Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100003279/qb0192sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100003279/qb0192Isup2.hkl |
CCDC reference: 144715
Transparent plate shaped crystals were obtained by means of slow evaporation from a solution of the compound in methanol at 25°.
The independent reflections included 181 Friedel-related data. The H atoms were allowed to ride on their parent atom with Uiso = xUeq (parent), where x = 1.5 for methyl and x = 1.2 for all others.
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXS93 (Sheldrick, 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ZORTEP (Zsolnai & Huttner, 1994); software used to prepare material for publication: SHELXL97.
C79H110O7 | Dx = 1.129 Mg m−3 |
Mr = 1171.67 | Melting point: 105° K |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 33.654 (9) Å | Cell parameters from 4620 reflections |
b = 30.229 (8) Å | θ = 1.2–26.4° |
c = 6.798 (2) Å | µ = 0.07 mm−1 |
β = 94.74 (1)° | T = 123 K |
V = 6892.3 (3) Å3 | Plate, colourless |
Z = 4 | 0.4 × 0.10 × 0.02 mm |
F(000) = 2560 |
Bruker 1K CCD area-detector diffractometer | 6169 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.179 |
Graphite monochromator | θmax = 29.1°, θmin = 1.2° |
ϕ and ω scans | h = −45→45 |
79109 measured reflections | k = −40→40 |
17107 independent reflections | l = −9→9 |
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)] = 0.071 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.130 | H-atom parameters constrained |
S = 1.02 | Calculated w = 1/[σ2(Fo2) + (0.0576P)2 + 3.1481P] where P = (Fo2 + 2Fc2)/3 |
14105 reflections | (Δ/σ)max = −0.085 |
775 parameters | Δρmax = 0.29 e Å−3 |
48 restraints | Δρmin = −0.28 e Å−3 |
C79H110O7 | V = 6892.3 (3) Å3 |
Mr = 1171.67 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 33.654 (9) Å | µ = 0.07 mm−1 |
b = 30.229 (8) Å | T = 123 K |
c = 6.798 (2) Å | 0.4 × 0.10 × 0.02 mm |
β = 94.74 (1)° |
Bruker 1K CCD area-detector diffractometer | 6169 reflections with I > 2σ(I) |
79109 measured reflections | Rint = 0.179 |
17107 independent reflections |
R[F2 > 2σ(F2)] = 0.071 | 48 restraints |
wR(F2) = 0.130 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.29 e Å−3 |
14105 reflections | Δρmin = −0.28 e Å−3 |
775 parameters |
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 on F2 for ALL reflections except for 3002 with very negative F2 or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F2, conventional R- factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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 | ||
O1 | 0.34159 (4) | 0.69363 (5) | 0.8342 (2) | 0.0271 (4) | |
O2 | 0.74191 (4) | 0.68854 (5) | 1.6701 (2) | 0.0287 (4) | |
O3 | 0.37072 (4) | 0.41731 (5) | 1.2353 (2) | 0.0241 (4) | |
O4 | 0.77545 (4) | 0.43772 (5) | 1.9784 (2) | 0.0282 (4) | |
O5 | 0.56110 (4) | 0.57962 (4) | 1.1894 (2) | 0.0198 (4) | |
O6 | 0.61162 (4) | 0.53044 (4) | 1.1870 (2) | 0.0223 (4) | |
O7 | 0.54632 (4) | 0.51066 (4) | 1.1633 (2) | 0.0200 (4) | |
C1 | 0.33308 (7) | 0.67900 (7) | 0.6349 (3) | 0.0274 (6) | |
H1A | 0.33969 | 0.64722 | 0.6243 | 0.033* | |
H1B | 0.34947 | 0.69580 | 0.5462 | 0.033* | |
C2 | 0.28949 (7) | 0.68619 (8) | 0.5747 (4) | 0.0320 (7) | |
H2A | 0.28131 | 0.71548 | 0.6224 | 0.038* | |
H2B | 0.27362 | 0.66334 | 0.6372 | 0.038* | |
C3 | 0.28086 (7) | 0.68396 (8) | 0.3522 (3) | 0.0311 (7) | |
H3A | 0.29354 | 0.70966 | 0.2923 | 0.037* | |
H3B | 0.29323 | 0.65684 | 0.3031 | 0.037* | |
C4 | 0.23683 (7) | 0.68375 (8) | 0.2843 (4) | 0.0350 (7) | |
H4A | 0.22392 | 0.70923 | 0.3447 | 0.042* | |
H4B | 0.22469 | 0.65643 | 0.3328 | 0.042* | |
C5 | 0.22826 (7) | 0.68616 (8) | 0.0621 (4) | 0.0377 (8) | |
H5A | 0.24224 | 0.66144 | 0.0017 | 0.045* | |
H5B | 0.23947 | 0.71410 | 0.0147 | 0.045* | |
C6 | 0.18425 (7) | 0.68403 (8) | −0.0093 (4) | 0.0398 (8) | |
H6A | 0.16990 | 0.70789 | 0.0552 | 0.048* | |
H6B | 0.17322 | 0.65541 | 0.0314 | 0.048* | |
C7 | 0.17679 (7) | 0.68879 (8) | −0.2322 (4) | 0.0408 (8) | |
H7A | 0.18843 | 0.71715 | −0.2721 | 0.049* | |
H7B | 0.19101 | 0.66468 | −0.2956 | 0.049* | |
C8 | 0.13313 (8) | 0.68757 (9) | −0.3101 (4) | 0.0491 (9) | |
H8A | 0.11885 | 0.71214 | −0.2503 | 0.059* | |
H8B | 0.12117 | 0.65946 | −0.2691 | 0.059* | |
C9 | 0.12738 (8) | 0.69146 (9) | −0.5338 (4) | 0.0545 (9) | |
H9A | 0.14028 | 0.71902 | −0.5747 | 0.065* | |
H9B | 0.14095 | 0.66630 | −0.5932 | 0.065* | |
C10 | 0.08389 (9) | 0.69190 (11) | −0.6139 (5) | 0.0763 (12) | |
H10A | 0.08221 | 0.69445 | −0.7581 | 0.114* | |
H10B | 0.07036 | 0.71715 | −0.5585 | 0.114* | |
H10C | 0.07103 | 0.66438 | −0.5769 | 0.114* | |
C11 | 0.74911 (7) | 0.69651 (8) | 1.8775 (3) | 0.0283 (7) | |
H11A | 0.73147 | 0.67761 | 1.9514 | 0.034* | |
H11B | 0.74349 | 0.72784 | 1.9073 | 0.034* | |
C12 | 0.79222 (7) | 0.68592 (8) | 1.9378 (3) | 0.0289 (7) | |
H12A | 0.80966 | 0.70591 | 1.8681 | 0.035* | |
H12B | 0.79804 | 0.65512 | 1.8998 | 0.035* | |
C13 | 0.80093 (7) | 0.69145 (8) | 2.1614 (3) | 0.0309 (7) | |
H13A | 0.79311 | 0.72167 | 2.1989 | 0.037* | |
H13B | 0.78427 | 0.67027 | 2.2293 | 0.037* | |
C14 | 0.84445 (7) | 0.68404 (8) | 2.2332 (3) | 0.0301 (7) | |
H14A | 0.85236 | 0.65385 | 2.1956 | 0.036* | |
H14B | 0.86116 | 0.70531 | 2.1661 | 0.036* | |
C15 | 0.85257 (7) | 0.68943 (8) | 2.4545 (4) | 0.0370 (7) | |
H15A | 0.84414 | 0.71946 | 2.4915 | 0.044* | |
H15B | 0.83595 | 0.66792 | 2.5208 | 0.044* | |
C16 | 0.89572 (7) | 0.68288 (9) | 2.5311 (4) | 0.0417 (8) | |
H16A | 0.91238 | 0.70456 | 2.4661 | 0.050* | |
H16B | 0.90428 | 0.65291 | 2.4937 | 0.050* | |
C17 | 0.90317 (8) | 0.68806 (9) | 2.7533 (4) | 0.0455 (8) | |
H17A | 0.89315 | 0.71740 | 2.7909 | 0.055* | |
H17B | 0.88747 | 0.66535 | 2.8176 | 0.055* | |
C18 | 0.94614 (9) | 0.68402 (10) | 2.8324 (4) | 0.0626 (10) | |
H18A | 0.96197 | 0.70729 | 2.7726 | 0.075* | |
H18B | 0.95659 | 0.65494 | 2.7939 | 0.075* | |
C19 | 0.95124 (9) | 0.68850 (11) | 3.0592 (5) | 0.0715 (11) | |
H19A | 0.93883 | 0.71655 | 3.0977 | 0.086* | |
H19B | 0.93693 | 0.66391 | 3.1187 | 0.086* | |
C20 | 0.99371 (10) | 0.68794 (14) | 3.1403 (6) | 0.105 (2) | |
H20A | 0.99509 | 0.69088 | 3.2843 | 0.158* | |
H20B | 1.00796 | 0.71262 | 3.0845 | 0.158* | |
H20C | 1.00605 | 0.65995 | 3.1055 | 0.158* | |
C21 | 0.34653 (6) | 0.45616 (7) | 1.2493 (4) | 0.0279 (6) | |
H21A | 0.35638 | 0.48018 | 1.1670 | 0.033* | |
H21B | 0.34768 | 0.46653 | 1.3878 | 0.033* | |
C22 | 0.30429 (6) | 0.44422 (8) | 1.1778 (3) | 0.0274 (7) | |
H22A | 0.28604 | 0.46699 | 1.2238 | 0.033* | |
H22B | 0.29737 | 0.41563 | 1.2372 | 0.033* | |
C23 | 0.29776 (6) | 0.44052 (8) | 0.9529 (3) | 0.0278 (7) | |
H23A | 0.30918 | 0.46694 | 0.8925 | 0.033* | |
H23B | 0.31216 | 0.41422 | 0.9089 | 0.033* | |
C24 | 0.25368 (7) | 0.43665 (8) | 0.8800 (3) | 0.0264 (6) | |
H24A | 0.24308 | 0.40851 | 0.9287 | 0.032* | |
H24B | 0.23882 | 0.46115 | 0.9370 | 0.032* | |
C25 | 0.24625 (7) | 0.43803 (7) | 0.6558 (3) | 0.0286 (7) | |
H25A | 0.25805 | 0.46549 | 0.6067 | 0.034* | |
H25B | 0.26007 | 0.41269 | 0.5993 | 0.034* | |
C26 | 0.20223 (7) | 0.43640 (8) | 0.5823 (3) | 0.0284 (7) | |
H26A | 0.19062 | 0.40848 | 0.6277 | 0.034* | |
H26B | 0.18824 | 0.46120 | 0.6420 | 0.034* | |
C27 | 0.19493 (7) | 0.43923 (8) | 0.3591 (3) | 0.0277 (7) | |
H27A | 0.20905 | 0.41444 | 0.3000 | 0.033* | |
H27B | 0.20673 | 0.46711 | 0.3143 | 0.033* | |
C28 | 0.15129 (7) | 0.43774 (8) | 0.2813 (3) | 0.0315 (7) | |
H28A | 0.13692 | 0.46216 | 0.3416 | 0.038* | |
H28B | 0.13953 | 0.40953 | 0.3223 | 0.038* | |
C29 | 0.14514 (7) | 0.44169 (8) | 0.0577 (4) | 0.0336 (7) | |
H29A | 0.15729 | 0.46977 | 0.0176 | 0.040* | |
H29B | 0.15961 | 0.41720 | −0.0016 | 0.040* | |
C30 | 0.10209 (8) | 0.44065 (9) | −0.0268 (4) | 0.0495 (9) | |
H30A | 0.10099 | 0.44337 | −0.1708 | 0.074* | |
H30B | 0.08754 | 0.46529 | 0.0275 | 0.074* | |
H30C | 0.08987 | 0.41261 | 0.0082 | 0.074* | |
C31 | 0.78218 (6) | 0.43497 (8) | 2.1890 (3) | 0.0257 (6) | |
H31A | 0.77199 | 0.40644 | 2.2356 | 0.031* | |
H31B | 0.76784 | 0.45919 | 2.2510 | 0.031* | |
C32 | 0.82638 (7) | 0.43861 (8) | 2.2464 (3) | 0.0277 (7) | |
H32A | 0.83640 | 0.46703 | 2.1976 | 0.033* | |
H32B | 0.84050 | 0.41435 | 2.1835 | 0.033* | |
C33 | 0.83528 (6) | 0.43613 (8) | 2.4705 (3) | 0.0263 (6) | |
H33A | 0.82160 | 0.46095 | 2.5318 | 0.032* | |
H33B | 0.82406 | 0.40824 | 2.5186 | 0.032* | |
C34 | 0.87967 (6) | 0.43800 (8) | 2.5383 (3) | 0.0284 (7) | |
H34A | 0.89368 | 0.41420 | 2.4717 | 0.034* | |
H34B | 0.89063 | 0.46666 | 2.4976 | 0.034* | |
C35 | 0.88788 (7) | 0.43285 (8) | 2.7607 (3) | 0.0323 (7) | |
H35A | 0.87791 | 0.40358 | 2.7997 | 0.039* | |
H35B | 0.87261 | 0.45570 | 2.8266 | 0.039* | |
C36 | 0.93188 (7) | 0.43675 (9) | 2.8357 (3) | 0.0334 (7) | |
H36A | 0.94746 | 0.41474 | 2.7664 | 0.040* | |
H36B | 0.94165 | 0.46653 | 2.8030 | 0.040* | |
C37 | 0.93908 (7) | 0.42945 (9) | 3.0569 (4) | 0.0398 (8) | |
H37A | 0.93202 | 0.39853 | 3.0870 | 0.048* | |
H37B | 0.92105 | 0.44908 | 3.1248 | 0.048* | |
C38 | 0.98193 (7) | 0.43812 (9) | 3.1402 (4) | 0.0406 (8) | |
H38A | 1.00020 | 0.41991 | 3.0669 | 0.049* | |
H38B | 0.98846 | 0.46958 | 3.1186 | 0.049* | |
C39 | 0.98896 (8) | 0.42784 (10) | 3.3572 (4) | 0.0517 (9) | |
H39A | 0.98386 | 0.39596 | 3.3768 | 0.062* | |
H39B | 0.96936 | 0.44458 | 3.4287 | 0.062* | |
C40 | 1.03084 (8) | 0.43871 (11) | 3.4492 (4) | 0.0623 (10) | |
H40A | 1.03279 | 0.43103 | 3.5898 | 0.093* | |
H40B | 1.03601 | 0.47039 | 3.4344 | 0.093* | |
H40C | 1.05054 | 0.42167 | 3.3825 | 0.093* | |
C41 | 0.38082 (6) | 0.69201 (6) | 0.9073 (3) | 0.0210 (6) | |
C42 | 0.39019 (6) | 0.71267 (7) | 1.0882 (3) | 0.0212 (6) | |
H42A | 0.36962 | 0.72602 | 1.1553 | 0.025* | |
C43 | 0.42903 (6) | 0.71400 (7) | 1.1713 (3) | 0.0202 (6) | |
H43A | 0.43485 | 0.72877 | 1.2936 | 0.024* | |
C44 | 0.46014 (6) | 0.69385 (6) | 1.0778 (3) | 0.0194 (6) | |
C45 | 0.44967 (6) | 0.67219 (7) | 0.8987 (3) | 0.0196 (6) | |
H45A | 0.46992 | 0.65775 | 0.8333 | 0.024* | |
C46 | 0.41098 (6) | 0.67110 (7) | 0.8139 (3) | 0.0221 (6) | |
H46A | 0.40495 | 0.65614 | 0.6922 | 0.027* | |
C47 | 0.50213 (6) | 0.69464 (6) | 1.1623 (3) | 0.0163 (6) | |
C48 | 0.51773 (6) | 0.73017 (7) | 1.2761 (3) | 0.0193 (6) | |
H48A | 0.50114 | 0.75458 | 1.3016 | 0.023* | |
C49 | 0.55730 (6) | 0.72990 (6) | 1.3516 (3) | 0.0198 (6) | |
H49A | 0.56739 | 0.75465 | 1.4260 | 0.024* | |
C50 | 0.58287 (6) | 0.69446 (6) | 1.3221 (3) | 0.0193 (6) | |
C51 | 0.56667 (6) | 0.65764 (6) | 1.2159 (3) | 0.0163 (5) | |
C52 | 0.52743 (6) | 0.65909 (6) | 1.1341 (3) | 0.0176 (6) | |
H52A | 0.51745 | 0.63487 | 1.0558 | 0.021* | |
C53 | 0.62472 (6) | 0.69486 (6) | 1.4100 (3) | 0.0189 (6) | |
C54 | 0.63390 (6) | 0.71046 (7) | 1.6001 (3) | 0.0216 (6) | |
H54A | 0.61306 | 0.72241 | 1.6699 | 0.026* | |
C55 | 0.67221 (6) | 0.70939 (7) | 1.6929 (3) | 0.0234 (6) | |
H55A | 0.67731 | 0.72010 | 1.8239 | 0.028* | |
C56 | 0.70304 (6) | 0.69241 (7) | 1.5912 (3) | 0.0227 (6) | |
C57 | 0.69499 (6) | 0.67823 (7) | 1.3985 (3) | 0.0229 (6) | |
H57A | 0.71606 | 0.66748 | 1.3269 | 0.028* | |
C58 | 0.65654 (6) | 0.67955 (7) | 1.3092 (3) | 0.0213 (6) | |
H58A | 0.65168 | 0.66984 | 1.1765 | 0.026* | |
C59 | 0.41126 (6) | 0.42174 (6) | 1.2818 (3) | 0.0186 (6) | |
C60 | 0.43178 (6) | 0.38227 (7) | 1.3179 (3) | 0.0206 (6) | |
H60A | 0.41792 | 0.35489 | 1.3067 | 0.025* | |
C61 | 0.47235 (6) | 0.38287 (7) | 1.3702 (3) | 0.0198 (6) | |
H61A | 0.48586 | 0.35588 | 1.4018 | 0.024* | |
C62 | 0.49387 (6) | 0.42249 (6) | 1.3775 (3) | 0.0181 (6) | |
C63 | 0.47294 (6) | 0.46151 (7) | 1.3356 (3) | 0.0197 (6) | |
H63A | 0.48705 | 0.48874 | 1.3369 | 0.024* | |
C64 | 0.43183 (6) | 0.46158 (7) | 1.2920 (3) | 0.0213 (6) | |
H64A | 0.41793 | 0.48870 | 1.2694 | 0.026* | |
C65 | 0.53716 (6) | 0.42239 (6) | 1.4467 (3) | 0.0195 (6) | |
C66 | 0.54877 (6) | 0.40077 (7) | 1.6237 (3) | 0.0242 (6) | |
H66A | 0.52920 | 0.38564 | 1.6910 | 0.029* | |
C67 | 0.58791 (6) | 0.40070 (7) | 1.7041 (3) | 0.0217 (6) | |
H67A | 0.59470 | 0.38498 | 1.8231 | 0.026* | |
C68 | 0.61760 (6) | 0.42332 (6) | 1.6133 (3) | 0.0176 (6) | |
C69 | 0.60633 (6) | 0.44343 (6) | 1.4322 (3) | 0.0190 (6) | |
H69A | 0.62615 | 0.45787 | 1.3639 | 0.023* | |
C70 | 0.56705 (6) | 0.44313 (6) | 1.3479 (3) | 0.0180 (6) | |
C71 | 0.65906 (6) | 0.42628 (7) | 1.7091 (3) | 0.0209 (6) | |
C72 | 0.66633 (6) | 0.42003 (7) | 1.9123 (3) | 0.0271 (6) | |
H72A | 0.64470 | 0.41330 | 1.9886 | 0.032* | |
C73 | 0.70480 (6) | 0.42348 (7) | 2.0058 (3) | 0.0265 (6) | |
H73A | 0.70901 | 0.41882 | 2.1442 | 0.032* | |
C74 | 0.73650 (6) | 0.43355 (7) | 1.8994 (3) | 0.0230 (6) | |
C75 | 0.72999 (6) | 0.43971 (7) | 1.6976 (3) | 0.0257 (6) | |
H75A | 0.75180 | 0.44621 | 1.6222 | 0.031* | |
C76 | 0.69183 (6) | 0.43644 (7) | 1.6048 (3) | 0.0223 (6) | |
H76A | 0.68792 | 0.44126 | 1.4665 | 0.027* | |
C77 | 0.58995 (6) | 0.61501 (6) | 1.2012 (3) | 0.0175 (6) | |
H77A | 0.60501 | 0.61529 | 1.0822 | 0.021* | |
H77B | 0.60904 | 0.61125 | 1.3188 | 0.021* | |
C78 | 0.57688 (6) | 0.53924 (7) | 1.1812 (3) | 0.0182 (6) | |
C79 | 0.55773 (6) | 0.46419 (6) | 1.1482 (3) | 0.0186 (6) | |
H79A | 0.58144 | 0.46203 | 1.0717 | 0.022* | |
H79B | 0.53572 | 0.44772 | 1.0756 | 0.022* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.0205 (8) | 0.0309 (9) | 0.0288 (9) | 0.0012 (7) | −0.0052 (7) | −0.0057 (7) |
O2 | 0.0227 (8) | 0.0386 (9) | 0.0242 (9) | 0.0026 (7) | −0.0031 (7) | −0.0025 (8) |
O3 | 0.0185 (8) | 0.0237 (8) | 0.0294 (9) | 0.0006 (7) | −0.0015 (7) | −0.0016 (7) |
O4 | 0.0202 (8) | 0.0406 (9) | 0.0230 (9) | 0.0006 (7) | −0.0041 (7) | 0.0021 (8) |
O5 | 0.0203 (8) | 0.0124 (7) | 0.0264 (9) | 0.0008 (6) | 0.0003 (7) | 0.0013 (6) |
O6 | 0.0180 (8) | 0.0190 (8) | 0.0299 (9) | 0.0026 (6) | 0.0025 (7) | 0.0012 (7) |
O7 | 0.0212 (8) | 0.0142 (7) | 0.0244 (9) | −0.0005 (6) | 0.0007 (7) | 0.0025 (7) |
C1 | 0.0276 (13) | 0.0277 (13) | 0.0259 (14) | 0.0014 (11) | −0.0046 (11) | −0.0067 (11) |
C2 | 0.0258 (13) | 0.0279 (13) | 0.041 (2) | 0.0026 (11) | −0.0071 (12) | −0.0071 (12) |
C3 | 0.0322 (14) | 0.0249 (13) | 0.034 (2) | 0.0005 (11) | −0.0089 (12) | 0.0010 (11) |
C4 | 0.0293 (14) | 0.0313 (14) | 0.042 (2) | 0.0067 (11) | −0.0108 (13) | −0.0081 (12) |
C5 | 0.041 (2) | 0.0312 (14) | 0.039 (2) | 0.0044 (12) | −0.0129 (13) | −0.0011 (12) |
C6 | 0.041 (2) | 0.0347 (14) | 0.041 (2) | 0.0089 (12) | −0.0162 (13) | −0.0091 (13) |
C7 | 0.044 (2) | 0.0327 (14) | 0.042 (2) | 0.0038 (13) | −0.0179 (14) | −0.0053 (13) |
C8 | 0.052 (2) | 0.0363 (15) | 0.054 (2) | 0.0110 (14) | −0.024 (2) | −0.0143 (14) |
C9 | 0.068 (2) | 0.040 (2) | 0.050 (2) | 0.0027 (15) | −0.028 (2) | −0.0009 (14) |
C10 | 0.070 (2) | 0.072 (2) | 0.078 (2) | 0.006 (2) | −0.046 (2) | −0.004 (2) |
C11 | 0.0236 (13) | 0.0342 (13) | 0.0262 (14) | 0.0018 (11) | −0.0036 (11) | −0.0038 (11) |
C12 | 0.0266 (13) | 0.0271 (13) | 0.0324 (15) | 0.0005 (11) | −0.0024 (12) | 0.0002 (11) |
C13 | 0.0297 (14) | 0.0340 (13) | 0.0279 (15) | 0.0045 (11) | −0.0045 (12) | −0.0028 (11) |
C14 | 0.0295 (13) | 0.0287 (13) | 0.0307 (15) | −0.0005 (11) | −0.0057 (12) | 0.0014 (11) |
C15 | 0.041 (2) | 0.0348 (14) | 0.034 (2) | 0.0037 (12) | −0.0084 (13) | −0.0048 (12) |
C16 | 0.040 (2) | 0.044 (2) | 0.039 (2) | −0.0044 (13) | −0.0108 (14) | 0.0038 (13) |
C17 | 0.049 (2) | 0.047 (2) | 0.037 (2) | 0.0011 (14) | −0.0165 (14) | −0.0035 (14) |
C18 | 0.059 (2) | 0.071 (2) | 0.052 (2) | −0.004 (2) | −0.029 (2) | 0.003 (2) |
C19 | 0.062 (2) | 0.092 (2) | 0.056 (2) | 0.000 (2) | −0.023 (2) | −0.004 (2) |
C20 | 0.063 (2) | 0.152 (4) | 0.096 (3) | 0.011 (3) | −0.022 (2) | −0.023 (3) |
C21 | 0.0268 (13) | 0.0289 (13) | 0.0276 (14) | 0.0072 (11) | −0.0001 (11) | −0.0048 (11) |
C22 | 0.0186 (12) | 0.0341 (14) | 0.0299 (14) | 0.0021 (10) | 0.0034 (11) | −0.0051 (11) |
C23 | 0.0216 (13) | 0.0346 (13) | 0.0271 (14) | −0.0002 (11) | 0.0019 (11) | −0.0045 (11) |
C24 | 0.0278 (13) | 0.0304 (13) | 0.0210 (13) | −0.0012 (11) | 0.0012 (11) | −0.0010 (11) |
C25 | 0.0264 (13) | 0.0249 (12) | 0.0342 (15) | −0.0004 (11) | 0.0015 (12) | 0.0007 (11) |
C26 | 0.0293 (14) | 0.0300 (13) | 0.0256 (14) | −0.0010 (11) | 0.0011 (12) | −0.0030 (11) |
C27 | 0.0255 (13) | 0.0304 (13) | 0.0270 (14) | 0.0016 (11) | 0.0017 (11) | −0.0046 (11) |
C28 | 0.0326 (14) | 0.0321 (13) | 0.0289 (15) | 0.0004 (11) | −0.0025 (12) | 0.0047 (11) |
C29 | 0.0335 (14) | 0.0373 (14) | 0.0287 (15) | 0.0035 (12) | −0.0046 (12) | 0.0021 (12) |
C30 | 0.041 (2) | 0.059 (2) | 0.045 (2) | 0.0047 (14) | −0.0157 (15) | −0.0049 (15) |
C31 | 0.0256 (13) | 0.0310 (13) | 0.0195 (13) | 0.0006 (10) | −0.0051 (11) | 0.0001 (10) |
C32 | 0.0268 (13) | 0.0267 (12) | 0.0286 (14) | 0.0007 (11) | −0.0032 (12) | −0.0014 (11) |
C33 | 0.0214 (12) | 0.0321 (13) | 0.0250 (14) | −0.0021 (11) | −0.0001 (11) | 0.0007 (11) |
C34 | 0.0252 (13) | 0.0321 (13) | 0.0272 (14) | −0.0013 (11) | −0.0019 (12) | −0.0031 (11) |
C35 | 0.0302 (14) | 0.0396 (14) | 0.0268 (14) | −0.0003 (12) | −0.0001 (12) | −0.0018 (12) |
C36 | 0.0238 (13) | 0.050 (2) | 0.0253 (15) | 0.0012 (12) | −0.0036 (12) | −0.0008 (12) |
C37 | 0.0318 (15) | 0.061 (2) | 0.0259 (15) | −0.0010 (13) | −0.0035 (13) | 0.0026 (13) |
C38 | 0.0303 (15) | 0.066 (2) | 0.0251 (15) | −0.0026 (13) | −0.0017 (13) | 0.0005 (14) |
C39 | 0.033 (2) | 0.087 (2) | 0.034 (2) | 0.000 (2) | −0.0083 (14) | 0.001 (2) |
C40 | 0.044 (2) | 0.103 (3) | 0.037 (2) | −0.005 (2) | −0.013 (2) | −0.001 (2) |
C41 | 0.0192 (12) | 0.0193 (11) | 0.0244 (13) | −0.0029 (10) | 0.0009 (11) | 0.0024 (10) |
C42 | 0.0213 (12) | 0.0186 (11) | 0.0243 (13) | 0.0035 (10) | 0.0055 (11) | −0.0002 (10) |
C43 | 0.0211 (12) | 0.0171 (11) | 0.0224 (13) | 0.0000 (10) | 0.0014 (10) | −0.0007 (10) |
C44 | 0.0222 (12) | 0.0129 (10) | 0.0230 (13) | −0.0019 (9) | 0.0013 (10) | 0.0013 (10) |
C45 | 0.0202 (12) | 0.0183 (11) | 0.0209 (13) | 0.0002 (9) | 0.0054 (10) | 0.0015 (10) |
C46 | 0.0233 (12) | 0.0215 (12) | 0.0214 (13) | −0.0004 (10) | 0.0006 (11) | −0.0007 (10) |
C47 | 0.0188 (11) | 0.0149 (11) | 0.0154 (12) | −0.0019 (9) | 0.0034 (10) | 0.0038 (9) |
C48 | 0.0214 (12) | 0.0196 (11) | 0.0170 (12) | 0.0026 (10) | 0.0029 (10) | −0.0011 (10) |
C49 | 0.0263 (12) | 0.0169 (11) | 0.0165 (12) | −0.0032 (10) | 0.0040 (10) | −0.0011 (10) |
C50 | 0.0209 (12) | 0.0190 (11) | 0.0184 (13) | −0.0009 (10) | 0.0035 (10) | 0.0032 (9) |
C51 | 0.0180 (11) | 0.0177 (11) | 0.0135 (12) | 0.0004 (9) | 0.0035 (10) | 0.0017 (9) |
C52 | 0.0221 (12) | 0.0162 (11) | 0.0143 (12) | −0.0043 (9) | −0.0001 (10) | −0.0007 (9) |
C53 | 0.0226 (12) | 0.0141 (11) | 0.0197 (13) | −0.0024 (9) | −0.0008 (10) | −0.0019 (9) |
C54 | 0.0193 (12) | 0.0167 (11) | 0.0285 (14) | −0.0010 (10) | 0.0004 (11) | −0.0020 (10) |
C55 | 0.0331 (13) | 0.0178 (11) | 0.0189 (13) | −0.0049 (10) | 0.0002 (11) | −0.0025 (10) |
C56 | 0.0176 (12) | 0.0205 (11) | 0.0295 (14) | −0.0022 (10) | −0.0020 (11) | 0.0018 (10) |
C57 | 0.0215 (12) | 0.0194 (12) | 0.0283 (14) | 0.0007 (10) | 0.0047 (11) | −0.0029 (10) |
C58 | 0.0250 (12) | 0.0207 (12) | 0.0186 (13) | −0.0018 (10) | 0.0037 (11) | −0.0002 (10) |
C59 | 0.0170 (11) | 0.0254 (12) | 0.0132 (12) | −0.0007 (10) | 0.0006 (10) | −0.0012 (10) |
C60 | 0.0251 (12) | 0.0196 (11) | 0.0179 (13) | −0.0058 (10) | 0.0050 (10) | −0.0014 (10) |
C61 | 0.0225 (12) | 0.0188 (11) | 0.0181 (13) | −0.0005 (10) | 0.0013 (10) | 0.0026 (10) |
C62 | 0.0225 (12) | 0.0216 (11) | 0.0107 (12) | 0.0014 (10) | 0.0043 (10) | −0.0001 (9) |
C63 | 0.0238 (12) | 0.0195 (11) | 0.0156 (12) | −0.0049 (10) | 0.0013 (10) | 0.0000 (10) |
C64 | 0.0225 (12) | 0.0226 (12) | 0.0190 (13) | 0.0041 (10) | 0.0025 (10) | 0.0010 (10) |
C65 | 0.0219 (12) | 0.0157 (11) | 0.0206 (13) | 0.0012 (10) | 0.0013 (10) | −0.0010 (10) |
C66 | 0.0258 (13) | 0.0225 (12) | 0.0250 (14) | −0.0026 (10) | 0.0059 (11) | 0.0044 (10) |
C67 | 0.0239 (13) | 0.0204 (12) | 0.0200 (13) | 0.0004 (10) | −0.0036 (11) | 0.0041 (10) |
C68 | 0.0164 (11) | 0.0150 (11) | 0.0209 (13) | 0.0008 (9) | −0.0008 (10) | −0.0012 (10) |
C69 | 0.0233 (12) | 0.0127 (11) | 0.0215 (13) | −0.0007 (9) | 0.0060 (11) | −0.0045 (9) |
C70 | 0.0231 (12) | 0.0137 (11) | 0.0171 (12) | 0.0020 (9) | 0.0006 (10) | −0.0012 (9) |
C71 | 0.0227 (12) | 0.0152 (11) | 0.0244 (13) | 0.0020 (10) | −0.0010 (11) | −0.0024 (10) |
C72 | 0.0238 (12) | 0.0312 (13) | 0.0264 (14) | 0.0010 (11) | 0.0034 (11) | 0.0005 (11) |
C73 | 0.0258 (13) | 0.0338 (13) | 0.0190 (13) | 0.0030 (11) | −0.0031 (11) | 0.0009 (11) |
C74 | 0.0161 (12) | 0.0226 (12) | 0.0299 (14) | −0.0007 (10) | −0.0010 (11) | −0.0012 (11) |
C75 | 0.0205 (12) | 0.0330 (13) | 0.0234 (14) | 0.0002 (10) | 0.0009 (11) | 0.0021 (11) |
C76 | 0.0276 (13) | 0.0218 (12) | 0.0174 (13) | 0.0006 (10) | 0.0014 (11) | 0.0003 (10) |
C77 | 0.0199 (11) | 0.0136 (10) | 0.0190 (12) | −0.0029 (9) | 0.0011 (10) | 0.0019 (9) |
C78 | 0.0221 (12) | 0.0216 (12) | 0.0111 (12) | 0.0018 (10) | 0.0024 (10) | −0.0001 (9) |
C79 | 0.0225 (12) | 0.0102 (10) | 0.0230 (13) | 0.0014 (9) | 0.0002 (10) | −0.0014 (9) |
O1—C41 | 1.373 (2) | C30—H30B | 0.98 |
O1—C1 | 1.432 (3) | C30—H30C | 0.98 |
O2—C56 | 1.377 (2) | C31—C32 | 1.511 (3) |
O2—C11 | 1.431 (3) | C31—H31A | 0.99 |
O3—C59 | 1.381 (2) | C31—H31B | 0.99 |
O3—C21 | 1.437 (2) | C32—C33 | 1.530 (3) |
O4—C74 | 1.381 (2) | C32—H32A | 0.99 |
O4—C31 | 1.433 (3) | C32—H32B | 0.99 |
O5—C78 | 1.334 (2) | C33—C34 | 1.528 (3) |
O5—C77 | 1.442 (2) | C33—H33A | 0.99 |
O6—C78 | 1.196 (2) | C33—H33B | 0.99 |
O7—C78 | 1.341 (2) | C34—C35 | 1.523 (3) |
O7—C79 | 1.462 (2) | C34—H34A | 0.99 |
C1—C2 | 1.506 (3) | C34—H34B | 0.99 |
C1—H1A | 0.99 | C35—C36 | 1.530 (3) |
C1—H1B | 0.99 | C35—H35A | 0.99 |
C2—C3 | 1.518 (3) | C35—H35B | 0.99 |
C2—H2A | 0.99 | C36—C37 | 1.519 (3) |
C2—H2B | 0.99 | C36—H36A | 0.99 |
C3—C4 | 1.515 (3) | C36—H36B | 0.99 |
C3—H3A | 0.99 | C37—C38 | 1.528 (3) |
C3—H3B | 0.99 | C37—H37A | 0.99 |
C4—C5 | 1.515 (3) | C37—H37B | 0.99 |
C4—H4A | 0.99 | C38—C39 | 1.507 (3) |
C4—H4B | 0.99 | C38—H38A | 0.99 |
C5—C6 | 1.521 (3) | C38—H38B | 0.99 |
C5—H5A | 0.99 | C39—C40 | 1.530 (4) |
C5—H5B | 0.99 | C39—H39A | 0.99 |
C6—C7 | 1.522 (3) | C39—H39B | 0.99 |
C6—H6A | 0.99 | C40—H40A | 0.98 |
C6—H6B | 0.99 | C40—H40B | 0.98 |
C7—C8 | 1.521 (3) | C40—H40C | 0.98 |
C7—H7A | 0.99 | C41—C42 | 1.392 (3) |
C7—H7B | 0.99 | C41—C46 | 1.393 (3) |
C8—C9 | 1.522 (4) | C42—C43 | 1.381 (3) |
C8—H8A | 0.99 | C42—H42A | 0.95 |
C8—H8B | 0.99 | C43—C44 | 1.407 (3) |
C9—C10 | 1.519 (4) | C43—H43A | 0.95 |
C9—H9A | 0.99 | C44—C45 | 1.402 (3) |
C9—H9B | 0.99 | C44—C47 | 1.481 (3) |
C10—H10A | 0.98 | C45—C46 | 1.380 (3) |
C10—H10B | 0.98 | C45—H45A | 0.95 |
C10—H10C | 0.98 | C46—H46A | 0.95 |
C11—C12 | 1.509 (3) | C47—C52 | 1.394 (3) |
C11—H11A | 0.99 | C47—C48 | 1.400 (3) |
C11—H11B | 0.99 | C48—C49 | 1.387 (3) |
C12—C13 | 1.533 (3) | C48—H48A | 0.95 |
C12—H12A | 0.99 | C49—C50 | 1.399 (3) |
C12—H12B | 0.99 | C49—H49A | 0.95 |
C13—C14 | 1.522 (3) | C50—C51 | 1.411 (3) |
C13—H13A | 0.99 | C50—C53 | 1.484 (3) |
C13—H13B | 0.99 | C51—C52 | 1.391 (3) |
C14—C15 | 1.515 (3) | C51—C77 | 1.516 (3) |
C14—H14A | 0.99 | C52—H52A | 0.95 |
C14—H14B | 0.99 | C53—C54 | 1.387 (3) |
C15—C16 | 1.515 (3) | C53—C58 | 1.397 (3) |
C15—H15A | 0.99 | C54—C55 | 1.388 (3) |
C15—H15B | 0.99 | C54—H54A | 0.95 |
C16—C17 | 1.519 (3) | C55—C56 | 1.391 (3) |
C16—H16A | 0.99 | C55—H55A | 0.95 |
C16—H16B | 0.99 | C56—C57 | 1.384 (3) |
C17—C18 | 1.506 (4) | C57—C58 | 1.384 (3) |
C17—H17A | 0.99 | C57—H57A | 0.95 |
C17—H17B | 0.99 | C58—H58A | 0.95 |
C18—C19 | 1.543 (4) | C59—C64 | 1.388 (3) |
C18—H18A | 0.99 | C59—C60 | 1.390 (3) |
C18—H18B | 0.99 | C60—C61 | 1.382 (3) |
C19—C20 | 1.489 (4) | C60—H60A | 0.95 |
C19—H19A | 0.99 | C61—C62 | 1.398 (3) |
C19—H19B | 0.99 | C61—H61A | 0.95 |
C20—H20A | 0.98 | C62—C63 | 1.391 (3) |
C20—H20B | 0.98 | C62—C65 | 1.494 (3) |
C20—H20C | 0.98 | C63—C64 | 1.391 (3) |
C21—C22 | 1.508 (3) | C63—H63A | 0.95 |
C21—H21A | 0.99 | C64—H64A | 0.95 |
C21—H21B | 0.99 | C65—C66 | 1.396 (3) |
C22—C23 | 1.531 (3) | C65—C70 | 1.403 (3) |
C22—H22A | 0.99 | C66—C67 | 1.384 (3) |
C22—H22B | 0.99 | C66—H66A | 0.95 |
C23—C24 | 1.529 (3) | C67—C68 | 1.396 (3) |
C23—H23A | 0.99 | C67—H67A | 0.95 |
C23—H23B | 0.99 | C68—C69 | 1.397 (3) |
C24—C25 | 1.525 (3) | C68—C71 | 1.493 (3) |
C24—H24A | 0.99 | C69—C70 | 1.397 (3) |
C24—H24B | 0.99 | C69—H69A | 0.95 |
C25—C26 | 1.525 (3) | C70—C79 | 1.508 (3) |
C25—H25A | 0.99 | C71—C76 | 1.393 (3) |
C25—H25B | 0.99 | C71—C72 | 1.396 (3) |
C26—C27 | 1.520 (3) | C72—C73 | 1.398 (3) |
C26—H26A | 0.99 | C72—H72A | 0.95 |
C26—H26B | 0.99 | C73—C74 | 1.372 (3) |
C27—C28 | 1.520 (3) | C73—H73A | 0.95 |
C27—H27A | 0.99 | C74—C75 | 1.384 (3) |
C27—H27B | 0.99 | C75—C76 | 1.387 (3) |
C28—C29 | 1.521 (3) | C75—H75A | 0.95 |
C28—H28A | 0.99 | C76—H76A | 0.95 |
C28—H28B | 0.99 | C77—H77A | 0.99 |
C29—C30 | 1.514 (3) | C77—H77B | 0.99 |
C29—H29A | 0.99 | C79—H79A | 0.99 |
C29—H29B | 0.99 | C79—H79B | 0.99 |
C30—H30A | 0.98 | ||
C41—O1—C1 | 116.3 (2) | H30B—C30—H30C | 109.5 |
C56—O2—C11 | 116.6 (2) | O4—C31—C32 | 109.0 (2) |
C59—O3—C21 | 117.4 (2) | O4—C31—H31A | 109.89 (11) |
C74—O4—C31 | 116.7 (2) | C32—C31—H31A | 109.89 (12) |
C78—O5—C77 | 114.4 (2) | O4—C31—H31B | 109.90 (11) |
C78—O7—C79 | 114.9 (2) | C32—C31—H31B | 109.89 (12) |
O1—C1—C2 | 109.1 (2) | H31A—C31—H31B | 108.3 |
O1—C1—H1A | 109.86 (11) | C31—C32—C33 | 111.2 (2) |
C2—C1—H1A | 109.86 (12) | C31—C32—H32A | 109.40 (12) |
O1—C1—H1B | 109.87 (11) | C33—C32—H32A | 109.40 (12) |
C2—C1—H1B | 109.87 (13) | C31—C32—H32B | 109.40 (12) |
H1A—C1—H1B | 108.3 | C33—C32—H32B | 109.39 (12) |
C1—C2—C3 | 111.5 (2) | H32A—C32—H32B | 108.0 |
C1—C2—H2A | 109.32 (12) | C34—C33—C32 | 113.9 (2) |
C3—C2—H2A | 109.32 (12) | C34—C33—H33A | 108.78 (12) |
C1—C2—H2B | 109.33 (13) | C32—C33—H33A | 108.78 (12) |
C3—C2—H2B | 109.33 (12) | C34—C33—H33B | 108.79 (12) |
H2A—C2—H2B | 108.0 | C32—C33—H33B | 108.79 (12) |
C4—C3—C2 | 114.0 (2) | H33A—C33—H33B | 107.7 |
C4—C3—H3A | 108.76 (13) | C35—C34—C33 | 112.9 (2) |
C2—C3—H3A | 108.77 (12) | C35—C34—H34A | 109.01 (13) |
C4—C3—H3B | 108.77 (13) | C33—C34—H34A | 109.01 (12) |
C2—C3—H3B | 108.76 (12) | C35—C34—H34B | 109.02 (13) |
H3A—C3—H3B | 107.7 | C33—C34—H34B | 109.02 (12) |
C3—C4—C5 | 113.9 (2) | H34A—C34—H34B | 107.8 |
C3—C4—H4A | 108.79 (13) | C34—C35—C36 | 114.5 (2) |
C5—C4—H4A | 108.79 (13) | C34—C35—H35A | 108.65 (13) |
C3—C4—H4B | 108.78 (13) | C36—C35—H35A | 108.65 (13) |
C5—C4—H4B | 108.78 (13) | C34—C35—H35B | 108.64 (13) |
H4A—C4—H4B | 107.7 | C36—C35—H35B | 108.64 (13) |
C4—C5—C6 | 114.6 (2) | H35A—C35—H35B | 107.6 |
C4—C5—H5A | 108.62 (13) | C37—C36—C35 | 112.9 (2) |
C6—C5—H5A | 108.62 (13) | C37—C36—H36A | 109.00 (14) |
C4—C5—H5B | 108.61 (13) | C35—C36—H36A | 109.00 (13) |
C6—C5—H5B | 108.61 (14) | C37—C36—H36B | 109.00 (14) |
H5A—C5—H5B | 107.6 | C35—C36—H36B | 109.01 (13) |
C5—C6—C7 | 112.9 (2) | H36A—C36—H36B | 107.8 |
C5—C6—H6A | 109.00 (13) | C36—C37—C38 | 114.2 (2) |
C7—C6—H6A | 109.01 (13) | C36—C37—H37A | 108.70 (14) |
C5—C6—H6B | 108.99 (13) | C38—C37—H37A | 108.70 (15) |
C7—C6—H6B | 108.99 (13) | C36—C37—H37B | 108.69 (14) |
H6A—C6—H6B | 107.8 | C38—C37—H37B | 108.69 (14) |
C8—C7—C6 | 114.8 (2) | H37A—C37—H37B | 107.6 |
C8—C7—H7A | 108.57 (14) | C39—C38—C37 | 113.3 (2) |
C6—C7—H7A | 108.56 (13) | C39—C38—H38A | 108.93 (15) |
C8—C7—H7B | 108.57 (14) | C37—C38—H38A | 108.92 (14) |
C6—C7—H7B | 108.57 (13) | C39—C38—H38B | 108.9 (2) |
H7A—C7—H7B | 107.5 | C37—C38—H38B | 108.93 (15) |
C7—C8—C9 | 112.7 (2) | H38A—C38—H38B | 107.7 |
C7—C8—H8A | 109.06 (14) | C38—C39—C40 | 114.9 (2) |
C9—C8—H8A | 109.06 (15) | C38—C39—H39A | 108.5 (2) |
C7—C8—H8B | 109.06 (14) | C40—C39—H39A | 108.5 (2) |
C9—C8—H8B | 109.06 (15) | C38—C39—H39B | 108.54 (15) |
H8A—C8—H8B | 107.8 | C40—C39—H39B | 108.5 (2) |
C10—C9—C8 | 113.5 (3) | H39A—C39—H39B | 107.5 |
C10—C9—H9A | 108.9 (2) | C39—C40—H40A | 109.5 (2) |
C8—C9—H9A | 108.88 (15) | C39—C40—H40B | 109.5 (2) |
C10—C9—H9B | 108.9 (2) | H40A—C40—H40B | 109.5 |
C8—C9—H9B | 108.88 (14) | C39—C40—H40C | 109.5 (2) |
H9A—C9—H9B | 107.7 | H40A—C40—H40C | 109.5 |
C9—C10—H10A | 109.5 (2) | H40B—C40—H40C | 109.5 |
C9—C10—H10B | 109.5 (2) | O1—C41—C42 | 116.4 (2) |
H10A—C10—H10B | 109.5 | O1—C41—C46 | 124.5 (2) |
C9—C10—H10C | 109.5 (2) | C42—C41—C46 | 119.1 (2) |
H10A—C10—H10C | 109.5 | C43—C42—C41 | 120.8 (2) |
H10B—C10—H10C | 109.5 | C43—C42—H42A | 119.60 (13) |
O2—C11—C12 | 108.2 (2) | C41—C42—H42A | 119.61 (12) |
O2—C11—H11A | 110.06 (11) | C42—C43—C44 | 121.1 (2) |
C12—C11—H11A | 110.05 (13) | C42—C43—H43A | 119.43 (13) |
O2—C11—H11B | 110.05 (11) | C44—C43—H43A | 119.44 (11) |
C12—C11—H11B | 110.06 (12) | C45—C44—C43 | 116.8 (2) |
H11A—C11—H11B | 108.4 | C45—C44—C47 | 120.5 (2) |
C11—C12—C13 | 110.3 (2) | C43—C44—C47 | 122.7 (2) |
C11—C12—H12A | 109.59 (13) | C46—C45—C44 | 122.3 (2) |
C13—C12—H12A | 109.59 (12) | C46—C45—H45A | 118.84 (13) |
C11—C12—H12B | 109.60 (12) | C44—C45—H45A | 118.84 (12) |
C13—C12—H12B | 109.60 (12) | C45—C46—C41 | 119.8 (2) |
H12A—C12—H12B | 108.1 | C45—C46—H46A | 120.10 (13) |
C14—C13—C12 | 113.7 (2) | C41—C46—H46A | 120.11 (12) |
C14—C13—H13A | 108.82 (12) | C52—C47—C48 | 117.5 (2) |
C12—C13—H13A | 108.82 (12) | C52—C47—C44 | 120.5 (2) |
C14—C13—H13B | 108.82 (13) | C48—C47—C44 | 121.9 (2) |
C12—C13—H13B | 108.82 (12) | C49—C48—C47 | 120.3 (2) |
H13A—C13—H13B | 107.7 | C49—C48—H48A | 119.84 (12) |
C15—C14—C13 | 113.1 (2) | C47—C48—H48A | 119.84 (11) |
C15—C14—H14A | 108.96 (13) | C48—C49—C50 | 122.3 (2) |
C13—C14—H14A | 108.96 (12) | C48—C49—H49A | 118.85 (12) |
C15—C14—H14B | 108.97 (13) | C50—C49—H49A | 118.85 (11) |
C13—C14—H14B | 108.96 (13) | C49—C50—C51 | 117.5 (2) |
H14A—C14—H14B | 107.8 | C49—C50—C53 | 120.7 (2) |
C16—C15—C14 | 114.6 (2) | C51—C50—C53 | 121.7 (2) |
C16—C15—H15A | 108.61 (14) | C52—C51—C50 | 119.6 (2) |
C14—C15—H15A | 108.61 (13) | C52—C51—C77 | 118.6 (2) |
C16—C15—H15B | 108.61 (14) | C50—C51—C77 | 121.6 (2) |
C14—C15—H15B | 108.62 (13) | C51—C52—C47 | 122.7 (2) |
H15A—C15—H15B | 107.6 | C51—C52—H52A | 118.67 (12) |
C15—C16—C17 | 113.8 (2) | C47—C52—H52A | 118.67 (11) |
C15—C16—H16A | 108.80 (14) | C54—C53—C58 | 116.7 (2) |
C17—C16—H16A | 108.80 (14) | C54—C53—C50 | 120.6 (2) |
C15—C16—H16B | 108.80 (14) | C58—C53—C50 | 122.7 (2) |
C17—C16—H16B | 108.80 (14) | C53—C54—C55 | 122.9 (2) |
H16A—C16—H16B | 107.7 | C53—C54—H54A | 118.57 (12) |
C18—C17—C16 | 114.9 (2) | C55—C54—H54A | 118.57 (13) |
C18—C17—H17A | 108.5 (2) | C54—C55—C56 | 119.1 (2) |
C16—C17—H17A | 108.53 (14) | C54—C55—H55A | 120.46 (13) |
C18—C17—H17B | 108.5 (2) | C56—C55—H55A | 120.47 (12) |
C16—C17—H17B | 108.53 (14) | O2—C56—C57 | 116.6 (2) |
H17A—C17—H17B | 107.5 | O2—C56—C55 | 124.1 (2) |
C17—C18—C19 | 112.0 (3) | C57—C56—C55 | 119.3 (2) |
C17—C18—H18A | 109.2 (2) | C58—C57—C56 | 120.6 (2) |
C19—C18—H18A | 109.2 (2) | C58—C57—H57A | 119.70 (13) |
C17—C18—H18B | 109.2 (2) | C56—C57—H57A | 119.70 (12) |
C19—C18—H18B | 109.2 (2) | C57—C58—C53 | 121.4 (2) |
H18A—C18—H18B | 107.9 | C57—C58—H58A | 119.28 (13) |
C20—C19—C18 | 113.1 (3) | C53—C58—H58A | 119.28 (12) |
C20—C19—H19A | 109.0 (2) | O3—C59—C64 | 125.1 (2) |
C18—C19—H19A | 109.0 (2) | O3—C59—C60 | 115.1 (2) |
C20—C19—H19B | 109.0 (2) | C64—C59—C60 | 119.8 (2) |
C18—C19—H19B | 109.0 (2) | C61—C60—C59 | 120.0 (2) |
H19A—C19—H19B | 107.8 | C61—C60—H60A | 120.01 (12) |
C19—C20—H20A | 109.5 (2) | C59—C60—H60A | 120.01 (11) |
C19—C20—H20B | 109.5 (2) | C60—C61—C62 | 121.2 (2) |
H20A—C20—H20B | 109.5 | C60—C61—H61A | 119.39 (12) |
C19—C20—H20C | 109.5 (2) | C62—C61—H61A | 119.40 (11) |
H20A—C20—H20C | 109.5 | C63—C62—C61 | 117.8 (2) |
H20B—C20—H20C | 109.5 | C63—C62—C65 | 122.0 (2) |
O3—C21—C22 | 107.9 (2) | C61—C62—C65 | 119.9 (2) |
O3—C21—H21A | 110.13 (11) | C64—C63—C62 | 121.5 (2) |
C22—C21—H21A | 110.12 (13) | C64—C63—H63A | 119.24 (12) |
O3—C21—H21B | 110.13 (11) | C62—C63—H63A | 119.24 (12) |
C22—C21—H21B | 110.12 (13) | C59—C64—C63 | 119.5 (2) |
H21A—C21—H21B | 108.4 | C59—C64—H64A | 120.24 (12) |
C21—C22—C23 | 113.1 (2) | C63—C64—H64A | 120.24 (12) |
C21—C22—H22A | 108.95 (12) | C66—C65—C70 | 117.5 (2) |
C23—C22—H22A | 108.95 (12) | C66—C65—C62 | 118.0 (2) |
C21—C22—H22B | 108.95 (12) | C70—C65—C62 | 124.6 (2) |
C23—C22—H22B | 108.95 (12) | C67—C66—C65 | 122.0 (2) |
H22A—C22—H22B | 107.8 | C67—C66—H66A | 118.98 (13) |
C24—C23—C22 | 112.6 (2) | C65—C66—H66A | 118.98 (12) |
C24—C23—H23A | 109.07 (12) | C66—C67—C68 | 121.2 (2) |
C22—C23—H23A | 109.08 (12) | C66—C67—H67A | 119.42 (13) |
C24—C23—H23B | 109.07 (12) | C68—C67—H67A | 119.43 (11) |
C22—C23—H23B | 109.08 (12) | C67—C68—C69 | 116.8 (2) |
H23A—C23—H23B | 107.8 | C67—C68—C71 | 120.9 (2) |
C25—C24—C23 | 113.3 (2) | C69—C68—C71 | 122.3 (2) |
C25—C24—H24A | 108.91 (12) | C68—C69—C70 | 122.5 (2) |
C23—C24—H24A | 108.90 (12) | C68—C69—H69A | 118.73 (12) |
C25—C24—H24B | 108.91 (12) | C70—C69—H69A | 118.73 (12) |
C23—C24—H24B | 108.90 (12) | C69—C70—C65 | 119.8 (2) |
H24A—C24—H24B | 107.7 | C69—C70—C79 | 119.1 (2) |
C26—C25—C24 | 113.6 (2) | C65—C70—C79 | 121.1 (2) |
C26—C25—H25A | 108.84 (12) | C76—C71—C72 | 116.9 (2) |
C24—C25—H25A | 108.84 (12) | C76—C71—C68 | 122.8 (2) |
C26—C25—H25B | 108.83 (12) | C72—C71—C68 | 120.3 (2) |
C24—C25—H25B | 108.84 (12) | C71—C72—C73 | 121.3 (2) |
H25A—C25—H25B | 107.7 | C71—C72—H72A | 119.34 (12) |
C27—C26—C25 | 113.4 (2) | C73—C72—H72A | 119.34 (13) |
C27—C26—H26A | 108.88 (12) | C74—C73—C72 | 120.5 (2) |
C25—C26—H26A | 108.89 (12) | C74—C73—H73A | 119.73 (12) |
C27—C26—H26B | 108.88 (12) | C72—C73—H73A | 119.73 (14) |
C25—C26—H26B | 108.88 (12) | C73—C74—O4 | 124.8 (2) |
H26A—C26—H26B | 107.7 | C73—C74—C75 | 119.1 (2) |
C26—C27—C28 | 114.7 (2) | O4—C74—C75 | 116.2 (2) |
C26—C27—H27A | 108.59 (12) | C74—C75—C76 | 120.4 (2) |
C28—C27—H27A | 108.59 (13) | C74—C75—H75A | 119.79 (12) |
C26—C27—H27B | 108.59 (12) | C76—C75—H75A | 119.79 (13) |
C28—C27—H27B | 108.60 (13) | C75—C76—C71 | 121.7 (2) |
H27A—C27—H27B | 107.6 | C75—C76—H76A | 119.13 (13) |
C27—C28—C29 | 113.1 (2) | C71—C76—H76A | 119.13 (12) |
C27—C28—H28A | 108.95 (13) | O5—C77—C51 | 106.6 (2) |
C29—C28—H28A | 108.95 (13) | O5—C77—H77A | 110.42 (10) |
C27—C28—H28B | 108.95 (13) | C51—C77—H77A | 110.41 (11) |
C29—C28—H28B | 108.95 (13) | O5—C77—H77B | 110.41 (10) |
H28A—C28—H28B | 107.8 | C51—C77—H77B | 110.41 (11) |
C30—C29—C28 | 115.1 (2) | H77A—C77—H77B | 108.6 |
C30—C29—H29A | 108.50 (14) | O6—C78—O5 | 126.4 (2) |
C28—C29—H29A | 108.50 (13) | O6—C78—O7 | 126.8 (2) |
C30—C29—H29B | 108.49 (14) | O5—C78—O7 | 106.7 (2) |
C28—C29—H29B | 108.49 (13) | O7—C79—C70 | 112.3 (2) |
H29A—C29—H29B | 107.5 | O7—C79—H79A | 109.15 (10) |
C29—C30—H30A | 109.47 (15) | C70—C79—H79A | 109.16 (11) |
C29—C30—H30B | 109.47 (14) | O7—C79—H79B | 109.15 (10) |
H30A—C30—H30B | 109.5 | C70—C79—H79B | 109.15 (11) |
C29—C30—H30C | 109.48 (14) | H79A—C79—H79B | 107.9 |
H30A—C30—H30C | 109.5 | ||
C41—O1—C1—C2 | −175.8 (2) | C51—C50—C53—C58 | 43.7 (3) |
O1—C1—C2—C3 | 163.7 (2) | C58—C53—C54—C55 | −3.0 (3) |
C1—C2—C3—C4 | 170.9 (2) | C50—C53—C54—C55 | 176.5 (2) |
C2—C3—C4—C5 | 174.2 (2) | C53—C54—C55—C56 | 0.7 (3) |
C3—C4—C5—C6 | 177.6 (2) | C11—O2—C56—C57 | −170.4 (2) |
C4—C5—C6—C7 | 177.2 (2) | C11—O2—C56—C55 | 9.5 (3) |
C5—C6—C7—C8 | −179.1 (2) | C54—C55—C56—O2 | −178.1 (2) |
C6—C7—C8—C9 | −178.8 (2) | C54—C55—C56—C57 | 1.9 (3) |
C7—C8—C9—C10 | −178.0 (2) | O2—C56—C57—C58 | 177.9 (2) |
C56—O2—C11—C12 | 174.0 (2) | C55—C56—C57—C58 | −2.0 (3) |
O2—C11—C12—C13 | −176.9 (2) | C56—C57—C58—C53 | −0.4 (3) |
C11—C12—C13—C14 | −176.6 (2) | C54—C53—C58—C57 | 2.8 (3) |
C12—C13—C14—C15 | −179.8 (2) | C50—C53—C58—C57 | −176.7 (2) |
C13—C14—C15—C16 | −179.2 (2) | C21—O3—C59—C64 | −17.2 (3) |
C14—C15—C16—C17 | −179.5 (2) | C21—O3—C59—C60 | 163.4 (2) |
C15—C16—C17—C18 | −177.0 (2) | O3—C59—C60—C61 | −178.5 (2) |
C16—C17—C18—C19 | −178.6 (2) | C64—C59—C60—C61 | 2.1 (3) |
C17—C18—C19—C20 | −175.8 (3) | C59—C60—C61—C62 | −3.5 (3) |
C59—O3—C21—C22 | 175.9 (2) | C60—C61—C62—C63 | 1.7 (3) |
O3—C21—C22—C23 | −76.0 (2) | C60—C61—C62—C65 | 176.1 (2) |
C21—C22—C23—C24 | −169.7 (2) | C61—C62—C63—C64 | 1.4 (3) |
C22—C23—C24—C25 | 173.7 (2) | C65—C62—C63—C64 | −172.9 (2) |
C23—C24—C25—C26 | −177.3 (2) | O3—C59—C64—C63 | −178.4 (2) |
C24—C25—C26—C27 | 178.2 (2) | C60—C59—C64—C63 | 0.9 (3) |
C25—C26—C27—C28 | −179.9 (2) | C62—C63—C64—C59 | −2.7 (3) |
C26—C27—C28—C29 | 178.7 (2) | C63—C62—C65—C66 | 124.6 (2) |
C27—C28—C29—C30 | −179.7 (2) | C61—C62—C65—C66 | −49.6 (3) |
C74—O4—C31—C32 | 178.0 (2) | C63—C62—C65—C70 | −54.4 (3) |
O4—C31—C32—C33 | 179.7 (2) | C61—C62—C65—C70 | 131.5 (2) |
C31—C32—C33—C34 | 178.0 (2) | C70—C65—C66—C67 | 2.1 (3) |
C32—C33—C34—C35 | −176.7 (2) | C62—C65—C66—C67 | −176.9 (2) |
C33—C34—C35—C36 | −177.2 (2) | C65—C66—C67—C68 | 1.5 (3) |
C34—C35—C36—C37 | −177.5 (2) | C66—C67—C68—C69 | −4.0 (3) |
C35—C36—C37—C38 | −173.6 (2) | C66—C67—C68—C71 | 174.9 (2) |
C36—C37—C38—C39 | −176.3 (2) | C67—C68—C69—C70 | 3.0 (3) |
C37—C38—C39—C40 | −176.5 (2) | C71—C68—C69—C70 | −175.9 (2) |
C1—O1—C41—C42 | 170.0 (2) | C68—C69—C70—C65 | 0.6 (3) |
C1—O1—C41—C46 | −10.5 (3) | C68—C69—C70—C79 | −177.8 (2) |
O1—C41—C42—C43 | −178.1 (2) | C66—C65—C70—C69 | −3.1 (3) |
C46—C41—C42—C43 | 2.4 (3) | C62—C65—C70—C69 | 175.9 (2) |
C41—C42—C43—C44 | −1.2 (3) | C66—C65—C70—C79 | 175.2 (2) |
C42—C43—C44—C45 | −0.6 (3) | C62—C65—C70—C79 | −5.8 (3) |
C42—C43—C44—C47 | 179.9 (2) | C67—C68—C71—C76 | 160.5 (2) |
C43—C44—C45—C46 | 1.3 (3) | C69—C68—C71—C76 | −20.7 (3) |
C47—C44—C45—C46 | −179.3 (2) | C67—C68—C71—C72 | −21.3 (3) |
C44—C45—C46—C41 | −0.1 (3) | C69—C68—C71—C72 | 157.5 (2) |
O1—C41—C46—C45 | 178.8 (2) | C76—C71—C72—C73 | −0.5 (3) |
C42—C41—C46—C45 | −1.8 (3) | C68—C71—C72—C73 | −178.8 (2) |
C45—C44—C47—C52 | −32.6 (3) | C71—C72—C73—C74 | 0.6 (3) |
C43—C44—C47—C52 | 146.8 (2) | C72—C73—C74—O4 | 179.9 (2) |
C45—C44—C47—C48 | 148.8 (2) | C72—C73—C74—C75 | −0.8 (3) |
C43—C44—C47—C48 | −31.7 (3) | C31—O4—C74—C73 | −5.6 (3) |
C52—C47—C48—C49 | 1.9 (3) | C31—O4—C74—C75 | 175.1 (2) |
C44—C47—C48—C49 | −179.5 (2) | C73—C74—C75—C76 | 1.0 (3) |
C47—C48—C49—C50 | −1.3 (3) | O4—C74—C75—C76 | −179.6 (2) |
C48—C49—C50—C51 | −1.8 (3) | C74—C75—C76—C71 | −1.0 (3) |
C48—C49—C50—C53 | −178.3 (2) | C72—C71—C76—C75 | 0.7 (3) |
C49—C50—C51—C52 | 4.4 (3) | C68—C71—C76—C75 | 178.9 (2) |
C53—C50—C51—C52 | −179.2 (2) | C78—O5—C77—C51 | −178.2 (2) |
C49—C50—C51—C77 | −171.0 (2) | C52—C51—C77—O5 | −27.2 (3) |
C53—C50—C51—C77 | 5.5 (3) | C50—C51—C77—O5 | 148.2 (2) |
C50—C51—C52—C47 | −4.0 (3) | C77—O5—C78—O6 | 1.7 (3) |
C77—C51—C52—C47 | 171.5 (2) | C77—O5—C78—O7 | −177.7 (2) |
C48—C47—C52—C51 | 0.8 (3) | C79—O7—C78—O6 | −0.5 (3) |
C44—C47—C52—C51 | −177.8 (2) | C79—O7—C78—O5 | 178.9 (2) |
C49—C50—C53—C54 | 40.6 (3) | C78—O7—C79—C70 | 85.2 (2) |
C51—C50—C53—C54 | −135.7 (2) | C69—C70—C79—O7 | −91.8 (2) |
C49—C50—C53—C58 | −139.9 (2) | C65—C70—C79—O7 | 89.8 (2) |
Experimental details
Crystal data | |
Chemical formula | C79H110O7 |
Mr | 1171.67 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 123 |
a, b, c (Å) | 33.654 (9), 30.229 (8), 6.798 (2) |
β (°) | 94.74 (1) |
V (Å3) | 6892.3 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.07 |
Crystal size (mm) | 0.4 × 0.10 × 0.02 |
Data collection | |
Diffractometer | Bruker 1K CCD area-detector diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 79109, 17107, 6169 |
Rint | 0.179 |
(sin θ/λ)max (Å−1) | 0.685 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.071, 0.130, 1.02 |
No. of reflections | 14105 |
No. of parameters | 775 |
No. of restraints | 48 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.29, −0.28 |
Computer programs: SMART (Bruker, 1998), SMART, SHELXTL (Bruker, 1998), SHELXS93 (Sheldrick, 1993), SHELXL97 (Sheldrick, 1997), ZORTEP (Zsolnai & Huttner, 1994), SHELXL97.
Planes | Θ |
P1 \wedge P2 | 33.01 (7) |
P2 \wedge P3 | 41.68 (8) |
P4 \wedge P5 | 53.14 (8) |
P5 \wedge P6 | 21.36 (9) |
P1 \wedge P7 | 26.44 (9) |
P3 \wedge P8 | 12.56 (8) |
P4 \wedge P9 | 75.77 (9) |
P6 \wedge P10 | 2.40 (9) |
P2 \wedge P11 | 28.45 (6) |
P5 \wedge P11 | 63.64 (6) |
Definition of planes: P1 = C41–C46; P2 = C47–C52; P3 = C53–C58; P4 = C59–C64; P5 = C65–C70; P6 = C71–C76; P7 = O1, C1–C10; P8 = O2, C11–C20; P9 = O3, C21–C30; P10 = O4, C31–C40; P11 = O5, O6, O7, C77, C78, C79. |