Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807052567/cv2323sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807052567/cv2323Isup2.hkl |
CCDC reference: 636270
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.004 Å
- R factor = 0.034
- wR factor = 0.089
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S4
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.01 From the CIF: _reflns_number_total 3815 Count of symmetry unique reflns 2132 Completeness (_total/calc) 178.94% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1683 Fraction of Friedel pairs measured 0.789 Are heavy atom types Z>Si present yes PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
To an ethanol (10 ml) solution of 4,4'-thiodibenzenethiol (1 mmol) was added an ethanol (5 ml) solution of iodine (2 mmol). The mixture was stirred for 4 h at room temperature, and a pale yellow solution was obtained and filtered. The filtrate was left undisturbed at room temperature for two weeks. Crystals of the title compound suitable for X-ray analysis were grown from an ethanol solution (yield 63%).
All H atoms were placed in geometrically idealized positions (C—H = 0.93 Å) and treated as riding on their parent atoms, with Uiso(H)=1.2Ueq(C).
In the title compound (Fig. 1), the S—S bond lengths are 2.0600 (11) Å [S2—S5] and 2.0589 (12) Å [S3—S6], which are consistent with the reported values (Ogawa et al., 1999). The intramolecular distances C2···C20 and C8···C18 are 4.418 (5) and 7.281 (7) Å, respectively.
For S—S bond lengths, see: Ogawa et al. (1999).
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
Fig. 1. The molecular structure of the title compound, showing 30% probability displacement ellipsoids and atomic numbering. H atoms have been omited for clarity. |
C24H16S6 | F(000) = 1024 |
Mr = 496.73 | Dx = 1.508 Mg m−3 |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 5516 reflections |
a = 14.6300 (15) Å | θ = 2.8–28.2° |
b = 25.025 (3) Å | µ = 0.64 mm−1 |
c = 5.9754 (6) Å | T = 298 K |
V = 2187.7 (4) Å3 | Block, colourless |
Z = 4 | 0.33 × 0.11 × 0.08 mm |
Bruker SMART CCD area-detector diffractometer | 3815 independent reflections |
Radiation source: fine-focus sealed tube | 3452 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
φ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −17→12 |
Tmin = 0.818, Tmax = 0.951 | k = −29→29 |
11286 measured reflections | l = −7→6 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.089 | w = 1/[σ2(Fo2) + (0.051P)2 + 0.7742P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
3815 reflections | Δρmax = 0.25 e Å−3 |
272 parameters | Δρmin = −0.21 e Å−3 |
1 restraint | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (8) |
C24H16S6 | V = 2187.7 (4) Å3 |
Mr = 496.73 | Z = 4 |
Orthorhombic, Pna21 | Mo Kα radiation |
a = 14.6300 (15) Å | µ = 0.64 mm−1 |
b = 25.025 (3) Å | T = 298 K |
c = 5.9754 (6) Å | 0.33 × 0.11 × 0.08 mm |
Bruker SMART CCD area-detector diffractometer | 3815 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3452 reflections with I > 2σ(I) |
Tmin = 0.818, Tmax = 0.951 | Rint = 0.029 |
11286 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.089 | Δρmax = 0.25 e Å−3 |
S = 1.00 | Δρmin = −0.21 e Å−3 |
3815 reflections | Absolute structure: Flack (1983) |
272 parameters | Absolute structure parameter: 0.02 (8) |
1 restraint |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
S1 | 0.04551 (7) | 0.61284 (3) | −0.25432 (16) | 0.0556 (3) | |
S2 | 0.19406 (5) | 0.42222 (3) | 0.33953 (16) | 0.04216 (19) | |
S3 | 0.10998 (5) | 0.81877 (3) | 0.33467 (17) | 0.0505 (2) | |
S4 | 0.42460 (7) | 0.63478 (3) | 0.83251 (19) | 0.0586 (2) | |
S5 | 0.33401 (5) | 0.42247 (3) | 0.30183 (15) | 0.0479 (2) | |
S6 | 0.24892 (6) | 0.82644 (3) | 0.29017 (17) | 0.0495 (2) | |
C1 | 0.09121 (19) | 0.56196 (11) | −0.0797 (5) | 0.0373 (7) | |
C2 | 0.1331 (2) | 0.57092 (12) | 0.1244 (6) | 0.0428 (8) | |
H2 | 0.1401 | 0.6057 | 0.1765 | 0.051* | |
C3 | 0.1646 (2) | 0.52860 (11) | 0.2518 (6) | 0.0393 (7) | |
H3 | 0.1903 | 0.5349 | 0.3916 | 0.047* | |
C4 | 0.15771 (19) | 0.47662 (11) | 0.1706 (5) | 0.0355 (7) | |
C5 | 0.1188 (2) | 0.46789 (11) | −0.0373 (5) | 0.0373 (7) | |
H5 | 0.1156 | 0.4333 | −0.0940 | 0.045* | |
C6 | 0.08465 (19) | 0.50999 (11) | −0.1612 (6) | 0.0400 (6) | |
H6 | 0.0573 | 0.5036 | −0.2992 | 0.048* | |
C7 | 0.0574 (2) | 0.67187 (12) | −0.0927 (5) | 0.0400 (7) | |
C8 | 0.0130 (2) | 0.67842 (12) | 0.1109 (6) | 0.0441 (8) | |
H8 | −0.0272 | 0.6523 | 0.1620 | 0.053* | |
C9 | 0.0283 (2) | 0.72354 (12) | 0.2371 (6) | 0.0415 (7) | |
H9 | 0.0011 | 0.7270 | 0.3771 | 0.050* | |
C10 | 0.0843 (2) | 0.76392 (12) | 0.1554 (5) | 0.0385 (7) | |
C11 | 0.1210 (2) | 0.75951 (13) | −0.0562 (5) | 0.0425 (7) | |
H11 | 0.1532 | 0.7880 | −0.1178 | 0.051* | |
C12 | 0.11021 (19) | 0.71307 (11) | −0.1764 (6) | 0.0418 (7) | |
H12 | 0.1386 | 0.7094 | −0.3148 | 0.050* | |
C13 | 0.4031 (2) | 0.57457 (12) | 0.6845 (6) | 0.0404 (7) | |
C14 | 0.4422 (2) | 0.56461 (12) | 0.4793 (6) | 0.0431 (8) | |
H14 | 0.4823 | 0.5893 | 0.4168 | 0.052* | |
C15 | 0.42192 (19) | 0.51778 (11) | 0.3656 (6) | 0.0394 (7) | |
H15 | 0.4460 | 0.5119 | 0.2237 | 0.047* | |
C16 | 0.3658 (2) | 0.47972 (11) | 0.4632 (5) | 0.0378 (7) | |
C17 | 0.3322 (2) | 0.48796 (13) | 0.6754 (6) | 0.0451 (8) | |
H17 | 0.2985 | 0.4613 | 0.7457 | 0.054* | |
C18 | 0.3483 (2) | 0.53591 (12) | 0.7850 (6) | 0.0436 (7) | |
H18 | 0.3226 | 0.5422 | 0.9249 | 0.052* | |
C19 | 0.3718 (2) | 0.68490 (12) | 0.6690 (6) | 0.0392 (7) | |
C20 | 0.3303 (2) | 0.67732 (12) | 0.4636 (6) | 0.0462 (8) | |
H20 | 0.3279 | 0.6433 | 0.4016 | 0.055* | |
C21 | 0.2923 (2) | 0.72005 (11) | 0.3493 (6) | 0.0446 (7) | |
H21 | 0.2652 | 0.7145 | 0.2104 | 0.053* | |
C22 | 0.2943 (2) | 0.77105 (11) | 0.4405 (5) | 0.0378 (7) | |
C23 | 0.3359 (2) | 0.77856 (12) | 0.6463 (6) | 0.0414 (7) | |
H23 | 0.3380 | 0.8126 | 0.7088 | 0.050* | |
C24 | 0.37435 (19) | 0.73607 (11) | 0.7594 (6) | 0.0410 (7) | |
H24 | 0.4022 | 0.7417 | 0.8973 | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
S1 | 0.0788 (6) | 0.0384 (4) | 0.0496 (5) | 0.0030 (4) | −0.0241 (5) | 0.0010 (4) |
S2 | 0.0472 (4) | 0.0278 (3) | 0.0515 (5) | −0.0022 (3) | −0.0025 (4) | 0.0039 (4) |
S3 | 0.0544 (4) | 0.0424 (4) | 0.0547 (5) | 0.0143 (3) | −0.0033 (5) | −0.0102 (4) |
S4 | 0.0803 (6) | 0.0408 (4) | 0.0545 (5) | 0.0112 (4) | −0.0296 (5) | −0.0075 (5) |
S5 | 0.0467 (4) | 0.0367 (4) | 0.0603 (6) | 0.0083 (3) | −0.0029 (4) | −0.0104 (4) |
S6 | 0.0575 (5) | 0.0309 (4) | 0.0602 (6) | −0.0033 (3) | −0.0076 (4) | 0.0049 (4) |
C1 | 0.0365 (15) | 0.0324 (15) | 0.0430 (19) | 0.0011 (12) | −0.0013 (13) | 0.0013 (13) |
C2 | 0.0506 (19) | 0.0294 (15) | 0.048 (2) | 0.0001 (13) | −0.0111 (16) | −0.0056 (14) |
C3 | 0.0466 (16) | 0.0314 (15) | 0.0399 (18) | 0.0009 (12) | −0.0067 (15) | −0.0029 (13) |
C4 | 0.0340 (15) | 0.0303 (15) | 0.0423 (18) | 0.0009 (12) | 0.0043 (14) | 0.0008 (13) |
C5 | 0.0396 (16) | 0.0292 (15) | 0.0431 (18) | −0.0018 (12) | 0.0027 (14) | −0.0050 (13) |
C6 | 0.0436 (15) | 0.0404 (15) | 0.0361 (16) | −0.0034 (12) | −0.0025 (15) | −0.0047 (16) |
C7 | 0.0420 (16) | 0.0339 (15) | 0.0442 (19) | 0.0049 (12) | −0.0109 (14) | 0.0035 (13) |
C8 | 0.0432 (18) | 0.0398 (18) | 0.049 (2) | −0.0031 (14) | 0.0014 (15) | 0.0115 (15) |
C9 | 0.0381 (15) | 0.0490 (18) | 0.0374 (17) | 0.0071 (13) | 0.0047 (14) | 0.0066 (15) |
C10 | 0.0391 (16) | 0.0332 (15) | 0.0431 (19) | 0.0098 (13) | −0.0050 (14) | 0.0022 (14) |
C11 | 0.0466 (18) | 0.0396 (17) | 0.0414 (18) | −0.0044 (13) | 0.0014 (15) | 0.0039 (14) |
C12 | 0.0454 (15) | 0.0447 (16) | 0.0353 (17) | 0.0023 (12) | 0.0015 (16) | 0.0020 (15) |
C13 | 0.0436 (17) | 0.0351 (16) | 0.0425 (18) | 0.0078 (13) | −0.0116 (14) | −0.0011 (14) |
C14 | 0.0453 (17) | 0.0351 (16) | 0.049 (2) | 0.0006 (13) | 0.0002 (15) | 0.0065 (15) |
C15 | 0.0399 (15) | 0.0384 (15) | 0.0398 (18) | 0.0071 (12) | 0.0025 (14) | 0.0014 (15) |
C16 | 0.0365 (16) | 0.0359 (16) | 0.0411 (18) | 0.0043 (12) | −0.0040 (14) | 0.0018 (14) |
C17 | 0.0402 (18) | 0.049 (2) | 0.046 (2) | −0.0048 (14) | 0.0010 (15) | 0.0024 (16) |
C18 | 0.0414 (15) | 0.0526 (18) | 0.0368 (18) | 0.0068 (13) | −0.0003 (14) | −0.0012 (16) |
C19 | 0.0378 (16) | 0.0340 (15) | 0.0458 (19) | 0.0053 (13) | −0.0046 (14) | −0.0050 (14) |
C20 | 0.058 (2) | 0.0341 (16) | 0.046 (2) | 0.0079 (14) | −0.0123 (16) | −0.0108 (15) |
C21 | 0.0536 (17) | 0.0387 (15) | 0.0413 (17) | 0.0072 (13) | −0.0118 (17) | −0.0070 (16) |
C22 | 0.0383 (16) | 0.0288 (14) | 0.0464 (18) | 0.0001 (12) | 0.0010 (14) | −0.0018 (13) |
C23 | 0.0432 (17) | 0.0324 (16) | 0.049 (2) | −0.0024 (13) | 0.0013 (15) | −0.0109 (14) |
C24 | 0.0420 (16) | 0.0383 (16) | 0.0428 (18) | −0.0012 (12) | −0.0057 (15) | −0.0081 (14) |
S1—C7 | 1.773 (3) | C9—H9 | 0.9300 |
S1—C1 | 1.777 (3) | C10—C11 | 1.379 (5) |
S2—C4 | 1.776 (3) | C11—C12 | 1.376 (4) |
S2—S5 | 2.0600 (11) | C11—H11 | 0.9300 |
S3—C10 | 1.781 (3) | C12—H12 | 0.9300 |
S3—S6 | 2.0589 (12) | C13—C14 | 1.376 (5) |
S4—C19 | 1.768 (3) | C13—C18 | 1.393 (4) |
S4—C13 | 1.775 (3) | C14—C15 | 1.387 (4) |
S5—C16 | 1.789 (3) | C14—H14 | 0.9300 |
S6—C22 | 1.780 (3) | C15—C16 | 1.386 (4) |
C1—C2 | 1.383 (4) | C15—H15 | 0.9300 |
C1—C6 | 1.392 (4) | C16—C17 | 1.376 (5) |
C2—C3 | 1.383 (4) | C17—C18 | 1.387 (4) |
C2—H2 | 0.9300 | C17—H17 | 0.9300 |
C3—C4 | 1.392 (4) | C18—H18 | 0.9300 |
C3—H3 | 0.9300 | C19—C20 | 1.382 (4) |
C4—C5 | 1.384 (4) | C19—C24 | 1.390 (4) |
C5—C6 | 1.381 (4) | C20—C21 | 1.386 (4) |
C5—H5 | 0.9300 | C20—H20 | 0.9300 |
C6—H6 | 0.9300 | C21—C22 | 1.388 (4) |
C7—C12 | 1.383 (4) | C21—H21 | 0.9300 |
C7—C8 | 1.389 (5) | C22—C23 | 1.385 (5) |
C8—C9 | 1.376 (5) | C23—C24 | 1.380 (4) |
C8—H8 | 0.9300 | C23—H23 | 0.9300 |
C9—C10 | 1.390 (4) | C24—H24 | 0.9300 |
C7—S1—C1 | 103.91 (14) | C11—C12—C7 | 120.4 (3) |
C4—S2—S5 | 103.48 (10) | C11—C12—H12 | 119.8 |
C10—S3—S6 | 101.69 (11) | C7—C12—H12 | 119.8 |
C19—S4—C13 | 104.44 (15) | C14—C13—C18 | 119.9 (3) |
C16—S5—S2 | 101.66 (10) | C14—C13—S4 | 121.6 (3) |
C22—S6—S3 | 103.33 (11) | C18—C13—S4 | 118.5 (3) |
C2—C1—C6 | 119.4 (3) | C13—C14—C15 | 120.0 (3) |
C2—C1—S1 | 124.6 (2) | C13—C14—H14 | 120.0 |
C6—C1—S1 | 116.0 (2) | C15—C14—H14 | 120.0 |
C3—C2—C1 | 120.6 (3) | C16—C15—C14 | 120.1 (3) |
C3—C2—H2 | 119.7 | C16—C15—H15 | 119.9 |
C1—C2—H2 | 119.7 | C14—C15—H15 | 119.9 |
C2—C3—C4 | 120.0 (3) | C17—C16—C15 | 119.8 (3) |
C2—C3—H3 | 120.0 | C17—C16—S5 | 121.6 (2) |
C4—C3—H3 | 120.0 | C15—C16—S5 | 118.5 (3) |
C5—C4—C3 | 119.3 (3) | C16—C17—C18 | 120.3 (3) |
C5—C4—S2 | 120.8 (2) | C16—C17—H17 | 119.9 |
C3—C4—S2 | 119.8 (2) | C18—C17—H17 | 119.9 |
C6—C5—C4 | 120.6 (3) | C17—C18—C13 | 119.7 (3) |
C6—C5—H5 | 119.7 | C17—C18—H18 | 120.2 |
C4—C5—H5 | 119.7 | C13—C18—H18 | 120.2 |
C5—C6—C1 | 120.0 (3) | C20—C19—C24 | 118.9 (3) |
C5—C6—H6 | 120.0 | C20—C19—S4 | 125.8 (2) |
C1—C6—H6 | 120.0 | C24—C19—S4 | 115.3 (2) |
C12—C7—C8 | 119.4 (3) | C19—C20—C21 | 120.5 (3) |
C12—C7—S1 | 118.6 (3) | C19—C20—H20 | 119.7 |
C8—C7—S1 | 122.0 (2) | C21—C20—H20 | 119.7 |
C9—C8—C7 | 120.0 (3) | C20—C21—C22 | 120.5 (3) |
C9—C8—H8 | 120.0 | C20—C21—H21 | 119.8 |
C7—C8—H8 | 120.0 | C22—C21—H21 | 119.8 |
C8—C9—C10 | 120.0 (3) | C23—C22—C21 | 118.9 (3) |
C8—C9—H9 | 120.0 | C23—C22—S6 | 120.4 (2) |
C10—C9—H9 | 120.0 | C21—C22—S6 | 120.6 (2) |
C11—C10—C9 | 119.6 (3) | C24—C23—C22 | 120.6 (3) |
C11—C10—S3 | 122.1 (2) | C24—C23—H23 | 119.7 |
C9—C10—S3 | 118.3 (2) | C22—C23—H23 | 119.7 |
C12—C11—C10 | 120.1 (3) | C23—C24—C19 | 120.6 (3) |
C12—C11—H11 | 119.9 | C23—C24—H24 | 119.7 |
C10—C11—H11 | 119.9 | C19—C24—H24 | 119.7 |
C4—S2—S5—C16 | 73.11 (15) | S1—C7—C12—C11 | 180.0 (2) |
C10—S3—S6—C22 | −73.89 (15) | C19—S4—C13—C14 | 67.7 (3) |
C7—S1—C1—C2 | −5.4 (3) | C19—S4—C13—C18 | −115.1 (3) |
C7—S1—C1—C6 | 175.8 (2) | C18—C13—C14—C15 | 4.6 (5) |
C6—C1—C2—C3 | −2.9 (5) | S4—C13—C14—C15 | −178.2 (2) |
S1—C1—C2—C3 | 178.3 (3) | C13—C14—C15—C16 | −3.2 (4) |
C1—C2—C3—C4 | 2.7 (5) | C14—C15—C16—C17 | −1.6 (4) |
C2—C3—C4—C5 | −0.3 (4) | C14—C15—C16—S5 | 175.0 (2) |
C2—C3—C4—S2 | −177.5 (2) | S2—S5—C16—C17 | 47.7 (3) |
S5—S2—C4—C5 | 103.3 (2) | S2—S5—C16—C15 | −128.9 (2) |
S5—S2—C4—C3 | −79.6 (2) | C15—C16—C17—C18 | 5.0 (5) |
C3—C4—C5—C6 | −1.8 (4) | S5—C16—C17—C18 | −171.5 (2) |
S2—C4—C5—C6 | 175.3 (2) | C16—C17—C18—C13 | −3.7 (5) |
C4—C5—C6—C1 | 1.6 (4) | C14—C13—C18—C17 | −1.2 (5) |
C2—C1—C6—C5 | 0.8 (4) | S4—C13—C18—C17 | −178.4 (2) |
S1—C1—C6—C5 | 179.7 (2) | C13—S4—C19—C20 | −4.6 (3) |
C1—S1—C7—C12 | 119.6 (2) | C13—S4—C19—C24 | 176.0 (2) |
C1—S1—C7—C8 | −62.4 (3) | C24—C19—C20—C21 | 0.3 (5) |
C12—C7—C8—C9 | −5.9 (5) | S4—C19—C20—C21 | −179.0 (3) |
S1—C7—C8—C9 | 176.2 (2) | C19—C20—C21—C22 | −0.8 (5) |
C7—C8—C9—C10 | 3.5 (5) | C20—C21—C22—C23 | 0.8 (5) |
C8—C9—C10—C11 | 2.8 (4) | C20—C21—C22—S6 | 177.9 (3) |
C8—C9—C10—S3 | −174.6 (2) | S3—S6—C22—C23 | −104.9 (2) |
S6—S3—C10—C11 | −43.3 (3) | S3—S6—C22—C21 | 78.0 (3) |
S6—S3—C10—C9 | 134.0 (2) | C21—C22—C23—C24 | −0.4 (5) |
C9—C10—C11—C12 | −6.7 (5) | S6—C22—C23—C24 | −177.5 (2) |
S3—C10—C11—C12 | 170.6 (2) | C22—C23—C24—C19 | −0.1 (5) |
C10—C11—C12—C7 | 4.3 (5) | C20—C19—C24—C23 | 0.1 (5) |
C8—C7—C12—C11 | 2.0 (5) | S4—C19—C24—C23 | 179.5 (2) |
Experimental details
Crystal data | |
Chemical formula | C24H16S6 |
Mr | 496.73 |
Crystal system, space group | Orthorhombic, Pna21 |
Temperature (K) | 298 |
a, b, c (Å) | 14.6300 (15), 25.025 (3), 5.9754 (6) |
V (Å3) | 2187.7 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.64 |
Crystal size (mm) | 0.33 × 0.11 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.818, 0.951 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11286, 3815, 3452 |
Rint | 0.029 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.089, 1.00 |
No. of reflections | 3815 |
No. of parameters | 272 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.25, −0.21 |
Absolute structure | Flack (1983) |
Absolute structure parameter | 0.02 (8) |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b).
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In the title compound (Fig. 1), the S—S bond lengths are 2.0600 (11) Å [S2—S5] and 2.0589 (12) Å [S3—S6], which are consistent with the reported values (Ogawa et al., 1999). The intramolecular distances C2···C20 and C8···C18 are 4.418 (5) and 7.281 (7) Å, respectively.