Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806054432/hg2158sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806054432/hg2158Isup2.hkl |
CCDC reference: 636676
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.039
- wR factor = 0.098
- Data-to-parameter ratio = 9.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT432_ALERT_2_B Short Inter X...Y Contact O8 .. C25 .. 2.88 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.56 Ratio PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT410_ALERT_2_C Short Intra H...H Contact H7A .. H15A .. 1.98 Ang. PLAT717_ALERT_1_C D...A Unknown or Inconsistent Label ..........
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 27.47 From the CIF: _reflns_number_total 3660 Count of symmetry unique reflns 3668 Completeness (_total/calc) 99.78% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present no PLAT791_ALERT_1_G Confirm the Absolute Configuration of C1 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C4 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C9 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C16 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C18 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C20 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C22 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C29 = . R
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 9 ALERT level G = General alerts; check 12 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: COLLECT (Bruker Nonius, 2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXTL/PC (Sheldrick, 2001); molecular graphics: SHELXTL/PC; software used to prepare material for publication: SHELXTL/PC.
C31H38O10·0.25H2O | F(000) = 1226 |
Mr = 575.12 | Dx = 1.331 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 24546 reflections |
a = 12.5030 (2) Å | θ = 2.9–27.5° |
b = 13.7366 (2) Å | µ = 0.10 mm−1 |
c = 16.7164 (4) Å | T = 150 K |
V = 2871.02 (9) Å3 | Needle, colourless |
Z = 4 | 0.28 × 0.20 × 0.18 mm |
Bruker Nonius KappaCCD area-detector diffractometer | 3660 independent reflections |
Radiation source: fine-focus sealed tube | 2970 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 2.9° |
φ scans, and ω scans with κ offsets | h = −14→16 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −17→17 |
Tmin = 0.905, Tmax = 0.988 | l = −21→19 |
24546 measured reflections |
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)] = 0.039 | H-atom parameters constrained |
wR(F2) = 0.098 | w = 1/[σ2(Fo2) + (0.0534P)2 + 0.3768P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
3660 reflections | Δρmax = 0.18 e Å−3 |
382 parameters | Δρmin = −0.18 e Å−3 |
0 restraints | Extinction correction: SHELXTL/PC (Sheldrick, 2001), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0103 (14) |
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 | Occ. (<1) | |
O1 | 0.26234 (14) | 0.14471 (13) | 0.54925 (10) | 0.0412 (4) | |
O2 | 0.23418 (17) | 0.07301 (14) | 0.66430 (11) | 0.0535 (5) | |
O3 | 0.34446 (14) | 0.17750 (13) | 0.29332 (10) | 0.0414 (4) | |
O4 | 0.02444 (15) | 0.65269 (15) | 0.68120 (11) | 0.0494 (5) | |
O5 | 0.32497 (14) | 0.44549 (14) | 0.69337 (10) | 0.0410 (4) | |
O6 | 0.4330 (2) | 0.4697 (2) | 0.79861 (15) | 0.0856 (8) | |
O7 | 0.28205 (13) | 0.70216 (11) | 0.46856 (10) | 0.0334 (4) | |
O8 | 0.24304 (16) | 0.69452 (13) | 0.33789 (11) | 0.0480 (5) | |
O9 | 0.38944 (13) | 0.46334 (11) | 0.43976 (11) | 0.0365 (4) | |
O10 | 0.45104 (13) | 0.61471 (11) | 0.41759 (10) | 0.0360 (4) | |
C1 | 0.13840 (17) | 0.27738 (17) | 0.50867 (13) | 0.0284 (5) | |
C2 | 0.13062 (18) | 0.36442 (16) | 0.45148 (13) | 0.0297 (5) | |
H2A | 0.2002 | 0.3988 | 0.4502 | 0.036* | |
H2B | 0.1154 | 0.3405 | 0.3968 | 0.036* | |
C3 | 0.04339 (19) | 0.43555 (18) | 0.47653 (14) | 0.0328 (5) | |
H3A | −0.0268 | 0.4026 | 0.4726 | 0.039* | |
H3B | 0.0429 | 0.4910 | 0.4387 | 0.039* | |
C4 | 0.05712 (18) | 0.47488 (16) | 0.56180 (14) | 0.0319 (5) | |
H4A | −0.0171 | 0.4869 | 0.5818 | 0.038* | |
C5 | 0.10451 (18) | 0.40047 (18) | 0.61844 (13) | 0.0317 (5) | |
C6 | 0.13541 (18) | 0.31132 (17) | 0.59544 (13) | 0.0296 (5) | |
C7 | 0.1698 (2) | 0.23551 (19) | 0.65587 (14) | 0.0402 (6) | |
H7A | 0.2194 | 0.2670 | 0.6941 | 0.048* | |
H7B | 0.1058 | 0.2152 | 0.6864 | 0.048* | |
C8 | 0.2232 (2) | 0.1454 (2) | 0.62445 (15) | 0.0388 (6) | |
C9 | 0.24956 (18) | 0.22997 (17) | 0.49757 (14) | 0.0313 (5) | |
H9A | 0.3055 | 0.2789 | 0.5122 | 0.038* | |
C10 | 0.27362 (18) | 0.19230 (16) | 0.41549 (14) | 0.0320 (5) | |
C11 | 0.2368 (2) | 0.10369 (18) | 0.37960 (17) | 0.0437 (6) | |
H11A | 0.1900 | 0.0573 | 0.4031 | 0.052* | |
C12 | 0.2808 (2) | 0.09846 (19) | 0.30682 (17) | 0.0452 (6) | |
H12A | 0.2693 | 0.0471 | 0.2698 | 0.054* | |
C13 | 0.33851 (19) | 0.23301 (18) | 0.36070 (14) | 0.0358 (5) | |
H13A | 0.3754 | 0.2928 | 0.3681 | 0.043* | |
C14 | 0.04822 (19) | 0.20452 (17) | 0.49362 (15) | 0.0344 (5) | |
H14A | −0.0209 | 0.2371 | 0.5001 | 0.052* | |
H14B | 0.0537 | 0.1508 | 0.5320 | 0.052* | |
H14C | 0.0541 | 0.1789 | 0.4391 | 0.052* | |
C15 | 0.1067 (2) | 0.4326 (2) | 0.70476 (14) | 0.0383 (6) | |
H15A | 0.1480 | 0.3847 | 0.7364 | 0.046* | |
H15B | 0.0327 | 0.4335 | 0.7258 | 0.046* | |
C16 | 0.1572 (2) | 0.5352 (2) | 0.71583 (14) | 0.0387 (6) | |
H16A | 0.1419 | 0.5576 | 0.7716 | 0.046* | |
C17 | 0.0958 (2) | 0.59886 (19) | 0.65894 (15) | 0.0377 (6) | |
C18 | 0.11776 (18) | 0.57665 (17) | 0.57052 (14) | 0.0322 (5) | |
C19 | 0.0624 (2) | 0.65428 (19) | 0.51965 (15) | 0.0386 (6) | |
H19A | −0.0146 | 0.6538 | 0.5309 | 0.058* | |
H19B | 0.0742 | 0.6403 | 0.4629 | 0.058* | |
H19C | 0.0919 | 0.7184 | 0.5326 | 0.058* | |
C20 | 0.24197 (17) | 0.56439 (16) | 0.55623 (13) | 0.0299 (5) | |
H20A | 0.2543 | 0.4925 | 0.5563 | 0.036* | |
C21 | 0.31012 (19) | 0.60348 (19) | 0.62724 (14) | 0.0363 (5) | |
C22 | 0.2793 (2) | 0.5425 (2) | 0.70149 (15) | 0.0402 (6) | |
H22A | 0.3121 | 0.5739 | 0.7495 | 0.048* | |
C23 | 0.2910 (2) | 0.7120 (2) | 0.64773 (17) | 0.0461 (7) | |
H23A | 0.3206 | 0.7529 | 0.6051 | 0.069* | |
H23B | 0.3262 | 0.7277 | 0.6985 | 0.069* | |
H23C | 0.2140 | 0.7241 | 0.6525 | 0.069* | |
C24 | 0.43104 (19) | 0.5914 (2) | 0.61175 (16) | 0.0446 (7) | |
H24A | 0.4453 | 0.5254 | 0.5924 | 0.067* | |
H24B | 0.4705 | 0.6026 | 0.6616 | 0.067* | |
H24C | 0.4541 | 0.6387 | 0.5714 | 0.067* | |
C25 | 0.4033 (2) | 0.4199 (3) | 0.74428 (17) | 0.0545 (8) | |
C26 | 0.4504 (3) | 0.3230 (3) | 0.7240 (2) | 0.0676 (10) | |
H26A | 0.4411 | 0.2785 | 0.7693 | 0.101* | |
H26B | 0.5268 | 0.3306 | 0.7126 | 0.101* | |
H26C | 0.4142 | 0.2963 | 0.6768 | 0.101* | |
C27 | 0.26202 (19) | 0.74272 (17) | 0.39643 (15) | 0.0352 (5) | |
C28 | 0.2646 (2) | 0.85107 (18) | 0.39891 (19) | 0.0487 (7) | |
H28A | 0.1974 | 0.8769 | 0.3774 | 0.073* | |
H28B | 0.3246 | 0.8748 | 0.3666 | 0.073* | |
H28C | 0.2734 | 0.8728 | 0.4544 | 0.073* | |
C29 | 0.27521 (18) | 0.59806 (16) | 0.47185 (13) | 0.0294 (5) | |
H29A | 0.2170 | 0.5779 | 0.4343 | 0.035* | |
C30 | 0.37850 (18) | 0.55084 (16) | 0.44242 (13) | 0.0289 (5) | |
C31 | 0.5518 (2) | 0.5740 (2) | 0.38994 (16) | 0.0412 (6) | |
H31A | 0.5925 | 0.6243 | 0.3616 | 0.062* | |
H31B | 0.5376 | 0.5195 | 0.3537 | 0.062* | |
H31C | 0.5932 | 0.5509 | 0.4359 | 0.062* | |
O1W | 0.3507 (8) | −0.0739 (8) | 0.6079 (6) | 0.077 (3)* | 0.25 |
H1W | 0.3137 | −0.0277 | 0.6255 | 0.116* | 0.25 |
H2W | 0.4080 | −0.0626 | 0.6325 | 0.116* | 0.25 |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.0400 (9) | 0.0471 (10) | 0.0364 (9) | 0.0104 (8) | 0.0006 (8) | 0.0107 (8) |
O2 | 0.0631 (12) | 0.0517 (11) | 0.0457 (11) | 0.0062 (10) | −0.0022 (10) | 0.0192 (10) |
O3 | 0.0464 (10) | 0.0446 (10) | 0.0334 (9) | 0.0058 (8) | 0.0027 (8) | 0.0001 (8) |
O4 | 0.0454 (10) | 0.0569 (11) | 0.0459 (11) | 0.0050 (9) | 0.0121 (9) | −0.0167 (10) |
O5 | 0.0408 (9) | 0.0564 (11) | 0.0258 (8) | 0.0041 (8) | −0.0023 (7) | 0.0005 (8) |
O6 | 0.0927 (19) | 0.109 (2) | 0.0552 (14) | −0.0016 (16) | −0.0388 (14) | −0.0022 (15) |
O7 | 0.0392 (9) | 0.0256 (8) | 0.0353 (9) | 0.0014 (7) | 0.0036 (7) | −0.0017 (7) |
O8 | 0.0637 (12) | 0.0437 (10) | 0.0365 (10) | 0.0017 (9) | 0.0000 (9) | 0.0041 (9) |
O9 | 0.0348 (9) | 0.0296 (9) | 0.0451 (10) | 0.0026 (7) | 0.0063 (8) | −0.0014 (8) |
O10 | 0.0335 (8) | 0.0337 (8) | 0.0407 (9) | −0.0006 (7) | 0.0092 (8) | −0.0003 (7) |
C1 | 0.0259 (11) | 0.0329 (12) | 0.0264 (11) | −0.0017 (9) | 0.0005 (9) | −0.0013 (9) |
C2 | 0.0321 (11) | 0.0338 (12) | 0.0232 (10) | −0.0011 (9) | −0.0002 (9) | −0.0016 (10) |
C3 | 0.0332 (12) | 0.0359 (12) | 0.0292 (11) | 0.0014 (10) | −0.0023 (10) | −0.0015 (10) |
C4 | 0.0253 (11) | 0.0379 (12) | 0.0326 (12) | 0.0009 (9) | 0.0060 (10) | −0.0019 (10) |
C5 | 0.0281 (11) | 0.0408 (13) | 0.0263 (11) | −0.0050 (10) | 0.0035 (9) | 0.0000 (10) |
C6 | 0.0266 (11) | 0.0375 (12) | 0.0247 (10) | −0.0052 (9) | 0.0010 (9) | 0.0012 (10) |
C7 | 0.0483 (14) | 0.0451 (14) | 0.0270 (12) | −0.0036 (12) | −0.0016 (11) | 0.0056 (11) |
C8 | 0.0347 (12) | 0.0486 (15) | 0.0331 (12) | −0.0031 (11) | −0.0040 (11) | 0.0075 (12) |
C9 | 0.0297 (12) | 0.0347 (12) | 0.0294 (11) | 0.0004 (9) | −0.0008 (9) | 0.0048 (10) |
C10 | 0.0281 (11) | 0.0321 (12) | 0.0358 (12) | 0.0042 (9) | 0.0008 (10) | 0.0020 (10) |
C11 | 0.0510 (15) | 0.0304 (12) | 0.0497 (15) | −0.0003 (11) | 0.0112 (13) | −0.0019 (12) |
C12 | 0.0528 (15) | 0.0360 (13) | 0.0469 (15) | 0.0042 (12) | 0.0039 (13) | −0.0069 (12) |
C13 | 0.0387 (13) | 0.0389 (13) | 0.0298 (12) | 0.0014 (10) | −0.0013 (10) | 0.0005 (10) |
C14 | 0.0305 (11) | 0.0371 (13) | 0.0358 (13) | −0.0041 (10) | −0.0001 (11) | −0.0020 (11) |
C15 | 0.0378 (13) | 0.0491 (14) | 0.0281 (12) | −0.0020 (11) | 0.0059 (10) | −0.0015 (11) |
C16 | 0.0431 (14) | 0.0495 (15) | 0.0236 (11) | −0.0031 (12) | 0.0047 (10) | −0.0098 (11) |
C17 | 0.0336 (12) | 0.0423 (13) | 0.0373 (13) | −0.0036 (11) | 0.0069 (11) | −0.0091 (11) |
C18 | 0.0305 (12) | 0.0357 (12) | 0.0304 (12) | 0.0009 (10) | 0.0034 (10) | −0.0054 (10) |
C19 | 0.0342 (13) | 0.0389 (13) | 0.0428 (13) | 0.0055 (11) | 0.0048 (11) | −0.0048 (12) |
C20 | 0.0302 (11) | 0.0309 (11) | 0.0285 (11) | −0.0005 (9) | 0.0020 (10) | −0.0041 (10) |
C21 | 0.0341 (12) | 0.0441 (14) | 0.0306 (12) | −0.0052 (10) | 0.0031 (10) | −0.0069 (11) |
C22 | 0.0411 (14) | 0.0542 (15) | 0.0254 (11) | −0.0037 (12) | 0.0005 (11) | −0.0095 (11) |
C23 | 0.0475 (15) | 0.0505 (15) | 0.0402 (14) | −0.0091 (12) | 0.0049 (12) | −0.0190 (13) |
C24 | 0.0326 (13) | 0.0652 (18) | 0.0359 (14) | −0.0075 (12) | −0.0025 (11) | −0.0064 (13) |
C25 | 0.0472 (15) | 0.085 (2) | 0.0311 (14) | 0.0005 (16) | −0.0039 (13) | 0.0087 (15) |
C26 | 0.0542 (18) | 0.098 (3) | 0.0508 (17) | 0.0233 (19) | 0.0046 (15) | 0.0210 (18) |
C27 | 0.0310 (12) | 0.0351 (12) | 0.0395 (14) | 0.0029 (10) | 0.0062 (11) | 0.0032 (11) |
C28 | 0.0441 (15) | 0.0340 (13) | 0.0679 (19) | 0.0037 (12) | −0.0004 (14) | 0.0100 (14) |
C29 | 0.0332 (12) | 0.0260 (11) | 0.0291 (11) | 0.0017 (9) | 0.0026 (10) | −0.0007 (9) |
C30 | 0.0312 (11) | 0.0316 (13) | 0.0240 (10) | −0.0004 (9) | −0.0003 (9) | 0.0013 (9) |
C31 | 0.0318 (12) | 0.0488 (14) | 0.0430 (14) | −0.0001 (11) | 0.0117 (11) | −0.0017 (12) |
O1—C8 | 1.349 (3) | C14—H14B | 0.9800 |
O1—C9 | 1.464 (3) | C14—H14C | 0.9800 |
O2—C8 | 1.205 (3) | C15—C16 | 1.555 (4) |
O3—C13 | 1.362 (3) | C15—H15A | 0.9900 |
O3—C12 | 1.365 (3) | C15—H15B | 0.9900 |
O4—C17 | 1.217 (3) | C16—C17 | 1.503 (4) |
O5—C25 | 1.344 (3) | C16—C22 | 1.548 (3) |
O5—C22 | 1.457 (3) | C16—H16A | 1.0000 |
O6—C25 | 1.196 (4) | C17—C18 | 1.534 (3) |
O7—C27 | 1.352 (3) | C18—C19 | 1.530 (3) |
O7—C29 | 1.434 (3) | C18—C20 | 1.580 (3) |
O8—C27 | 1.205 (3) | C19—H19A | 0.9800 |
O9—C30 | 1.210 (3) | C19—H19B | 0.9800 |
O10—C30 | 1.328 (3) | C19—H19C | 0.9800 |
O10—C31 | 1.454 (3) | C20—C29 | 1.541 (3) |
C1—C6 | 1.524 (3) | C20—C21 | 1.557 (3) |
C1—C14 | 1.528 (3) | C20—H20A | 1.0000 |
C1—C2 | 1.534 (3) | C21—C24 | 1.543 (3) |
C1—C9 | 1.546 (3) | C21—C22 | 1.546 (4) |
C2—C3 | 1.523 (3) | C21—C23 | 1.548 (4) |
C2—H2A | 0.9900 | C22—H22A | 1.0000 |
C2—H2B | 0.9900 | C23—H23A | 0.9800 |
C3—C4 | 1.534 (3) | C23—H23B | 0.9800 |
C3—H3A | 0.9900 | C23—H23C | 0.9800 |
C3—H3B | 0.9900 | C24—H24A | 0.9800 |
C4—C5 | 1.514 (3) | C24—H24B | 0.9800 |
C4—C18 | 1.597 (3) | C24—H24C | 0.9800 |
C4—H4A | 1.0000 | C25—C26 | 1.495 (5) |
C5—C6 | 1.340 (3) | C26—H26A | 0.9800 |
C5—C15 | 1.509 (3) | C26—H26B | 0.9800 |
C6—C7 | 1.513 (3) | C26—H26C | 0.9800 |
C7—C8 | 1.501 (4) | C27—C28 | 1.489 (3) |
C7—H7A | 0.9900 | C28—H28A | 0.9800 |
C7—H7B | 0.9900 | C28—H28B | 0.9800 |
C9—C10 | 1.497 (3) | C28—H28C | 0.9800 |
C9—H9A | 1.0000 | C29—C30 | 1.527 (3) |
C10—C13 | 1.345 (3) | C29—H29A | 1.0000 |
C10—C11 | 1.433 (4) | C31—H31A | 0.9800 |
C11—C12 | 1.337 (4) | C31—H31B | 0.9800 |
C11—H11A | 0.9500 | C31—H31C | 0.9800 |
C12—H12A | 0.9500 | O1W—H1W | 0.8401 |
C13—H13A | 0.9500 | O1W—H2W | 0.8401 |
C14—H14A | 0.9800 | ||
C8—O1—C9 | 120.31 (19) | O4—C17—C16 | 122.3 (2) |
C13—O3—C12 | 106.06 (19) | O4—C17—C18 | 123.1 (2) |
C25—O5—C22 | 117.8 (2) | C16—C17—C18 | 113.7 (2) |
C27—O7—C29 | 115.74 (18) | C19—C18—C17 | 108.4 (2) |
C30—O10—C31 | 115.91 (18) | C19—C18—C20 | 115.8 (2) |
C6—C1—C14 | 109.81 (18) | C17—C18—C20 | 110.04 (19) |
C6—C1—C2 | 110.68 (18) | C19—C18—C4 | 110.15 (19) |
C14—C1—C2 | 111.17 (18) | C17—C18—C4 | 100.21 (19) |
C6—C1—C9 | 105.38 (18) | C20—C18—C4 | 111.07 (18) |
C14—C1—C9 | 111.56 (18) | C18—C19—H19A | 109.5 |
C2—C1—C9 | 108.09 (17) | C18—C19—H19B | 109.5 |
C3—C2—C1 | 111.97 (18) | H19A—C19—H19B | 109.5 |
C3—C2—H2A | 109.2 | C18—C19—H19C | 109.5 |
C1—C2—H2A | 109.2 | H19A—C19—H19C | 109.5 |
C3—C2—H2B | 109.2 | H19B—C19—H19C | 109.5 |
C1—C2—H2B | 109.2 | C29—C20—C21 | 116.53 (19) |
H2A—C2—H2B | 107.9 | C29—C20—C18 | 111.80 (19) |
C2—C3—C4 | 113.66 (19) | C21—C20—C18 | 112.70 (18) |
C2—C3—H3A | 108.8 | C29—C20—H20A | 104.8 |
C4—C3—H3A | 108.8 | C21—C20—H20A | 104.8 |
C2—C3—H3B | 108.8 | C18—C20—H20A | 104.8 |
C4—C3—H3B | 108.8 | C24—C21—C22 | 108.7 (2) |
H3A—C3—H3B | 107.7 | C24—C21—C23 | 107.0 (2) |
C5—C4—C3 | 112.77 (19) | C22—C21—C23 | 107.8 (2) |
C5—C4—C18 | 110.37 (18) | C24—C21—C20 | 111.8 (2) |
C3—C4—C18 | 116.51 (19) | C22—C21—C20 | 106.79 (19) |
C5—C4—H4A | 105.4 | C23—C21—C20 | 114.6 (2) |
C3—C4—H4A | 105.4 | O5—C22—C21 | 108.84 (19) |
C18—C4—H4A | 105.4 | O5—C22—C16 | 110.0 (2) |
C6—C5—C15 | 122.4 (2) | C21—C22—C16 | 113.9 (2) |
C6—C5—C4 | 123.4 (2) | O5—C22—H22A | 108.0 |
C15—C5—C4 | 114.1 (2) | C21—C22—H22A | 108.0 |
C5—C6—C7 | 121.3 (2) | C16—C22—H22A | 108.0 |
C5—C6—C1 | 124.0 (2) | C21—C23—H23A | 109.5 |
C7—C6—C1 | 114.7 (2) | C21—C23—H23B | 109.5 |
C8—C7—C6 | 117.4 (2) | H23A—C23—H23B | 109.5 |
C8—C7—H7A | 107.9 | C21—C23—H23C | 109.5 |
C6—C7—H7A | 107.9 | H23A—C23—H23C | 109.5 |
C8—C7—H7B | 107.9 | H23B—C23—H23C | 109.5 |
C6—C7—H7B | 107.9 | C21—C24—H24A | 109.5 |
H7A—C7—H7B | 107.2 | C21—C24—H24B | 109.5 |
O2—C8—O1 | 117.9 (2) | H24A—C24—H24B | 109.5 |
O2—C8—C7 | 122.5 (2) | C21—C24—H24C | 109.5 |
O1—C8—C7 | 119.5 (2) | H24A—C24—H24C | 109.5 |
O1—C9—C10 | 104.03 (18) | H24B—C24—H24C | 109.5 |
O1—C9—C1 | 111.36 (17) | O6—C25—O5 | 123.9 (3) |
C10—C9—C1 | 115.87 (18) | O6—C25—C26 | 124.0 (3) |
O1—C9—H9A | 108.4 | O5—C25—C26 | 112.1 (3) |
C10—C9—H9A | 108.4 | C25—C26—H26A | 109.5 |
C1—C9—H9A | 108.4 | C25—C26—H26B | 109.5 |
C13—C10—C11 | 105.2 (2) | H26A—C26—H26B | 109.5 |
C13—C10—C9 | 127.0 (2) | C25—C26—H26C | 109.5 |
C11—C10—C9 | 127.8 (2) | H26A—C26—H26C | 109.5 |
C12—C11—C10 | 107.1 (2) | H26B—C26—H26C | 109.5 |
C12—C11—H11A | 126.4 | O8—C27—O7 | 122.3 (2) |
C10—C11—H11A | 126.4 | O8—C27—C28 | 125.2 (2) |
C11—C12—O3 | 110.3 (2) | O7—C27—C28 | 112.5 (2) |
C11—C12—H12A | 124.8 | C27—C28—H28A | 109.5 |
O3—C12—H12A | 124.8 | C27—C28—H28B | 109.5 |
C10—C13—O3 | 111.3 (2) | H28A—C28—H28B | 109.5 |
C10—C13—H13A | 124.4 | C27—C28—H28C | 109.5 |
O3—C13—H13A | 124.4 | H28A—C28—H28C | 109.5 |
C1—C14—H14A | 109.5 | H28B—C28—H28C | 109.5 |
C1—C14—H14B | 109.5 | O7—C29—C30 | 111.16 (18) |
H14A—C14—H14B | 109.5 | O7—C29—C20 | 110.51 (18) |
C1—C14—H14C | 109.5 | C30—C29—C20 | 113.30 (18) |
H14A—C14—H14C | 109.5 | O7—C29—H29A | 107.2 |
H14B—C14—H14C | 109.5 | C30—C29—H29A | 107.2 |
C5—C15—C16 | 112.7 (2) | C20—C29—H29A | 107.2 |
C5—C15—H15A | 109.1 | O9—C30—O10 | 124.5 (2) |
C16—C15—H15A | 109.1 | O9—C30—C29 | 122.0 (2) |
C5—C15—H15B | 109.1 | O10—C30—C29 | 113.43 (18) |
C16—C15—H15B | 109.1 | O10—C31—H31A | 109.5 |
H15A—C15—H15B | 107.8 | O10—C31—H31B | 109.5 |
C17—C16—C22 | 111.6 (2) | H31A—C31—H31B | 109.5 |
C17—C16—C15 | 104.2 (2) | O10—C31—H31C | 109.5 |
C22—C16—C15 | 116.2 (2) | H31A—C31—H31C | 109.5 |
C17—C16—H16A | 108.2 | H31B—C31—H31C | 109.5 |
C22—C16—H16A | 108.2 | H1W—O1W—H2W | 99.1 |
C15—C16—H16A | 108.2 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O2 | 0.84 | 1.82 | 2.662 (11) | 180 |
O1W—H2W···O6i | 0.84 | 2.34 | 3.180 (11) | 180 |
C2—H2A···O9 | 0.99 | 2.53 | 3.515 (3) | 172 |
C3—H3B···O6ii | 0.99 | 2.42 | 3.260 (3) | 142 |
C7—H7A···O8iii | 0.99 | 2.51 | 3.372 (3) | 146 |
C12—H12A···O2iv | 0.95 | 2.42 | 3.355 (3) | 170 |
C15—H15A···O8iii | 0.99 | 2.43 | 3.396 (3) | 164 |
C20—H20A···O5 | 1.00 | 2.54 | 3.000 (3) | 108 |
C22—H22A···O6 | 1.00 | 2.24 | 2.707 (4) | 107 |
C23—H23A···07 | 0.98 | 2.43 | 3.000 (3) | 116 |
C24—H24C···O10 | 0.98 | 2.59 | 3.271 (3) | 126 |
C26—H26A···O8iii | 0.98 | 2.60 | 3.087 (4) | 111 |
Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) −x+1/2, −y+1, z−1/2; (iii) −x+1/2, −y+1, z+1/2; (iv) −x+1/2, −y, z−1/2. |
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