Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806007161/tk2005sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806007161/tk2005Isup2.hkl |
CCDC reference: 608504
Key indicators
- Single-crystal X-ray study
- T = 180 K
- Mean (C-C) = 0.004 Å
- R factor = 0.026
- wR factor = 0.060
- Data-to-parameter ratio = 11.6
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 24.10 Deg.
Author Response: ..The rather low theta full is due to the used apparatus. The Stoe IPDS because of the fixed phi spindle does not allow easy access to the cusp of data along the mount axis. This is an instrumentation-based restriction, which we have little control over. |
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
Author Response: ...The rather low theta full is due to the used apparatus. The Stoe IPDS because of the fixed phi spindle does not allow easy access to the cusp of data along the mount axis. This is an instrumentation-based restriction, which we have little control over. |
Alert level B THETM01_ALERT_3_B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5745
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 24.10 From the CIF: _diffrn_reflns_theta_full 24.10 From the CIF: _reflns_number_total 2733 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 2963 Completeness (_total/calc) 92.24% PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.92 PLAT023_ALERT_3_C Resolution (too) Low [sin(th)/Lambda < 0.6]..... 24.10 Deg. PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
2 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 6 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS Software (Stoe, 1996); cell refinement: IPDS Software; data reduction: X-RED (Stoe, 1996); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
C14H12O4S8 | Z = 2 |
Mr = 500.72 | F(000) = 512 |
Triclinic, P1 | Dx = 1.783 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.3867 (7) Å | Cell parameters from 8000 reflections |
b = 11.0716 (13) Å | θ = 1.7–26.1° |
c = 14.1462 (16) Å | µ = 0.98 mm−1 |
α = 106.009 (11)° | T = 180 K |
β = 90.107 (12)° | Plate, orange–yellow |
γ = 103.453 (12)° | 0.5 × 0.3 × 0.02 mm |
V = 932.78 (18) Å3 |
Stoe IPDS diffractometer | 2733 independent reflections |
Radiation source: fine-focus sealed tube | 2225 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
φ scans | θmax = 24.1°, θmin = 2.0° |
Absorption correction: multi-scan (Blessing, 1995) | h = −6→6 |
Tmin = 0.712, Tmax = 0.979 | k = −12→12 |
7398 measured reflections | l = −16→16 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0364P)2] where P = (Fo2 + 2Fc2)/3 |
2733 reflections | (Δ/σ)max < 0.001 |
235 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.28 e Å−3 |
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 | 0.5883 (4) | −0.07113 (19) | 0.12969 (15) | 0.0150 (5) | |
C2 | 0.6865 (4) | 0.0104 (2) | 0.21550 (15) | 0.0164 (5) | |
C3 | 0.5017 (4) | −0.20101 (19) | −0.05357 (15) | 0.0160 (5) | |
C4 | 0.3127 (4) | −0.2170 (2) | −0.01319 (15) | 0.0173 (5) | |
C5 | 0.9444 (4) | 0.20572 (19) | 0.33307 (14) | 0.0140 (5) | |
C6 | 0.7574 (4) | 0.1947 (2) | 0.37568 (15) | 0.0158 (5) | |
C7 | 0.3319 (4) | −0.4177 (2) | −0.22100 (16) | 0.0208 (5) | |
H7 | 0.2401 | −0.4078 | −0.2726 | 0.025* | |
C8 | 0.1844 (4) | −0.4514 (2) | −0.14301 (16) | 0.0210 (5) | |
H8 | 0.0637 | −0.5233 | −0.1768 | 0.025* | |
C9 | 1.1541 (4) | 0.3042 (2) | 0.51084 (15) | 0.0163 (5) | |
H9 | 1.2873 | 0.3557 | 0.5506 | 0.02* | |
C10 | 0.9671 (4) | 0.3515 (2) | 0.56182 (15) | 0.0176 (5) | |
H10 | 1.0108 | 0.4463 | 0.5801 | 0.021* | |
C11 | 0.5316 (4) | −0.5621 (2) | −0.19549 (19) | 0.0303 (6) | |
H11A | 0.6513 | −0.4931 | −0.1594 | 0.036* | |
H11B | 0.5885 | −0.6352 | −0.2295 | 0.036* | |
C12 | 0.3742 (5) | −0.6013 (2) | −0.12472 (19) | 0.0315 (6) | |
H12A | 0.2575 | −0.6731 | −0.1601 | 0.038* | |
H12B | 0.4457 | −0.6294 | −0.077 | 0.038* | |
C13 | 1.1188 (5) | 0.1488 (2) | 0.59729 (17) | 0.0298 (6) | |
H13A | 1.2437 | 0.2003 | 0.6414 | 0.036* | |
H13B | 1.11 | 0.0582 | 0.5907 | 0.036* | |
C14 | 0.9190 (5) | 0.1837 (2) | 0.63898 (18) | 0.0335 (7) | |
H14A | 0.7943 | 0.131 | 0.5952 | 0.04* | |
H14B | 0.9017 | 0.166 | 0.7024 | 0.04* | |
O1 | 0.4305 (3) | −0.51882 (15) | −0.26616 (11) | 0.0256 (4) | |
O2 | 0.2891 (3) | −0.49318 (14) | −0.07471 (11) | 0.0241 (4) | |
O3 | 1.1416 (3) | 0.17242 (14) | 0.50242 (11) | 0.0214 (4) | |
O4 | 0.9314 (3) | 0.31811 (15) | 0.65083 (10) | 0.0243 (4) | |
S1 | 0.73390 (10) | −0.11429 (5) | 0.02499 (4) | 0.01928 (15) | |
S2 | 0.31341 (10) | −0.15205 (5) | 0.11500 (4) | 0.02103 (15) | |
S3 | 0.96642 (10) | 0.07803 (5) | 0.23044 (4) | 0.01908 (15) | |
S4 | 0.55056 (10) | 0.05490 (5) | 0.32345 (4) | 0.01799 (15) | |
S5 | 0.54342 (11) | −0.26324 (5) | −0.17755 (4) | 0.02258 (16) | |
S6 | 0.07267 (11) | −0.31886 (6) | −0.07728 (4) | 0.02771 (17) | |
S7 | 1.17817 (10) | 0.32490 (5) | 0.38831 (4) | 0.01849 (15) | |
S8 | 0.70916 (10) | 0.30355 (6) | 0.48407 (4) | 0.02335 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0171 (14) | 0.0120 (10) | 0.0146 (11) | 0.0033 (9) | 0.0020 (9) | 0.0017 (8) |
C2 | 0.0169 (15) | 0.0165 (11) | 0.0144 (11) | 0.0023 (9) | 0.0007 (9) | 0.0037 (9) |
C3 | 0.0200 (15) | 0.0143 (11) | 0.0126 (11) | 0.0047 (9) | −0.0004 (9) | 0.0018 (9) |
C4 | 0.0171 (15) | 0.0173 (11) | 0.0158 (11) | 0.0073 (9) | −0.0029 (9) | −0.0008 (9) |
C5 | 0.0164 (15) | 0.0139 (10) | 0.0099 (10) | 0.0020 (9) | −0.0012 (9) | 0.0019 (8) |
C6 | 0.0162 (15) | 0.0180 (11) | 0.0121 (11) | 0.0054 (9) | −0.0010 (9) | 0.0013 (9) |
C7 | 0.0211 (15) | 0.0210 (12) | 0.0165 (11) | 0.0063 (10) | −0.0047 (10) | −0.0022 (9) |
C8 | 0.0130 (15) | 0.0225 (12) | 0.0215 (12) | 0.0032 (10) | −0.0031 (9) | −0.0026 (10) |
C9 | 0.0148 (14) | 0.0179 (11) | 0.0120 (11) | 0.0018 (9) | −0.0012 (9) | −0.0008 (9) |
C10 | 0.0118 (14) | 0.0215 (12) | 0.0140 (11) | 0.0008 (9) | −0.0021 (9) | −0.0009 (9) |
C11 | 0.0236 (18) | 0.0253 (13) | 0.0374 (15) | 0.0124 (11) | −0.0038 (12) | −0.0039 (11) |
C12 | 0.040 (2) | 0.0194 (12) | 0.0329 (14) | 0.0095 (11) | −0.0054 (12) | 0.0023 (10) |
C13 | 0.044 (2) | 0.0264 (13) | 0.0207 (12) | 0.0081 (12) | −0.0049 (11) | 0.0089 (10) |
C14 | 0.0383 (19) | 0.0385 (15) | 0.0202 (13) | −0.0051 (12) | 0.0001 (11) | 0.0145 (11) |
O1 | 0.0260 (11) | 0.0239 (9) | 0.0209 (8) | 0.0067 (7) | 0.0032 (7) | −0.0039 (7) |
O2 | 0.0283 (12) | 0.0194 (8) | 0.0231 (8) | 0.0054 (7) | 0.0011 (7) | 0.0038 (7) |
O3 | 0.0272 (11) | 0.0180 (8) | 0.0189 (8) | 0.0083 (7) | −0.0008 (7) | 0.0030 (6) |
O4 | 0.0235 (11) | 0.0333 (9) | 0.0118 (8) | 0.0040 (7) | 0.0043 (7) | 0.0017 (7) |
S1 | 0.0161 (4) | 0.0188 (3) | 0.0168 (3) | 0.0004 (2) | 0.0033 (2) | −0.0017 (2) |
S2 | 0.0163 (4) | 0.0255 (3) | 0.0154 (3) | 0.0031 (2) | 0.0037 (2) | −0.0022 (2) |
S3 | 0.0169 (4) | 0.0191 (3) | 0.0156 (3) | 0.0022 (2) | 0.0037 (2) | −0.0022 (2) |
S4 | 0.0144 (4) | 0.0218 (3) | 0.0135 (3) | 0.0005 (2) | 0.0014 (2) | 0.0012 (2) |
S5 | 0.0300 (4) | 0.0211 (3) | 0.0125 (3) | 0.0021 (3) | 0.0045 (2) | 0.0017 (2) |
S6 | 0.0139 (4) | 0.0335 (3) | 0.0275 (3) | 0.0095 (3) | −0.0040 (2) | −0.0077 (3) |
S7 | 0.0168 (4) | 0.0179 (3) | 0.0154 (3) | −0.0019 (2) | 0.0032 (2) | 0.0012 (2) |
S8 | 0.0152 (4) | 0.0311 (3) | 0.0177 (3) | 0.0106 (3) | −0.0008 (2) | −0.0071 (2) |
C1—C2 | 1.345 (3) | C9—O3 | 1.414 (3) |
C1—S2 | 1.759 (2) | C9—C10 | 1.519 (3) |
C1—S1 | 1.763 (2) | C9—S7 | 1.812 (2) |
C2—S3 | 1.758 (2) | C9—H9 | 0.98 |
C2—S4 | 1.766 (2) | C10—O4 | 1.412 (3) |
C3—C4 | 1.332 (3) | C10—S8 | 1.863 (2) |
C3—S5 | 1.744 (2) | C10—H10 | 0.98 |
C3—S1 | 1.760 (2) | C11—O1 | 1.432 (3) |
C4—S6 | 1.752 (2) | C11—C12 | 1.497 (4) |
C4—S2 | 1.756 (2) | C11—H11A | 0.97 |
C5—C6 | 1.334 (3) | C11—H11B | 0.97 |
C5—S3 | 1.757 (2) | C12—O2 | 1.438 (3) |
C5—S7 | 1.758 (2) | C12—H12A | 0.97 |
C6—S8 | 1.747 (2) | C12—H12B | 0.97 |
C6—S4 | 1.761 (2) | C13—O3 | 1.438 (3) |
C7—O1 | 1.412 (3) | C13—C14 | 1.494 (4) |
C7—C8 | 1.520 (3) | C13—H13A | 0.97 |
C7—S5 | 1.862 (2) | C13—H13B | 0.97 |
C7—H7 | 0.98 | C14—O4 | 1.435 (3) |
C8—O2 | 1.408 (3) | C14—H14A | 0.97 |
C8—S6 | 1.807 (2) | C14—H14B | 0.97 |
C8—H8 | 0.98 | ||
C2—C1—S2 | 123.50 (18) | O4—C10—H10 | 106.2 |
C2—C1—S1 | 121.62 (19) | C9—C10—H10 | 106.2 |
S2—C1—S1 | 114.71 (11) | S8—C10—H10 | 106.2 |
C1—C2—S3 | 122.21 (18) | O1—C11—C12 | 110.9 (2) |
C1—C2—S4 | 123.75 (19) | O1—C11—H11A | 109.5 |
S3—C2—S4 | 114.00 (11) | C12—C11—H11A | 109.5 |
C4—C3—S5 | 126.00 (17) | O1—C11—H11B | 109.5 |
C4—C3—S1 | 117.72 (16) | C12—C11—H11B | 109.5 |
S5—C3—S1 | 116.24 (13) | H11A—C11—H11B | 108 |
C3—C4—S6 | 123.41 (16) | O2—C12—C11 | 109.4 (2) |
C3—C4—S2 | 117.62 (17) | O2—C12—H12A | 109.8 |
S6—C4—S2 | 118.22 (14) | C11—C12—H12A | 109.8 |
C6—C5—S3 | 117.34 (16) | O2—C12—H12B | 109.8 |
C6—C5—S7 | 122.42 (16) | C11—C12—H12B | 109.8 |
S3—C5—S7 | 119.15 (13) | H12A—C12—H12B | 108.2 |
C5—C6—S8 | 124.65 (17) | O3—C13—C14 | 109.5 (2) |
C5—C6—S4 | 117.54 (15) | O3—C13—H13A | 109.8 |
S8—C6—S4 | 117.67 (13) | C14—C13—H13A | 109.8 |
O1—C7—C8 | 111.80 (19) | O3—C13—H13B | 109.8 |
O1—C7—S5 | 109.16 (17) | C14—C13—H13B | 109.8 |
C8—C7—S5 | 115.07 (14) | H13A—C13—H13B | 108.2 |
O1—C7—H7 | 106.8 | O4—C14—C13 | 110.4 (2) |
C8—C7—H7 | 106.8 | O4—C14—H14A | 109.6 |
S5—C7—H7 | 106.8 | C13—C14—H14A | 109.6 |
O2—C8—C7 | 112.1 (2) | O4—C14—H14B | 109.6 |
O2—C8—S6 | 109.16 (14) | C13—C14—H14B | 109.6 |
C7—C8—S6 | 112.73 (16) | H14A—C14—H14B | 108.1 |
O2—C8—H8 | 107.5 | C7—O1—C11 | 112.29 (17) |
C7—C8—H8 | 107.5 | C8—O2—C12 | 110.44 (17) |
S6—C8—H8 | 107.5 | C9—O3—C13 | 110.46 (16) |
O3—C9—C10 | 113.11 (18) | C10—O4—C14 | 112.40 (16) |
O3—C9—S7 | 107.57 (13) | C3—S1—C1 | 94.21 (11) |
C10—C9—S7 | 112.84 (16) | C4—S2—C1 | 94.44 (10) |
O3—C9—H9 | 107.7 | C5—S3—C2 | 93.03 (10) |
C10—C9—H9 | 107.7 | C6—S4—C2 | 92.79 (10) |
S7—C9—H9 | 107.7 | C3—S5—C7 | 104.94 (10) |
O4—C10—C9 | 112.10 (19) | C4—S6—C8 | 97.45 (11) |
O4—C10—S8 | 110.19 (15) | C5—S7—C9 | 96.55 (10) |
C9—C10—S8 | 115.40 (14) | C6—S8—C10 | 104.25 (11) |
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