Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011876/ya6243sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011876/ya6243Isup2.hkl |
CCDC reference: 272137
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.014 Å
- R factor = 0.066
- wR factor = 0.185
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT340_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 14
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.638 0.835 Tmin' and Tmax expected: 0.745 0.835 RR' = 0.856 Please check that your absorption correction is appropriate. PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 47 Perc. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Bruker,1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: program (reference)?.
C15H10O4S7 | F(000) = 976 |
Mr = 478.65 | Dx = 1.614 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.3011 (17) Å | Cell parameters from 61 reflections |
b = 12.3846 (13) Å | θ = 5.0–12.4° |
c = 14.187 (2) Å | µ = 0.82 mm−1 |
β = 114.338 (11)° | T = 293 K |
V = 1969.2 (5) Å3 | Prism, yellow |
Z = 4 | 0.35 × 0.31 × 0.22 mm |
Bruker P4 diffractometer | 1760 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.054 |
Graphite monochromator | θmax = 26.0°, θmin = 1.8° |
ω scans | h = −15→1 |
Absorption correction: ψ scan (XSCANS; Bruker, 1996) | k = −15→1 |
Tmin = 0.638, Tmax = 0.835 | l = −16→17 |
4637 measured reflections | 3 standard reflections every 97 reflections |
3768 independent reflections | intensity decay: none |
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)] = 0.066 | H-atom parameters constrained |
wR(F2) = 0.185 | w = 1/[σ2(Fo2) + (0.02P)2 + 8.6426P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max < 0.001 |
3768 reflections | Δρmax = 0.45 e Å−3 |
236 parameters | Δρmin = −0.61 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0058 (5) |
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 | ||
C1 | 0.2457 (6) | 0.0431 (6) | 0.7436 (6) | 0.0566 (19) | |
C2 | 0.2542 (6) | 0.2114 (5) | 0.6363 (6) | 0.0507 (17) | |
C3 | 0.2592 (6) | 0.1257 (5) | 0.5788 (6) | 0.0512 (17) | |
C4 | 0.0041 (7) | 0.2093 (5) | 0.3911 (6) | 0.0546 (18) | |
C5 | −0.0152 (7) | 0.3075 (6) | 0.3411 (6) | 0.067 (2) | |
H5A | 0.0103 | 0.3195 | 0.2887 | 0.080* | |
C6 | −0.0735 (8) | 0.3883 (7) | 0.3705 (8) | 0.086 (3) | |
H6A | −0.0903 | 0.4545 | 0.3365 | 0.103* | |
C7 | −0.1064 (9) | 0.3681 (8) | 0.4520 (9) | 0.092 (3) | |
H7A | −0.1434 | 0.4226 | 0.4731 | 0.111* | |
C8 | −0.0860 (8) | 0.2715 (7) | 0.5012 (8) | 0.078 (3) | |
H8A | −0.1104 | 0.2599 | 0.5543 | 0.093* | |
C9 | −0.0288 (7) | 0.1904 (6) | 0.4723 (6) | 0.060 (2) | |
H9A | −0.0127 | 0.1244 | 0.5066 | 0.072* | |
C10 | 0.5008 (7) | 0.3092 (6) | 0.6254 (7) | 0.060 (2) | |
C11 | 0.5045 (8) | 0.3362 (7) | 0.5339 (7) | 0.069 (2) | |
H11A | 0.4677 | 0.3989 | 0.4993 | 0.083* | |
C12 | 0.5636 (9) | 0.2693 (8) | 0.4930 (8) | 0.086 (3) | |
H12A | 0.5686 | 0.2871 | 0.4312 | 0.103* | |
C13 | 0.6146 (10) | 0.1771 (9) | 0.5439 (9) | 0.096 (3) | |
H13A | 0.6514 | 0.1309 | 0.5143 | 0.115* | |
C14 | 0.6139 (10) | 0.1487 (9) | 0.6390 (9) | 0.101 (3) | |
H14A | 0.6522 | 0.0866 | 0.6738 | 0.121* | |
C15 | 0.5540 (8) | 0.2165 (7) | 0.6798 (8) | 0.077 (3) | |
H15A | 0.5497 | 0.2001 | 0.7422 | 0.092* | |
O1 | 0.0505 (5) | 0.0036 (4) | 0.3867 (5) | 0.0680 (15) | |
O2 | 0.0800 (5) | 0.1239 (4) | 0.2604 (4) | 0.0734 (16) | |
O3 | 0.4577 (6) | 0.3687 (5) | 0.7831 (5) | 0.0806 (17) | |
O4 | 0.4231 (6) | 0.5022 (4) | 0.6431 (5) | 0.0827 (18) | |
S1 | 0.2345 (2) | −0.0353 (2) | 0.8307 (2) | 0.0842 (8) | |
S2 | 0.2488 (2) | 0.18389 (17) | 0.75328 (18) | 0.0681 (6) | |
S3 | 0.25720 (19) | −0.00028 (15) | 0.63162 (18) | 0.0613 (6) | |
S4 | 0.26486 (18) | 0.13498 (16) | 0.45786 (17) | 0.0613 (6) | |
S5 | 0.08245 (19) | 0.10653 (15) | 0.35960 (17) | 0.0591 (5) | |
S6 | 0.24298 (19) | 0.34592 (16) | 0.59385 (19) | 0.0680 (6) | |
S7 | 0.4226 (2) | 0.39319 (16) | 0.67563 (17) | 0.0641 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.039 (4) | 0.066 (4) | 0.066 (5) | 0.011 (3) | 0.023 (4) | 0.008 (4) |
C2 | 0.045 (4) | 0.052 (4) | 0.056 (4) | 0.003 (3) | 0.023 (4) | −0.002 (3) |
C3 | 0.046 (4) | 0.052 (4) | 0.063 (5) | 0.003 (3) | 0.030 (4) | 0.000 (3) |
C4 | 0.058 (5) | 0.049 (4) | 0.065 (5) | −0.006 (3) | 0.033 (4) | 0.004 (3) |
C5 | 0.072 (5) | 0.069 (5) | 0.062 (5) | −0.006 (4) | 0.032 (5) | 0.014 (4) |
C6 | 0.089 (7) | 0.067 (5) | 0.105 (8) | 0.023 (5) | 0.043 (6) | 0.033 (5) |
C7 | 0.087 (7) | 0.092 (7) | 0.106 (9) | 0.019 (6) | 0.049 (7) | 0.013 (6) |
C8 | 0.086 (6) | 0.067 (5) | 0.103 (8) | −0.004 (5) | 0.062 (6) | 0.007 (5) |
C9 | 0.065 (5) | 0.055 (4) | 0.071 (5) | −0.006 (4) | 0.039 (5) | 0.009 (4) |
C10 | 0.053 (5) | 0.056 (4) | 0.076 (6) | −0.002 (4) | 0.032 (4) | 0.003 (4) |
C11 | 0.074 (6) | 0.066 (5) | 0.066 (6) | −0.014 (4) | 0.028 (5) | −0.003 (4) |
C12 | 0.108 (8) | 0.090 (7) | 0.079 (7) | −0.022 (6) | 0.058 (6) | −0.010 (6) |
C13 | 0.101 (8) | 0.097 (8) | 0.106 (9) | 0.013 (6) | 0.059 (7) | −0.007 (7) |
C14 | 0.114 (8) | 0.093 (7) | 0.115 (9) | 0.037 (6) | 0.064 (8) | 0.025 (6) |
C15 | 0.086 (6) | 0.072 (6) | 0.086 (7) | 0.015 (5) | 0.049 (6) | 0.015 (5) |
O1 | 0.085 (4) | 0.047 (3) | 0.082 (4) | −0.009 (3) | 0.044 (3) | 0.010 (3) |
O2 | 0.094 (4) | 0.076 (4) | 0.061 (4) | −0.023 (3) | 0.043 (3) | −0.008 (3) |
O3 | 0.091 (4) | 0.088 (4) | 0.065 (4) | −0.011 (3) | 0.034 (4) | −0.012 (3) |
O4 | 0.107 (5) | 0.043 (3) | 0.103 (5) | −0.007 (3) | 0.048 (4) | 0.000 (3) |
S1 | 0.0830 (17) | 0.0954 (17) | 0.0823 (17) | 0.0036 (14) | 0.0421 (14) | 0.0269 (14) |
S2 | 0.0757 (14) | 0.0637 (12) | 0.0784 (15) | 0.0091 (11) | 0.0455 (13) | −0.0024 (11) |
S3 | 0.0655 (13) | 0.0492 (10) | 0.0775 (14) | 0.0004 (9) | 0.0378 (11) | −0.0005 (9) |
S4 | 0.0642 (12) | 0.0657 (12) | 0.0695 (13) | −0.0066 (10) | 0.0432 (11) | −0.0053 (10) |
S5 | 0.0714 (13) | 0.0509 (10) | 0.0666 (13) | −0.0126 (9) | 0.0401 (11) | −0.0029 (9) |
S6 | 0.0655 (13) | 0.0505 (11) | 0.0899 (17) | 0.0074 (10) | 0.0340 (12) | 0.0019 (10) |
S7 | 0.0758 (14) | 0.0500 (11) | 0.0705 (14) | −0.0047 (10) | 0.0342 (12) | −0.0038 (9) |
C1—S1 | 1.622 (7) | C9—H9A | 0.9300 |
C1—S3 | 1.736 (8) | C10—C11 | 1.360 (11) |
C1—S2 | 1.749 (8) | C10—C15 | 1.388 (11) |
C2—C3 | 1.355 (9) | C10—S7 | 1.755 (8) |
C2—S2 | 1.722 (7) | C11—C12 | 1.378 (11) |
C2—S6 | 1.758 (7) | C11—H11A | 0.9300 |
C3—S3 | 1.735 (7) | C12—C13 | 1.359 (13) |
C3—S4 | 1.750 (7) | C12—H12A | 0.9300 |
C4—C5 | 1.379 (10) | C13—C14 | 1.397 (14) |
C4—C9 | 1.389 (10) | C13—H13A | 0.9300 |
C4—S5 | 1.762 (7) | C14—C15 | 1.391 (11) |
C5—C6 | 1.392 (11) | C14—H14A | 0.9300 |
C5—H5A | 0.9300 | C15—H15A | 0.9300 |
C6—C7 | 1.396 (13) | O1—S5 | 1.433 (5) |
C6—H6A | 0.9300 | O2—S5 | 1.412 (5) |
C7—C8 | 1.356 (12) | O3—S7 | 1.435 (6) |
C7—H7A | 0.9300 | O4—S7 | 1.427 (5) |
C8—C9 | 1.382 (10) | S4—S5 | 2.127 (3) |
C8—H8A | 0.9300 | S6—S7 | 2.111 (3) |
S1—C1—S3 | 125.2 (5) | C10—C11—H11A | 120.5 |
S1—C1—S2 | 122.8 (5) | C12—C11—H11A | 120.5 |
S3—C1—S2 | 111.9 (4) | C13—C12—C11 | 119.3 (9) |
C3—C2—S2 | 117.0 (5) | C13—C12—H12A | 120.4 |
C3—C2—S6 | 123.6 (6) | C11—C12—H12A | 120.4 |
S2—C2—S6 | 119.3 (4) | C12—C13—C14 | 122.7 (9) |
C2—C3—S3 | 115.6 (5) | C12—C13—H13A | 118.7 |
C2—C3—S4 | 124.7 (6) | C14—C13—H13A | 118.7 |
S3—C3—S4 | 119.7 (4) | C15—C14—C13 | 117.7 (9) |
C5—C4—C9 | 121.9 (7) | C15—C14—H14A | 121.1 |
C5—C4—S5 | 120.1 (6) | C13—C14—H14A | 121.1 |
C9—C4—S5 | 117.8 (6) | C10—C15—C14 | 118.5 (8) |
C4—C5—C6 | 118.7 (7) | C10—C15—H15A | 120.8 |
C4—C5—H5A | 120.7 | C14—C15—H15A | 120.8 |
C6—C5—H5A | 120.7 | C2—S2—C1 | 97.4 (3) |
C5—C6—C7 | 118.8 (8) | C3—S3—C1 | 97.9 (3) |
C5—C6—H6A | 120.6 | C3—S4—S5 | 100.0 (2) |
C7—C6—H6A | 120.6 | O2—S5—O1 | 120.5 (3) |
C8—C7—C6 | 122.0 (9) | O2—S5—C4 | 110.7 (4) |
C8—C7—H7A | 119.0 | O1—S5—C4 | 109.6 (3) |
C6—C7—H7A | 119.0 | O2—S5—S4 | 102.2 (3) |
C7—C8—C9 | 119.8 (8) | O1—S5—S4 | 107.7 (3) |
C7—C8—H8A | 120.1 | C4—S5—S4 | 104.7 (3) |
C9—C8—H8A | 120.1 | C2—S6—S7 | 99.1 (3) |
C8—C9—C4 | 118.8 (7) | O4—S7—O3 | 120.3 (4) |
C8—C9—H9A | 120.6 | O4—S7—C10 | 110.7 (4) |
C4—C9—H9A | 120.6 | O3—S7—C10 | 109.3 (4) |
C11—C10—C15 | 122.7 (8) | O4—S7—S6 | 103.2 (3) |
C11—C10—S7 | 118.8 (6) | O3—S7—S6 | 108.3 (3) |
C15—C10—S7 | 118.4 (6) | C10—S7—S6 | 103.7 (3) |
C10—C11—C12 | 119.1 (9) | ||
S2—C2—C3—S3 | 0.8 (8) | S4—C3—S3—C1 | −177.8 (4) |
S6—C2—C3—S3 | −174.7 (4) | S1—C1—S3—C3 | 177.7 (5) |
S2—C2—C3—S4 | 179.8 (4) | S2—C1—S3—C3 | −2.8 (5) |
S6—C2—C3—S4 | 4.3 (10) | C2—C3—S4—S5 | −99.1 (6) |
C9—C4—C5—C6 | −2.5 (13) | S3—C3—S4—S5 | 79.8 (4) |
S5—C4—C5—C6 | −177.7 (7) | C5—C4—S5—O2 | −21.2 (8) |
C4—C5—C6—C7 | 2.3 (14) | C9—C4—S5—O2 | 163.5 (6) |
C5—C6—C7—C8 | −1.8 (17) | C5—C4—S5—O1 | −156.4 (7) |
C6—C7—C8—C9 | 1.4 (17) | C9—C4—S5—O1 | 28.3 (8) |
C7—C8—C9—C4 | −1.5 (14) | C5—C4—S5—S4 | 88.3 (7) |
C5—C4—C9—C8 | 2.1 (12) | C9—C4—S5—S4 | −87.0 (6) |
S5—C4—C9—C8 | 177.4 (7) | C3—S4—S5—O2 | 174.3 (3) |
C15—C10—C11—C12 | −0.2 (13) | C3—S4—S5—O1 | −57.8 (3) |
S7—C10—C11—C12 | −178.6 (7) | C3—S4—S5—C4 | 58.8 (3) |
C10—C11—C12—C13 | 1.3 (14) | C3—C2—S6—S7 | −101.5 (6) |
C11—C12—C13—C14 | −2.7 (17) | S2—C2—S6—S7 | 83.0 (4) |
C12—C13—C14—C15 | 2.7 (18) | C11—C10—S7—O4 | −28.9 (8) |
C11—C10—C15—C14 | 0.2 (14) | C15—C10—S7—O4 | 152.5 (7) |
S7—C10—C15—C14 | 178.7 (8) | C11—C10—S7—O3 | −163.6 (6) |
C13—C14—C15—C10 | −1.4 (16) | C15—C10—S7—O3 | 17.9 (8) |
C3—C2—S2—C1 | −2.5 (6) | C11—C10—S7—S6 | 81.1 (7) |
S6—C2—S2—C1 | 173.3 (4) | C15—C10—S7—S6 | −97.4 (7) |
S1—C1—S2—C2 | −177.3 (5) | C2—S6—S7—O4 | 178.2 (4) |
S3—C1—S2—C2 | 3.1 (5) | C2—S6—S7—O3 | −53.3 (4) |
C2—C3—S3—C1 | 1.2 (6) | C2—S6—S7—C10 | 62.8 (4) |
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