 | −0.3376 | 0.7619 | 0.060* | |
| C14 | 0.8066 (3) | −0.3445 (3) | 0.6410 (2) | 0.0505 (8) | |
| H14 | 0.7685 | −0.4226 | 0.6491 | 0.061* | |
| C15 | 0.7735 (3) | −0.2815 (3) | 0.56220 (19) | 0.0448 (7) | |
| H15 | 0.7137 | −0.3175 | 0.5157 | 0.054* | |
| C16 | 0.6823 (2) | 0.1408 (3) | 0.53043 (16) | 0.0376 (6) | |
| H16A | 0.6906 | 0.1968 | 0.5813 | 0.045* | |
| H16B | 0.6560 | 0.0507 | 0.5403 | 0.045* | |
| C17 | 0.5954 (2) | 0.2036 (3) | 0.45391 (16) | 0.0396 (6) | |
| C18 | 0.5232 (2) | 0.1274 (4) | 0.38632 (19) | 0.0502 (8) | |
| C19 | 0.4486 (3) | 0.1900 (5) | 0.3150 (2) | 0.0661 (11) | |
| H19 | 0.4009 | 0.1372 | 0.2695 | 0.079* | |
| C20 | 0.4435 (3) | 0.3273 (5) | 0.3101 (2) | 0.0685 (11) | |
| H20 | 0.3933 | 0.3699 | 0.2606 | 0.082* | |
| C21 | 0.5114 (3) | 0.4044 (4) | 0.37701 (19) | 0.0564 (9) | |
| C22 | 0.5870 (2) | 0.3432 (3) | 0.44836 (17) | 0.0437 (7) | |
| H22 | 0.6336 | 0.3972 | 0.4938 | 0.052* |
| Cl1 | 0.0454 (4) | 0.0807 (7) | 0.0762 (6) | −0.0194 (4) | 0.0274 (4) | −0.0311 (5) |
| Cl2 | 0.0780 (7) | 0.0882 (8) | 0.0780 (6) | 0.0331 (6) | 0.0310 (5) | 0.0324 (6) |
| S1 | 0.0355 (3) | 0.0382 (4) | 0.0259 (3) | −0.0025 (3) | 0.0048 (2) | −0.0050 (3) |
| O1 | 0.0316 (10) | 0.0547 (13) | 0.0402 (10) | −0.0033 (9) | −0.0006 (8) | −0.0019 (9) |
| O2 | 0.0582 (13) | 0.0452 (12) | 0.0332 (10) | −0.0025 (10) | 0.0124 (9) | −0.0114 (9) |
| O3 | 0.0569 (12) | 0.0388 (11) | 0.0303 (9) | −0.0066 (10) | 0.0160 (9) | −0.0086 (8) |
| O4 | 0.0440 (11) | 0.0395 (11) | 0.0358 (10) | −0.0041 (9) | 0.0102 (8) | −0.0087 (8) |
| N1 | 0.0342 (11) | 0.0379 (12) | 0.0265 (10) | −0.0022 (10) | 0.0100 (9) | −0.0041 (9) |
| C1 | 0.0311 (13) | 0.0375 (15) | 0.0310 (13) | −0.0010 (11) | 0.0082 (10) | −0.0024 (11) |
| C2 | 0.0414 (15) | 0.0378 (15) | 0.0399 (15) | −0.0015 (12) | 0.0108 (12) | −0.0062 (12) |
| C3 | 0.0529 (18) | 0.0349 (16) | 0.0515 (17) | 0.0000 (13) | 0.0178 (14) | 0.0047 (13) |
| C4 | 0.0578 (19) | 0.0464 (18) | 0.0389 (15) | −0.0002 (15) | 0.0146 (14) | 0.0081 (13) |
| C5 | 0.0469 (16) | 0.0474 (17) | 0.0304 (13) | −0.0005 (13) | 0.0117 (12) | −0.0024 (12) |
| C6 | 0.0305 (12) | 0.0366 (14) | 0.0276 (11) | −0.0021 (11) | 0.0092 (10) | −0.0020 (11) |
| C7 | 0.0281 (12) | 0.0398 (15) | 0.0290 (12) | −0.0016 (11) | 0.0088 (10) | −0.0074 (11) |
| C8 | 0.0276 (12) | 0.0380 (14) | 0.0246 (11) | −0.0008 (11) | 0.0066 (9) | −0.0035 (10) |
| C9 | 0.0274 (12) | 0.0388 (15) | 0.0337 (13) | −0.0021 (11) | 0.0103 (10) | −0.0028 (11) |
| C10 | 0.0379 (14) | 0.0354 (14) | 0.0349 (13) | 0.0042 (12) | 0.0140 (11) | 0.0028 (11) |
| C11 | 0.0391 (15) | 0.0417 (16) | 0.0387 (14) | 0.0041 (12) | 0.0119 (12) | 0.0034 (12) |
| C12 | 0.0454 (16) | 0.0536 (19) | 0.0365 (15) | 0.0096 (14) | 0.0102 (13) | 0.0026 (13) |
| C13 | 0.062 (2) | 0.0496 (19) | 0.0413 (16) | 0.0147 (16) | 0.0226 (15) | 0.0116 (14) |
| C14 | 0.067 (2) | 0.0375 (17) | 0.0579 (19) | 0.0017 (15) | 0.0351 (17) | 0.0071 (14) |
| C15 | 0.0504 (17) | 0.0423 (17) | 0.0449 (16) | −0.0002 (13) | 0.0206 (14) | −0.0016 (13) |
| C16 | 0.0365 (14) | 0.0490 (17) | 0.0306 (13) | −0.0006 (12) | 0.0156 (11) | −0.0037 (12) |
| C17 | 0.0292 (13) | 0.0628 (19) | 0.0296 (13) | 0.0001 (13) | 0.0138 (11) | −0.0029 (12) |
| C18 | 0.0313 (14) | 0.079 (2) | 0.0444 (16) | −0.0037 (15) | 0.0190 (13) | −0.0138 (16) |
| C19 | 0.0351 (17) | 0.119 (4) | 0.0399 (18) | −0.002 (2) | 0.0073 (14) | −0.013 (2) |
| C20 | 0.0389 (18) | 0.124 (4) | 0.0366 (17) | 0.018 (2) | 0.0057 (14) | 0.015 (2) |
| C21 | 0.0395 (16) | 0.088 (3) | 0.0434 (17) | 0.0170 (17) | 0.0171 (14) | 0.0127 (17) |
| C22 | 0.0343 (14) | 0.065 (2) | 0.0340 (14) | 0.0068 (14) | 0.0142 (12) | 0.0029 (13) |
| Cl1—C18 | 1.736 (4) | C9—C10 | 1.486 (3) |
| Cl2—C21 | 1.738 (4) | C10—C15 | 1.389 (4) |
| S1—O1 | 1.425 (2) | C10—C11 | 1.391 (4) |
| S1—O2 | 1.4268 (19) | C11—C12 | 1.386 (4) |
| S1—N1 | 1.640 (2) | C11—H11 | 0.9500 |
| S1—C1 | 1.759 (3) | C12—C13 | 1.375 (4) |
| O3—C7 | 1.333 (3) | C12—H12 | 0.9500 |
| O3—H3O | 0.8400 | C13—C14 | 1.384 (4) |
| O4—C9 | 1.247 (3) | C13—H13 | 0.9500 |
| N1—C8 | 1.440 (3) | C14—C15 | 1.384 (4) |
| N1—C16 | 1.491 (3) | C14—H14 | 0.9500 |
| C1—C2 | 1.384 (4) | C15—H15 | 0.9500 |
| C1—C6 | 1.397 (3) | C16—C17 | 1.506 (4) |
| C2—C3 | 1.386 (4) | C16—H16A | 0.9900 |
| C2—H2 | 0.9500 | C16—H16B | 0.9900 |
| C3—C4 | 1.372 (4) | C17—C22 | 1.389 (4) |
| C3—H3 | 0.9500 | C17—C18 | 1.404 (4) |
| C4—C5 | 1.379 (4) | C18—C19 | 1.387 (5) |
| C4—H4 | 0.9500 | C19—C20 | 1.365 (6) |
| C5—C6 | 1.396 (4) | C19—H19 | 0.9500 |
| C5—H5 | 0.9500 | C20—C21 | 1.383 (5) |
| C6—C7 | 1.467 (4) | C20—H20 | 0.9500 |
| C7—C8 | 1.368 (3) | C21—C22 | 1.386 (4) |
| C8—C9 | 1.448 (4) | C22—H22 | 0.9500 |
| O1—S1—O2 | 119.62 (12) | C12—C11—C10 | 119.7 (3) |
| O1—S1—N1 | 107.33 (12) | C12—C11—H11 | 120.1 |
| O2—S1—N1 | 107.70 (12) | C10—C11—H11 | 120.1 |
| O1—S1—C1 | 108.03 (12) | C13—C12—C11 | 120.1 (3) |
| O2—S1—C1 | 110.19 (12) | C13—C12—H12 | 119.9 |
| N1—S1—C1 | 102.62 (11) | C11—C12—H12 | 119.9 |
| C7—O3—H3O | 109.5 | C12—C13—C14 | 120.5 (3) |
| C8—N1—C16 | 116.06 (19) | C12—C13—H13 | 119.7 |
| C8—N1—S1 | 114.13 (16) | C14—C13—H13 | 119.7 |
| C16—N1—S1 | 119.42 (18) | C13—C14—C15 | 119.8 (3) |
| C2—C1—C6 | 121.6 (2) | C13—C14—H14 | 120.1 |
| C2—C1—S1 | 120.8 (2) | C15—C14—H14 | 120.1 |
| C6—C1—S1 | 117.5 (2) | C14—C15—C10 | 120.0 (3) |
| C1—C2—C3 | 119.0 (3) | C14—C15—H15 | 120.0 |
| C1—C2—H2 | 120.5 | C10—C15—H15 | 120.0 |
| C3—C2—H2 | 120.5 | N1—C16—C17 | 113.8 (2) |
| C4—C3—C2 | 120.1 (3) | N1—C16—H16A | 108.8 |
| C4—C3—H3 | 120.0 | C17—C16—H16A | 108.8 |
| C2—C3—H3 | 120.0 | N1—C16—H16B | 108.8 |
| C3—C4—C5 | 121.2 (3) | C17—C16—H16B | 108.8 |
| C3—C4—H4 | 119.4 | H16A—C16—H16B | 107.7 |
| C5—C4—H4 | 119.4 | C22—C17—C18 | 118.0 (3) |
| C4—C5—C6 | 120.1 (3) | C22—C17—C16 | 119.1 (3) |
| C4—C5—H5 | 120.0 | C18—C17—C16 | 122.9 (3) |
| C6—C5—H5 | 120.0 | C19—C18—C17 | 120.7 (3) |
| C5—C6—C1 | 118.1 (2) | C19—C18—Cl1 | 118.4 (3) |
| C5—C6—C7 | 121.3 (2) | C17—C18—Cl1 | 120.8 (3) |
| C1—C6—C7 | 120.6 (2) | C20—C19—C18 | 120.3 (3) |
| O3—C7—C8 | 121.4 (2) | C20—C19—H19 | 119.9 |
| O3—C7—C6 | 114.9 (2) | C18—C19—H19 | 119.9 |
| C8—C7—C6 | 123.7 (2) | C19—C20—C21 | 119.9 (3) |
| C7—C8—N1 | 119.5 (2) | C19—C20—H20 | 120.0 |
| C7—C8—C9 | 121.2 (2) | C21—C20—H20 | 120.0 |
| N1—C8—C9 | 119.2 (2) | C20—C21—C22 | 120.4 (4) |
| O4—C9—C8 | 119.6 (2) | C20—C21—Cl2 | 120.1 (3) |
| O4—C9—C10 | 119.6 (2) | C22—C21—Cl2 | 119.4 (3) |
| C8—C9—C10 | 120.8 (2) | C21—C22—C17 | 120.5 (3) |
| C15—C10—C11 | 119.9 (3) | C21—C22—H22 | 119.7 |
| C15—C10—C9 | 119.4 (2) | C17—C22—H22 | 119.7 |
| C11—C10—C9 | 120.5 (2) | ||
| O1—S1—N1—C8 | −61.89 (19) | S1—N1—C8—C9 | 138.3 (2) |
| O2—S1—N1—C8 | 168.09 (17) | C7—C8—C9—O4 | −16.1 (4) |
| C1—S1—N1—C8 | 51.8 (2) | N1—C8—C9—O4 | 161.9 (2) |
| O1—S1—N1—C16 | 154.46 (18) | C7—C8—C9—C10 | 162.6 (2) |
| O2—S1—N1—C16 | 24.5 (2) | N1—C8—C9—C10 | −19.5 (3) |
| C1—S1—N1—C16 | −91.83 (19) | O4—C9—C10—C15 | −36.4 (4) |
| O1—S1—C1—C2 | −96.7 (2) | C8—C9—C10—C15 | 144.9 (3) |
| O2—S1—C1—C2 | 35.6 (3) | O4—C9—C10—C11 | 138.0 (3) |
| N1—S1—C1—C2 | 150.1 (2) | C8—C9—C10—C11 | −40.7 (4) |
| O1—S1—C1—C6 | 80.8 (2) | C15—C10—C11—C12 | 0.3 (4) |
| O2—S1—C1—C6 | −146.9 (2) | C9—C10—C11—C12 | −174.1 (3) |
| N1—S1—C1—C6 | −32.4 (2) | C10—C11—C12—C13 | −0.7 (4) |
| C6—C1—C2—C3 | −0.8 (4) | C11—C12—C13—C14 | 0.0 (4) |
| S1—C1—C2—C3 | 176.6 (2) | C12—C13—C14—C15 | 1.1 (5) |
| C1—C2—C3—C4 | 0.3 (4) | C13—C14—C15—C10 | −1.5 (4) |
| C2—C3—C4—C5 | 0.3 (5) | C11—C10—C15—C14 | 0.8 (4) |
| C3—C4—C5—C6 | −0.5 (5) | C9—C10—C15—C14 | 175.3 (3) |
| C4—C5—C6—C1 | 0.0 (4) | C8—N1—C16—C17 | −62.6 (3) |
| C4—C5—C6—C7 | −179.3 (3) | S1—N1—C16—C17 | 80.4 (3) |
| C2—C1—C6—C5 | 0.7 (4) | N1—C16—C17—C22 | −86.3 (3) |
| S1—C1—C6—C5 | −176.8 (2) | N1—C16—C17—C18 | 92.3 (3) |
| C2—C1—C6—C7 | −180.0 (2) | C22—C17—C18—C19 | 2.1 (4) |
| S1—C1—C6—C7 | 2.5 (3) | C16—C17—C18—C19 | −176.5 (3) |
| C5—C6—C7—O3 | 16.2 (4) | C22—C17—C18—Cl1 | −177.5 (2) |
| C1—C6—C7—O3 | −163.1 (2) | C16—C17—C18—Cl1 | 3.9 (4) |
| C5—C6—C7—C8 | −166.5 (2) | C17—C18—C19—C20 | −0.7 (5) |
| C1—C6—C7—C8 | 14.2 (4) | Cl1—C18—C19—C20 | 178.9 (3) |
| O3—C7—C8—N1 | −175.6 (2) | C18—C19—C20—C21 | −1.2 (5) |
| C6—C7—C8—N1 | 7.3 (4) | C19—C20—C21—C22 | 1.8 (5) |
| O3—C7—C8—C9 | 2.3 (4) | C19—C20—C21—Cl2 | −177.8 (3) |
| C6—C7—C8—C9 | −174.8 (2) | C20—C21—C22—C17 | −0.4 (4) |
| C16—N1—C8—C7 | 101.2 (3) | Cl2—C21—C22—C17 | 179.2 (2) |
| S1—N1—C8—C7 | −43.8 (3) | C18—C17—C22—C21 | −1.5 (4) |
| C16—N1—C8—C9 | −76.8 (3) | C16—C17—C22—C21 | 177.1 (2) |
| H··· | ||||
| C3—H3···O4i | 0.95 | 2.60 | 3.310 (4) | 132 |
| O3—H3 | 0.84 | 1.80 | 2.539 (3) | 146 |
| C11—H11···N1 | 0.95 | 2.62 | 3.003 (3) | 105 |
| C16—H16 | 0.99 | 2.45 | 2.862 (3) | 105 |
| C16—H16 | 0.99 | 2.67 | 3.120 (3) | 108 |
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| C3—H3⋯O4i | 0.95 | 2.60 | 3.310 (4) | 132 |
| O3—H3 | 0.84 | 1.80 | 2.539 (3) | 146 |
Symmetry code: (i) .