| Literature DB >> 21589450 |
Peter John, Saima Khizar, Islam Ullah Khan, Shahzad Sharif, Edward R T Tiekink.
Abstract
When viewed down the central S⋯N axis of the title compound, C(20)H(26)Entities:
Year: 2010 PMID: 21589450 PMCID: PMC3011401 DOI: 10.1107/S1600536810045708
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| C20H26N2O3S | |
| Monoclinic, | Mo |
| Hall symbol: -P 2ybc | Cell parameters from 7015 reflections |
| θ = 3.0–27.8° | |
| µ = 0.19 mm−1 | |
| β = 97.194 (1)° | Block, colourless |
| 0.28 × 0.14 × 0.08 mm | |
| Bruker APEXII CCD diffractometer | 4079 independent reflections |
| Radiation source: fine-focus sealed tube | 3325 reflections with |
| graphite | |
| φ and ω scans | θmax = 26.5°, θmin = 2.6° |
| Absorption correction: multi-scan ( | |
| 16612 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 | |
| 4079 reflections | (Δ/σ)max = 0.001 |
| 240 parameters | Δρmax = 0.24 e Å−3 |
| 0 restraints | Δρmin = −0.26 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 |
| S1 | 1.12740 (5) | 0.72075 (4) | 0.249229 (18) | 0.03937 (14) | |
| O1 | 1.07590 (16) | 0.82013 (10) | 0.28110 (6) | 0.0509 (3) | |
| O2 | 1.25922 (15) | 0.73062 (12) | 0.21059 (6) | 0.0536 (3) | |
| O3 | 0.27644 (17) | 0.53664 (14) | 0.04014 (7) | 0.0694 (4) | |
| N1 | 1.18549 (16) | 0.62329 (11) | 0.30379 (6) | 0.0376 (3) | |
| N2 | 0.52634 (17) | 0.52003 (13) | 0.09842 (7) | 0.0475 (4) | |
| C1 | 1.2726 (2) | 0.52088 (16) | 0.28259 (8) | 0.0476 (4) | |
| H1A | 1.1913 | 0.4620 | 0.2683 | 0.057* | |
| H1B | 1.3306 | 0.5419 | 0.2470 | 0.057* | |
| C2 | 1.3933 (3) | 0.4738 (2) | 0.33407 (12) | 0.0874 (8) | |
| H2A | 1.4686 | 0.5337 | 0.3505 | 0.131* | |
| H2B | 1.4551 | 0.4123 | 0.3178 | 0.131* | |
| H2C | 1.3347 | 0.4450 | 0.3673 | 0.131* | |
| C3 | 1.06969 (18) | 0.60395 (13) | 0.34975 (7) | 0.0339 (3) | |
| C4 | 1.06258 (19) | 0.68223 (14) | 0.39837 (7) | 0.0389 (3) | |
| H4 | 1.1336 | 0.7456 | 0.4015 | 0.047* | |
| C5 | 0.9517 (2) | 0.66828 (15) | 0.44270 (7) | 0.0422 (4) | |
| C6 | 0.8482 (2) | 0.57149 (16) | 0.43848 (8) | 0.0442 (4) | |
| C7 | 0.8584 (2) | 0.49348 (15) | 0.39000 (8) | 0.0488 (4) | |
| H7 | 0.7902 | 0.4286 | 0.3873 | 0.059* | |
| C8 | 0.9669 (2) | 0.50905 (14) | 0.34545 (8) | 0.0440 (4) | |
| H8 | 0.9704 | 0.4559 | 0.3129 | 0.053* | |
| C9 | 0.9443 (3) | 0.7571 (2) | 0.49396 (9) | 0.0631 (5) | |
| H9A | 1.0265 | 0.8155 | 0.4903 | 0.095* | |
| H9B | 0.9660 | 0.7207 | 0.5347 | 0.095* | |
| H9C | 0.8355 | 0.7916 | 0.4896 | 0.095* | |
| C10 | 0.7272 (3) | 0.5500 (2) | 0.48570 (10) | 0.0673 (6) | |
| H10A | 0.7868 | 0.5468 | 0.5276 | 0.101* | |
| H10B | 0.6708 | 0.4781 | 0.4761 | 0.101* | |
| H10C | 0.6471 | 0.6114 | 0.4834 | 0.101* | |
| C11 | 0.95077 (19) | 0.66426 (14) | 0.20256 (7) | 0.0377 (3) | |
| C12 | 0.7959 (2) | 0.68032 (16) | 0.22264 (8) | 0.0454 (4) | |
| H12 | 0.7859 | 0.7231 | 0.2589 | 0.055* | |
| C13 | 0.6567 (2) | 0.63238 (16) | 0.18843 (8) | 0.0477 (4) | |
| H13 | 0.5526 | 0.6421 | 0.2020 | 0.057* | |
| C14 | 0.67146 (19) | 0.56991 (14) | 0.13400 (8) | 0.0410 (4) | |
| C15 | 0.8263 (2) | 0.55379 (15) | 0.11401 (8) | 0.0435 (4) | |
| H15 | 0.8359 | 0.5115 | 0.0775 | 0.052* | |
| C16 | 0.96666 (19) | 0.60077 (15) | 0.14841 (7) | 0.0422 (4) | |
| H16 | 1.0710 | 0.5898 | 0.1353 | 0.051* | |
| C17 | 0.5128 (2) | 0.39364 (17) | 0.09782 (10) | 0.0592 (5) | |
| H17A | 0.6237 | 0.3608 | 0.1001 | 0.071* | |
| H17B | 0.4510 | 0.3697 | 0.0579 | 0.071* | |
| C18 | 0.4287 (4) | 0.3465 (2) | 0.15098 (12) | 0.0839 (7) | |
| H18A | 0.4904 | 0.3684 | 0.1907 | 0.126* | |
| H18B | 0.4241 | 0.2639 | 0.1480 | 0.126* | |
| H18C | 0.3177 | 0.3768 | 0.1484 | 0.126* | |
| C19 | 0.4017 (2) | 0.58325 (17) | 0.06710 (8) | 0.0485 (4) | |
| C20 | 0.4223 (3) | 0.71197 (17) | 0.06548 (9) | 0.0564 (5) | |
| H20A | 0.3588 | 0.7423 | 0.0280 | 0.085* | |
| H20B | 0.5379 | 0.7305 | 0.0652 | 0.085* | |
| H20C | 0.3834 | 0.7454 | 0.1022 | 0.085* |
| S1 | 0.0372 (2) | 0.0426 (3) | 0.0387 (2) | −0.00274 (16) | 0.00612 (16) | 0.00737 (16) |
| O1 | 0.0619 (8) | 0.0375 (6) | 0.0527 (7) | 0.0004 (6) | 0.0049 (6) | 0.0032 (5) |
| O2 | 0.0408 (6) | 0.0717 (9) | 0.0498 (7) | −0.0092 (6) | 0.0114 (5) | 0.0127 (6) |
| O3 | 0.0518 (8) | 0.0747 (10) | 0.0762 (9) | −0.0066 (7) | −0.0140 (7) | −0.0079 (8) |
| N1 | 0.0376 (7) | 0.0394 (7) | 0.0365 (6) | 0.0037 (5) | 0.0071 (5) | 0.0036 (5) |
| N2 | 0.0397 (7) | 0.0436 (8) | 0.0584 (9) | 0.0001 (6) | 0.0028 (6) | −0.0044 (7) |
| C1 | 0.0457 (9) | 0.0479 (10) | 0.0514 (9) | 0.0085 (8) | 0.0142 (8) | 0.0004 (8) |
| C2 | 0.0891 (17) | 0.0869 (18) | 0.0821 (16) | 0.0473 (14) | −0.0048 (13) | 0.0050 (14) |
| C3 | 0.0342 (7) | 0.0354 (8) | 0.0323 (7) | −0.0006 (6) | 0.0043 (6) | 0.0021 (6) |
| C4 | 0.0388 (8) | 0.0380 (8) | 0.0392 (8) | −0.0052 (7) | 0.0018 (6) | −0.0018 (6) |
| C5 | 0.0413 (8) | 0.0477 (9) | 0.0367 (8) | 0.0048 (7) | 0.0021 (7) | −0.0035 (7) |
| C6 | 0.0393 (8) | 0.0528 (10) | 0.0416 (8) | 0.0021 (7) | 0.0086 (7) | 0.0060 (7) |
| C7 | 0.0494 (10) | 0.0434 (9) | 0.0544 (10) | −0.0142 (8) | 0.0095 (8) | 0.0013 (8) |
| C8 | 0.0530 (10) | 0.0379 (9) | 0.0416 (8) | −0.0073 (7) | 0.0082 (7) | −0.0068 (7) |
| C9 | 0.0642 (12) | 0.0715 (13) | 0.0544 (11) | 0.0027 (10) | 0.0107 (10) | −0.0209 (10) |
| C10 | 0.0596 (12) | 0.0847 (16) | 0.0622 (11) | −0.0031 (11) | 0.0254 (10) | 0.0073 (11) |
| C11 | 0.0340 (8) | 0.0451 (9) | 0.0343 (7) | 0.0036 (7) | 0.0061 (6) | 0.0065 (7) |
| C12 | 0.0404 (9) | 0.0559 (10) | 0.0414 (8) | 0.0047 (8) | 0.0104 (7) | −0.0042 (8) |
| C13 | 0.0339 (8) | 0.0619 (11) | 0.0490 (9) | 0.0029 (8) | 0.0122 (7) | −0.0034 (8) |
| C14 | 0.0351 (8) | 0.0438 (9) | 0.0439 (8) | 0.0014 (7) | 0.0038 (7) | 0.0027 (7) |
| C15 | 0.0428 (9) | 0.0504 (10) | 0.0380 (8) | 0.0055 (7) | 0.0080 (7) | −0.0016 (7) |
| C16 | 0.0344 (8) | 0.0541 (10) | 0.0396 (8) | 0.0058 (7) | 0.0110 (6) | 0.0046 (7) |
| C17 | 0.0519 (11) | 0.0488 (11) | 0.0774 (13) | 0.0015 (8) | 0.0105 (9) | −0.0121 (10) |
| C18 | 0.112 (2) | 0.0563 (13) | 0.0870 (16) | −0.0039 (13) | 0.0250 (15) | 0.0065 (12) |
| C19 | 0.0429 (9) | 0.0578 (11) | 0.0445 (9) | 0.0004 (8) | 0.0043 (7) | −0.0042 (8) |
| C20 | 0.0589 (11) | 0.0538 (11) | 0.0549 (10) | 0.0054 (9) | 0.0002 (9) | 0.0030 (9) |
| S1—O1 | 1.4256 (13) | C9—H9A | 0.9600 |
| S1—O2 | 1.4301 (12) | C9—H9B | 0.9600 |
| S1—N1 | 1.6458 (13) | C9—H9C | 0.9600 |
| S1—C11 | 1.7608 (16) | C10—H10A | 0.9600 |
| O3—C19 | 1.226 (2) | C10—H10B | 0.9600 |
| N1—C3 | 1.4534 (18) | C10—H10C | 0.9600 |
| N1—C1 | 1.480 (2) | C11—C12 | 1.386 (2) |
| N2—C19 | 1.352 (2) | C11—C16 | 1.386 (2) |
| N2—C14 | 1.436 (2) | C12—C13 | 1.379 (2) |
| N2—C17 | 1.470 (2) | C12—H12 | 0.9300 |
| C1—C2 | 1.478 (3) | C13—C14 | 1.384 (2) |
| C1—H1A | 0.9700 | C13—H13 | 0.9300 |
| C1—H1B | 0.9700 | C14—C15 | 1.385 (2) |
| C2—H2A | 0.9600 | C15—C16 | 1.383 (2) |
| C2—H2B | 0.9600 | C15—H15 | 0.9300 |
| C2—H2C | 0.9600 | C16—H16 | 0.9300 |
| C3—C8 | 1.376 (2) | C17—C18 | 1.494 (3) |
| C3—C4 | 1.383 (2) | C17—H17A | 0.9700 |
| C4—C5 | 1.390 (2) | C17—H17B | 0.9700 |
| C4—H4 | 0.9300 | C18—H18A | 0.9600 |
| C5—C6 | 1.396 (2) | C18—H18B | 0.9600 |
| C5—C9 | 1.506 (2) | C18—H18C | 0.9600 |
| C6—C7 | 1.382 (2) | C19—C20 | 1.503 (3) |
| C6—C10 | 1.508 (2) | C20—H20A | 0.9600 |
| C7—C8 | 1.382 (2) | C20—H20B | 0.9600 |
| C7—H7 | 0.9300 | C20—H20C | 0.9600 |
| C8—H8 | 0.9300 | ||
| O1—S1—O2 | 119.46 (8) | H9B—C9—H9C | 109.5 |
| O1—S1—N1 | 107.13 (7) | C6—C10—H10A | 109.5 |
| O2—S1—N1 | 107.03 (7) | C6—C10—H10B | 109.5 |
| O1—S1—C11 | 107.71 (8) | H10A—C10—H10B | 109.5 |
| O2—S1—C11 | 108.45 (7) | C6—C10—H10C | 109.5 |
| N1—S1—C11 | 106.37 (7) | H10A—C10—H10C | 109.5 |
| C3—N1—C1 | 116.91 (12) | H10B—C10—H10C | 109.5 |
| C3—N1—S1 | 115.41 (10) | C12—C11—C16 | 120.59 (15) |
| C1—N1—S1 | 116.17 (10) | C12—C11—S1 | 118.50 (12) |
| C19—N2—C14 | 123.41 (15) | C16—C11—S1 | 120.86 (12) |
| C19—N2—C17 | 119.09 (15) | C13—C12—C11 | 119.53 (15) |
| C14—N2—C17 | 117.48 (15) | C13—C12—H12 | 120.2 |
| C2—C1—N1 | 111.47 (16) | C11—C12—H12 | 120.2 |
| C2—C1—H1A | 109.3 | C12—C13—C14 | 120.17 (15) |
| N1—C1—H1A | 109.3 | C12—C13—H13 | 119.9 |
| C2—C1—H1B | 109.3 | C14—C13—H13 | 119.9 |
| N1—C1—H1B | 109.3 | C15—C14—C13 | 120.26 (15) |
| H1A—C1—H1B | 108.0 | C15—C14—N2 | 119.64 (15) |
| C1—C2—H2A | 109.5 | C13—C14—N2 | 120.09 (14) |
| C1—C2—H2B | 109.5 | C16—C15—C14 | 119.88 (15) |
| H2A—C2—H2B | 109.5 | C16—C15—H15 | 120.1 |
| C1—C2—H2C | 109.5 | C14—C15—H15 | 120.1 |
| H2A—C2—H2C | 109.5 | C15—C16—C11 | 119.56 (14) |
| H2B—C2—H2C | 109.5 | C15—C16—H16 | 120.2 |
| C8—C3—C4 | 119.57 (14) | C11—C16—H16 | 120.2 |
| C8—C3—N1 | 120.92 (13) | N2—C17—C18 | 113.53 (17) |
| C4—C3—N1 | 119.50 (13) | N2—C17—H17A | 108.9 |
| C3—C4—C5 | 121.45 (14) | C18—C17—H17A | 108.9 |
| C3—C4—H4 | 119.3 | N2—C17—H17B | 108.9 |
| C5—C4—H4 | 119.3 | C18—C17—H17B | 108.9 |
| C4—C5—C6 | 118.84 (15) | H17A—C17—H17B | 107.7 |
| C4—C5—C9 | 119.93 (16) | C17—C18—H18A | 109.5 |
| C6—C5—C9 | 121.23 (16) | C17—C18—H18B | 109.5 |
| C7—C6—C5 | 118.90 (15) | H18A—C18—H18B | 109.5 |
| C7—C6—C10 | 119.53 (17) | C17—C18—H18C | 109.5 |
| C5—C6—C10 | 121.57 (16) | H18A—C18—H18C | 109.5 |
| C8—C7—C6 | 121.90 (15) | H18B—C18—H18C | 109.5 |
| C8—C7—H7 | 119.0 | O3—C19—N2 | 120.85 (18) |
| C6—C7—H7 | 119.0 | O3—C19—C20 | 120.99 (18) |
| C3—C8—C7 | 119.31 (15) | N2—C19—C20 | 118.16 (16) |
| C3—C8—H8 | 120.3 | C19—C20—H20A | 109.5 |
| C7—C8—H8 | 120.3 | C19—C20—H20B | 109.5 |
| C5—C9—H9A | 109.5 | H20A—C20—H20B | 109.5 |
| C5—C9—H9B | 109.5 | C19—C20—H20C | 109.5 |
| H9A—C9—H9B | 109.5 | H20A—C20—H20C | 109.5 |
| C5—C9—H9C | 109.5 | H20B—C20—H20C | 109.5 |
| H9A—C9—H9C | 109.5 | ||
| O1—S1—N1—C3 | 48.43 (12) | O2—S1—C11—C12 | −159.96 (14) |
| O2—S1—N1—C3 | 177.67 (10) | N1—S1—C11—C12 | 85.22 (14) |
| C11—S1—N1—C3 | −66.55 (12) | O1—S1—C11—C16 | 153.43 (13) |
| O1—S1—N1—C1 | −169.22 (12) | O2—S1—C11—C16 | 22.83 (16) |
| O2—S1—N1—C1 | −39.98 (14) | N1—S1—C11—C16 | −91.99 (14) |
| C11—S1—N1—C1 | 75.80 (13) | C16—C11—C12—C13 | 0.2 (3) |
| C3—N1—C1—C2 | −68.9 (2) | S1—C11—C12—C13 | −177.06 (13) |
| S1—N1—C1—C2 | 149.37 (17) | C11—C12—C13—C14 | −0.8 (3) |
| C1—N1—C3—C8 | −39.7 (2) | C12—C13—C14—C15 | 0.9 (3) |
| S1—N1—C3—C8 | 102.32 (16) | C12—C13—C14—N2 | 180.00 (16) |
| C1—N1—C3—C4 | 140.40 (15) | C19—N2—C14—C15 | −114.12 (19) |
| S1—N1—C3—C4 | −77.54 (16) | C17—N2—C14—C15 | 67.4 (2) |
| C8—C3—C4—C5 | −1.0 (2) | C19—N2—C14—C13 | 66.8 (2) |
| N1—C3—C4—C5 | 178.83 (13) | C17—N2—C14—C13 | −111.71 (19) |
| C3—C4—C5—C6 | 1.4 (2) | C13—C14—C15—C16 | −0.3 (3) |
| C3—C4—C5—C9 | −178.33 (16) | N2—C14—C15—C16 | −179.42 (15) |
| C4—C5—C6—C7 | −0.7 (2) | C14—C15—C16—C11 | −0.4 (3) |
| C9—C5—C6—C7 | 179.10 (17) | C12—C11—C16—C15 | 0.4 (2) |
| C4—C5—C6—C10 | 178.90 (16) | S1—C11—C16—C15 | 177.57 (13) |
| C9—C5—C6—C10 | −1.3 (3) | C19—N2—C17—C18 | −89.7 (2) |
| C5—C6—C7—C8 | −0.5 (3) | C14—N2—C17—C18 | 88.9 (2) |
| C10—C6—C7—C8 | 179.92 (17) | C14—N2—C19—O3 | −176.18 (16) |
| C4—C3—C8—C7 | −0.2 (2) | C17—N2—C19—O3 | 2.3 (3) |
| N1—C3—C8—C7 | 179.99 (15) | C14—N2—C19—C20 | 4.7 (2) |
| C6—C7—C8—C3 | 0.9 (3) | C17—N2—C19—C20 | −176.83 (17) |
| O1—S1—C11—C12 | −29.36 (15) |
| Cg1 is the centroid of the C3–C8 ring. |
| H··· | ||||
| C8—H8···O1i | 0.93 | 2.54 | 3.455 (2) | 170 |
| C10—H10a···Cg1ii | 0.96 | 2.93 | 3.728 (2) | 142 |
Hydrogen-bond geometry (Å, °)
Cg1 is the centroid of the C3–C8 ring.
| H⋯ | ||||
|---|---|---|---|---|
| C8—H8⋯O1i | 0.93 | 2.54 | 3.455 (2) | 170 |
| C10—H10a⋯ | 0.96 | 2.93 | 3.728 (2) | 142 |
Symmetry codes: (i) ; (ii) .