Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801020487/om6071sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801020487/om6071Isup2.hkl |
CCDC reference: 180555
Modest restraints (DFIX and DELU) were applied to first and second nearest-atom distances in the hydrocarbon tails of the cholesterol molecules. Despite being restrained to nominal values, most carbon–carbon bond distances appear short. This implies a wagging motion of the chain ends, with presumably kidney-shaped atoms modeled as ellipsoids with shortened bonds. The choice of extreme thermal motion or disorder in the tails of the cholesterol molecules presented a difficulty. After refining several models we have chosen to model only the two most obvious cases (C25_2 and C21_3, C22_3, C23_3) as disordered. Given the limited data, no convincing improvement was achieved by modeling additional atoms as disordered. The weight parameters were arrived at by an iterative procedure in which the mean standard uncertainties of the oxygen and ordered carbon-atom coordinates were minimized. This resulted in significantly lower s.u.'s for the atom coordinates, and allowed the S parameters to deviate more from unity.
Data collection: Syntex P1 Software (Sparks, 1970); cell refinement: Syntex P1 Software; data reduction: SYNOUT (Sparks, 1970); program(s) used to solve structure: Patterson search (Schilling, 1970) and MULTAN (Germain et al., 1971); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1994); software used to prepare material for publication: SHELXL97.
| Fig. 1. Atom numbering in the title cholesterol molecule. Fig. 2. One cell of the cholesterol hemimethanol solvate structure showing 25% probability displacement ellipsoids. |
C27H46O·0.5CH4O | Z = 4 |
Mr = 402.66 | F(000) = 900 |
Triclinic, P1 | Dx = 1.017 Mg m−3 |
a = 12.2735 (17) Å | Cu Kα radiation, λ = 1.54180 Å |
b = 34.237 (7) Å | Cell parameters from 15 reflections |
c = 6.2739 (8) Å | θ = 24–31° |
α = 90.224 (14)° | µ = 0.45 mm−1 |
β = 93.705 (10)° | T = 293 K |
γ = 91.576 (14)° | Plate, colourless |
V = 2629.8 (7) Å3 | 0.50 × 0.30 × 0.10 mm |
Syntex P1 diffractometer | Rint = 0.000 |
Radiation source: fine-focus sealed tube | θmax = 57.4°, θmin = 2.6° |
Graphite monochromator | h = 0→13 |
ω–2θ scans | k = −37→37 |
7176 measured reflections | l = −6→6 |
7176 independent reflections | 3 standard reflections every 50 reflections |
5452 reflections with I > 2σ(I) | intensity decay: 6% |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.102 | H atoms treated by a mixture of independent and constrained refinement |
S = 2.09 | w = 1/[σ2(Fo2) + (0.0171P)2] where P = (Fo2 + 2Fc2)/3 |
6750 reflections | (Δ/σ)max = 0.001 |
1097 parameters | Δρmax = 0.17 e Å−3 |
393 restraints | Δρmin = −0.15 e Å−3 |
C27H46O·0.5CH4O | γ = 91.576 (14)° |
Mr = 402.66 | V = 2629.8 (7) Å3 |
Triclinic, P1 | Z = 4 |
a = 12.2735 (17) Å | Cu Kα radiation |
b = 34.237 (7) Å | µ = 0.45 mm−1 |
c = 6.2739 (8) Å | T = 293 K |
α = 90.224 (14)° | 0.50 × 0.30 × 0.10 mm |
β = 93.705 (10)° |
Syntex P1 diffractometer | Rint = 0.000 |
7176 measured reflections | θmax = 57.4° |
7176 independent reflections | 3 standard reflections every 50 reflections |
5452 reflections with I > 2σ(I) | intensity decay: 6% |
R[F2 > 2σ(F2)] = 0.054 | 393 restraints |
wR(F2) = 0.102 | H atoms treated by a mixture of independent and constrained refinement |
S = 2.09 | Δρmax = 0.17 e Å−3 |
6750 reflections | Δρmin = −0.15 e Å−3 |
1097 parameters |
Experimental. All reflections in the theta range 57.4 to 60.0 were recorded but no intensity above background was found. One hemisphere of reciprocal space was covered. |
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. 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) | |
O03_1 | 0.1829 (4) | 0.52123 (12) | 0.4856 (9) | 0.1178 (16) | |
H03_1 | 0.129 (6) | 0.5158 (7) | 0.579 (11) | 0.141* | |
C01_1 | 0.3514 (4) | 0.61027 (16) | 0.3822 (10) | 0.0894 (18) | |
H01A_1 | 0.4109 | 0.6137 | 0.2888 | 0.107* | |
H01B_1 | 0.3805 | 0.6159 | 0.5268 | 0.107* | |
C02_1 | 0.3119 (5) | 0.56788 (17) | 0.3705 (11) | 0.099 (2) | |
H02A_1 | 0.2893 | 0.5610 | 0.2239 | 0.119* | |
H02B_1 | 0.3711 | 0.5511 | 0.4180 | 0.119* | |
C03_1 | 0.2181 (5) | 0.56163 (17) | 0.5081 (11) | 0.0872 (17) | |
H03C_1 | 0.2430 | 0.5668 | 0.6573 | 0.105* | |
C04_1 | 0.1275 (4) | 0.58819 (15) | 0.4450 (9) | 0.0799 (16) | |
H04A_1 | 0.0699 | 0.5848 | 0.5427 | 0.096* | |
H04B_1 | 0.0975 | 0.5811 | 0.3028 | 0.096* | |
C05_1 | 0.1651 (4) | 0.63044 (15) | 0.4469 (8) | 0.0609 (13) | |
C06_1 | 0.1153 (4) | 0.65668 (16) | 0.5534 (8) | 0.0697 (14) | |
H06_1 | 0.0571 | 0.6481 | 0.6305 | 0.084* | |
C07_1 | 0.1447 (4) | 0.69951 (15) | 0.5613 (8) | 0.0734 (15) | |
H07A_1 | 0.1783 | 0.7060 | 0.7015 | 0.088* | |
H07B_1 | 0.0784 | 0.7142 | 0.5414 | 0.088* | |
C08_1 | 0.2221 (4) | 0.71187 (14) | 0.3934 (8) | 0.0597 (13) | |
H08_1 | 0.1803 | 0.7132 | 0.2552 | 0.072* | |
C09_1 | 0.3101 (4) | 0.68176 (14) | 0.3764 (7) | 0.0608 (13) | |
H09_1 | 0.3461 | 0.6800 | 0.5199 | 0.073* | |
C10_1 | 0.2652 (4) | 0.63989 (15) | 0.3210 (8) | 0.0664 (14) | |
C11_1 | 0.3990 (4) | 0.69637 (16) | 0.2324 (10) | 0.0912 (19) | |
H11A_1 | 0.4591 | 0.6785 | 0.2435 | 0.109* | |
H11B_1 | 0.3693 | 0.6959 | 0.0853 | 0.109* | |
C12_1 | 0.4428 (4) | 0.73738 (16) | 0.2871 (10) | 0.0878 (18) | |
H12A_1 | 0.4813 | 0.7372 | 0.4271 | 0.105* | |
H12B_1 | 0.4948 | 0.7452 | 0.1843 | 0.105* | |
C13_1 | 0.3536 (4) | 0.76712 (16) | 0.2873 (8) | 0.0671 (14) | |
C14_1 | 0.2728 (4) | 0.75164 (14) | 0.4444 (8) | 0.0629 (13) | |
H14_1 | 0.3157 | 0.7486 | 0.5803 | 0.075* | |
C15_1 | 0.1983 (4) | 0.78577 (15) | 0.4785 (10) | 0.0891 (18) | |
H15A_1 | 0.1677 | 0.7842 | 0.6171 | 0.107* | |
H15B_1 | 0.1391 | 0.7862 | 0.3684 | 0.107* | |
C16_1 | 0.2756 (5) | 0.82251 (16) | 0.4648 (10) | 0.0924 (19) | |
H16A_1 | 0.2438 | 0.8413 | 0.3655 | 0.111* | |
H16B_1 | 0.2881 | 0.8349 | 0.6038 | 0.111* | |
C17_1 | 0.3840 (4) | 0.80754 (16) | 0.3855 (9) | 0.0782 (16) | |
H17_1 | 0.4323 | 0.8030 | 0.5131 | 0.094* | |
C18_1 | 0.2983 (5) | 0.77241 (17) | 0.0610 (9) | 0.0982 (19) | |
H18A_1 | 0.2422 | 0.7913 | 0.0662 | 0.147* | |
H18B_1 | 0.2665 | 0.7479 | 0.0104 | 0.147* | |
H18C_1 | 0.3518 | 0.7813 | −0.0342 | 0.147* | |
C19_1 | 0.2285 (5) | 0.63642 (17) | 0.0774 (8) | 0.0977 (19) | |
H19A_1 | 0.1740 | 0.6553 | 0.0419 | 0.147* | |
H19B_1 | 0.1986 | 0.6106 | 0.0470 | 0.147* | |
H19C_1 | 0.2904 | 0.6412 | −0.0058 | 0.147* | |
C20_1 | 0.4405 (5) | 0.83934 (18) | 0.2564 (12) | 0.108 (2) | |
H20_1 | 0.3909 | 0.8475 | 0.1370 | 0.130* | |
C21_1 | 0.5468 (6) | 0.8253 (2) | 0.1714 (14) | 0.144 (3) | |
H21A_1 | 0.5798 | 0.8459 | 0.0920 | 0.216* | |
H21B_1 | 0.5313 | 0.8030 | 0.0798 | 0.216* | |
H21C_1 | 0.5961 | 0.8181 | 0.2889 | 0.216* | |
C22_1 | 0.4691 (8) | 0.8750 (2) | 0.4087 (19) | 0.196 (5) | |
H22A_1 | 0.4014 | 0.8835 | 0.4630 | 0.236* | |
H22B_1 | 0.5138 | 0.8655 | 0.5299 | 0.236* | |
C23_1 | 0.5192 (11) | 0.9057 (3) | 0.336 (3) | 0.299 (9) | |
H23A_1 | 0.4814 | 0.9118 | 0.1999 | 0.359* | |
H23B_1 | 0.5916 | 0.8976 | 0.3041 | 0.359* | |
C24_1 | 0.5349 (13) | 0.9445 (4) | 0.460 (3) | 0.315 (10) | |
H24A_1 | 0.5675 | 0.9635 | 0.3681 | 0.378* | |
H24B_1 | 0.4632 | 0.9536 | 0.4894 | 0.378* | |
C25_1 | 0.5981 (19) | 0.9442 (7) | 0.653 (3) | 0.47 (2) | |
H25_1 | 0.5854 | 0.9217 | 0.7458 | 0.569* | |
C26_1 | 0.7053 (18) | 0.9439 (6) | 0.537 (5) | 0.463 (19) | |
H26A_1 | 0.7665 | 0.9439 | 0.6400 | 0.695* | |
H26B_1 | 0.7100 | 0.9668 | 0.4493 | 0.695* | |
H26C_1 | 0.7059 | 0.9210 | 0.4485 | 0.695* | |
C27_1 | 0.5904 (17) | 0.9862 (5) | 0.763 (4) | 0.52 (2) | |
H27A_1 | 0.6336 | 0.9868 | 0.8961 | 0.785* | |
H27B_1 | 0.5157 | 0.9910 | 0.7885 | 0.785* | |
H27C_1 | 0.6173 | 1.0059 | 0.6700 | 0.785* | |
O03_2 | 0.3038 (4) | 0.46414 (13) | 0.3475 (9) | 0.1279 (19) | |
H03_2 | 0.257 (5) | 0.4827 (17) | 0.374 (11) | 0.154* | |
C01_2 | 0.1222 (4) | 0.37655 (16) | 0.4297 (10) | 0.0825 (17) | |
H01A_2 | 0.0500 | 0.3691 | 0.3685 | 0.099* | |
H01B_2 | 0.1174 | 0.3792 | 0.5827 | 0.099* | |
C02_2 | 0.1543 (5) | 0.41596 (17) | 0.3411 (11) | 0.0964 (19) | |
H02A_2 | 0.1015 | 0.4351 | 0.3768 | 0.116* | |
H02B_2 | 0.1543 | 0.4143 | 0.1867 | 0.116* | |
C03_2 | 0.2684 (5) | 0.42884 (18) | 0.4346 (11) | 0.0920 (19) | |
H03C_2 | 0.2658 | 0.4321 | 0.5894 | 0.110* | |
C04_2 | 0.3487 (4) | 0.39775 (17) | 0.3917 (10) | 0.0894 (18) | |
H04A_2 | 0.3578 | 0.3966 | 0.2394 | 0.107* | |
H04B_2 | 0.4189 | 0.4050 | 0.4625 | 0.107* | |
C05_2 | 0.3143 (4) | 0.35807 (17) | 0.4664 (9) | 0.0708 (15) | |
C06_2 | 0.3803 (4) | 0.33699 (19) | 0.5927 (9) | 0.0819 (17) | |
H06_2 | 0.4471 | 0.3485 | 0.6403 | 0.098* | |
C07_2 | 0.3561 (4) | 0.29626 (19) | 0.6648 (8) | 0.0817 (17) | |
H07A_2 | 0.3431 | 0.2968 | 0.8157 | 0.098* | |
H07B_2 | 0.4195 | 0.2805 | 0.6474 | 0.098* | |
C08_2 | 0.2574 (4) | 0.27713 (15) | 0.5421 (8) | 0.0639 (14) | |
H08_2 | 0.2786 | 0.2697 | 0.3999 | 0.077* | |
C09_2 | 0.1665 (4) | 0.30656 (16) | 0.5165 (8) | 0.0638 (14) | |
H09_2 | 0.1537 | 0.3157 | 0.6608 | 0.077* | |
C10_2 | 0.1998 (4) | 0.34363 (16) | 0.3881 (8) | 0.0662 (14) | |
C11_2 | 0.0579 (4) | 0.28734 (16) | 0.4266 (9) | 0.0804 (16) | |
H11A_2 | 0.0001 | 0.3058 | 0.4379 | 0.096* | |
H11B_2 | 0.0635 | 0.2817 | 0.2762 | 0.096* | |
C12_2 | 0.0261 (4) | 0.24938 (16) | 0.5407 (9) | 0.0796 (17) | |
H12A_2 | 0.0094 | 0.2555 | 0.6859 | 0.096* | |
H12B_2 | −0.0392 | 0.2378 | 0.4679 | 0.096* | |
C13_2 | 0.1171 (4) | 0.21994 (16) | 0.5452 (8) | 0.0664 (14) | |
C14_2 | 0.2181 (4) | 0.24098 (16) | 0.6537 (8) | 0.0671 (14) | |
H14_2 | 0.1957 | 0.2500 | 0.7923 | 0.081* | |
C15_2 | 0.2983 (5) | 0.20820 (19) | 0.7040 (10) | 0.102 (2) | |
H15A_2 | 0.3480 | 0.2151 | 0.8256 | 0.122* | |
H15B_2 | 0.3405 | 0.2029 | 0.5822 | 0.122* | |
C16_2 | 0.2253 (5) | 0.1728 (2) | 0.7546 (11) | 0.105 (2) | |
H16A_2 | 0.2346 | 0.1664 | 0.9050 | 0.126* | |
H16B_2 | 0.2437 | 0.1502 | 0.6714 | 0.126* | |
C17_2 | 0.1052 (4) | 0.18472 (17) | 0.6948 (9) | 0.0786 (16) | |
H17_2 | 0.0767 | 0.1948 | 0.8259 | 0.094* | |
C18_2 | 0.1385 (5) | 0.20632 (18) | 0.3183 (8) | 0.0991 (19) | |
H18A_2 | 0.1960 | 0.1878 | 0.3253 | 0.149* | |
H18B_2 | 0.1596 | 0.2284 | 0.2351 | 0.149* | |
H18C_2 | 0.0731 | 0.1942 | 0.2527 | 0.149* | |
C19_2 | 0.2000 (5) | 0.33482 (17) | 0.1478 (8) | 0.0918 (18) | |
H19A_2 | 0.1287 | 0.3256 | 0.0955 | 0.138* | |
H19B_2 | 0.2523 | 0.3151 | 0.1242 | 0.138* | |
H19C_2 | 0.2194 | 0.3582 | 0.0734 | 0.138* | |
C20_2 | 0.0321 (5) | 0.1498 (2) | 0.6243 (12) | 0.105 (2) | |
H20_2 | 0.0663 | 0.1357 | 0.5112 | 0.126* | |
C21_2 | −0.0835 (5) | 0.1601 (2) | 0.5440 (12) | 0.127 (3) | |
H21A_2 | −0.1243 | 0.1367 | 0.5031 | 0.191* | |
H21B_2 | −0.0803 | 0.1770 | 0.4228 | 0.191* | |
H21C_2 | −0.1186 | 0.1732 | 0.6555 | 0.191* | |
C22_2 | 0.0259 (8) | 0.1221 (3) | 0.8275 (19) | 0.187 (5) | |
H22A_2 | 0.0998 | 0.1175 | 0.8846 | 0.224* | |
H22B_2 | −0.0109 | 0.1358 | 0.9364 | 0.224* | |
C23_2 | −0.0273 (10) | 0.0863 (3) | 0.789 (2) | 0.285 (8) | |
H23A_2 | −0.0040 | 0.0760 | 0.6558 | 0.342* | |
H23B_2 | −0.1049 | 0.0908 | 0.7689 | 0.342* | |
C24_2 | −0.0110 (12) | 0.0547 (5) | 0.959 (3) | 0.337 (13) | |
H24A_2 | −0.0232 | 0.0296 | 0.8878 | 0.404* | |
H24B_2 | 0.0652 | 0.0561 | 1.0108 | 0.404* | |
C25_2 | −0.0714 (18) | 0.0540 (7) | 1.135 (4) | 0.273 (18) | 0.60 (3) |
H25A_2 | −0.0470 | 0.0749 | 1.2354 | 0.328* | 0.60 (3) |
C25'_2 | −0.0973 (18) | 0.0309 (8) | 1.021 (4) | 0.29 (3) | 0.40 (3) |
H25D_2 | −0.1199 | 0.0110 | 0.9134 | 0.348* | 0.40 (3) |
C26_2 | −0.0445 (12) | 0.0125 (4) | 1.232 (2) | 0.285 (7) | |
H26A_2 | −0.0825 | 0.0088 | 1.3595 | 0.428* | |
H26B_2 | 0.0327 | 0.0111 | 1.2653 | 0.428* | |
H26C_2 | −0.0675 | −0.0074 | 1.1296 | 0.428* | |
C27_2 | −0.1933 (12) | 0.0538 (6) | 1.092 (4) | 0.423 (16) | |
H27A_2 | −0.2276 | 0.0531 | 1.2257 | 0.635* | |
H27B_2 | −0.2163 | 0.0311 | 1.0090 | 0.635* | |
H27C_2 | −0.2138 | 0.0769 | 1.0156 | 0.635* | |
O03_3 | 0.6596 (4) | 0.52112 (12) | 0.3104 (8) | 0.1163 (18) | |
H03_3 | 0.619 (6) | 0.5126 (9) | 0.231 (12) | 0.140* | |
C01_3 | 0.7837 (5) | 0.62178 (16) | 0.3648 (8) | 0.0854 (17) | |
H01A_3 | 0.8531 | 0.6306 | 0.4340 | 0.102* | |
H01B_3 | 0.7264 | 0.6342 | 0.4374 | 0.102* | |
C02_3 | 0.7716 (5) | 0.57771 (16) | 0.3920 (9) | 0.0871 (17) | |
H02A_3 | 0.8320 | 0.5650 | 0.3306 | 0.104* | |
H02B_3 | 0.7736 | 0.5715 | 0.5429 | 0.104* | |
C03_3 | 0.6654 (5) | 0.56260 (17) | 0.2840 (10) | 0.0874 (17) | |
H03C_3 | 0.6048 | 0.5742 | 0.3537 | 0.105* | |
C04_3 | 0.6581 (5) | 0.57375 (16) | 0.0492 (9) | 0.0856 (17) | |
H04A_3 | 0.7122 | 0.5596 | −0.0239 | 0.103* | |
H04B_3 | 0.5866 | 0.5659 | −0.0139 | 0.103* | |
C05_3 | 0.6763 (4) | 0.61705 (16) | 0.0158 (8) | 0.0687 (14) | |
C06_3 | 0.6088 (4) | 0.63771 (17) | −0.1082 (9) | 0.0777 (16) | |
H06_3 | 0.5467 | 0.6246 | −0.1677 | 0.093* | |
C07_3 | 0.6216 (4) | 0.67984 (16) | −0.1627 (8) | 0.0720 (14) | |
H07A_3 | 0.5672 | 0.6945 | −0.0932 | 0.086* | |
H07B_3 | 0.6082 | 0.6829 | −0.3158 | 0.086* | |
C08_3 | 0.7356 (4) | 0.69684 (15) | −0.0946 (7) | 0.0580 (13) | |
H08_3 | 0.7868 | 0.6885 | −0.1983 | 0.070* | |
C09_3 | 0.7727 (4) | 0.68042 (14) | 0.1274 (7) | 0.0611 (13) | |
H09_3 | 0.7150 | 0.6868 | 0.2215 | 0.073* | |
C10_3 | 0.7785 (4) | 0.63547 (15) | 0.1296 (8) | 0.0629 (13) | |
C11_3 | 0.8760 (4) | 0.70160 (15) | 0.2228 (8) | 0.0755 (15) | |
H11A_3 | 0.8866 | 0.6943 | 0.3717 | 0.091* | |
H11B_3 | 0.9379 | 0.6923 | 0.1503 | 0.091* | |
C12_3 | 0.8767 (4) | 0.74588 (15) | 0.2101 (8) | 0.0740 (15) | |
H12A_3 | 0.8246 | 0.7559 | 0.3052 | 0.089* | |
H12B_3 | 0.9486 | 0.7562 | 0.2579 | 0.089* | |
C13_3 | 0.8480 (4) | 0.75985 (14) | −0.0142 (7) | 0.0590 (13) | |
C14_3 | 0.7374 (4) | 0.74023 (14) | −0.0872 (7) | 0.0588 (13) | |
H14_3 | 0.6876 | 0.7471 | 0.0221 | 0.071* | |
C15_3 | 0.6991 (4) | 0.76305 (16) | −0.2862 (9) | 0.0813 (16) | |
H15A_3 | 0.6201 | 0.7644 | −0.2978 | 0.098* | |
H15B_3 | 0.7228 | 0.7508 | −0.4143 | 0.098* | |
C16_3 | 0.7527 (5) | 0.80443 (17) | −0.2543 (9) | 0.0962 (19) | |
H16A_3 | 0.7991 | 0.8106 | −0.3696 | 0.115* | |
H16B_3 | 0.6972 | 0.8240 | −0.2506 | 0.115* | |
C17_3 | 0.8210 (4) | 0.80332 (15) | −0.0382 (8) | 0.0736 (15) | |
H17_3 | 0.7698 | 0.8086 | 0.0713 | 0.088* | |
C18_3 | 0.9390 (4) | 0.74950 (17) | −0.1623 (8) | 0.0801 (16) | |
H18A_3 | 0.9199 | 0.7585 | −0.3043 | 0.120* | |
H18B_3 | 0.9470 | 0.7217 | −0.1647 | 0.120* | |
H18C_3 | 1.0067 | 0.7619 | −0.1100 | 0.120* | |
C19_3 | 0.8791 (4) | 0.62103 (17) | 0.0208 (9) | 0.0890 (17) | |
H19A_3 | 0.9442 | 0.6324 | 0.0911 | 0.133* | |
H19B_3 | 0.8744 | 0.6286 | −0.1266 | 0.133* | |
H19C_3 | 0.8812 | 0.5931 | 0.0301 | 0.133* | |
C20_3 | 0.9118 (6) | 0.83462 (18) | −0.0071 (14) | 0.107 (2) | |
H20_3 | 0.9687 | 0.8246 | −0.0936 | 0.128* | |
C21_3 | 0.9655 (12) | 0.8377 (4) | 0.197 (2) | 0.160 (7) | 0.636 (10) |
H21A_3 | 1.0206 | 0.8581 | 0.1974 | 0.239* | 0.636 (10) |
H21B_3 | 0.9989 | 0.8134 | 0.2332 | 0.239* | 0.636 (10) |
H21C_3 | 0.9136 | 0.8436 | 0.2996 | 0.239* | 0.636 (10) |
C22_3 | 0.8848 (11) | 0.8737 (3) | −0.1154 (19) | 0.125 (5) | 0.636 (10) |
H22A_3 | 0.8656 | 0.8685 | −0.2654 | 0.150* | 0.636 (10) |
H22B_3 | 0.8206 | 0.8837 | −0.0539 | 0.150* | 0.636 (10) |
C23_3 | 0.9724 (14) | 0.9053 (4) | −0.100 (2) | 0.183 (9) | 0.636 (10) |
H23A_3 | 1.0109 | 0.9036 | 0.0391 | 0.220* | 0.636 (10) |
H23B_3 | 0.9369 | 0.9303 | −0.1064 | 0.220* | 0.636 (10) |
C21'_3 | 0.862 (2) | 0.8664 (6) | 0.160 (3) | 0.158 (12) | 0.364 (10) |
H21D_3 | 0.8287 | 0.8526 | 0.2721 | 0.237* | 0.364 (10) |
H21E_3 | 0.8088 | 0.8819 | 0.0834 | 0.237* | 0.364 (10) |
H21F_3 | 0.9205 | 0.8831 | 0.2196 | 0.237* | 0.364 (10) |
C22'_3 | 0.9590 (13) | 0.8520 (5) | −0.168 (2) | 0.096 (6) | 0.364 (10) |
H22D_3 | 0.9067 | 0.8691 | −0.2396 | 0.116* | 0.364 (10) |
H22E_3 | 0.9764 | 0.8322 | −0.2703 | 0.116* | 0.364 (10) |
C23'_3 | 1.0664 (14) | 0.8767 (5) | −0.102 (3) | 0.125 (8) | 0.364 (10) |
H23D_3 | 1.0641 | 0.8884 | 0.0386 | 0.150* | 0.364 (10) |
H23E_3 | 1.1314 | 0.8614 | −0.1079 | 0.150* | 0.364 (10) |
C24_3 | 1.0583 (10) | 0.9055 (3) | −0.2704 (18) | 0.211 (5) | |
H24A_3 | 1.0939 | 0.8806 | −0.2619 | 0.253* | |
H24B_3 | 1.0189 | 0.9064 | −0.4093 | 0.253* | |
C25_3 | 1.1445 (15) | 0.9360 (5) | −0.267 (3) | 0.310 (10) | |
H25_3 | 1.1016 | 0.9587 | −0.2323 | 0.371* | |
C26_3 | 1.2205 (16) | 0.9370 (7) | −0.092 (3) | 0.408 (16) | |
H26A_3 | 1.1860 | 0.9279 | 0.0328 | 0.612* | |
H26B_3 | 1.2480 | 0.9633 | −0.0680 | 0.612* | |
H26C_3 | 1.2798 | 0.9203 | −0.1191 | 0.612* | |
C27_3 | 1.1783 (16) | 0.9480 (6) | −0.473 (3) | 0.451 (17) | |
H27A_3 | 1.1177 | 0.9452 | −0.5774 | 0.677* | |
H27B_3 | 1.2366 | 0.9319 | −0.5138 | 0.677* | |
H27C_3 | 1.2032 | 0.9748 | −0.4663 | 0.677* | |
O03_4 | 0.8078 (4) | 0.48701 (12) | 0.5852 (8) | 0.1149 (16) | |
H03_4 | 0.764 (5) | 0.4988 (12) | 0.472 (11) | 0.138* | |
C01_4 | 0.7955 (4) | 0.37707 (15) | 0.5893 (8) | 0.0733 (15) | |
H01A_4 | 0.8465 | 0.3585 | 0.5394 | 0.088* | |
H01B_4 | 0.7263 | 0.3725 | 0.5083 | 0.088* | |
C02_4 | 0.8374 (5) | 0.41792 (16) | 0.5407 (9) | 0.0850 (17) | |
H02A_4 | 0.9109 | 0.4217 | 0.6056 | 0.102* | |
H02B_4 | 0.8407 | 0.4208 | 0.3875 | 0.102* | |
C03_4 | 0.7653 (5) | 0.44855 (17) | 0.6233 (11) | 0.0925 (19) | |
H03C_4 | 0.6927 | 0.4456 | 0.5498 | 0.111* | |
C04_4 | 0.7549 (5) | 0.44307 (16) | 0.8608 (10) | 0.0904 (18) | |
H04A_4 | 0.7038 | 0.4617 | 0.9101 | 0.108* | |
H04B_4 | 0.8253 | 0.4485 | 0.9359 | 0.108* | |
C05_4 | 0.7158 (5) | 0.40182 (16) | 0.9153 (8) | 0.0703 (14) | |
C06_4 | 0.6313 (5) | 0.39738 (18) | 1.0307 (9) | 0.0825 (16) | |
H06_4 | 0.5964 | 0.4196 | 1.0735 | 0.099* | |
C07_4 | 0.5873 (4) | 0.35791 (16) | 1.0982 (8) | 0.0723 (15) | |
H07A_4 | 0.5181 | 0.3524 | 1.0191 | 0.087* | |
H07B_4 | 0.5737 | 0.3591 | 1.2486 | 0.087* | |
C08_4 | 0.6635 (4) | 0.32475 (15) | 1.0624 (7) | 0.0583 (13) | |
H08_4 | 0.7221 | 0.3256 | 1.1763 | 0.070* | |
C09_4 | 0.7153 (4) | 0.32984 (14) | 0.8455 (7) | 0.0566 (12) | |
H09_4 | 0.6540 | 0.3307 | 0.7377 | 0.068* | |
C10_4 | 0.7791 (4) | 0.36890 (15) | 0.8268 (7) | 0.0601 (13) | |
C11_4 | 0.7794 (4) | 0.29374 (14) | 0.7905 (8) | 0.0646 (13) | |
H11A_4 | 0.8010 | 0.2962 | 0.6450 | 0.078* | |
H11B_4 | 0.8456 | 0.2934 | 0.8836 | 0.078* | |
C12_4 | 0.7174 (4) | 0.25464 (15) | 0.8107 (7) | 0.0687 (14) | |
H12A_4 | 0.7660 | 0.2335 | 0.7855 | 0.082* | |
H12B_4 | 0.6572 | 0.2530 | 0.7027 | 0.082* | |
C13_4 | 0.6727 (4) | 0.24988 (15) | 1.0335 (8) | 0.0614 (13) | |
C14_4 | 0.6055 (4) | 0.28636 (15) | 1.0689 (7) | 0.0615 (14) | |
H14_4 | 0.5500 | 0.2865 | 0.9494 | 0.074* | |
C15_4 | 0.5436 (4) | 0.27589 (17) | 1.2647 (8) | 0.0777 (16) | |
H15A_4 | 0.4754 | 0.2896 | 1.2634 | 0.093* | |
H15B_4 | 0.5871 | 0.2826 | 1.3950 | 0.093* | |
C16_4 | 0.5222 (5) | 0.23178 (19) | 1.2489 (9) | 0.0923 (18) | |
H16A_4 | 0.4447 | 0.2260 | 1.2227 | 0.111* | |
H16B_4 | 0.5473 | 0.2193 | 1.3809 | 0.111* | |
C17_4 | 0.5864 (4) | 0.21675 (16) | 1.0592 (9) | 0.0737 (15) | |
H17_4 | 0.5359 | 0.2176 | 0.9319 | 0.088* | |
C18_4 | 0.7684 (4) | 0.24564 (17) | 1.2015 (8) | 0.0786 (16) | |
H18A_4 | 0.8072 | 0.2225 | 1.1721 | 0.118* | |
H18B_4 | 0.7408 | 0.2438 | 1.3410 | 0.118* | |
H18C_4 | 0.8170 | 0.2680 | 1.1966 | 0.118* | |
C19_4 | 0.8926 (4) | 0.36795 (16) | 0.9491 (8) | 0.0785 (16) | |
H19A_4 | 0.9336 | 0.3471 | 0.8941 | 0.118* | |
H19B_4 | 0.8835 | 0.3638 | 1.0982 | 0.118* | |
H19C_4 | 0.9311 | 0.3924 | 0.9308 | 0.118* | |
C20_4 | 0.6182 (6) | 0.17456 (18) | 1.0850 (12) | 0.104 (2) | |
H20_4 | 0.6705 | 0.1730 | 1.2092 | 0.124* | |
C21_4 | 0.6709 (8) | 0.1597 (2) | 0.8973 (17) | 0.178 (4) | |
H21A_4 | 0.6897 | 0.1330 | 0.9203 | 0.266* | |
H21B_4 | 0.7358 | 0.1751 | 0.8764 | 0.266* | |
H21C_4 | 0.6214 | 0.1614 | 0.7730 | 0.266* | |
C22_4 | 0.5179 (8) | 0.1482 (2) | 1.1270 (17) | 0.175 (4) | |
H22A_4 | 0.4783 | 0.1602 | 1.2380 | 0.210* | |
H22B_4 | 0.4697 | 0.1470 | 0.9981 | 0.210* | |
C23_4 | 0.5438 (9) | 0.1087 (3) | 1.191 (2) | 0.255 (7) | |
H23A_4 | 0.6168 | 0.1090 | 1.2601 | 0.306* | |
H23B_4 | 0.5442 | 0.0925 | 1.0640 | 0.306* | |
C24_4 | 0.4599 (15) | 0.0891 (6) | 1.351 (4) | 0.474 (19) | |
H24A_4 | 0.4904 | 0.0650 | 1.4062 | 0.569* | |
H24B_4 | 0.4541 | 0.1066 | 1.4718 | 0.569* | |
C25_4 | 0.3614 (12) | 0.0813 (5) | 1.265 (3) | 0.271 (8) | |
H25_4 | 0.3282 | 0.1046 | 1.2010 | 0.325* | |
C27_4 | 0.2815 (15) | 0.0584 (6) | 1.401 (4) | 0.52 (2) | |
H27A_4 | 0.2128 | 0.0545 | 1.3203 | 0.786* | |
H27B_4 | 0.2707 | 0.0729 | 1.5287 | 0.786* | |
H27C_4 | 0.3112 | 0.0335 | 1.4379 | 0.786* | |
C26_4 | 0.387 (3) | 0.0515 (8) | 1.097 (5) | 0.59 (3) | |
H26A_4 | 0.3203 | 0.0427 | 1.0212 | 0.889* | |
H26B_4 | 0.4218 | 0.0297 | 1.1654 | 0.889* | |
H26C_4 | 0.4347 | 0.0633 | 0.9991 | 0.889* | |
O_5 | 0.4736 (4) | 0.48828 (14) | 0.1161 (9) | 0.1127 (15) | |
H28_5 | 0.419 (5) | 0.4783 (19) | 0.197 (6) | 0.135* | |
C_5 | 0.4369 (7) | 0.4879 (3) | −0.1008 (16) | 0.169 (4) | |
H29A_5 | 0.3702 | 0.4726 | −0.1194 | 0.253* | |
H29B_5 | 0.4913 | 0.4766 | −0.1837 | 0.253* | |
H29C_5 | 0.4243 | 0.5141 | −0.1475 | 0.253* | |
O_6 | 1.0135 (4) | 0.5077 (2) | 0.7302 (11) | 0.151 (2) | |
H28_6 | 0.942 (7) | 0.507 (3) | 0.692 (4) | 0.181* | |
C_6 | 1.0284 (8) | 0.5072 (3) | 0.9446 (18) | 0.195 (4) | |
H29A_6 | 1.0911 | 0.4922 | 0.9856 | 0.292* | |
H29B_6 | 0.9650 | 0.4957 | 1.0038 | 0.292* | |
H29C_6 | 1.0397 | 0.5335 | 0.9974 | 0.292* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O03_1 | 0.108 (4) | 0.071 (3) | 0.177 (5) | −0.001 (2) | 0.033 (3) | 0.001 (3) |
C01_1 | 0.061 (4) | 0.079 (4) | 0.131 (5) | 0.015 (3) | 0.019 (3) | −0.005 (4) |
C02_1 | 0.082 (4) | 0.076 (4) | 0.142 (6) | 0.009 (3) | 0.022 (4) | 0.002 (4) |
C03_1 | 0.087 (4) | 0.067 (4) | 0.109 (5) | 0.010 (3) | 0.011 (4) | 0.002 (3) |
C04_1 | 0.077 (4) | 0.077 (4) | 0.086 (4) | −0.002 (3) | 0.007 (3) | 0.000 (3) |
C05_1 | 0.049 (3) | 0.075 (4) | 0.058 (3) | 0.001 (3) | −0.002 (2) | −0.003 (3) |
C06_1 | 0.057 (3) | 0.079 (4) | 0.074 (4) | −0.006 (3) | 0.012 (3) | −0.003 (3) |
C07_1 | 0.063 (3) | 0.087 (4) | 0.071 (4) | 0.006 (3) | 0.010 (3) | −0.007 (3) |
C08_1 | 0.059 (3) | 0.071 (4) | 0.050 (3) | 0.010 (3) | 0.008 (2) | −0.010 (3) |
C09_1 | 0.052 (3) | 0.075 (4) | 0.056 (3) | 0.006 (3) | 0.005 (2) | −0.010 (3) |
C10_1 | 0.065 (3) | 0.073 (4) | 0.063 (3) | 0.006 (3) | 0.010 (3) | −0.006 (3) |
C11_1 | 0.072 (4) | 0.078 (4) | 0.128 (5) | 0.000 (3) | 0.040 (4) | −0.017 (4) |
C12_1 | 0.067 (4) | 0.080 (4) | 0.120 (5) | −0.004 (3) | 0.027 (3) | −0.015 (4) |
C13_1 | 0.058 (3) | 0.081 (4) | 0.062 (3) | −0.003 (3) | 0.010 (3) | −0.011 (3) |
C14_1 | 0.057 (3) | 0.073 (4) | 0.060 (3) | 0.006 (3) | 0.007 (2) | −0.011 (3) |
C15_1 | 0.075 (4) | 0.075 (4) | 0.120 (5) | 0.003 (3) | 0.029 (3) | −0.025 (3) |
C16_1 | 0.091 (4) | 0.074 (4) | 0.114 (5) | 0.004 (3) | 0.019 (4) | −0.017 (4) |
C17_1 | 0.063 (3) | 0.079 (4) | 0.093 (4) | 0.005 (3) | 0.003 (3) | −0.016 (3) |
C18_1 | 0.126 (5) | 0.099 (5) | 0.069 (4) | −0.012 (4) | 0.002 (4) | −0.003 (3) |
C19_1 | 0.127 (5) | 0.101 (5) | 0.064 (4) | −0.026 (4) | 0.013 (3) | −0.019 (3) |
C20_1 | 0.091 (5) | 0.075 (4) | 0.161 (7) | −0.002 (4) | 0.038 (4) | −0.002 (4) |
C21_1 | 0.113 (6) | 0.102 (5) | 0.225 (9) | −0.011 (4) | 0.085 (6) | −0.011 (5) |
C22_1 | 0.176 (9) | 0.054 (5) | 0.373 (15) | −0.037 (5) | 0.144 (9) | −0.041 (7) |
C23_1 | 0.225 (14) | 0.178 (12) | 0.50 (3) | −0.016 (11) | 0.066 (15) | −0.121 (15) |
C24_1 | 0.259 (17) | 0.165 (12) | 0.52 (3) | −0.018 (11) | 0.07 (2) | −0.089 (16) |
C25_1 | 0.52 (5) | 0.51 (4) | 0.39 (3) | 0.18 (4) | −0.07 (3) | −0.28 (3) |
C26_1 | 0.37 (3) | 0.24 (2) | 0.77 (6) | 0.01 (2) | −0.04 (3) | −0.06 (3) |
C27_1 | 0.57 (4) | 0.28 (2) | 0.69 (5) | −0.04 (2) | −0.14 (4) | −0.27 (3) |
O03_2 | 0.094 (3) | 0.079 (3) | 0.215 (6) | −0.010 (3) | 0.048 (3) | −0.003 (3) |
C01_2 | 0.054 (3) | 0.085 (4) | 0.109 (5) | 0.006 (3) | 0.003 (3) | −0.016 (4) |
C02_2 | 0.071 (4) | 0.078 (4) | 0.140 (6) | 0.008 (3) | 0.006 (4) | −0.012 (4) |
C03_2 | 0.073 (4) | 0.081 (4) | 0.123 (5) | 0.002 (4) | 0.018 (4) | −0.018 (4) |
C04_2 | 0.063 (4) | 0.095 (5) | 0.111 (5) | 0.003 (3) | 0.009 (3) | −0.014 (4) |
C05_2 | 0.050 (3) | 0.086 (4) | 0.076 (4) | 0.003 (3) | 0.005 (3) | −0.011 (3) |
C06_2 | 0.050 (3) | 0.113 (5) | 0.082 (4) | −0.004 (3) | 0.000 (3) | −0.015 (4) |
C07_2 | 0.046 (3) | 0.134 (5) | 0.065 (4) | 0.008 (3) | −0.008 (3) | −0.005 (3) |
C08_2 | 0.049 (3) | 0.096 (4) | 0.047 (3) | 0.011 (3) | 0.000 (2) | −0.006 (3) |
C09_2 | 0.043 (3) | 0.090 (4) | 0.058 (3) | 0.014 (3) | −0.005 (2) | −0.013 (3) |
C10_2 | 0.050 (3) | 0.081 (4) | 0.066 (4) | 0.007 (3) | −0.009 (2) | −0.012 (3) |
C11_2 | 0.052 (3) | 0.082 (4) | 0.103 (4) | 0.007 (3) | −0.023 (3) | −0.001 (3) |
C12_2 | 0.054 (3) | 0.087 (4) | 0.097 (4) | 0.011 (3) | −0.012 (3) | −0.001 (3) |
C13_2 | 0.061 (3) | 0.082 (4) | 0.056 (3) | 0.015 (3) | −0.002 (3) | −0.005 (3) |
C14_2 | 0.053 (3) | 0.095 (4) | 0.053 (3) | 0.010 (3) | −0.004 (2) | 0.000 (3) |
C15_2 | 0.069 (4) | 0.129 (5) | 0.109 (5) | 0.033 (4) | 0.002 (3) | 0.032 (4) |
C16_2 | 0.077 (4) | 0.125 (5) | 0.114 (5) | 0.015 (4) | 0.002 (4) | 0.042 (4) |
C17_2 | 0.067 (4) | 0.094 (4) | 0.075 (4) | 0.015 (3) | 0.005 (3) | 0.011 (3) |
C18_2 | 0.135 (5) | 0.102 (5) | 0.061 (4) | 0.002 (4) | 0.010 (3) | −0.007 (3) |
C19_2 | 0.102 (4) | 0.109 (5) | 0.064 (4) | 0.014 (4) | −0.004 (3) | −0.009 (3) |
C20_2 | 0.090 (5) | 0.093 (5) | 0.133 (6) | 0.012 (4) | 0.003 (4) | 0.015 (4) |
C21_2 | 0.096 (5) | 0.114 (6) | 0.168 (7) | −0.007 (4) | −0.025 (5) | 0.017 (5) |
C22_2 | 0.138 (7) | 0.126 (8) | 0.286 (13) | −0.039 (6) | −0.050 (7) | 0.094 (8) |
C23_2 | 0.195 (13) | 0.206 (13) | 0.45 (2) | 0.018 (10) | −0.063 (13) | 0.142 (15) |
C24_2 | 0.288 (19) | 0.30 (2) | 0.43 (3) | 0.024 (15) | 0.003 (18) | 0.25 (2) |
C25_2 | 0.32 (3) | 0.33 (4) | 0.17 (3) | 0.19 (3) | −0.01 (2) | 0.04 (2) |
C25'_2 | 0.25 (4) | 0.50 (7) | 0.13 (3) | 0.09 (3) | 0.08 (2) | 0.20 (4) |
C26_2 | 0.321 (18) | 0.247 (15) | 0.286 (18) | 0.020 (13) | 0.002 (14) | 0.099 (13) |
C27_2 | 0.244 (19) | 0.43 (3) | 0.61 (4) | 0.12 (2) | 0.06 (2) | 0.22 (3) |
O03_3 | 0.109 (4) | 0.085 (3) | 0.148 (5) | −0.016 (2) | −0.040 (3) | 0.030 (3) |
C01_3 | 0.105 (4) | 0.082 (4) | 0.067 (4) | −0.001 (3) | −0.013 (3) | 0.004 (3) |
C02_3 | 0.098 (4) | 0.076 (4) | 0.083 (4) | −0.014 (3) | −0.021 (3) | 0.020 (3) |
C03_3 | 0.082 (4) | 0.069 (4) | 0.109 (5) | −0.004 (3) | −0.006 (3) | 0.023 (3) |
C04_3 | 0.091 (4) | 0.082 (4) | 0.080 (4) | −0.012 (3) | −0.020 (3) | 0.006 (3) |
C05_3 | 0.068 (4) | 0.073 (4) | 0.064 (3) | −0.003 (3) | −0.003 (3) | −0.001 (3) |
C06_3 | 0.064 (4) | 0.089 (4) | 0.078 (4) | −0.010 (3) | −0.009 (3) | 0.002 (3) |
C07_3 | 0.060 (3) | 0.087 (4) | 0.068 (4) | 0.002 (3) | −0.001 (3) | 0.011 (3) |
C08_3 | 0.050 (3) | 0.077 (4) | 0.047 (3) | 0.004 (3) | 0.003 (2) | 0.002 (3) |
C09_3 | 0.062 (3) | 0.066 (4) | 0.055 (3) | −0.001 (3) | 0.006 (2) | 0.001 (3) |
C10_3 | 0.060 (3) | 0.074 (4) | 0.055 (3) | 0.000 (3) | 0.001 (2) | 0.000 (3) |
C11_3 | 0.078 (4) | 0.080 (4) | 0.064 (3) | −0.010 (3) | −0.015 (3) | 0.005 (3) |
C12_3 | 0.080 (4) | 0.080 (4) | 0.060 (3) | −0.004 (3) | −0.006 (3) | 0.007 (3) |
C13_3 | 0.052 (3) | 0.070 (4) | 0.055 (3) | −0.001 (3) | 0.009 (2) | 0.003 (3) |
C14_3 | 0.056 (3) | 0.069 (4) | 0.053 (3) | 0.011 (3) | 0.012 (2) | 0.008 (3) |
C15_3 | 0.069 (3) | 0.094 (4) | 0.078 (4) | −0.009 (3) | −0.009 (3) | 0.021 (3) |
C16_3 | 0.097 (4) | 0.092 (5) | 0.098 (5) | −0.003 (4) | −0.009 (4) | 0.026 (4) |
C17_3 | 0.069 (3) | 0.076 (4) | 0.077 (4) | −0.002 (3) | 0.009 (3) | 0.009 (3) |
C18_3 | 0.059 (3) | 0.108 (4) | 0.075 (4) | −0.003 (3) | 0.020 (3) | −0.003 (3) |
C19_3 | 0.070 (4) | 0.094 (4) | 0.104 (5) | 0.009 (3) | 0.008 (3) | −0.007 (3) |
C20_3 | 0.100 (5) | 0.081 (5) | 0.139 (7) | −0.009 (4) | 0.002 (5) | 0.001 (5) |
C21_3 | 0.185 (14) | 0.102 (9) | 0.176 (13) | −0.047 (9) | −0.091 (11) | 0.055 (8) |
C22_3 | 0.187 (14) | 0.070 (8) | 0.113 (10) | −0.022 (9) | −0.026 (9) | 0.029 (7) |
C23_3 | 0.31 (2) | 0.110 (11) | 0.122 (11) | −0.094 (14) | −0.009 (12) | 0.027 (9) |
C21'_3 | 0.23 (3) | 0.14 (2) | 0.099 (17) | −0.10 (2) | 0.032 (17) | −0.028 (15) |
C22'_3 | 0.073 (12) | 0.106 (16) | 0.110 (15) | 0.021 (11) | 0.000 (10) | 0.007 (12) |
C23'_3 | 0.104 (15) | 0.124 (19) | 0.15 (2) | −0.009 (13) | 0.035 (14) | −0.006 (14) |
C24_3 | 0.286 (15) | 0.163 (11) | 0.179 (12) | −0.062 (10) | 0.006 (10) | −0.017 (9) |
C25_3 | 0.39 (3) | 0.249 (16) | 0.28 (2) | −0.172 (18) | 0.061 (18) | 0.025 (16) |
C26_3 | 0.36 (3) | 0.51 (3) | 0.33 (2) | −0.29 (2) | 0.00 (2) | 0.04 (2) |
C27_3 | 0.45 (3) | 0.52 (3) | 0.40 (3) | 0.00 (2) | 0.15 (2) | 0.28 (3) |
O03_4 | 0.114 (3) | 0.082 (3) | 0.143 (4) | −0.017 (3) | −0.029 (3) | 0.037 (3) |
C01_4 | 0.077 (4) | 0.086 (4) | 0.056 (3) | −0.001 (3) | −0.004 (3) | 0.009 (3) |
C02_4 | 0.100 (4) | 0.087 (4) | 0.066 (4) | 0.001 (4) | −0.004 (3) | 0.011 (3) |
C03_4 | 0.089 (4) | 0.078 (5) | 0.107 (5) | −0.001 (4) | −0.026 (4) | 0.020 (4) |
C04_4 | 0.095 (4) | 0.075 (4) | 0.102 (5) | 0.011 (3) | 0.007 (4) | −0.012 (4) |
C05_4 | 0.069 (4) | 0.068 (4) | 0.073 (4) | 0.010 (3) | −0.006 (3) | −0.008 (3) |
C06_4 | 0.072 (4) | 0.093 (5) | 0.084 (4) | 0.019 (3) | 0.004 (3) | −0.013 (3) |
C07_4 | 0.057 (3) | 0.095 (4) | 0.065 (3) | 0.015 (3) | 0.004 (3) | −0.007 (3) |
C08_4 | 0.049 (3) | 0.082 (4) | 0.044 (3) | 0.008 (3) | 0.000 (2) | 0.000 (3) |
C09_4 | 0.055 (3) | 0.068 (3) | 0.047 (3) | 0.012 (3) | −0.003 (2) | −0.003 (2) |
C10_4 | 0.053 (3) | 0.075 (4) | 0.052 (3) | 0.006 (3) | −0.005 (2) | 0.000 (3) |
C11_4 | 0.066 (3) | 0.070 (4) | 0.059 (3) | 0.006 (3) | 0.010 (3) | −0.003 (3) |
C12_4 | 0.074 (3) | 0.077 (4) | 0.055 (3) | 0.006 (3) | 0.004 (3) | 0.001 (3) |
C13_4 | 0.050 (3) | 0.081 (4) | 0.053 (3) | 0.005 (3) | −0.003 (2) | 0.005 (3) |
C14_4 | 0.051 (3) | 0.088 (4) | 0.045 (3) | 0.006 (3) | 0.000 (2) | 0.001 (3) |
C15_4 | 0.061 (3) | 0.107 (5) | 0.068 (4) | 0.013 (3) | 0.014 (3) | 0.012 (3) |
C16_4 | 0.079 (4) | 0.116 (5) | 0.082 (4) | −0.018 (4) | 0.020 (3) | 0.009 (4) |
C17_4 | 0.061 (3) | 0.084 (4) | 0.075 (4) | −0.004 (3) | −0.002 (3) | 0.013 (3) |
C18_4 | 0.062 (3) | 0.105 (4) | 0.067 (4) | 0.005 (3) | −0.008 (3) | 0.011 (3) |
C19_4 | 0.053 (3) | 0.095 (4) | 0.085 (4) | 0.003 (3) | −0.014 (3) | 0.000 (3) |
C20_4 | 0.102 (5) | 0.081 (5) | 0.128 (6) | −0.012 (4) | 0.011 (4) | 0.020 (4) |
C21_4 | 0.212 (9) | 0.088 (6) | 0.247 (11) | 0.024 (6) | 0.112 (9) | 0.011 (6) |
C22_4 | 0.203 (10) | 0.077 (6) | 0.248 (11) | −0.020 (6) | 0.048 (8) | 0.024 (6) |
C23_4 | 0.232 (13) | 0.168 (10) | 0.370 (19) | −0.072 (10) | 0.095 (13) | 0.068 (11) |
C24_4 | 0.31 (3) | 0.36 (3) | 0.75 (5) | −0.14 (2) | 0.04 (3) | 0.11 (3) |
C25_4 | 0.202 (14) | 0.239 (16) | 0.37 (2) | −0.051 (13) | 0.029 (15) | 0.005 (14) |
C27_4 | 0.34 (2) | 0.34 (3) | 0.92 (7) | −0.08 (2) | 0.29 (3) | 0.20 (3) |
C26_4 | 0.63 (6) | 0.53 (5) | 0.63 (6) | 0.03 (4) | 0.12 (4) | −0.26 (4) |
O_5 | 0.088 (3) | 0.119 (4) | 0.130 (4) | −0.023 (3) | 0.008 (3) | −0.013 (3) |
C_5 | 0.149 (8) | 0.205 (10) | 0.147 (8) | −0.001 (7) | −0.032 (6) | 0.000 (7) |
O_6 | 0.115 (4) | 0.191 (5) | 0.146 (5) | −0.036 (4) | 0.015 (4) | 0.024 (4) |
C_6 | 0.190 (10) | 0.246 (12) | 0.142 (9) | −0.060 (8) | −0.010 (7) | −0.002 (9) |
O03_1—C03_1 | 1.442 (6) | C01_3—C10_3 | 1.548 (7) |
C01_1—C02_1 | 1.517 (7) | C02_3—C03_3 | 1.506 (7) |
C01_1—C10_1 | 1.519 (7) | C03_3—C04_3 | 1.521 (7) |
C02_1—C03_1 | 1.494 (8) | C04_3—C05_3 | 1.511 (7) |
C03_1—C04_1 | 1.491 (7) | C05_3—C06_3 | 1.321 (7) |
C04_1—C05_1 | 1.506 (7) | C05_3—C10_3 | 1.523 (7) |
C05_1—C06_1 | 1.306 (6) | C06_3—C07_3 | 1.490 (7) |
C05_1—C10_1 | 1.531 (7) | C07_3—C08_3 | 1.535 (6) |
C06_1—C07_1 | 1.500 (7) | C08_3—C14_3 | 1.485 (6) |
C07_1—C08_1 | 1.517 (6) | C08_3—C09_3 | 1.549 (6) |
C08_1—C14_1 | 1.506 (6) | C09_3—C11_3 | 1.529 (6) |
C08_1—C09_1 | 1.522 (6) | C09_3—C10_3 | 1.542 (6) |
C09_1—C11_1 | 1.536 (6) | C10_3—C19_3 | 1.541 (7) |
C09_1—C10_1 | 1.552 (6) | C11_3—C12_3 | 1.518 (7) |
C10_1—C19_1 | 1.568 (7) | C12_3—C13_3 | 1.511 (6) |
C11_1—C12_1 | 1.520 (7) | C13_3—C17_3 | 1.539 (7) |
C12_1—C13_1 | 1.515 (7) | C13_3—C14_3 | 1.540 (6) |
C13_1—C14_1 | 1.529 (7) | C13_3—C18_3 | 1.546 (6) |
C13_1—C17_1 | 1.539 (7) | C14_3—C15_3 | 1.531 (6) |
C13_1—C18_1 | 1.548 (7) | C15_3—C16_3 | 1.552 (7) |
C14_1—C15_1 | 1.526 (6) | C16_3—C17_3 | 1.549 (7) |
C15_1—C16_1 | 1.561 (7) | C17_3—C20_3 | 1.528 (7) |
C16_1—C17_1 | 1.550 (7) | C20_3—C22'_3 | 1.331 (13) |
C17_1—C20_1 | 1.536 (8) | C20_3—C21_3 | 1.403 (11) |
C20_1—C21_1 | 1.531 (8) | C20_3—C22_3 | 1.538 (10) |
C20_1—C22_1 | 1.565 (10) | C20_3—C21'_3 | 1.661 (15) |
C22_1—C23_1 | 1.302 (12) | C22_3—C23_3 | 1.502 (12) |
C23_1—C24_1 | 1.540 (12) | C23_3—C24_3 | 1.547 (14) |
C24_1—C25_1 | 1.395 (18) | C22'_3—C23'_3 | 1.578 (16) |
C25_1—C26_1 | 1.55 (2) | C23'_3—C24_3 | 1.449 (16) |
C25_1—C27_1 | 1.600 (17) | C24_3—C25_3 | 1.465 (12) |
O03_2—C03_2 | 1.398 (7) | C25_3—C26_3 | 1.396 (15) |
C01_2—C02_2 | 1.513 (7) | C25_3—C27_3 | 1.443 (14) |
C01_2—C10_2 | 1.528 (6) | O03_4—C03_4 | 1.429 (6) |
C02_2—C03_2 | 1.535 (8) | C01_4—C02_4 | 1.516 (7) |
C03_2—C04_2 | 1.505 (7) | C01_4—C10_4 | 1.542 (6) |
C04_2—C05_2 | 1.497 (7) | C02_4—C03_4 | 1.502 (7) |
C05_2—C06_2 | 1.326 (7) | C03_4—C04_4 | 1.515 (8) |
C05_2—C10_2 | 1.528 (7) | C04_4—C05_4 | 1.526 (7) |
C06_2—C07_2 | 1.496 (7) | C05_4—C06_4 | 1.309 (7) |
C07_2—C08_2 | 1.523 (7) | C05_4—C10_4 | 1.510 (7) |
C08_2—C14_2 | 1.507 (7) | C06_4—C07_4 | 1.513 (8) |
C08_2—C09_2 | 1.526 (6) | C07_4—C08_4 | 1.515 (6) |
C09_2—C11_2 | 1.542 (6) | C08_4—C14_4 | 1.479 (6) |
C09_2—C10_2 | 1.565 (7) | C08_4—C09_4 | 1.548 (6) |
C10_2—C19_2 | 1.537 (7) | C09_4—C11_4 | 1.533 (6) |
C11_2—C12_2 | 1.539 (7) | C09_4—C10_4 | 1.540 (6) |
C12_2—C13_2 | 1.524 (7) | C10_4—C19_4 | 1.547 (6) |
C13_2—C14_2 | 1.535 (7) | C11_4—C12_4 | 1.531 (6) |
C13_2—C18_2 | 1.537 (7) | C12_4—C13_4 | 1.542 (6) |
C13_2—C17_2 | 1.541 (7) | C13_4—C18_4 | 1.537 (6) |
C14_2—C15_2 | 1.533 (7) | C13_4—C14_4 | 1.539 (6) |
C15_2—C16_2 | 1.534 (8) | C13_4—C17_4 | 1.547 (7) |
C16_2—C17_2 | 1.564 (7) | C14_4—C15_4 | 1.525 (7) |
C17_2—C20_2 | 1.522 (8) | C15_4—C16_4 | 1.527 (7) |
C20_2—C21_2 | 1.526 (8) | C16_4—C17_4 | 1.562 (7) |
C20_2—C22_2 | 1.596 (10) | C17_4—C20_4 | 1.513 (7) |
C22_2—C23_2 | 1.386 (11) | C20_4—C21_4 | 1.475 (10) |
C23_2—C24_2 | 1.531 (12) | C20_4—C22_4 | 1.543 (9) |
C24_2—C25_2 | 1.365 (17) | C22_4—C23_4 | 1.451 (10) |
C24_2—C25'_2 | 1.394 (18) | C23_4—C24_4 | 1.620 (15) |
C25_2—C27_2 | 1.502 (19) | C24_4—C25_4 | 1.312 (16) |
C25_2—C26_2 | 1.582 (18) | C25_4—C26_4 | 1.516 (17) |
C25'_2—C27_2 | 1.52 (2) | C25_4—C27_4 | 1.540 (14) |
C25'_2—C26_2 | 1.574 (19) | O_5—C_5 | 1.406 (8) |
O03_3—C03_3 | 1.431 (6) | O_6—C_6 | 1.346 (9) |
C01_3—C02_3 | 1.523 (7) | ||
C02_1—C01_1—C10_1 | 115.1 (5) | O03_3—C03_3—C02_3 | 108.2 (4) |
C03_1—C02_1—C01_1 | 110.2 (5) | O03_3—C03_3—C04_3 | 111.5 (5) |
O03_1—C03_1—C04_1 | 111.1 (5) | C02_3—C03_3—C04_3 | 110.4 (5) |
O03_1—C03_1—C02_1 | 107.4 (5) | C05_3—C04_3—C03_3 | 112.6 (5) |
C04_1—C03_1—C02_1 | 110.9 (5) | C06_3—C05_3—C04_3 | 122.1 (5) |
C03_1—C04_1—C05_1 | 112.1 (5) | C06_3—C05_3—C10_3 | 121.7 (5) |
C06_1—C05_1—C04_1 | 121.1 (5) | C04_3—C05_3—C10_3 | 116.1 (5) |
C06_1—C05_1—C10_1 | 123.2 (5) | C05_3—C06_3—C07_3 | 126.9 (5) |
C04_1—C05_1—C10_1 | 115.7 (5) | C06_3—C07_3—C08_3 | 112.6 (4) |
C05_1—C06_1—C07_1 | 125.2 (5) | C14_3—C08_3—C07_3 | 111.9 (4) |
C06_1—C07_1—C08_1 | 113.2 (4) | C14_3—C08_3—C09_3 | 110.1 (4) |
C14_1—C08_1—C07_1 | 110.9 (4) | C07_3—C08_3—C09_3 | 109.1 (4) |
C14_1—C08_1—C09_1 | 110.5 (4) | C11_3—C09_3—C10_3 | 114.2 (4) |
C07_1—C08_1—C09_1 | 110.1 (4) | C11_3—C09_3—C08_3 | 111.8 (4) |
C08_1—C09_1—C11_1 | 111.1 (4) | C10_3—C09_3—C08_3 | 113.1 (4) |
C08_1—C09_1—C10_1 | 114.1 (4) | C05_3—C10_3—C19_3 | 108.6 (4) |
C11_1—C09_1—C10_1 | 113.9 (4) | C05_3—C10_3—C09_3 | 110.4 (4) |
C01_1—C10_1—C05_1 | 107.9 (4) | C19_3—C10_3—C09_3 | 112.0 (4) |
C01_1—C10_1—C09_1 | 109.9 (4) | C05_3—C10_3—C01_3 | 108.0 (4) |
C05_1—C10_1—C09_1 | 110.1 (4) | C19_3—C10_3—C01_3 | 109.4 (4) |
C01_1—C10_1—C19_1 | 110.7 (4) | C09_3—C10_3—C01_3 | 108.4 (4) |
C05_1—C10_1—C19_1 | 107.5 (4) | C12_3—C11_3—C09_3 | 115.9 (4) |
C09_1—C10_1—C19_1 | 110.6 (4) | C13_3—C12_3—C11_3 | 111.9 (4) |
C12_1—C11_1—C09_1 | 113.8 (4) | C12_3—C13_3—C17_3 | 116.4 (4) |
C13_1—C12_1—C11_1 | 112.8 (4) | C12_3—C13_3—C14_3 | 106.9 (4) |
C12_1—C13_1—C14_1 | 105.7 (4) | C17_3—C13_3—C14_3 | 101.0 (4) |
C12_1—C13_1—C17_1 | 117.4 (4) | C12_3—C13_3—C18_3 | 110.2 (4) |
C14_1—C13_1—C17_1 | 100.8 (4) | C17_3—C13_3—C18_3 | 109.9 (4) |
C12_1—C13_1—C18_1 | 111.4 (5) | C14_3—C13_3—C18_3 | 112.1 (4) |
C14_1—C13_1—C18_1 | 111.8 (4) | C08_3—C14_3—C15_3 | 119.6 (4) |
C17_1—C13_1—C18_1 | 109.2 (5) | C08_3—C14_3—C13_3 | 115.5 (4) |
C08_1—C14_1—C15_1 | 118.9 (4) | C15_3—C14_3—C13_3 | 104.3 (4) |
C08_1—C14_1—C13_1 | 115.8 (4) | C14_3—C15_3—C16_3 | 105.1 (4) |
C15_1—C14_1—C13_1 | 104.5 (4) | C17_3—C16_3—C15_3 | 106.0 (4) |
C14_1—C15_1—C16_1 | 103.7 (4) | C20_3—C17_3—C13_3 | 120.0 (4) |
C17_1—C16_1—C15_1 | 106.0 (4) | C20_3—C17_3—C16_3 | 115.6 (5) |
C20_1—C17_1—C13_1 | 121.2 (5) | C13_3—C17_3—C16_3 | 103.2 (4) |
C20_1—C17_1—C16_1 | 110.4 (5) | C22'_3—C20_3—C21_3 | 117.8 (10) |
C13_1—C17_1—C16_1 | 104.6 (4) | C22'_3—C20_3—C17_3 | 123.4 (9) |
C21_1—C20_1—C17_1 | 111.8 (5) | C21_3—C20_3—C17_3 | 116.8 (7) |
C21_1—C20_1—C22_1 | 108.1 (6) | C21_3—C20_3—C22_3 | 115.3 (8) |
C17_1—C20_1—C22_1 | 108.0 (6) | C17_3—C20_3—C22_3 | 114.0 (6) |
C23_1—C22_1—C20_1 | 119.4 (10) | C22'_3—C20_3—C21'_3 | 112.5 (10) |
C22_1—C23_1—C24_1 | 123.3 (13) | C17_3—C20_3—C21'_3 | 103.8 (8) |
C25_1—C24_1—C23_1 | 117.6 (15) | C23_3—C22_3—C20_3 | 117.0 (10) |
C24_1—C25_1—C26_1 | 92 (2) | C22_3—C23_3—C24_3 | 117.7 (11) |
C24_1—C25_1—C27_1 | 107.7 (17) | C20_3—C22'_3—C23'_3 | 114.9 (12) |
C26_1—C25_1—C27_1 | 107.6 (17) | C24_3—C23'_3—C22'_3 | 98.2 (12) |
C02_2—C01_2—C10_2 | 115.2 (5) | C23'_3—C24_3—C25_3 | 116.7 (12) |
C01_2—C02_2—C03_2 | 110.0 (5) | C25_3—C24_3—C23_3 | 120.3 (11) |
O03_2—C03_2—C04_2 | 109.1 (5) | C26_3—C25_3—C27_3 | 119.4 (15) |
O03_2—C03_2—C02_2 | 111.9 (6) | C26_3—C25_3—C24_3 | 117.2 (13) |
C04_2—C03_2—C02_2 | 109.5 (5) | C27_3—C25_3—C24_3 | 115.5 (14) |
C05_2—C04_2—C03_2 | 113.3 (5) | C02_4—C01_4—C10_4 | 115.3 (4) |
C06_2—C05_2—C04_2 | 121.4 (5) | C03_4—C02_4—C01_4 | 111.5 (5) |
C06_2—C05_2—C10_2 | 122.6 (5) | O03_4—C03_4—C02_4 | 111.3 (5) |
C04_2—C05_2—C10_2 | 116.0 (5) | O03_4—C03_4—C04_4 | 109.5 (5) |
C05_2—C06_2—C07_2 | 125.3 (5) | C02_4—C03_4—C04_4 | 109.8 (4) |
C06_2—C07_2—C08_2 | 113.0 (4) | C03_4—C04_4—C05_4 | 112.5 (5) |
C14_2—C08_2—C07_2 | 111.3 (4) | C06_4—C05_4—C10_4 | 125.1 (5) |
C14_2—C08_2—C09_2 | 110.4 (4) | C06_4—C05_4—C04_4 | 119.0 (5) |
C07_2—C08_2—C09_2 | 109.2 (4) | C10_4—C05_4—C04_4 | 115.9 (5) |
C08_2—C09_2—C11_2 | 112.0 (4) | C05_4—C06_4—C07_4 | 123.3 (5) |
C08_2—C09_2—C10_2 | 112.9 (4) | C06_4—C07_4—C08_4 | 113.7 (4) |
C11_2—C09_2—C10_2 | 112.5 (4) | C14_4—C08_4—C07_4 | 111.3 (4) |
C01_2—C10_2—C05_2 | 106.9 (4) | C14_4—C08_4—C09_4 | 110.0 (4) |
C01_2—C10_2—C19_2 | 110.7 (4) | C07_4—C08_4—C09_4 | 110.0 (4) |
C05_2—C10_2—C19_2 | 108.2 (4) | C11_4—C09_4—C10_4 | 114.4 (4) |
C01_2—C10_2—C09_2 | 109.5 (4) | C11_4—C09_4—C08_4 | 111.0 (4) |
C05_2—C10_2—C09_2 | 109.8 (4) | C10_4—C09_4—C08_4 | 113.3 (4) |
C19_2—C10_2—C09_2 | 111.5 (4) | C05_4—C10_4—C09_4 | 110.2 (4) |
C12_2—C11_2—C09_2 | 113.9 (4) | C05_4—C10_4—C01_4 | 108.7 (4) |
C13_2—C12_2—C11_2 | 111.9 (4) | C09_4—C10_4—C01_4 | 109.1 (4) |
C12_2—C13_2—C14_2 | 105.9 (4) | C05_4—C10_4—C19_4 | 108.8 (4) |
C12_2—C13_2—C18_2 | 111.0 (4) | C09_4—C10_4—C19_4 | 111.5 (4) |
C14_2—C13_2—C18_2 | 111.4 (4) | C01_4—C10_4—C19_4 | 108.6 (4) |
C12_2—C13_2—C17_2 | 116.5 (4) | C12_4—C11_4—C09_4 | 115.0 (4) |
C14_2—C13_2—C17_2 | 100.6 (4) | C11_4—C12_4—C13_4 | 111.6 (4) |
C18_2—C13_2—C17_2 | 110.8 (5) | C18_4—C13_4—C14_4 | 113.0 (4) |
C08_2—C14_2—C15_2 | 119.1 (4) | C18_4—C13_4—C12_4 | 109.4 (4) |
C08_2—C14_2—C13_2 | 115.5 (4) | C14_4—C13_4—C12_4 | 105.9 (4) |
C15_2—C14_2—C13_2 | 104.2 (5) | C18_4—C13_4—C17_4 | 110.0 (4) |
C14_2—C15_2—C16_2 | 104.4 (4) | C14_4—C13_4—C17_4 | 101.4 (4) |
C15_2—C16_2—C17_2 | 106.3 (5) | C12_4—C13_4—C17_4 | 116.9 (4) |
C20_2—C17_2—C13_2 | 120.1 (5) | C08_4—C14_4—C15_4 | 119.0 (4) |
C20_2—C17_2—C16_2 | 112.1 (5) | C08_4—C14_4—C13_4 | 117.1 (4) |
C13_2—C17_2—C16_2 | 104.3 (4) | C15_4—C14_4—C13_4 | 103.3 (4) |
C17_2—C20_2—C21_2 | 114.5 (5) | C14_4—C15_4—C16_4 | 105.1 (4) |
C17_2—C20_2—C22_2 | 106.4 (6) | C15_4—C16_4—C17_4 | 106.9 (4) |
C21_2—C20_2—C22_2 | 109.1 (6) | C20_4—C17_4—C13_4 | 121.7 (4) |
C23_2—C22_2—C20_2 | 115.2 (10) | C20_4—C17_4—C16_4 | 112.6 (5) |
C22_2—C23_2—C24_2 | 117.5 (12) | C13_4—C17_4—C16_4 | 102.6 (4) |
C25_2—C24_2—C23_2 | 120.8 (14) | C21_4—C20_4—C17_4 | 112.2 (6) |
C25'_2—C24_2—C23_2 | 122.0 (13) | C21_4—C20_4—C22_4 | 109.5 (7) |
C24_2—C25_2—C27_2 | 116.3 (18) | C17_4—C20_4—C22_4 | 110.9 (6) |
C24_2—C25_2—C26_2 | 101.8 (15) | C23_4—C22_4—C20_4 | 114.4 (8) |
C27_2—C25_2—C26_2 | 105.5 (16) | C22_4—C23_4—C24_4 | 114.2 (12) |
C24_2—C25'_2—C27_2 | 113.4 (19) | C25_4—C24_4—C23_4 | 114.8 (16) |
C24_2—C25'_2—C26_2 | 100.9 (16) | C24_4—C25_4—C26_4 | 100 (2) |
C27_2—C25'_2—C26_2 | 105.0 (15) | C24_4—C25_4—C27_4 | 117.5 (16) |
C02_3—C01_3—C10_3 | 114.3 (4) | C26_4—C25_4—C27_4 | 102.5 (13) |
C03_3—C02_3—C01_3 | 110.6 (5) |
Experimental details
Crystal data | |
Chemical formula | C27H46O·0.5CH4O |
Mr | 402.66 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 12.2735 (17), 34.237 (7), 6.2739 (8) |
α, β, γ (°) | 90.224 (14), 93.705 (10), 91.576 (14) |
V (Å3) | 2629.8 (7) |
Z | 4 |
Radiation type | Cu Kα |
µ (mm−1) | 0.45 |
Crystal size (mm) | 0.50 × 0.30 × 0.10 |
Data collection | |
Diffractometer | Syntex P1 diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7176, 7176, 5452 |
Rint | 0.000 |
θmax (°) | 57.4 |
(sin θ/λ)max (Å−1) | 0.546 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.102, 2.09 |
No. of reflections | 6750 |
No. of parameters | 1097 |
No. of restraints | 393 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.17, −0.15 |
Computer programs: Syntex P1 Software (Sparks, 1970), Syntex P1 Software, SYNOUT (Sparks, 1970), Patterson search (Schilling, 1970) and MULTAN (Germain et al., 1971), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 1994), SHELXL97.
The unit cell of cholesterol hemimethanol solvate, (I), has been reported by Klötzer (1936), a preliminary report by us (Hsieh & Nordman, 1978) gave the unit cell and space group. In this paper, the refined structure is presented. All reported structures of cholesterol and its solvates have asymmetric units containing multiple cholesterol molecules. Room-temperature cholesterol has eight (Shieh et al., 1981), its high-temperature form 16 (Hsu & Nordman, 1983; Hsu et al., 2002), cholesterol hydrate eight (Craven, 1979), and monoclinic and triclinic cholesterol hemiethanolate each eight (Shieh et al., 1982). With only four cholesterol molecules in the asymmetric unit, the present sructure is the simplest of the group. Furthermore, cholesterol hemimethanol solvate lacks any obvious pseudosymmetry, as distinct from the aforementioned structures, which exhibit several forms of pseudosymmetry. The hydrogen-bonded chain.. C1—C2—M1—C3—C4—M2—C1-.. is similar to the cholesterol–ethanol chains found in both forms of cholesterol hemiethanolate. The structure differs from other cholesterol structures in the relative orientation of adjacent molecules; the mean planes of the steroid groups of molecules hydrogen bonded to each other are very nearly parallel, while the planes of laterally adjacent molecules are approximately perpendicular to one another. The cholesterol molecule, in all its crystal forms, shows extreme thermal motion or disorder in the hydrocarbon tails. In the hemimethanolate there is clear disorder in the tails of molecules 2 and 3.