Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804005768/ya6197sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804005768/ya6197Isup2.hkl |
CCDC reference: 238798
Key indicators
- Single-crystal X-ray study
- T = 93 K
- Mean (C-C) = 0.003 Å
- R factor = 0.033
- wR factor = 0.088
- Data-to-parameter ratio = 17.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.80 mm PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C8 H10 O S PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 C H Cl3
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 27.50 From the CIF: _reflns_number_total 11046 Count of symmetry unique reflns 6130 Completeness (_total/calc) 180.20% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 4916 Fraction of Friedel pairs measured 0.802 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 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 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: PROCESS-AUTO (Rigaku Corporation, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
C40H26O4·2C8H10OS·CHCl3 | F(000) = 2080 |
Mr = 998.42 | Dx = 1.366 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71075 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 41152 reflections |
a = 13.8789 (15) Å | θ = 3.1–27.5° |
b = 15.410 (2) Å | µ = 0.33 mm−1 |
c = 22.705 (2) Å | T = 93 K |
V = 4856.0 (10) Å3 | Block, yellow |
Z = 4 | 0.8 × 0.8 × 0.6 mm |
Rigaku R-AXIS RAPID diffractometer | 10476 reflections with I > 2σ(I) |
ω scans | Rint = 0.040 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995). | θmax = 27.5°, θmin = 3° |
Tmin = 0.779, Tmax = 0.828 | h = −15→18 |
40838 measured reflections | k = −19→19 |
11046 independent reflections | l = −29→28 |
Refinement on F2 | w = 1/[σ2(Fo2) + (0.03P)2 + 3.7498P] where P = (Fo2 + 2Fc2)/3 |
Least-squares matrix: full | (Δ/σ)max = 0.007 |
R[F2 > 2σ(F2)] = 0.033 | Δρmax = 0.27 e Å−3 |
wR(F2) = 0.088 | Δρmin = −0.37 e Å−3 |
S = 1.05 | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
11046 reflections | Extinction coefficient: 0.00146 (18) |
641 parameters | Absolute structure: Flack (1983), 4963 Friedel pairs |
0 restraints | Absolute structure parameter: −0.01 (4) |
H atoms treated by a mixture of independent and constrained refinement |
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. |
x | y | z | Uiso*/Ueq | ||
Cl1 | 0.76606 (4) | 0.59308 (4) | −0.08901 (3) | 0.03354 (12) | |
Cl2 | 0.87539 (4) | 0.48607 (5) | −0.16979 (3) | 0.04138 (15) | |
Cl3 | 0.66691 (4) | 0.47732 (4) | −0.16851 (3) | 0.03682 (14) | |
S2 | 0.66926 (4) | 0.19513 (4) | 0.24223 (2) | 0.02850 (12) | |
S1 | 0.91769 (4) | 0.15684 (3) | −0.08317 (2) | 0.02370 (11) | |
O1 | 0.71990 (11) | 0.32386 (10) | −0.04027 (6) | 0.0236 (3) | |
H1 | 0.768 (3) | 0.293 (2) | −0.0289 (14) | 0.056 (10)* | |
O2 | 0.75189 (10) | 0.24517 (10) | 0.10786 (7) | 0.0232 (3) | |
H2 | 0.760 (2) | 0.2003 (18) | 0.1284 (12) | 0.031 (7)* | |
O3 | 0.85372 (11) | 0.06919 (9) | 0.05650 (6) | 0.0218 (3) | |
H3 | 0.8564 (19) | 0.1166 (17) | 0.0381 (12) | 0.026 (7)* | |
O4 | 0.68286 (11) | −0.02080 (10) | 0.13120 (7) | 0.0256 (3) | |
H4 | 0.712 (2) | 0.023 (2) | 0.1480 (13) | 0.040 (8)* | |
O6 | 0.71915 (12) | 0.13309 (10) | 0.20096 (7) | 0.0287 (3) | |
O5 | 0.84929 (10) | 0.18993 (10) | −0.03659 (6) | 0.0232 (3) | |
C16 | 1.10223 (14) | 0.37986 (13) | 0.02766 (9) | 0.0208 (4) | |
H12 | 1.1613 | 0.3515 | 0.0365 | 0.025* | |
C19 | 0.93000 (15) | 0.46618 (12) | 0.00364 (9) | 0.0205 (4) | |
H15 | 0.8723 | 0.4974 | −0.0039 | 0.025* | |
C18 | 1.01517 (16) | 0.49573 (14) | −0.01913 (10) | 0.0250 (4) | |
H14 | 1.0154 | 0.5457 | −0.0436 | 0.03* | |
C17 | 1.10242 (15) | 0.45300 (13) | −0.00673 (10) | 0.0236 (4) | |
H13 | 1.1613 | 0.4748 | −0.0221 | 0.028* | |
C20 | 0.92647 (14) | 0.38986 (12) | 0.03829 (8) | 0.0171 (4) | |
C15 | 1.01467 (14) | 0.34637 (13) | 0.05005 (8) | 0.0177 (4) | |
C14 | 1.01163 (14) | 0.26826 (12) | 0.08288 (9) | 0.0171 (4) | |
H11 | 1.0703 | 0.2394 | 0.0919 | 0.02* | |
C13 | 0.92695 (14) | 0.23328 (12) | 0.10183 (8) | 0.0161 (3) | |
C12 | 0.83873 (13) | 0.27759 (12) | 0.09004 (8) | 0.0171 (4) | |
C11 | 0.83799 (14) | 0.35563 (12) | 0.06029 (8) | 0.0174 (4) | |
C23 | 0.92672 (13) | 0.15116 (13) | 0.13659 (8) | 0.0175 (4) | |
C22 | 0.88899 (14) | 0.07296 (13) | 0.11214 (9) | 0.0181 (4) | |
C21 | 0.88716 (14) | −0.00289 (13) | 0.14483 (8) | 0.0188 (4) | |
C30 | 0.92327 (14) | −0.00206 (13) | 0.20406 (9) | 0.0195 (4) | |
C25 | 0.96120 (14) | 0.07575 (13) | 0.22815 (9) | 0.0196 (4) | |
C24 | 0.96269 (14) | 0.15102 (13) | 0.19265 (9) | 0.0189 (4) | |
H16 | 0.9894 | 0.203 | 0.2082 | 0.023* | |
C26 | 0.99385 (14) | 0.07689 (14) | 0.28750 (9) | 0.0226 (4) | |
H17 | 1.0199 | 0.1288 | 0.3035 | 0.027* | |
C27 | 0.98827 (16) | 0.00423 (15) | 0.32180 (10) | 0.0264 (4) | |
H18 | 1.0088 | 0.006 | 0.3617 | 0.032* | |
C28 | 0.95200 (16) | −0.07321 (15) | 0.29775 (10) | 0.0281 (5) | |
H19 | 0.9491 | −0.1238 | 0.3216 | 0.034* | |
C29 | 0.92074 (16) | −0.07697 (14) | 0.24047 (9) | 0.0243 (4) | |
H20 | 0.8972 | −0.1302 | 0.225 | 0.029* | |
C31 | 0.84259 (16) | −0.08173 (13) | 0.11912 (8) | 0.0217 (4) | |
C32 | 0.74329 (15) | −0.08477 (13) | 0.11257 (9) | 0.0230 (4) | |
C33 | 0.69741 (16) | −0.15657 (14) | 0.08630 (10) | 0.0269 (4) | |
H21 | 0.6295 | −0.1561 | 0.081 | 0.032* | |
C34 | 0.74970 (18) | −0.22689 (14) | 0.06837 (9) | 0.0293 (5) | |
H22 | 0.7177 | −0.2748 | 0.0507 | 0.035* | |
C35 | 0.85121 (17) | −0.22914 (13) | 0.07580 (9) | 0.0273 (5) | |
C40 | 0.89814 (16) | −0.15521 (14) | 0.10029 (9) | 0.0242 (4) | |
C39 | 1.00001 (17) | −0.15786 (15) | 0.10592 (10) | 0.0291 (5) | |
H26 | 1.033 | −0.1089 | 0.1214 | 0.035* | |
C38 | 1.05137 (18) | −0.22954 (16) | 0.08949 (12) | 0.0353 (5) | |
H25 | 1.1194 | −0.2298 | 0.0939 | 0.042* | |
C37 | 1.0044 (2) | −0.30330 (16) | 0.06599 (11) | 0.0367 (6) | |
H24 | 1.0406 | −0.353 | 0.0548 | 0.044* | |
C36 | 0.9068 (2) | −0.30230 (15) | 0.05950 (10) | 0.0339 (5) | |
H23 | 0.8753 | −0.3518 | 0.0437 | 0.041* | |
C7 | 0.64822 (17) | 0.60202 (15) | 0.16331 (11) | 0.0305 (5) | |
H8 | 0.6261 | 0.6463 | 0.1891 | 0.037* | |
C8 | 0.73139 (18) | 0.55454 (15) | 0.17738 (10) | 0.0302 (5) | |
H9 | 0.7656 | 0.5674 | 0.2126 | 0.036* | |
C9 | 0.76393 (15) | 0.48993 (14) | 0.14105 (9) | 0.0242 (4) | |
H10 | 0.8203 | 0.4584 | 0.1513 | 0.029* | |
C10 | 0.71398 (14) | 0.46983 (12) | 0.08828 (9) | 0.0195 (4) | |
C5 | 0.62956 (14) | 0.51794 (13) | 0.07400 (9) | 0.0207 (4) | |
C4 | 0.57816 (15) | 0.49745 (13) | 0.02183 (9) | 0.0223 (4) | |
H6 | 0.522 | 0.5295 | 0.0119 | 0.027* | |
C6 | 0.59910 (16) | 0.58473 (14) | 0.11271 (10) | 0.0262 (4) | |
H7 | 0.5436 | 0.618 | 0.1032 | 0.031* | |
C3 | 0.60847 (15) | 0.43230 (14) | −0.01405 (9) | 0.0218 (4) | |
H5 | 0.5729 | 0.4183 | −0.0485 | 0.026* | |
C2 | 0.69263 (14) | 0.38552 (12) | −0.00011 (9) | 0.0184 (4) | |
C1 | 0.74601 (14) | 0.40290 (12) | 0.04950 (8) | 0.0178 (4) | |
C57 | 0.77114 (17) | 0.49217 (15) | −0.12591 (10) | 0.0292 (5) | |
H47 | 0.773 (2) | 0.4482 (17) | −0.0964 (12) | 0.035* | |
C54 | 0.73992 (17) | 0.08022 (16) | 0.32340 (10) | 0.0320 (5) | |
H30 | 0.7725 | 0.0546 | 0.291 | 0.038* | |
C51 | 0.64497 (17) | 0.15689 (18) | 0.41738 (11) | 0.0361 (5) | |
H27 | 0.6137 | 0.1833 | 0.45 | 0.043* | |
C52 | 0.70371 (18) | 0.0857 (2) | 0.42662 (11) | 0.0424 (6) | |
H28 | 0.712 | 0.0637 | 0.4654 | 0.051* | |
C53 | 0.75072 (18) | 0.04616 (19) | 0.37987 (11) | 0.0398 (6) | |
H29 | 0.7898 | −0.0036 | 0.3863 | 0.048* | |
C50 | 0.63072 (16) | 0.19054 (15) | 0.36131 (10) | 0.0279 (5) | |
C49 | 0.68156 (16) | 0.15143 (15) | 0.31513 (9) | 0.0256 (4) | |
C55 | 0.56062 (17) | 0.26421 (16) | 0.35160 (11) | 0.0344 (5) | |
H32 | 0.531 | 0.2804 | 0.3892 | 0.052* | |
H33 | 0.5104 | 0.2457 | 0.324 | 0.052* | |
H31 | 0.595 | 0.3143 | 0.3353 | 0.052* | |
C56 | 0.7547 (2) | 0.28362 (18) | 0.25142 (12) | 0.0465 (7) | |
H35 | 0.8187 | 0.2599 | 0.2599 | 0.07* | |
H36 | 0.734 | 0.3206 | 0.2842 | 0.07* | |
H34 | 0.7573 | 0.318 | 0.2152 | 0.07* | |
C46 | 0.78717 (16) | 0.23424 (15) | −0.15804 (9) | 0.0257 (4) | |
C41 | 0.86415 (15) | 0.17762 (13) | −0.15361 (9) | 0.0220 (4) | |
C42 | 0.90022 (17) | 0.13387 (15) | −0.20290 (10) | 0.0293 (5) | |
C43 | 0.85786 (17) | 0.15253 (16) | −0.25703 (10) | 0.0301 (5) | |
H37 | 0.8815 | 0.1247 | −0.2914 | 0.036* | |
C44 | 0.78244 (17) | 0.21035 (14) | −0.26209 (9) | 0.0269 (4) | |
H38 | 0.7554 | 0.2224 | −0.2996 | 0.032* | |
C45 | 0.74636 (17) | 0.25067 (15) | −0.21256 (10) | 0.0289 (5) | |
H39 | 0.6936 | 0.2897 | −0.2158 | 0.035* | |
C47 | 0.9803 (2) | 0.0681 (2) | −0.19856 (13) | 0.0531 (8) | |
H42 | 0.9832 | 0.0342 | −0.235 | 0.08* | |
H43 | 0.9681 | 0.0293 | −0.1652 | 0.08* | |
H41 | 1.0418 | 0.0982 | −0.1926 | 0.08* | |
C48 | 1.01104 (16) | 0.23655 (18) | −0.08747 (11) | 0.0343 (5) | |
H45 | 0.9823 | 0.2942 | −0.0923 | 0.051* | |
H46 | 1.0526 | 0.2239 | −0.1213 | 0.051* | |
H44 | 1.0494 | 0.2352 | −0.0512 | 0.051* | |
H40 | 0.765 (2) | 0.2579 (18) | −0.1232 (13) | 0.039 (7)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cl1 | 0.0371 (3) | 0.0283 (3) | 0.0353 (3) | −0.0014 (2) | −0.0057 (2) | 0.0014 (2) |
Cl2 | 0.0292 (3) | 0.0483 (4) | 0.0467 (4) | −0.0031 (3) | 0.0078 (3) | 0.0003 (3) |
Cl3 | 0.0276 (3) | 0.0467 (3) | 0.0362 (3) | −0.0012 (3) | −0.0017 (2) | −0.0096 (3) |
S2 | 0.0315 (3) | 0.0281 (3) | 0.0260 (3) | 0.0033 (2) | 0.0052 (2) | 0.0039 (2) |
S1 | 0.0244 (2) | 0.0281 (2) | 0.0186 (2) | 0.0064 (2) | 0.00005 (19) | −0.0006 (2) |
O1 | 0.0224 (7) | 0.0266 (8) | 0.0217 (7) | 0.0054 (6) | −0.0035 (6) | −0.0066 (6) |
O2 | 0.0177 (7) | 0.0220 (7) | 0.0300 (8) | −0.0015 (6) | 0.0026 (6) | 0.0086 (6) |
O3 | 0.0297 (8) | 0.0192 (7) | 0.0166 (7) | −0.0031 (6) | −0.0026 (6) | 0.0036 (6) |
O4 | 0.0246 (8) | 0.0262 (8) | 0.0260 (7) | −0.0029 (6) | −0.0029 (6) | 0.0035 (6) |
O6 | 0.0345 (9) | 0.0279 (8) | 0.0237 (7) | 0.0008 (7) | 0.0055 (6) | 0.0004 (6) |
O5 | 0.0230 (7) | 0.0286 (7) | 0.0179 (7) | 0.0031 (6) | 0.0022 (5) | 0.0001 (6) |
C16 | 0.0178 (9) | 0.0225 (9) | 0.0220 (9) | −0.0013 (7) | 0.0006 (7) | −0.0014 (8) |
C19 | 0.0224 (10) | 0.0174 (9) | 0.0218 (9) | 0.0001 (8) | −0.0012 (8) | 0.0009 (8) |
C18 | 0.0288 (11) | 0.0204 (10) | 0.0259 (10) | −0.0044 (8) | −0.0025 (8) | 0.0070 (8) |
C17 | 0.0212 (10) | 0.0232 (10) | 0.0265 (10) | −0.0059 (8) | 0.0028 (8) | 0.0021 (8) |
C20 | 0.0199 (9) | 0.0147 (8) | 0.0166 (9) | −0.0024 (7) | 0.0009 (7) | −0.0023 (7) |
C15 | 0.0163 (9) | 0.0206 (9) | 0.0162 (8) | −0.0008 (7) | −0.0010 (7) | −0.0023 (8) |
C14 | 0.0177 (9) | 0.0142 (8) | 0.0192 (9) | 0.0006 (7) | −0.0007 (7) | −0.0027 (7) |
C13 | 0.0203 (9) | 0.0131 (8) | 0.0150 (8) | −0.0006 (7) | −0.0004 (7) | −0.0006 (7) |
C12 | 0.0160 (8) | 0.0171 (8) | 0.0183 (8) | −0.0011 (7) | 0.0006 (7) | 0.0003 (7) |
C11 | 0.0171 (9) | 0.0200 (9) | 0.0152 (8) | 0.0004 (7) | −0.0006 (7) | −0.0017 (7) |
C23 | 0.0160 (8) | 0.0182 (9) | 0.0184 (9) | 0.0015 (7) | 0.0021 (7) | 0.0020 (7) |
C22 | 0.0178 (9) | 0.0189 (9) | 0.0177 (9) | 0.0010 (7) | 0.0003 (7) | 0.0002 (7) |
C21 | 0.0202 (9) | 0.0185 (9) | 0.0177 (9) | 0.0000 (7) | −0.0006 (7) | 0.0001 (7) |
C30 | 0.0179 (9) | 0.0208 (9) | 0.0198 (9) | 0.0014 (7) | −0.0003 (7) | 0.0013 (7) |
C25 | 0.0166 (9) | 0.0222 (10) | 0.0199 (9) | 0.0024 (7) | −0.0013 (7) | 0.0007 (8) |
C24 | 0.0171 (9) | 0.0187 (9) | 0.0209 (9) | 0.0006 (7) | −0.0016 (7) | −0.0013 (7) |
C26 | 0.0209 (10) | 0.0268 (10) | 0.0200 (10) | 0.0006 (8) | −0.0019 (7) | 0.0002 (8) |
C27 | 0.0270 (10) | 0.0307 (11) | 0.0214 (10) | 0.0037 (9) | −0.0039 (8) | 0.0023 (9) |
C28 | 0.0299 (11) | 0.0306 (11) | 0.0238 (10) | 0.0034 (9) | −0.0023 (9) | 0.0107 (9) |
C29 | 0.0272 (10) | 0.0205 (9) | 0.0252 (10) | −0.0001 (8) | −0.0008 (8) | 0.0033 (8) |
C31 | 0.0292 (10) | 0.0196 (9) | 0.0163 (9) | −0.0041 (8) | −0.0009 (8) | 0.0040 (7) |
C32 | 0.0292 (11) | 0.0200 (9) | 0.0199 (9) | −0.0028 (8) | −0.0017 (8) | 0.0068 (8) |
C33 | 0.0305 (11) | 0.0277 (10) | 0.0224 (10) | −0.0080 (9) | −0.0063 (8) | 0.0066 (9) |
C34 | 0.0433 (14) | 0.0248 (10) | 0.0198 (10) | −0.0119 (10) | −0.0068 (9) | 0.0020 (8) |
C35 | 0.0408 (13) | 0.0192 (10) | 0.0218 (10) | −0.0060 (9) | −0.0007 (9) | 0.0029 (8) |
C40 | 0.0341 (11) | 0.0197 (9) | 0.0188 (9) | −0.0036 (9) | 0.0004 (8) | 0.0021 (8) |
C39 | 0.0337 (12) | 0.0206 (10) | 0.0329 (12) | −0.0019 (9) | 0.0029 (9) | −0.0023 (9) |
C38 | 0.0333 (12) | 0.0325 (12) | 0.0400 (13) | 0.0014 (10) | 0.0039 (10) | −0.0037 (11) |
C37 | 0.0501 (16) | 0.0230 (11) | 0.0370 (13) | 0.0022 (11) | 0.0043 (11) | −0.0050 (10) |
C36 | 0.0547 (15) | 0.0184 (10) | 0.0285 (11) | −0.0049 (10) | −0.0019 (11) | −0.0019 (9) |
C7 | 0.0297 (12) | 0.0282 (11) | 0.0336 (12) | 0.0036 (9) | 0.0031 (9) | −0.0121 (9) |
C8 | 0.0298 (11) | 0.0337 (12) | 0.0271 (11) | 0.0014 (10) | −0.0043 (9) | −0.0085 (9) |
C9 | 0.0222 (10) | 0.0275 (10) | 0.0229 (10) | 0.0016 (9) | −0.0048 (8) | −0.0024 (8) |
C10 | 0.0194 (9) | 0.0183 (9) | 0.0208 (9) | −0.0017 (7) | 0.0008 (7) | 0.0002 (8) |
C5 | 0.0187 (9) | 0.0175 (9) | 0.0259 (10) | 0.0001 (7) | 0.0006 (7) | 0.0000 (8) |
C4 | 0.0194 (9) | 0.0210 (10) | 0.0265 (10) | 0.0025 (8) | −0.0018 (8) | 0.0029 (8) |
C6 | 0.0248 (10) | 0.0198 (10) | 0.0341 (11) | 0.0059 (8) | 0.0005 (9) | −0.0033 (9) |
C3 | 0.0195 (9) | 0.0262 (10) | 0.0197 (10) | −0.0007 (8) | −0.0034 (7) | 0.0011 (8) |
C2 | 0.0189 (9) | 0.0164 (9) | 0.0199 (9) | −0.0016 (7) | 0.0013 (7) | 0.0002 (7) |
C1 | 0.0176 (9) | 0.0159 (8) | 0.0201 (9) | −0.0021 (7) | 0.0001 (7) | 0.0025 (7) |
C57 | 0.0308 (11) | 0.0292 (11) | 0.0278 (11) | −0.0004 (10) | 0.0007 (9) | 0.0024 (9) |
C54 | 0.0287 (11) | 0.0399 (13) | 0.0273 (11) | 0.0044 (10) | 0.0049 (9) | 0.0028 (10) |
C51 | 0.0265 (11) | 0.0551 (15) | 0.0267 (11) | −0.0082 (11) | 0.0032 (9) | −0.0063 (12) |
C52 | 0.0327 (13) | 0.0699 (19) | 0.0245 (12) | −0.0022 (13) | −0.0021 (9) | 0.0066 (12) |
C53 | 0.0301 (13) | 0.0531 (16) | 0.0360 (13) | 0.0065 (11) | −0.0001 (10) | 0.0127 (12) |
C50 | 0.0207 (10) | 0.0314 (11) | 0.0317 (11) | −0.0082 (9) | 0.0020 (8) | −0.0050 (9) |
C49 | 0.0243 (10) | 0.0310 (11) | 0.0215 (10) | −0.0035 (9) | 0.0019 (8) | 0.0016 (8) |
C55 | 0.0284 (12) | 0.0346 (12) | 0.0402 (13) | −0.0043 (10) | 0.0099 (10) | −0.0070 (10) |
C56 | 0.0615 (19) | 0.0374 (14) | 0.0406 (14) | −0.0131 (13) | 0.0173 (13) | −0.0080 (11) |
C46 | 0.0316 (11) | 0.0280 (11) | 0.0175 (9) | 0.0035 (9) | −0.0013 (8) | −0.0042 (8) |
C41 | 0.0254 (10) | 0.0223 (10) | 0.0183 (9) | 0.0001 (8) | −0.0001 (7) | −0.0010 (8) |
C42 | 0.0294 (11) | 0.0313 (11) | 0.0272 (11) | 0.0044 (9) | 0.0010 (9) | −0.0062 (9) |
C43 | 0.0332 (12) | 0.0376 (12) | 0.0194 (10) | −0.0032 (10) | 0.0032 (8) | −0.0081 (9) |
C44 | 0.0333 (12) | 0.0255 (10) | 0.0220 (10) | −0.0070 (9) | −0.0012 (9) | −0.0002 (8) |
C45 | 0.0326 (12) | 0.0296 (11) | 0.0244 (10) | 0.0044 (9) | −0.0048 (9) | −0.0026 (9) |
C47 | 0.0492 (17) | 0.073 (2) | 0.0368 (15) | 0.0310 (16) | −0.0039 (13) | −0.0206 (14) |
C48 | 0.0238 (11) | 0.0530 (15) | 0.0260 (11) | −0.0065 (10) | −0.0012 (9) | −0.0025 (11) |
Cl1—C57 | 1.768 (2) | C40—C39 | 1.420 (3) |
Cl2—C57 | 1.759 (2) | C39—C38 | 1.366 (3) |
Cl3—C57 | 1.755 (2) | C39—H26 | 0.95 |
S2—O6 | 1.5072 (16) | C38—C37 | 1.415 (3) |
S2—C49 | 1.795 (2) | C38—H25 | 0.95 |
S2—C56 | 1.819 (3) | C37—C36 | 1.363 (4) |
S1—O5 | 1.5099 (15) | C37—H24 | 0.95 |
S1—C48 | 1.788 (2) | C36—H23 | 0.95 |
S1—C41 | 1.792 (2) | C7—C6 | 1.362 (3) |
O1—C2 | 1.370 (2) | C7—C8 | 1.403 (3) |
O1—H1 | 0.86 (4) | C7—H8 | 0.95 |
O2—C12 | 1.366 (2) | C8—C9 | 1.369 (3) |
O2—H2 | 0.84 (3) | C8—H9 | 0.95 |
O3—C22 | 1.356 (2) | C9—C10 | 1.418 (3) |
O3—H3 | 0.84 (3) | C9—H10 | 0.95 |
O4—C32 | 1.362 (3) | C10—C5 | 1.424 (3) |
O4—H4 | 0.87 (3) | C10—C1 | 1.427 (3) |
C16—C17 | 1.371 (3) | C5—C6 | 1.418 (3) |
C16—C15 | 1.415 (3) | C5—C4 | 1.418 (3) |
C16—H12 | 0.95 | C4—C3 | 1.360 (3) |
C19—C18 | 1.368 (3) | C4—H6 | 0.95 |
C19—C20 | 1.416 (3) | C6—H7 | 0.95 |
C19—H15 | 0.95 | C3—C2 | 1.409 (3) |
C18—C17 | 1.407 (3) | C3—H5 | 0.95 |
C18—H14 | 0.95 | C2—C1 | 1.375 (3) |
C17—H13 | 0.95 | C57—H47 | 0.95 (3) |
C20—C15 | 1.421 (3) | C54—C49 | 1.377 (3) |
C20—C11 | 1.427 (3) | C54—C53 | 1.393 (3) |
C15—C14 | 1.416 (3) | C54—H30 | 0.95 |
C14—C13 | 1.363 (3) | C51—C52 | 1.383 (4) |
C14—H11 | 0.95 | C51—C50 | 1.389 (3) |
C13—C12 | 1.427 (3) | C51—H27 | 0.95 |
C13—C23 | 1.491 (3) | C52—C53 | 1.387 (4) |
C12—C11 | 1.379 (3) | C52—H28 | 0.95 |
C11—C1 | 1.490 (3) | C53—H29 | 0.95 |
C23—C24 | 1.367 (3) | C50—C49 | 1.400 (3) |
C23—C22 | 1.426 (3) | C50—C55 | 1.511 (3) |
C22—C21 | 1.385 (3) | C55—H32 | 0.98 |
C21—C30 | 1.435 (3) | C55—H33 | 0.98 |
C21—C31 | 1.483 (3) | C55—H31 | 0.98 |
C30—C25 | 1.419 (3) | C56—H35 | 0.98 |
C30—C29 | 1.420 (3) | C56—H36 | 0.98 |
C25—C24 | 1.413 (3) | C56—H34 | 0.98 |
C25—C26 | 1.422 (3) | C46—C41 | 1.383 (3) |
C24—H16 | 0.95 | C46—C45 | 1.385 (3) |
C26—C27 | 1.366 (3) | C46—H40 | 0.93 (3) |
C26—H17 | 0.95 | C41—C42 | 1.399 (3) |
C27—C28 | 1.406 (3) | C42—C43 | 1.392 (3) |
C27—H18 | 0.95 | C42—C47 | 1.507 (3) |
C28—C29 | 1.372 (3) | C43—C44 | 1.379 (3) |
C28—H19 | 0.95 | C43—H37 | 0.95 |
C29—H20 | 0.95 | C44—C45 | 1.379 (3) |
C31—C32 | 1.387 (3) | C44—H38 | 0.95 |
C31—C40 | 1.435 (3) | C45—H39 | 0.95 |
C32—C33 | 1.409 (3) | C47—H42 | 0.98 |
C33—C34 | 1.366 (3) | C47—H43 | 0.98 |
C33—H21 | 0.95 | C47—H41 | 0.98 |
C34—C35 | 1.419 (3) | C48—H45 | 0.98 |
C34—H22 | 0.95 | C48—H46 | 0.98 |
C35—C36 | 1.415 (3) | C48—H44 | 0.98 |
C35—C40 | 1.425 (3) | ||
O6—S2—C49 | 106.96 (10) | C37—C36—H23 | 119.3 |
O6—S2—C56 | 104.32 (11) | C35—C36—H23 | 119.3 |
C49—S2—C56 | 96.52 (12) | C6—C7—C8 | 120.1 (2) |
O5—S1—C48 | 105.18 (10) | C6—C7—H8 | 119.9 |
O5—S1—C41 | 107.70 (9) | C8—C7—H8 | 119.9 |
C48—S1—C41 | 97.41 (11) | C9—C8—C7 | 120.9 (2) |
C2—O1—H1 | 113 (2) | C9—C8—H9 | 119.6 |
C12—O2—H2 | 110.5 (19) | C7—C8—H9 | 119.6 |
C22—O3—H3 | 114.1 (18) | C8—C9—C10 | 120.4 (2) |
C32—O4—H4 | 114.2 (19) | C8—C9—H10 | 119.8 |
C17—C16—C15 | 120.40 (19) | C10—C9—H10 | 119.8 |
C17—C16—H12 | 119.8 | C9—C10—C5 | 118.74 (18) |
C15—C16—H12 | 119.8 | C9—C10—C1 | 121.78 (18) |
C18—C19—C20 | 121.09 (19) | C5—C10—C1 | 119.48 (18) |
C18—C19—H15 | 119.5 | C6—C5—C4 | 121.96 (19) |
C20—C19—H15 | 119.5 | C6—C5—C10 | 118.82 (19) |
C19—C18—C17 | 120.81 (19) | C4—C5—C10 | 119.22 (18) |
C19—C18—H14 | 119.6 | C3—C4—C5 | 120.61 (19) |
C17—C18—H14 | 119.6 | C3—C4—H6 | 119.7 |
C16—C17—C18 | 119.80 (19) | C5—C4—H6 | 119.7 |
C16—C17—H13 | 120.1 | C7—C6—C5 | 121.0 (2) |
C18—C17—H13 | 120.1 | C7—C6—H7 | 119.5 |
C19—C20—C15 | 117.80 (18) | C5—C6—H7 | 119.5 |
C19—C20—C11 | 122.10 (18) | C4—C3—C2 | 119.98 (19) |
C15—C20—C11 | 120.09 (17) | C4—C3—H5 | 120 |
C16—C15—C14 | 121.64 (18) | C2—C3—H5 | 120 |
C16—C15—C20 | 120.03 (18) | O1—C2—C1 | 122.12 (17) |
C14—C15—C20 | 118.30 (17) | O1—C2—C3 | 115.73 (17) |
C13—C14—C15 | 121.86 (17) | C1—C2—C3 | 122.10 (18) |
C13—C14—H11 | 119.1 | C2—C1—C10 | 118.59 (18) |
C15—C14—H11 | 119.1 | C2—C1—C11 | 120.08 (17) |
C14—C13—C12 | 119.44 (17) | C10—C1—C11 | 121.25 (17) |
C14—C13—C23 | 120.30 (17) | Cl3—C57—Cl2 | 111.02 (13) |
C12—C13—C23 | 120.22 (17) | Cl3—C57—Cl1 | 110.06 (13) |
O2—C12—C11 | 117.22 (17) | Cl2—C57—Cl1 | 110.38 (13) |
O2—C12—C13 | 121.76 (16) | Cl3—C57—H47 | 108.1 (17) |
C11—C12—C13 | 121.01 (17) | Cl2—C57—H47 | 110.1 (17) |
C12—C11—C20 | 119.17 (17) | Cl1—C57—H47 | 107.1 (16) |
C12—C11—C1 | 120.87 (17) | C49—C54—C53 | 119.3 (2) |
C20—C11—C1 | 119.94 (16) | C49—C54—H30 | 120.4 |
C24—C23—C22 | 119.67 (18) | C53—C54—H30 | 120.4 |
C24—C23—C13 | 119.56 (18) | C52—C51—C50 | 121.3 (2) |
C22—C23—C13 | 120.77 (17) | C52—C51—H27 | 119.4 |
O3—C22—C21 | 117.17 (17) | C50—C51—H27 | 119.4 |
O3—C22—C23 | 122.09 (17) | C51—C52—C53 | 120.6 (2) |
C21—C22—C23 | 120.74 (18) | C51—C52—H28 | 119.7 |
C22—C21—C30 | 119.23 (18) | C53—C52—H28 | 119.7 |
C22—C21—C31 | 119.22 (17) | C52—C53—C54 | 119.2 (2) |
C30—C21—C31 | 121.45 (17) | C52—C53—H29 | 120.4 |
C25—C30—C29 | 118.13 (18) | C54—C53—H29 | 120.4 |
C25—C30—C21 | 119.88 (17) | C51—C50—C49 | 117.0 (2) |
C29—C30—C21 | 121.97 (18) | C51—C50—C55 | 120.4 (2) |
C24—C25—C30 | 118.64 (18) | C49—C50—C55 | 122.6 (2) |
C24—C25—C26 | 121.73 (19) | C54—C49—C50 | 122.5 (2) |
C30—C25—C26 | 119.60 (19) | C54—C49—S2 | 118.73 (17) |
C23—C24—C25 | 121.81 (19) | C50—C49—S2 | 118.76 (18) |
C23—C24—H16 | 119.1 | C50—C55—H32 | 109.5 |
C25—C24—H16 | 119.1 | C50—C55—H33 | 109.5 |
C27—C26—C25 | 120.8 (2) | H32—C55—H33 | 109.5 |
C27—C26—H17 | 119.6 | C50—C55—H31 | 109.5 |
C25—C26—H17 | 119.6 | H32—C55—H31 | 109.5 |
C26—C27—C28 | 119.6 (2) | H33—C55—H31 | 109.5 |
C26—C27—H18 | 120.2 | S2—C56—H35 | 109.5 |
C28—C27—H18 | 120.2 | S2—C56—H36 | 109.5 |
C29—C28—C27 | 121.2 (2) | H35—C56—H36 | 109.5 |
C29—C28—H19 | 119.4 | S2—C56—H34 | 109.5 |
C27—C28—H19 | 119.4 | H35—C56—H34 | 109.5 |
C28—C29—C30 | 120.6 (2) | H36—C56—H34 | 109.5 |
C28—C29—H20 | 119.7 | C41—C46—C45 | 119.8 (2) |
C30—C29—H20 | 119.7 | C41—C46—H40 | 116.7 (18) |
C32—C31—C40 | 118.38 (19) | C45—C46—H40 | 123.5 (18) |
C32—C31—C21 | 118.96 (19) | C46—C41—C42 | 121.5 (2) |
C40—C31—C21 | 122.66 (19) | C46—C41—S1 | 119.86 (16) |
O4—C32—C31 | 123.66 (19) | C42—C41—S1 | 118.64 (17) |
O4—C32—C33 | 114.94 (19) | C43—C42—C41 | 117.1 (2) |
C31—C32—C33 | 121.4 (2) | C43—C42—C47 | 120.5 (2) |
C34—C33—C32 | 120.6 (2) | C41—C42—C47 | 122.4 (2) |
C34—C33—H21 | 119.7 | C44—C43—C42 | 121.8 (2) |
C32—C33—H21 | 119.7 | C44—C43—H37 | 119.1 |
C33—C34—C35 | 120.7 (2) | C42—C43—H37 | 119.1 |
C33—C34—H22 | 119.6 | C45—C44—C43 | 119.9 (2) |
C35—C34—H22 | 119.6 | C45—C44—H38 | 120 |
C36—C35—C34 | 122.0 (2) | C43—C44—H38 | 120 |
C36—C35—C40 | 119.3 (2) | C44—C45—C46 | 119.9 (2) |
C34—C35—C40 | 118.7 (2) | C44—C45—H39 | 120.1 |
C39—C40—C35 | 117.8 (2) | C46—C45—H39 | 120.1 |
C39—C40—C31 | 122.1 (2) | C42—C47—H42 | 109.5 |
C35—C40—C31 | 120.1 (2) | C42—C47—H43 | 109.5 |
C38—C39—C40 | 121.2 (2) | H42—C47—H43 | 109.5 |
C38—C39—H26 | 119.4 | C42—C47—H41 | 109.5 |
C40—C39—H26 | 119.4 | H42—C47—H41 | 109.5 |
C39—C38—C37 | 120.8 (2) | H43—C47—H41 | 109.5 |
C39—C38—H25 | 119.6 | S1—C48—H45 | 109.5 |
C37—C38—H25 | 119.6 | S1—C48—H46 | 109.5 |
C36—C37—C38 | 119.3 (2) | H45—C48—H46 | 109.5 |
C36—C37—H24 | 120.3 | S1—C48—H44 | 109.5 |
C38—C37—H24 | 120.3 | H45—C48—H44 | 109.5 |
C37—C36—C35 | 121.5 (2) | H46—C48—H44 | 109.5 |
C20—C19—C18—C17 | −2.6 (3) | C34—C35—C40—C39 | −178.4 (2) |
C15—C16—C17—C18 | 0.9 (3) | C36—C35—C40—C31 | −177.65 (19) |
C19—C18—C17—C16 | 1.3 (3) | C34—C35—C40—C31 | 2.5 (3) |
C18—C19—C20—C15 | 1.8 (3) | C32—C31—C40—C39 | −179.38 (19) |
C18—C19—C20—C11 | −177.12 (19) | C21—C31—C40—C39 | 1.0 (3) |
C17—C16—C15—C14 | 176.37 (19) | C32—C31—C40—C35 | −0.3 (3) |
C17—C16—C15—C20 | −1.7 (3) | C21—C31—C40—C35 | −179.89 (18) |
C19—C20—C15—C16 | 0.4 (3) | C35—C40—C39—C38 | −1.3 (3) |
C11—C20—C15—C16 | 179.30 (18) | C31—C40—C39—C38 | 177.8 (2) |
C19—C20—C15—C14 | −177.77 (17) | C40—C39—C38—C37 | 0.4 (4) |
C11—C20—C15—C14 | 1.2 (3) | C39—C38—C37—C36 | 0.3 (4) |
C16—C15—C14—C13 | −176.40 (19) | C38—C37—C36—C35 | −0.1 (4) |
C20—C15—C14—C13 | 1.7 (3) | C34—C35—C36—C37 | 179.0 (2) |
C15—C14—C13—C12 | −2.0 (3) | C40—C35—C36—C37 | −0.8 (3) |
C15—C14—C13—C23 | −179.65 (17) | C6—C7—C8—C9 | −0.6 (4) |
C14—C13—C12—O2 | 179.75 (18) | C7—C8—C9—C10 | 0.1 (4) |
C23—C13—C12—O2 | −2.6 (3) | C8—C9—C10—C5 | −0.1 (3) |
C14—C13—C12—C11 | −0.6 (3) | C8—C9—C10—C1 | 180.0 (2) |
C23—C13—C12—C11 | 177.01 (17) | C9—C10—C5—C6 | 0.6 (3) |
O2—C12—C11—C20 | −176.93 (17) | C1—C10—C5—C6 | −179.46 (18) |
C13—C12—C11—C20 | 3.4 (3) | C9—C10—C5—C4 | −178.99 (19) |
O2—C12—C11—C1 | 1.3 (3) | C1—C10—C5—C4 | 0.9 (3) |
C13—C12—C11—C1 | −178.31 (17) | C6—C5—C4—C3 | −179.2 (2) |
C19—C20—C11—C12 | 175.20 (18) | C10—C5—C4—C3 | 0.5 (3) |
C15—C20—C11—C12 | −3.7 (3) | C8—C7—C6—C5 | 1.2 (4) |
C19—C20—C11—C1 | −3.1 (3) | C4—C5—C6—C7 | 178.4 (2) |
C15—C20—C11—C1 | 178.05 (17) | C10—C5—C6—C7 | −1.2 (3) |
C14—C13—C23—C24 | 69.0 (2) | C5—C4—C3—C2 | −1.2 (3) |
C12—C13—C23—C24 | −108.6 (2) | C4—C3—C2—O1 | −177.07 (18) |
C14—C13—C23—C22 | −111.3 (2) | C4—C3—C2—C1 | 0.5 (3) |
C12—C13—C23—C22 | 71.0 (2) | O1—C2—C1—C10 | 178.28 (17) |
C24—C23—C22—O3 | −179.04 (17) | C3—C2—C1—C10 | 0.8 (3) |
C13—C23—C22—O3 | 1.3 (3) | O1—C2—C1—C11 | 1.5 (3) |
C24—C23—C22—C21 | 0.9 (3) | C3—C2—C1—C11 | −175.94 (18) |
C13—C23—C22—C21 | −178.79 (17) | C9—C10—C1—C2 | 178.37 (19) |
O3—C22—C21—C30 | −179.71 (17) | C5—C10—C1—C2 | −1.5 (3) |
C23—C22—C21—C30 | 0.4 (3) | C9—C10—C1—C11 | −4.9 (3) |
O3—C22—C21—C31 | −3.4 (3) | C5—C10—C1—C11 | 175.20 (17) |
C23—C22—C21—C31 | 176.72 (18) | C12—C11—C1—C2 | −88.3 (2) |
C22—C21—C30—C25 | −0.7 (3) | C20—C11—C1—C2 | 89.9 (2) |
C31—C21—C30—C25 | −176.95 (19) | C12—C11—C1—C10 | 95.0 (2) |
C22—C21—C30—C29 | 178.07 (19) | C20—C11—C1—C10 | −86.8 (2) |
C31—C21—C30—C29 | 1.8 (3) | C50—C51—C52—C53 | 0.4 (4) |
C29—C30—C25—C24 | −179.02 (18) | C51—C52—C53—C54 | 1.5 (4) |
C21—C30—C25—C24 | −0.2 (3) | C49—C54—C53—C52 | −1.1 (4) |
C29—C30—C25—C26 | −0.9 (3) | C52—C51—C50—C49 | −2.6 (3) |
C21—C30—C25—C26 | 177.88 (18) | C52—C51—C50—C55 | 175.5 (2) |
C22—C23—C24—C25 | −1.9 (3) | C53—C54—C49—C50 | −1.2 (4) |
C13—C23—C24—C25 | 177.83 (17) | C53—C54—C49—S2 | 179.4 (2) |
C30—C25—C24—C23 | 1.5 (3) | C51—C50—C49—C54 | 3.0 (3) |
C26—C25—C24—C23 | −176.54 (19) | C55—C50—C49—C54 | −175.1 (2) |
C24—C25—C26—C27 | 177.4 (2) | C51—C50—C49—S2 | −177.64 (17) |
C30—C25—C26—C27 | −0.6 (3) | C55—C50—C49—S2 | 4.3 (3) |
C25—C26—C27—C28 | 1.6 (3) | O6—S2—C49—C54 | 7.7 (2) |
C26—C27—C28—C29 | −0.9 (3) | C56—S2—C49—C54 | −99.5 (2) |
C27—C28—C29—C30 | −0.7 (3) | O6—S2—C49—C50 | −171.73 (17) |
C25—C30—C29—C28 | 1.6 (3) | C56—S2—C49—C50 | 81.1 (2) |
C21—C30—C29—C28 | −177.2 (2) | C45—C46—C41—C42 | −2.2 (3) |
C22—C21—C31—C32 | −71.1 (3) | C45—C46—C41—S1 | 179.54 (18) |
C30—C21—C31—C32 | 105.2 (2) | O5—S1—C41—C46 | 14.7 (2) |
C22—C21—C31—C40 | 108.5 (2) | C48—S1—C41—C46 | −93.9 (2) |
C30—C21—C31—C40 | −75.2 (3) | O5—S1—C41—C42 | −163.65 (17) |
C40—C31—C32—O4 | 176.95 (18) | C48—S1—C41—C42 | 87.8 (2) |
C21—C31—C32—O4 | −3.4 (3) | C46—C41—C42—C43 | 2.6 (3) |
C40—C31—C32—C33 | −2.1 (3) | S1—C41—C42—C43 | −179.09 (18) |
C21—C31—C32—C33 | 177.48 (18) | C46—C41—C42—C47 | −176.5 (3) |
O4—C32—C33—C34 | −176.82 (19) | S1—C41—C42—C47 | 1.8 (3) |
C31—C32—C33—C34 | 2.3 (3) | C41—C42—C43—C44 | −1.1 (4) |
C32—C33—C34—C35 | 0.0 (3) | C47—C42—C43—C44 | 178.0 (3) |
C33—C34—C35—C36 | 177.8 (2) | C42—C43—C44—C45 | −0.7 (4) |
C33—C34—C35—C40 | −2.4 (3) | C43—C44—C45—C46 | 1.2 (3) |
C36—C35—C40—C39 | 1.5 (3) | C41—C46—C45—C44 | 0.2 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O5 | 0.86 (4) | 1.96 (3) | 2.737 (2) | 150 (3) |
O2—H2···O6 | 0.84 (3) | 2.03 (3) | 2.767 (2) | 147 (3) |
O3—H3···O5 | 0.84 (3) | 2.04 (3) | 2.816 (2) | 153 (2) |
O4—H4···O6 | 0.87 (3) | 2.08 (3) | 2.896 (2) | 155 (3) |
C57—H47···O1 | 0.95 (3) | 2.41 (3) | 3.319 (3) | 158 (2) |
C46—H40···O1 | 0.93 (3) | 2.23 (3) | 3.151 (3) | 175 (3) |
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