Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807025123/ez2076sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807025123/ez2076Isup2.hkl |
CCDC reference: 651525
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.002 Å
- R factor = 0.039
- wR factor = 0.101
- Data-to-parameter ratio = 11.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.57 Ratio
Alert level C PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.64 mm PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.65 Ratio PLAT412_ALERT_2_C Short Intra XH3 .. XHn H7A .. H27B .. 1.86 Ang.
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 28.00 From the CIF: _reflns_number_total 4236 Count of symmetry unique reflns 4238 Completeness (_total/calc) 99.95% 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 C3 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C5 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C8 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C9 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C10 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C14 = . S PLAT791_ALERT_1_G Confirm the Absolute Configuration of C17 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C18 = . R
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 9 ALERT level G = General alerts; check 8 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 2 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
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2003).
C37H54O2 | F(000) = 1168 |
Mr = 530.8 | Dx = 1.141 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 6693 reflections |
a = 6.7897 (1) Å | θ = 2.7–30.6° |
b = 12.0370 (2) Å | µ = 0.07 mm−1 |
c = 37.8246 (6) Å | T = 173 K |
V = 3091.31 (8) Å3 | Block, colourless |
Z = 4 | 0.64 × 0.56 × 0.16 mm |
Bruker SMART APEXII CCD area-detector diffractometer | 3995 reflections with I > 2σ(I) |
ω scans | Rint = 0.065 |
Absorption correction: integration (XPREP; Bruker, 1999) | θmax = 28°, θmin = 2.0° |
Tmin = 0.960, Tmax = 0.989 | h = −8→8 |
45207 measured reflections | k = −13→15 |
4236 independent reflections | l = −48→49 |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0631P)2 + 0.3893P] where P = (Fo2 + 2Fc2)/3 |
4236 reflections | (Δ/σ)max = 0.001 |
360 parameters | Δρmax = 0.30 e Å−3 |
0 restraints | Δρmin = −0.24 e Å−3 |
Experimental. Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) |
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 | ||
C1 | 0.2238 (2) | 0.66959 (13) | 0.22612 (4) | 0.0203 (3) | |
H1A | 0.1128 | 0.72 | 0.2317 | 0.024* | |
H1B | 0.3448 | 0.7024 | 0.2363 | 0.024* | |
C2 | 0.2468 (2) | 0.66287 (13) | 0.18584 (4) | 0.0212 (3) | |
H2A | 0.1222 | 0.637 | 0.175 | 0.025* | |
H2B | 0.2779 | 0.7373 | 0.1762 | 0.025* | |
C3 | 0.4108 (2) | 0.58281 (13) | 0.17718 (4) | 0.0197 (3) | |
H3 | 0.5332 | 0.6087 | 0.1893 | 0.024* | |
C4 | 0.3688 (2) | 0.46299 (13) | 0.18896 (4) | 0.0194 (3) | |
C5 | 0.3393 (2) | 0.47086 (13) | 0.22985 (3) | 0.0175 (3) | |
H5 | 0.4683 | 0.4991 | 0.2389 | 0.021* | |
C6 | 0.3117 (2) | 0.35937 (13) | 0.24870 (4) | 0.0220 (3) | |
H6A | 0.3941 | 0.3019 | 0.2372 | 0.026* | |
H6B | 0.1723 | 0.3358 | 0.2471 | 0.026* | |
C7 | 0.3717 (2) | 0.37190 (13) | 0.28754 (4) | 0.0211 (3) | |
H7A | 0.5141 | 0.3893 | 0.2887 | 0.025* | |
H7B | 0.3509 | 0.3001 | 0.2997 | 0.025* | |
C8 | 0.2561 (2) | 0.46341 (12) | 0.30742 (4) | 0.0178 (3) | |
C9 | 0.2326 (2) | 0.57017 (12) | 0.28433 (4) | 0.0170 (3) | |
H9 | 0.365 | 0.6064 | 0.285 | 0.02* | |
C10 | 0.1859 (2) | 0.55592 (13) | 0.24388 (4) | 0.0171 (3) | |
C11 | 0.0954 (2) | 0.65227 (13) | 0.30325 (4) | 0.0215 (3) | |
H11A | 0.1115 | 0.7267 | 0.2925 | 0.026* | |
H11B | −0.0428 | 0.6288 | 0.2996 | 0.026* | |
C12 | 0.1347 (2) | 0.66015 (13) | 0.34210 (4) | 0.0212 (3) | |
H12 | 0.0685 | 0.717 | 0.3548 | 0.025* | |
C13 | 0.2550 (2) | 0.59397 (13) | 0.36035 (4) | 0.0188 (3) | |
C14 | 0.3695 (2) | 0.50043 (13) | 0.34219 (4) | 0.0185 (3) | |
C15 | 0.3964 (3) | 0.39984 (14) | 0.36740 (4) | 0.0258 (3) | |
H15A | 0.273 | 0.356 | 0.3676 | 0.031* | |
H15B | 0.502 | 0.3516 | 0.3579 | 0.031* | |
C16 | 0.4483 (3) | 0.43141 (14) | 0.40553 (4) | 0.0268 (3) | |
H16A | 0.5804 | 0.4662 | 0.4059 | 0.032* | |
H16B | 0.4544 | 0.3631 | 0.4201 | 0.032* | |
C17 | 0.2984 (3) | 0.51200 (15) | 0.42198 (4) | 0.0256 (3) | |
C18 | 0.2908 (2) | 0.61864 (14) | 0.39938 (4) | 0.0219 (3) | |
H18 | 0.1751 | 0.6626 | 0.4079 | 0.026* | |
C19 | 0.4737 (3) | 0.69286 (15) | 0.40412 (4) | 0.0256 (3) | |
H19A | 0.5889 | 0.654 | 0.3939 | 0.031* | |
H19B | 0.4538 | 0.7621 | 0.3905 | 0.031* | |
C20 | 0.5215 (3) | 0.72395 (16) | 0.44263 (4) | 0.0290 (4) | |
C21 | 0.5376 (3) | 0.61569 (17) | 0.46385 (4) | 0.0327 (4) | |
H21A | 0.6552 | 0.5742 | 0.4558 | 0.039* | |
H21B | 0.5569 | 0.6341 | 0.4891 | 0.039* | |
C22 | 0.3576 (3) | 0.54134 (17) | 0.46027 (4) | 0.0322 (4) | |
H22A | 0.2446 | 0.5786 | 0.4718 | 0.039* | |
H22B | 0.3829 | 0.4714 | 0.4733 | 0.039* | |
C23 | 0.5541 (2) | 0.39306 (14) | 0.18158 (4) | 0.0252 (3) | |
H23A | 0.5268 | 0.3149 | 0.1869 | 0.038* | |
H23B | 0.6625 | 0.4193 | 0.1965 | 0.038* | |
H23C | 0.5909 | 0.4005 | 0.1566 | 0.038* | |
C24 | 0.1971 (3) | 0.41062 (15) | 0.16858 (4) | 0.0261 (3) | |
H24A | 0.1638 | 0.3387 | 0.1792 | 0.039* | |
H24B | 0.2353 | 0.3998 | 0.1438 | 0.039* | |
H24C | 0.0823 | 0.4599 | 0.1697 | 0.039* | |
C25 | −0.0304 (2) | 0.52403 (15) | 0.23597 (4) | 0.0235 (3) | |
H25A | −0.0474 | 0.4438 | 0.2391 | 0.035* | |
H25B | −0.0628 | 0.5444 | 0.2116 | 0.035* | |
H25C | −0.1179 | 0.5637 | 0.2522 | 0.035* | |
C26 | 0.0536 (2) | 0.41393 (14) | 0.31691 (4) | 0.0237 (3) | |
H26A | −0.0134 | 0.4629 | 0.3338 | 0.036* | |
H26B | 0.0716 | 0.3404 | 0.3276 | 0.036* | |
H26C | −0.0263 | 0.407 | 0.2954 | 0.036* | |
C27 | 0.5789 (2) | 0.54578 (15) | 0.33350 (4) | 0.0243 (3) | |
H27A | 0.5692 | 0.6238 | 0.3263 | 0.036* | |
H27B | 0.6365 | 0.5021 | 0.3142 | 0.036* | |
H27C | 0.6626 | 0.54 | 0.3545 | 0.036* | |
C28 | 0.0943 (3) | 0.45846 (19) | 0.42306 (5) | 0.0358 (4) | |
H28A | 0.0015 | 0.509 | 0.4347 | 0.054* | |
H28B | 0.101 | 0.3886 | 0.4363 | 0.054* | |
H28C | 0.0495 | 0.4435 | 0.3989 | 0.054* | |
C29 | 0.7185 (3) | 0.7853 (2) | 0.44317 (5) | 0.0414 (5) | |
H29A | 0.7493 | 0.8078 | 0.4674 | 0.062* | |
H29B | 0.7102 | 0.8513 | 0.4281 | 0.062* | |
H29C | 0.8224 | 0.736 | 0.4343 | 0.062* | |
C30 | 0.3647 (4) | 0.80080 (18) | 0.45799 (5) | 0.0383 (5) | |
H30A | 0.2391 | 0.761 | 0.4595 | 0.057* | |
H30B | 0.3493 | 0.8658 | 0.4427 | 0.057* | |
H30C | 0.4049 | 0.825 | 0.4817 | 0.057* | |
C31 | 0.6289 (2) | 0.60710 (14) | 0.12809 (4) | 0.0239 (3) | |
C32 | 0.6434 (3) | 0.61319 (15) | 0.08868 (4) | 0.0276 (4) | |
C33 | 0.4794 (3) | 0.61160 (18) | 0.06693 (5) | 0.0372 (4) | |
H33 | 0.3514 | 0.6053 | 0.0769 | 0.045* | |
C34 | 0.5026 (4) | 0.6193 (2) | 0.03050 (5) | 0.0512 (6) | |
H34 | 0.3903 | 0.6181 | 0.0155 | 0.061* | |
C35 | 0.6872 (4) | 0.6287 (2) | 0.01612 (5) | 0.0568 (7) | |
H35 | 0.7023 | 0.633 | −0.0088 | 0.068* | |
C36 | 0.8492 (4) | 0.6317 (3) | 0.03738 (6) | 0.0606 (7) | |
H36 | 0.9764 | 0.639 | 0.0272 | 0.073* | |
C37 | 0.8293 (3) | 0.6243 (2) | 0.07390 (5) | 0.0453 (5) | |
H37 | 0.9425 | 0.6268 | 0.0887 | 0.054* | |
O1 | 0.44441 (16) | 0.58696 (10) | 0.13894 (3) | 0.0235 (2) | |
O2 | 0.76870 (18) | 0.61892 (13) | 0.14734 (3) | 0.0347 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0240 (7) | 0.0177 (7) | 0.0191 (6) | 0.0020 (6) | −0.0008 (5) | 0.0007 (5) |
C2 | 0.0248 (7) | 0.0197 (7) | 0.0191 (6) | 0.0006 (6) | 0.0001 (6) | 0.0023 (5) |
C3 | 0.0221 (7) | 0.0217 (8) | 0.0153 (6) | −0.0020 (6) | −0.0002 (5) | −0.0010 (5) |
C4 | 0.0212 (7) | 0.0191 (7) | 0.0180 (6) | −0.0021 (6) | −0.0002 (5) | −0.0031 (5) |
C5 | 0.0187 (6) | 0.0157 (7) | 0.0179 (6) | −0.0004 (6) | −0.0027 (5) | −0.0020 (5) |
C6 | 0.0291 (8) | 0.0159 (7) | 0.0209 (6) | 0.0006 (6) | −0.0025 (6) | −0.0018 (6) |
C7 | 0.0298 (7) | 0.0145 (7) | 0.0192 (6) | 0.0052 (6) | −0.0012 (6) | −0.0002 (5) |
C8 | 0.0189 (6) | 0.0163 (7) | 0.0181 (6) | 0.0011 (6) | −0.0006 (5) | −0.0001 (5) |
C9 | 0.0180 (6) | 0.0148 (7) | 0.0181 (6) | 0.0018 (5) | −0.0013 (5) | −0.0001 (5) |
C10 | 0.0167 (6) | 0.0169 (7) | 0.0178 (6) | 0.0005 (5) | −0.0019 (5) | 0.0001 (5) |
C11 | 0.0233 (7) | 0.0209 (8) | 0.0203 (6) | 0.0072 (6) | −0.0021 (5) | −0.0016 (6) |
C12 | 0.0237 (7) | 0.0193 (7) | 0.0204 (6) | 0.0051 (6) | 0.0014 (6) | −0.0016 (6) |
C13 | 0.0202 (7) | 0.0182 (7) | 0.0179 (6) | 0.0009 (6) | 0.0008 (5) | −0.0010 (5) |
C14 | 0.0202 (6) | 0.0179 (7) | 0.0174 (6) | 0.0030 (6) | −0.0011 (5) | −0.0002 (5) |
C15 | 0.0365 (9) | 0.0190 (8) | 0.0218 (7) | 0.0067 (7) | −0.0029 (6) | 0.0009 (6) |
C16 | 0.0376 (9) | 0.0226 (8) | 0.0202 (6) | 0.0075 (7) | −0.0029 (6) | 0.0030 (6) |
C17 | 0.0316 (8) | 0.0271 (9) | 0.0181 (6) | 0.0015 (7) | 0.0011 (6) | 0.0025 (6) |
C18 | 0.0262 (7) | 0.0222 (8) | 0.0174 (6) | 0.0038 (6) | 0.0014 (5) | −0.0015 (6) |
C19 | 0.0337 (8) | 0.0251 (8) | 0.0181 (6) | −0.0015 (7) | −0.0007 (6) | −0.0001 (6) |
C20 | 0.0357 (9) | 0.0308 (9) | 0.0205 (7) | −0.0011 (8) | −0.0021 (6) | −0.0037 (7) |
C21 | 0.0419 (10) | 0.0373 (10) | 0.0190 (7) | 0.0035 (9) | −0.0047 (7) | −0.0015 (7) |
C22 | 0.0456 (10) | 0.0335 (10) | 0.0174 (7) | 0.0026 (9) | 0.0008 (7) | 0.0033 (7) |
C23 | 0.0276 (8) | 0.0232 (8) | 0.0250 (7) | 0.0022 (7) | 0.0020 (6) | −0.0063 (6) |
C24 | 0.0296 (8) | 0.0275 (9) | 0.0212 (7) | −0.0087 (7) | −0.0030 (6) | −0.0037 (6) |
C25 | 0.0192 (7) | 0.0293 (9) | 0.0221 (6) | −0.0012 (7) | −0.0033 (5) | 0.0003 (6) |
C26 | 0.0230 (7) | 0.0232 (8) | 0.0250 (7) | −0.0048 (6) | −0.0007 (6) | 0.0016 (6) |
C27 | 0.0184 (7) | 0.0313 (9) | 0.0231 (7) | 0.0006 (6) | −0.0013 (5) | −0.0034 (6) |
C28 | 0.0382 (10) | 0.0400 (11) | 0.0292 (8) | −0.0059 (9) | 0.0060 (7) | 0.0043 (8) |
C29 | 0.0477 (11) | 0.0464 (12) | 0.0300 (8) | −0.0126 (10) | −0.0058 (8) | −0.0055 (8) |
C30 | 0.0543 (12) | 0.0344 (11) | 0.0262 (8) | 0.0039 (9) | 0.0033 (8) | −0.0074 (7) |
C31 | 0.0271 (7) | 0.0209 (8) | 0.0237 (7) | −0.0007 (6) | 0.0026 (6) | −0.0002 (6) |
C32 | 0.0348 (9) | 0.0249 (9) | 0.0231 (7) | −0.0010 (7) | 0.0058 (6) | −0.0015 (6) |
C33 | 0.0438 (10) | 0.0420 (11) | 0.0259 (8) | −0.0023 (9) | 0.0004 (8) | 0.0004 (8) |
C34 | 0.0677 (15) | 0.0616 (15) | 0.0241 (9) | −0.0036 (13) | −0.0045 (9) | 0.0006 (9) |
C35 | 0.0844 (18) | 0.0630 (16) | 0.0230 (8) | −0.0084 (15) | 0.0123 (10) | −0.0023 (9) |
C36 | 0.0609 (15) | 0.084 (2) | 0.0368 (11) | −0.0104 (15) | 0.0248 (11) | −0.0063 (12) |
C37 | 0.0403 (11) | 0.0625 (15) | 0.0330 (9) | −0.0056 (11) | 0.0109 (8) | −0.0052 (10) |
O1 | 0.0251 (5) | 0.0282 (6) | 0.0173 (5) | −0.0031 (5) | 0.0005 (4) | −0.0006 (4) |
O2 | 0.0251 (6) | 0.0501 (8) | 0.0287 (6) | −0.0051 (6) | 0.0000 (5) | 0.0000 (6) |
C1—C2 | 1.5335 (19) | C19—C20 | 1.538 (2) |
C1—C10 | 1.546 (2) | C19—H19A | 0.99 |
C1—H1A | 0.99 | C19—H19B | 0.99 |
C1—H1B | 0.99 | C20—C30 | 1.526 (3) |
C2—C3 | 1.508 (2) | C20—C29 | 1.528 (3) |
C2—H2A | 0.99 | C20—C21 | 1.534 (3) |
C2—H2B | 0.99 | C21—C22 | 1.521 (3) |
C3—O1 | 1.4652 (16) | C21—H21A | 0.99 |
C3—C4 | 1.536 (2) | C21—H21B | 0.99 |
C3—H3 | 1 | C22—H22A | 0.99 |
C4—C24 | 1.533 (2) | C22—H22B | 0.99 |
C4—C23 | 1.539 (2) | C23—H23A | 0.98 |
C4—C5 | 1.5626 (18) | C23—H23B | 0.98 |
C5—C6 | 1.531 (2) | C23—H23C | 0.98 |
C5—C10 | 1.554 (2) | C24—H24A | 0.98 |
C5—H5 | 1 | C24—H24B | 0.98 |
C6—C7 | 1.5318 (19) | C24—H24C | 0.98 |
C6—H6A | 0.99 | C25—H25A | 0.98 |
C6—H6B | 0.99 | C25—H25B | 0.98 |
C7—C8 | 1.547 (2) | C25—H25C | 0.98 |
C7—H7A | 0.99 | C26—H26A | 0.98 |
C7—H7B | 0.99 | C26—H26B | 0.98 |
C8—C26 | 1.541 (2) | C26—H26C | 0.98 |
C8—C9 | 1.562 (2) | C27—H27A | 0.98 |
C8—C14 | 1.5877 (19) | C27—H27B | 0.98 |
C9—C11 | 1.535 (2) | C27—H27C | 0.98 |
C9—C10 | 1.5719 (18) | C28—H28A | 0.98 |
C9—H9 | 1 | C28—H28B | 0.98 |
C10—C25 | 1.547 (2) | C28—H28C | 0.98 |
C11—C12 | 1.4967 (19) | C29—H29A | 0.98 |
C11—H11A | 0.99 | C29—H29B | 0.98 |
C11—H11B | 0.99 | C29—H29C | 0.98 |
C12—C13 | 1.333 (2) | C30—H30A | 0.98 |
C12—H12 | 0.95 | C30—H30B | 0.98 |
C13—C18 | 1.5256 (19) | C30—H30C | 0.98 |
C13—C14 | 1.531 (2) | C31—O2 | 1.204 (2) |
C14—C15 | 1.552 (2) | C31—O1 | 1.341 (2) |
C14—C27 | 1.558 (2) | C31—C32 | 1.496 (2) |
C15—C16 | 1.532 (2) | C32—C33 | 1.385 (3) |
C15—H15A | 0.99 | C32—C37 | 1.387 (3) |
C15—H15B | 0.99 | C33—C34 | 1.390 (2) |
C16—C17 | 1.538 (2) | C33—H33 | 0.95 |
C16—H16A | 0.99 | C34—C35 | 1.371 (4) |
C16—H16B | 0.99 | C34—H34 | 0.95 |
C17—C28 | 1.529 (3) | C35—C36 | 1.363 (4) |
C17—C18 | 1.543 (2) | C35—H35 | 0.95 |
C17—C22 | 1.544 (2) | C36—C37 | 1.391 (3) |
C18—C19 | 1.540 (2) | C36—H36 | 0.95 |
C18—H18 | 1 | C37—H37 | 0.95 |
C2—C1—C10 | 113.70 (12) | C19—C18—C17 | 113.01 (13) |
C2—C1—H1A | 108.8 | C13—C18—H18 | 106.8 |
C10—C1—H1A | 108.8 | C19—C18—H18 | 106.8 |
C2—C1—H1B | 108.8 | C17—C18—H18 | 106.8 |
C10—C1—H1B | 108.8 | C20—C19—C18 | 114.93 (13) |
H1A—C1—H1B | 107.7 | C20—C19—H19A | 108.5 |
C3—C2—C1 | 108.94 (12) | C18—C19—H19A | 108.5 |
C3—C2—H2A | 109.9 | C20—C19—H19B | 108.5 |
C1—C2—H2A | 109.9 | C18—C19—H19B | 108.5 |
C3—C2—H2B | 109.9 | H19A—C19—H19B | 107.5 |
C1—C2—H2B | 109.9 | C30—C20—C29 | 108.24 (16) |
H2A—C2—H2B | 108.3 | C30—C20—C21 | 111.43 (15) |
O1—C3—C2 | 107.92 (12) | C29—C20—C21 | 109.93 (16) |
O1—C3—C4 | 110.32 (12) | C30—C20—C19 | 111.15 (15) |
C2—C3—C4 | 113.58 (12) | C29—C20—C19 | 108.37 (14) |
O1—C3—H3 | 108.3 | C21—C20—C19 | 107.69 (14) |
C2—C3—H3 | 108.3 | C22—C21—C20 | 113.31 (15) |
C4—C3—H3 | 108.3 | C22—C21—H21A | 108.9 |
C24—C4—C3 | 112.42 (13) | C20—C21—H21A | 108.9 |
C24—C4—C23 | 107.79 (12) | C22—C21—H21B | 108.9 |
C3—C4—C23 | 108.01 (12) | C20—C21—H21B | 108.9 |
C24—C4—C5 | 115.15 (12) | H21A—C21—H21B | 107.7 |
C3—C4—C5 | 104.71 (11) | C21—C22—C17 | 115.29 (14) |
C23—C4—C5 | 108.51 (12) | C21—C22—H22A | 108.5 |
C6—C5—C10 | 109.68 (12) | C17—C22—H22A | 108.5 |
C6—C5—C4 | 115.05 (12) | C21—C22—H22B | 108.5 |
C10—C5—C4 | 117.63 (12) | C17—C22—H22B | 108.5 |
C6—C5—H5 | 104.3 | H22A—C22—H22B | 107.5 |
C10—C5—H5 | 104.3 | C4—C23—H23A | 109.5 |
C4—C5—H5 | 104.3 | C4—C23—H23B | 109.5 |
C5—C6—C7 | 109.14 (12) | H23A—C23—H23B | 109.5 |
C5—C6—H6A | 109.9 | C4—C23—H23C | 109.5 |
C7—C6—H6A | 109.9 | H23A—C23—H23C | 109.5 |
C5—C6—H6B | 109.9 | H23B—C23—H23C | 109.5 |
C7—C6—H6B | 109.9 | C4—C24—H24A | 109.5 |
H6A—C6—H6B | 108.3 | C4—C24—H24B | 109.5 |
C6—C7—C8 | 113.66 (12) | H24A—C24—H24B | 109.5 |
C6—C7—H7A | 108.8 | C4—C24—H24C | 109.5 |
C8—C7—H7A | 108.8 | H24A—C24—H24C | 109.5 |
C6—C7—H7B | 108.8 | H24B—C24—H24C | 109.5 |
C8—C7—H7B | 108.8 | C10—C25—H25A | 109.5 |
H7A—C7—H7B | 107.7 | C10—C25—H25B | 109.5 |
C26—C8—C7 | 106.90 (12) | H25A—C25—H25B | 109.5 |
C26—C8—C9 | 110.91 (12) | C10—C25—H25C | 109.5 |
C7—C8—C9 | 111.46 (11) | H25A—C25—H25C | 109.5 |
C26—C8—C14 | 110.37 (11) | H25B—C25—H25C | 109.5 |
C7—C8—C14 | 110.87 (11) | C8—C26—H26A | 109.5 |
C9—C8—C14 | 106.38 (11) | C8—C26—H26B | 109.5 |
C11—C9—C8 | 109.33 (11) | H26A—C26—H26B | 109.5 |
C11—C9—C10 | 113.69 (11) | C8—C26—H26C | 109.5 |
C8—C9—C10 | 118.36 (12) | H26A—C26—H26C | 109.5 |
C11—C9—H9 | 104.7 | H26B—C26—H26C | 109.5 |
C8—C9—H9 | 104.7 | C14—C27—H27A | 109.5 |
C10—C9—H9 | 104.7 | C14—C27—H27B | 109.5 |
C1—C10—C25 | 107.07 (13) | H27A—C27—H27B | 109.5 |
C1—C10—C5 | 108.87 (12) | C14—C27—H27C | 109.5 |
C25—C10—C5 | 114.00 (12) | H27A—C27—H27C | 109.5 |
C1—C10—C9 | 107.02 (12) | H27B—C27—H27C | 109.5 |
C25—C10—C9 | 114.00 (11) | C17—C28—H28A | 109.5 |
C5—C10—C9 | 105.61 (11) | C17—C28—H28B | 109.5 |
C12—C11—C9 | 112.99 (12) | H28A—C28—H28B | 109.5 |
C12—C11—H11A | 109 | C17—C28—H28C | 109.5 |
C9—C11—H11A | 109 | H28A—C28—H28C | 109.5 |
C12—C11—H11B | 109 | H28B—C28—H28C | 109.5 |
C9—C11—H11B | 109 | C20—C29—H29A | 109.5 |
H11A—C11—H11B | 107.8 | C20—C29—H29B | 109.5 |
C13—C12—C11 | 125.41 (14) | H29A—C29—H29B | 109.5 |
C13—C12—H12 | 117.3 | C20—C29—H29C | 109.5 |
C11—C12—H12 | 117.3 | H29A—C29—H29C | 109.5 |
C12—C13—C18 | 118.82 (14) | H29B—C29—H29C | 109.5 |
C12—C13—C14 | 121.21 (13) | C20—C30—H30A | 109.5 |
C18—C13—C14 | 119.78 (13) | C20—C30—H30B | 109.5 |
C13—C14—C15 | 110.97 (12) | H30A—C30—H30B | 109.5 |
C13—C14—C27 | 107.47 (13) | C20—C30—H30C | 109.5 |
C15—C14—C27 | 107.19 (12) | H30A—C30—H30C | 109.5 |
C13—C14—C8 | 109.38 (12) | H30B—C30—H30C | 109.5 |
C15—C14—C8 | 110.32 (12) | O2—C31—O1 | 124.94 (14) |
C27—C14—C8 | 111.47 (11) | O2—C31—C32 | 123.02 (15) |
C16—C15—C14 | 114.33 (13) | O1—C31—C32 | 112.04 (14) |
C16—C15—H15A | 108.7 | C33—C32—C37 | 119.60 (16) |
C14—C15—H15A | 108.7 | C33—C32—C31 | 122.59 (16) |
C16—C15—H15B | 108.7 | C37—C32—C31 | 117.77 (16) |
C14—C15—H15B | 108.7 | C32—C33—C34 | 119.8 (2) |
H15A—C15—H15B | 107.6 | C32—C33—H33 | 120.1 |
C15—C16—C17 | 112.65 (13) | C34—C33—H33 | 120.1 |
C15—C16—H16A | 109.1 | C35—C34—C33 | 120.2 (2) |
C17—C16—H16A | 109.1 | C35—C34—H34 | 119.9 |
C15—C16—H16B | 109.1 | C33—C34—H34 | 119.9 |
C17—C16—H16B | 109.1 | C36—C35—C34 | 120.37 (18) |
H16A—C16—H16B | 107.8 | C36—C35—H35 | 119.8 |
C28—C17—C16 | 110.18 (15) | C34—C35—H35 | 119.8 |
C28—C17—C18 | 109.57 (14) | C35—C36—C37 | 120.4 (2) |
C16—C17—C18 | 108.84 (12) | C35—C36—H36 | 119.8 |
C28—C17—C22 | 107.88 (14) | C37—C36—H36 | 119.8 |
C16—C17—C22 | 110.60 (14) | C32—C37—C36 | 119.6 (2) |
C18—C17—C22 | 109.76 (14) | C32—C37—H37 | 120.2 |
C13—C18—C19 | 110.72 (12) | C36—C37—H37 | 120.2 |
C13—C18—C17 | 112.31 (13) | C31—O1—C3 | 117.01 (12) |
C10—C1—C2—C3 | −56.44 (17) | C7—C8—C14—C13 | 177.83 (12) |
C1—C2—C3—O1 | −173.90 (12) | C9—C8—C14—C13 | 56.48 (14) |
C1—C2—C3—C4 | 63.46 (16) | C26—C8—C14—C15 | 58.41 (16) |
O1—C3—C4—C24 | −55.10 (16) | C7—C8—C14—C15 | −59.85 (16) |
C2—C3—C4—C24 | 66.20 (16) | C9—C8—C14—C15 | 178.81 (12) |
O1—C3—C4—C23 | 63.70 (15) | C26—C8—C14—C27 | 177.38 (13) |
C2—C3—C4—C23 | −175.00 (12) | C7—C8—C14—C27 | 59.12 (16) |
O1—C3—C4—C5 | 179.20 (11) | C9—C8—C14—C27 | −62.22 (15) |
C2—C3—C4—C5 | −59.50 (15) | C13—C14—C15—C16 | −41.70 (19) |
C24—C4—C5—C6 | 60.88 (18) | C27—C14—C15—C16 | 75.37 (17) |
C3—C4—C5—C6 | −175.15 (12) | C8—C14—C15—C16 | −163.09 (14) |
C23—C4—C5—C6 | −60.00 (16) | C14—C15—C16—C17 | 55.2 (2) |
C24—C4—C5—C10 | −70.76 (17) | C15—C16—C17—C28 | 60.95 (18) |
C3—C4—C5—C10 | 53.22 (16) | C15—C16—C17—C18 | −59.21 (19) |
C23—C4—C5—C10 | 168.37 (13) | C15—C16—C17—C22 | −179.86 (14) |
C10—C5—C6—C7 | −68.60 (15) | C12—C13—C18—C19 | −92.59 (17) |
C4—C5—C6—C7 | 156.08 (12) | C14—C13—C18—C19 | 82.48 (17) |
C5—C6—C7—C8 | 57.32 (17) | C12—C13—C18—C17 | 140.04 (15) |
C6—C7—C8—C26 | 78.92 (15) | C14—C13—C18—C17 | −44.89 (19) |
C6—C7—C8—C9 | −42.43 (17) | C28—C17—C18—C13 | −67.93 (17) |
C6—C7—C8—C14 | −160.73 (13) | C16—C17—C18—C13 | 52.61 (17) |
C26—C8—C9—C11 | 53.90 (15) | C22—C17—C18—C13 | 173.78 (14) |
C7—C8—C9—C11 | 172.89 (12) | C28—C17—C18—C19 | 165.93 (14) |
C14—C8—C9—C11 | −66.14 (14) | C16—C17—C18—C19 | −73.53 (16) |
C26—C8—C9—C10 | −78.43 (15) | C22—C17—C18—C19 | 47.64 (18) |
C7—C8—C9—C10 | 40.56 (17) | C13—C18—C19—C20 | 179.30 (14) |
C14—C8—C9—C10 | 161.53 (12) | C17—C18—C19—C20 | −53.72 (19) |
C2—C1—C10—C25 | −75.01 (15) | C18—C19—C20—C30 | −67.9 (2) |
C2—C1—C10—C5 | 48.67 (16) | C18—C19—C20—C29 | 173.33 (16) |
C2—C1—C10—C9 | 162.37 (12) | C18—C19—C20—C21 | 54.5 (2) |
C6—C5—C10—C1 | 176.78 (11) | C30—C20—C21—C22 | 68.38 (19) |
C4—C5—C10—C1 | −49.20 (16) | C29—C20—C21—C22 | −171.62 (15) |
C6—C5—C10—C25 | −63.77 (15) | C19—C20—C21—C22 | −53.75 (19) |
C4—C5—C10—C25 | 70.26 (17) | C20—C21—C22—C17 | 54.3 (2) |
C6—C5—C10—C9 | 62.16 (14) | C28—C17—C22—C21 | −168.41 (16) |
C4—C5—C10—C9 | −163.82 (12) | C16—C17—C22—C21 | 71.0 (2) |
C11—C9—C10—C1 | 63.99 (15) | C18—C17—C22—C21 | −49.1 (2) |
C8—C9—C10—C1 | −165.63 (12) | O2—C31—C32—C33 | −172.78 (19) |
C11—C9—C10—C25 | −54.20 (18) | O1—C31—C32—C33 | 7.4 (3) |
C8—C9—C10—C25 | 76.17 (17) | O2—C31—C32—C37 | 5.2 (3) |
C11—C9—C10—C5 | 179.88 (12) | O1—C31—C32—C37 | −174.68 (19) |
C8—C9—C10—C5 | −49.74 (16) | C37—C32—C33—C34 | 1.0 (3) |
C8—C9—C11—C12 | 42.11 (17) | C31—C32—C33—C34 | 179.0 (2) |
C10—C9—C11—C12 | 176.84 (13) | C32—C33—C34—C35 | −0.1 (4) |
C9—C11—C12—C13 | −8.9 (2) | C33—C34—C35—C36 | −0.7 (4) |
C11—C12—C13—C18 | 175.42 (15) | C34—C35—C36—C37 | 0.6 (4) |
C11—C12—C13—C14 | 0.4 (2) | C33—C32—C37—C36 | −1.1 (4) |
C12—C13—C14—C15 | −147.13 (15) | C31—C32—C37—C36 | −179.2 (2) |
C18—C13—C14—C15 | 37.92 (19) | C35—C36—C37—C32 | 0.3 (4) |
C12—C13—C14—C27 | 95.96 (17) | O2—C31—O1—C3 | 2.1 (3) |
C18—C13—C14—C27 | −78.98 (16) | C32—C31—O1—C3 | −178.04 (13) |
C12—C13—C14—C8 | −25.20 (19) | C2—C3—O1—C31 | 126.23 (15) |
C18—C13—C14—C8 | 159.86 (13) | C4—C3—O1—C31 | −109.16 (15) |
C26—C8—C14—C13 | −63.91 (15) |
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···O2 | 1.00 | 2.26 | 2.7148 (19) | 106 |
C23—H23C···O1 | 0.98 | 2.54 | 2.933 (2) | 104 |
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