Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803020610/ac6061sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803020610/ac6061Isup2.hkl |
CCDC reference: 225782
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.003 Å
- R factor = 0.034
- wR factor = 0.094
- Data-to-parameter ratio = 10.0
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT412_ALERT_2_C Short Intra XH3 .. XHn H14A .. H15B = 1.84 Ang. PLAT412_ALERT_2_C Short Intra XH3 .. XHn H37A .. H60C = 1.89 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 28.38 From the CIF: _reflns_number_total 6036 Count of symmetry unique reflns 6140 Completeness (_total/calc) 98.31% 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
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT and XPREP (Siemens, 1995); program(s) used to solve structure: SIR97 (Altomare et al., 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and WinGX32 (Farrugia, 1999); software used to prepare material for publication: enCIFer (CCDC, 2003).
C30H30O3 | Dx = 1.213 Mg m−3 |
Mr = 438.54 | Melting point: 441 K |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 9826 reflections |
a = 16.103 (3) Å | θ = 2.3–28.2° |
b = 10.8827 (19) Å | µ = 0.08 mm−1 |
c = 27.396 (5) Å | T = 150 K |
V = 4801.1 (15) Å3 | Multi-faced, colourless |
Z = 8 | 0.41 × 0.30 × 0.25 mm |
F(000) = 1872 |
Siemens SMART 1000 CCD diffractometer | 6036 independent reflections |
Radiation source: sealed tube | 5477 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
ω scans | θmax = 28.4°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1999) | h = −21→21 |
Tmin = 0.901, Tmax = 0.980 | k = −14→14 |
46026 measured reflections | l = −36→36 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0549P)2 + 0.8154P] where P = (Fo2 + 2Fc2)/3 |
6036 reflections | (Δ/σ)max = 0.001 |
601 parameters | Δρmax = 0.24 e Å−3 |
1 restraint | Δρmin = −0.19 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the torsion angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.08567 (11) | 0.16262 (15) | 0.53058 (7) | 0.0230 (3) | |
C2 | 0.13810 (11) | 0.12215 (16) | 0.49297 (7) | 0.0247 (4) | |
C3 | 0.10365 (11) | 0.08017 (16) | 0.44922 (7) | 0.0237 (4) | |
C4 | 0.01746 (11) | 0.06959 (16) | 0.44408 (7) | 0.0237 (4) | |
C5 | −0.03460 (11) | 0.11028 (16) | 0.48195 (7) | 0.0231 (4) | |
C6 | −0.00099 (11) | 0.16111 (16) | 0.52486 (7) | 0.0231 (3) | |
C7 | 0.12463 (12) | 0.20614 (17) | 0.57766 (7) | 0.0273 (4) | |
H7A | 0.0829 | 0.2055 | 0.6042 | 0.033* | |
H7B | 0.1709 | 0.1511 | 0.5870 | 0.033* | |
C8 | 0.20959 (12) | 0.37456 (17) | 0.60412 (7) | 0.0256 (4) | |
C9 | 0.23395 (13) | 0.31191 (18) | 0.64613 (7) | 0.0287 (4) | |
H9 | 0.2117 | 0.2331 | 0.6533 | 0.034* | |
C10 | 0.29142 (13) | 0.3665 (2) | 0.67747 (8) | 0.0327 (4) | |
H10 | 0.3090 | 0.3240 | 0.7059 | 0.039* | |
C11 | 0.32299 (13) | 0.48202 (19) | 0.66753 (9) | 0.0328 (4) | |
H11 | 0.3625 | 0.5183 | 0.6889 | 0.039* | |
C12 | 0.29670 (13) | 0.54464 (19) | 0.62628 (8) | 0.0327 (4) | |
H12 | 0.3175 | 0.6247 | 0.6198 | 0.039* | |
C13 | 0.24050 (13) | 0.49180 (18) | 0.59452 (8) | 0.0293 (4) | |
H13 | 0.2229 | 0.5351 | 0.5662 | 0.035* | |
C14 | 0.23115 (12) | 0.12228 (19) | 0.50043 (9) | 0.0329 (4) | |
H14A | 0.2587 | 0.0996 | 0.4698 | 0.049* | |
H14B | 0.2458 | 0.0628 | 0.5259 | 0.049* | |
H14C | 0.2493 | 0.2045 | 0.5104 | 0.049* | |
C15 | 0.15924 (13) | 0.04335 (17) | 0.40746 (8) | 0.0288 (4) | |
H15A | 0.1317 | 0.0610 | 0.3759 | 0.035* | |
H15B | 0.2120 | 0.0898 | 0.4088 | 0.035* | |
C16 | 0.22543 (11) | −0.14066 (18) | 0.37773 (7) | 0.0250 (4) | |
C17 | 0.26544 (12) | −0.07813 (19) | 0.34035 (8) | 0.0291 (4) | |
H17 | 0.2598 | 0.0084 | 0.3373 | 0.035* | |
C18 | 0.31395 (14) | −0.1443 (2) | 0.30743 (8) | 0.0370 (5) | |
H18 | 0.3414 | −0.1025 | 0.2816 | 0.044* | |
C19 | 0.32254 (15) | −0.2704 (2) | 0.31201 (10) | 0.0394 (5) | |
H19 | 0.3561 | −0.3146 | 0.2895 | 0.047* | |
C20 | 0.28221 (14) | −0.3320 (2) | 0.34935 (9) | 0.0359 (5) | |
H20 | 0.2877 | −0.4186 | 0.3522 | 0.043* | |
C21 | 0.23389 (13) | −0.26767 (18) | 0.38251 (8) | 0.0297 (4) | |
H21 | 0.2067 | −0.3098 | 0.4083 | 0.036* | |
C22 | −0.01893 (13) | 0.0150 (2) | 0.39809 (8) | 0.0336 (4) | |
H22A | 0.0177 | −0.0501 | 0.3860 | 0.050* | |
H22B | −0.0243 | 0.0793 | 0.3732 | 0.050* | |
H22C | −0.0738 | −0.0195 | 0.4053 | 0.050* | |
C23 | −0.12694 (11) | 0.10070 (18) | 0.47452 (8) | 0.0272 (4) | |
H23A | −0.1427 | 0.0152 | 0.4664 | 0.033* | |
H23B | −0.1568 | 0.1257 | 0.5045 | 0.033* | |
C24 | −0.21806 (11) | 0.15833 (17) | 0.40872 (7) | 0.0255 (4) | |
C25 | −0.21837 (13) | 0.20070 (19) | 0.36070 (8) | 0.0306 (4) | |
H25 | −0.1712 | 0.2419 | 0.3479 | 0.037* | |
C26 | −0.28781 (15) | 0.1825 (2) | 0.33182 (8) | 0.0381 (5) | |
H26 | −0.2882 | 0.2117 | 0.2992 | 0.046* | |
C27 | −0.35657 (14) | 0.1221 (2) | 0.35008 (9) | 0.0405 (5) | |
H27 | −0.4038 | 0.1087 | 0.3300 | 0.049* | |
C28 | −0.35602 (13) | 0.0814 (2) | 0.39801 (9) | 0.0391 (5) | |
H28 | −0.4035 | 0.0406 | 0.4107 | 0.047* | |
C29 | −0.28719 (13) | 0.09914 (19) | 0.42772 (8) | 0.0312 (4) | |
H29 | −0.2874 | 0.0712 | 0.4606 | 0.037* | |
C30 | −0.05678 (13) | 0.2138 (2) | 0.56444 (8) | 0.0315 (4) | |
H30A | −0.0270 | 0.2788 | 0.5820 | 0.047* | |
H30B | −0.0722 | 0.1485 | 0.5873 | 0.047* | |
H30C | −0.1070 | 0.2481 | 0.5495 | 0.047* | |
O1 | 0.15501 (10) | 0.32905 (12) | 0.57001 (6) | 0.0328 (3) | |
O2 | 0.17507 (9) | −0.08620 (12) | 0.41203 (5) | 0.0310 (3) | |
O3 | −0.14717 (8) | 0.18239 (12) | 0.43453 (5) | 0.0280 (3) | |
C31 | 0.16352 (12) | 0.84869 (16) | 0.56832 (7) | 0.0248 (4) | |
C32 | 0.25055 (11) | 0.84839 (16) | 0.57408 (7) | 0.0246 (4) | |
C33 | 0.28438 (12) | 0.89881 (17) | 0.61704 (7) | 0.0250 (4) | |
C34 | 0.23280 (12) | 0.94274 (16) | 0.65454 (7) | 0.0249 (4) | |
C35 | 0.14648 (12) | 0.93450 (16) | 0.64933 (7) | 0.0248 (4) | |
C36 | 0.11150 (11) | 0.89024 (16) | 0.60568 (7) | 0.0248 (4) | |
C37 | 0.12452 (13) | 0.80588 (17) | 0.52138 (8) | 0.0290 (4) | |
H37A | 0.0775 | 0.8601 | 0.5126 | 0.035* | |
H37B | 0.1658 | 0.8086 | 0.4946 | 0.035* | |
C38 | 0.04205 (12) | 0.63497 (17) | 0.49417 (7) | 0.0266 (4) | |
C39 | 0.01648 (13) | 0.69742 (19) | 0.45254 (8) | 0.0310 (4) | |
H39 | 0.0375 | 0.7770 | 0.4455 | 0.037* | |
C40 | −0.04039 (14) | 0.6418 (2) | 0.42121 (8) | 0.0353 (5) | |
H40 | −0.0589 | 0.6846 | 0.3930 | 0.042* | |
C41 | −0.07018 (13) | 0.5252 (2) | 0.43064 (9) | 0.0357 (5) | |
H41 | −0.1092 | 0.4883 | 0.4092 | 0.043* | |
C42 | −0.04290 (13) | 0.46233 (19) | 0.47160 (9) | 0.0347 (5) | |
H42 | −0.0624 | 0.3815 | 0.4778 | 0.042* | |
C43 | 0.01278 (13) | 0.51687 (18) | 0.50360 (8) | 0.0305 (4) | |
H43 | 0.0309 | 0.4738 | 0.5318 | 0.037* | |
C44 | 0.30586 (14) | 0.7943 (2) | 0.53498 (8) | 0.0330 (4) | |
H44A | 0.3254 | 0.8600 | 0.5134 | 0.050* | |
H44B | 0.2744 | 0.7340 | 0.5159 | 0.050* | |
H44C | 0.3536 | 0.7539 | 0.5503 | 0.050* | |
C45 | 0.37721 (12) | 0.90291 (18) | 0.62502 (8) | 0.0290 (4) | |
H45A | 0.4070 | 0.8783 | 0.5949 | 0.035* | |
H45B | 0.3950 | 0.9869 | 0.6341 | 0.035* | |
C46 | 0.46800 (12) | 0.83051 (17) | 0.68860 (8) | 0.0258 (4) | |
C47 | 0.53837 (12) | 0.88547 (19) | 0.66937 (8) | 0.0308 (4) | |
H47 | 0.5379 | 0.9187 | 0.6373 | 0.037* | |
C48 | 0.60990 (13) | 0.8911 (2) | 0.69802 (9) | 0.0373 (5) | |
H48 | 0.6585 | 0.9286 | 0.6852 | 0.045* | |
C49 | 0.61137 (14) | 0.8431 (2) | 0.74455 (9) | 0.0397 (5) | |
H49 | 0.6606 | 0.8478 | 0.7635 | 0.048* | |
C50 | 0.54088 (14) | 0.7882 (2) | 0.76359 (9) | 0.0372 (5) | |
H50 | 0.5417 | 0.7551 | 0.7957 | 0.045* | |
C51 | 0.46905 (13) | 0.78158 (18) | 0.73564 (8) | 0.0308 (4) | |
H51 | 0.4207 | 0.7437 | 0.7486 | 0.037* | |
C52 | 0.26994 (14) | 0.9984 (2) | 0.70038 (8) | 0.0350 (5) | |
H52A | 0.2823 | 0.9330 | 0.7239 | 0.052* | |
H52B | 0.2303 | 1.0562 | 0.7148 | 0.052* | |
H52C | 0.3213 | 1.0420 | 0.6921 | 0.052* | |
C53 | 0.09099 (13) | 0.97375 (17) | 0.69070 (8) | 0.0292 (4) | |
H53A | 0.0381 | 0.9274 | 0.6897 | 0.035* | |
H53B | 0.1184 | 0.9577 | 0.7224 | 0.035* | |
C54 | 0.02557 (12) | 1.15971 (18) | 0.71888 (7) | 0.0253 (4) | |
C55 | 0.01943 (13) | 1.28724 (19) | 0.71456 (8) | 0.0290 (4) | |
H55 | 0.0479 | 1.3286 | 0.6890 | 0.035* | |
C56 | −0.02808 (14) | 1.3533 (2) | 0.74738 (8) | 0.0345 (4) | |
H56 | −0.0318 | 1.4401 | 0.7445 | 0.041* | |
C57 | −0.07033 (15) | 1.2933 (2) | 0.78457 (9) | 0.0375 (5) | |
H57 | −0.1031 | 1.3385 | 0.8071 | 0.045* | |
C58 | −0.06407 (13) | 1.1677 (2) | 0.78836 (8) | 0.0355 (5) | |
H58 | −0.0933 | 1.1267 | 0.8137 | 0.043* | |
C59 | −0.01617 (12) | 1.09907 (18) | 0.75621 (7) | 0.0286 (4) | |
H59 | −0.0120 | 1.0124 | 0.7596 | 0.034* | |
C60 | 0.01854 (12) | 0.8895 (2) | 0.59861 (9) | 0.0336 (4) | |
H60A | −0.0066 | 0.9542 | 0.6186 | 0.050* | |
H60B | −0.0038 | 0.8095 | 0.6084 | 0.050* | |
H60C | 0.0056 | 0.9044 | 0.5642 | 0.050* | |
O4 | 0.09552 (10) | 0.68150 (12) | 0.52841 (6) | 0.0330 (3) | |
O5 | 0.39445 (8) | 0.81785 (12) | 0.66404 (6) | 0.0295 (3) | |
O6 | 0.07544 (9) | 1.10330 (12) | 0.68500 (5) | 0.0307 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0274 (9) | 0.0190 (8) | 0.0226 (9) | −0.0021 (6) | −0.0022 (7) | 0.0041 (7) |
C2 | 0.0228 (8) | 0.0207 (8) | 0.0307 (10) | −0.0016 (6) | −0.0017 (7) | 0.0054 (7) |
C3 | 0.0249 (9) | 0.0192 (8) | 0.0271 (9) | 0.0018 (6) | 0.0030 (7) | 0.0032 (7) |
C4 | 0.0268 (9) | 0.0196 (8) | 0.0247 (9) | 0.0014 (7) | −0.0017 (7) | 0.0002 (7) |
C5 | 0.0234 (8) | 0.0212 (8) | 0.0246 (9) | 0.0001 (6) | −0.0015 (7) | 0.0018 (7) |
C6 | 0.0259 (8) | 0.0207 (8) | 0.0227 (9) | −0.0003 (6) | 0.0004 (7) | 0.0029 (7) |
C7 | 0.0337 (10) | 0.0252 (9) | 0.0232 (10) | −0.0075 (7) | −0.0069 (8) | 0.0036 (7) |
C8 | 0.0259 (9) | 0.0259 (9) | 0.0249 (9) | −0.0014 (7) | −0.0048 (7) | −0.0001 (7) |
C9 | 0.0310 (10) | 0.0280 (9) | 0.0272 (9) | −0.0052 (8) | −0.0051 (8) | 0.0050 (8) |
C10 | 0.0320 (10) | 0.0372 (10) | 0.0289 (11) | −0.0009 (8) | −0.0083 (8) | 0.0034 (8) |
C11 | 0.0260 (9) | 0.0349 (10) | 0.0375 (11) | −0.0026 (8) | −0.0094 (8) | −0.0040 (9) |
C12 | 0.0302 (10) | 0.0280 (9) | 0.0400 (12) | −0.0051 (8) | −0.0027 (9) | −0.0006 (8) |
C13 | 0.0329 (10) | 0.0249 (9) | 0.0302 (10) | −0.0015 (7) | −0.0033 (8) | 0.0039 (7) |
C14 | 0.0217 (9) | 0.0368 (10) | 0.0402 (12) | −0.0022 (8) | −0.0017 (8) | 0.0077 (9) |
C15 | 0.0315 (9) | 0.0250 (9) | 0.0298 (10) | 0.0008 (7) | 0.0065 (8) | 0.0011 (8) |
C16 | 0.0228 (8) | 0.0301 (9) | 0.0221 (9) | 0.0017 (7) | 0.0002 (7) | −0.0014 (7) |
C17 | 0.0262 (9) | 0.0323 (10) | 0.0288 (10) | −0.0009 (7) | 0.0028 (7) | 0.0002 (8) |
C18 | 0.0336 (11) | 0.0469 (12) | 0.0305 (11) | −0.0011 (9) | 0.0094 (9) | 0.0010 (9) |
C19 | 0.0352 (12) | 0.0455 (13) | 0.0375 (13) | 0.0065 (9) | 0.0094 (10) | −0.0091 (10) |
C20 | 0.0342 (11) | 0.0331 (10) | 0.0406 (12) | 0.0063 (8) | 0.0004 (9) | −0.0043 (9) |
C21 | 0.0304 (10) | 0.0301 (10) | 0.0286 (10) | 0.0023 (7) | 0.0038 (8) | 0.0003 (8) |
C22 | 0.0351 (11) | 0.0378 (11) | 0.0279 (10) | 0.0040 (8) | −0.0047 (8) | −0.0079 (8) |
C23 | 0.0239 (9) | 0.0288 (9) | 0.0287 (9) | 0.0003 (7) | −0.0020 (8) | 0.0027 (8) |
C24 | 0.0227 (8) | 0.0253 (8) | 0.0283 (9) | 0.0032 (7) | −0.0025 (7) | −0.0021 (7) |
C25 | 0.0302 (10) | 0.0329 (10) | 0.0288 (10) | 0.0013 (8) | 0.0028 (8) | 0.0014 (8) |
C26 | 0.0430 (12) | 0.0405 (12) | 0.0309 (11) | 0.0035 (9) | −0.0072 (9) | 0.0012 (9) |
C27 | 0.0350 (11) | 0.0450 (12) | 0.0414 (12) | −0.0019 (9) | −0.0143 (9) | −0.0009 (10) |
C28 | 0.0259 (10) | 0.0442 (12) | 0.0472 (14) | −0.0042 (8) | −0.0041 (9) | 0.0031 (10) |
C29 | 0.0269 (9) | 0.0360 (10) | 0.0307 (10) | −0.0020 (8) | 0.0008 (8) | 0.0019 (8) |
C30 | 0.0335 (10) | 0.0350 (10) | 0.0259 (10) | 0.0018 (8) | 0.0043 (8) | −0.0032 (8) |
O1 | 0.0440 (8) | 0.0240 (7) | 0.0304 (8) | −0.0076 (6) | −0.0161 (7) | 0.0048 (6) |
O2 | 0.0363 (7) | 0.0252 (7) | 0.0314 (8) | 0.0049 (5) | 0.0131 (6) | 0.0027 (6) |
O3 | 0.0236 (6) | 0.0281 (6) | 0.0323 (7) | −0.0016 (5) | −0.0047 (6) | 0.0035 (6) |
C31 | 0.0281 (9) | 0.0210 (8) | 0.0253 (9) | −0.0032 (7) | −0.0047 (7) | 0.0056 (7) |
C32 | 0.0269 (9) | 0.0200 (8) | 0.0269 (9) | −0.0008 (7) | 0.0004 (7) | 0.0039 (7) |
C33 | 0.0244 (9) | 0.0227 (8) | 0.0278 (10) | −0.0001 (7) | −0.0017 (7) | 0.0045 (7) |
C34 | 0.0280 (9) | 0.0208 (8) | 0.0258 (9) | 0.0000 (7) | −0.0022 (7) | 0.0026 (7) |
C35 | 0.0270 (9) | 0.0197 (8) | 0.0278 (10) | 0.0000 (7) | 0.0011 (7) | 0.0038 (7) |
C36 | 0.0235 (8) | 0.0203 (8) | 0.0307 (10) | −0.0025 (6) | −0.0019 (7) | 0.0060 (7) |
C37 | 0.0351 (10) | 0.0237 (9) | 0.0281 (10) | −0.0062 (7) | −0.0051 (8) | 0.0054 (8) |
C38 | 0.0254 (9) | 0.0274 (9) | 0.0270 (9) | −0.0001 (7) | −0.0038 (7) | 0.0000 (8) |
C39 | 0.0332 (10) | 0.0273 (9) | 0.0325 (10) | −0.0018 (8) | −0.0063 (8) | 0.0032 (8) |
C40 | 0.0343 (11) | 0.0375 (11) | 0.0340 (12) | 0.0027 (8) | −0.0106 (9) | 0.0036 (9) |
C41 | 0.0275 (9) | 0.0380 (11) | 0.0415 (12) | −0.0028 (8) | −0.0096 (9) | −0.0049 (9) |
C42 | 0.0311 (10) | 0.0291 (10) | 0.0438 (12) | −0.0063 (8) | −0.0036 (9) | −0.0007 (9) |
C43 | 0.0314 (10) | 0.0284 (9) | 0.0316 (10) | −0.0019 (7) | −0.0045 (8) | 0.0030 (8) |
C44 | 0.0339 (11) | 0.0350 (10) | 0.0302 (11) | 0.0002 (8) | 0.0029 (9) | −0.0013 (9) |
C45 | 0.0251 (9) | 0.0313 (10) | 0.0306 (10) | −0.0023 (7) | −0.0032 (8) | 0.0053 (8) |
C46 | 0.0230 (8) | 0.0246 (8) | 0.0299 (10) | 0.0028 (7) | −0.0017 (7) | −0.0056 (7) |
C47 | 0.0284 (10) | 0.0349 (10) | 0.0292 (10) | −0.0002 (8) | −0.0016 (8) | −0.0005 (8) |
C48 | 0.0251 (10) | 0.0413 (11) | 0.0456 (13) | −0.0026 (8) | −0.0035 (9) | −0.0028 (10) |
C49 | 0.0331 (11) | 0.0424 (12) | 0.0435 (13) | 0.0023 (9) | −0.0136 (9) | −0.0039 (10) |
C50 | 0.0417 (12) | 0.0376 (11) | 0.0324 (11) | 0.0042 (9) | −0.0052 (9) | 0.0007 (9) |
C51 | 0.0299 (10) | 0.0286 (9) | 0.0338 (11) | 0.0035 (7) | 0.0008 (8) | 0.0007 (8) |
C52 | 0.0384 (11) | 0.0341 (10) | 0.0324 (11) | 0.0023 (8) | −0.0077 (9) | −0.0044 (9) |
C53 | 0.0324 (10) | 0.0242 (9) | 0.0309 (10) | −0.0006 (7) | 0.0058 (8) | 0.0046 (8) |
C54 | 0.0224 (8) | 0.0303 (9) | 0.0231 (9) | 0.0000 (7) | −0.0001 (7) | 0.0007 (7) |
C55 | 0.0293 (10) | 0.0302 (10) | 0.0275 (10) | 0.0006 (8) | 0.0027 (8) | 0.0034 (8) |
C56 | 0.0345 (10) | 0.0342 (10) | 0.0348 (11) | 0.0064 (8) | 0.0002 (9) | −0.0009 (9) |
C57 | 0.0335 (11) | 0.0490 (13) | 0.0300 (12) | 0.0098 (10) | 0.0045 (9) | −0.0046 (10) |
C58 | 0.0277 (10) | 0.0514 (12) | 0.0273 (10) | −0.0007 (9) | 0.0058 (8) | 0.0059 (9) |
C59 | 0.0256 (9) | 0.0327 (10) | 0.0274 (10) | −0.0012 (7) | 0.0000 (8) | 0.0050 (8) |
C60 | 0.0244 (9) | 0.0374 (10) | 0.0391 (11) | −0.0030 (8) | −0.0029 (8) | 0.0096 (9) |
O4 | 0.0445 (9) | 0.0239 (7) | 0.0306 (8) | −0.0069 (6) | −0.0149 (7) | 0.0063 (6) |
O5 | 0.0231 (6) | 0.0288 (6) | 0.0367 (8) | −0.0014 (5) | −0.0068 (6) | 0.0044 (6) |
O6 | 0.0375 (8) | 0.0241 (6) | 0.0305 (7) | 0.0023 (5) | 0.0117 (6) | 0.0037 (6) |
C1—C2 | 1.403 (3) | C31—C36 | 1.398 (3) |
C1—C6 | 1.404 (3) | C31—C32 | 1.410 (3) |
C1—C7 | 1.511 (3) | C31—C37 | 1.505 (3) |
C2—C3 | 1.398 (3) | C32—C33 | 1.408 (3) |
C2—C14 | 1.512 (3) | C32—C44 | 1.512 (3) |
C3—C4 | 1.400 (3) | C33—C34 | 1.405 (3) |
C3—C15 | 1.507 (3) | C33—C45 | 1.511 (3) |
C4—C5 | 1.405 (3) | C34—C35 | 1.400 (3) |
C4—C22 | 1.511 (3) | C34—C52 | 1.517 (3) |
C5—C6 | 1.407 (3) | C35—C36 | 1.407 (3) |
C5—C23 | 1.504 (2) | C35—C53 | 1.505 (3) |
C6—C30 | 1.520 (3) | C36—C60 | 1.510 (3) |
C7—O1 | 1.440 (2) | C37—O4 | 1.445 (2) |
C7—H7A | 0.9900 | C37—H37A | 0.9900 |
C7—H7B | 0.9900 | C37—H37B | 0.9900 |
C8—O1 | 1.375 (2) | C38—O4 | 1.370 (2) |
C8—C9 | 1.394 (3) | C38—C39 | 1.390 (3) |
C8—C13 | 1.394 (3) | C38—C43 | 1.393 (3) |
C9—C10 | 1.395 (3) | C39—C40 | 1.393 (3) |
C9—H9 | 0.9500 | C39—H39 | 0.9500 |
C10—C11 | 1.383 (3) | C40—C41 | 1.381 (3) |
C10—H10 | 0.9500 | C40—H40 | 0.9500 |
C11—C12 | 1.386 (3) | C41—C42 | 1.386 (3) |
C11—H11 | 0.9500 | C41—H41 | 0.9500 |
C12—C13 | 1.381 (3) | C42—C43 | 1.387 (3) |
C12—H12 | 0.9500 | C42—H42 | 0.9500 |
C13—H13 | 0.9500 | C43—H43 | 0.9500 |
C14—H14A | 0.9800 | C44—H44A | 0.9800 |
C14—H14B | 0.9800 | C44—H44B | 0.9800 |
C14—H14C | 0.9800 | C44—H44C | 0.9800 |
C15—O2 | 1.438 (2) | C45—O5 | 1.441 (2) |
C15—H15A | 0.9900 | C45—H45A | 0.9900 |
C15—H15B | 0.9900 | C45—H45B | 0.9900 |
C16—O2 | 1.376 (2) | C46—O5 | 1.369 (2) |
C16—C17 | 1.388 (3) | C46—C47 | 1.386 (3) |
C16—C21 | 1.395 (3) | C46—C51 | 1.394 (3) |
C17—C18 | 1.394 (3) | C47—C48 | 1.395 (3) |
C17—H17 | 0.9500 | C47—H47 | 0.9500 |
C18—C19 | 1.385 (3) | C48—C49 | 1.377 (4) |
C18—H18 | 0.9500 | C48—H48 | 0.9500 |
C19—C20 | 1.385 (4) | C49—C50 | 1.385 (3) |
C19—H19 | 0.9500 | C49—H49 | 0.9500 |
C20—C21 | 1.386 (3) | C50—C51 | 1.389 (3) |
C20—H20 | 0.9500 | C50—H50 | 0.9500 |
C21—H21 | 0.9500 | C51—H51 | 0.9500 |
C22—H22A | 0.9800 | C52—H52A | 0.9800 |
C22—H22B | 0.9800 | C52—H52B | 0.9800 |
C22—H22C | 0.9800 | C52—H52C | 0.9800 |
C23—O3 | 1.448 (2) | C53—O6 | 1.440 (2) |
C23—H23A | 0.9900 | C53—H53A | 0.9900 |
C23—H23B | 0.9900 | C53—H53B | 0.9900 |
C24—O3 | 1.368 (2) | C54—O6 | 1.372 (2) |
C24—C29 | 1.388 (3) | C54—C59 | 1.390 (3) |
C24—C25 | 1.394 (3) | C54—C55 | 1.396 (3) |
C25—C26 | 1.384 (3) | C55—C56 | 1.382 (3) |
C25—H25 | 0.9500 | C55—H55 | 0.9500 |
C26—C27 | 1.381 (3) | C56—C57 | 1.388 (3) |
C26—H26 | 0.9500 | C56—H56 | 0.9500 |
C27—C28 | 1.386 (4) | C57—C58 | 1.375 (3) |
C27—H27 | 0.9500 | C57—H57 | 0.9500 |
C28—C29 | 1.389 (3) | C58—C59 | 1.389 (3) |
C28—H28 | 0.9500 | C58—H58 | 0.9500 |
C29—H29 | 0.9500 | C59—H59 | 0.9500 |
C30—H30A | 0.9800 | C60—H60A | 0.9800 |
C30—H30B | 0.9800 | C60—H60B | 0.9800 |
C30—H30C | 0.9800 | C60—H60C | 0.9800 |
C2—C1—C6 | 120.83 (17) | C36—C31—C32 | 120.96 (18) |
C2—C1—C7 | 118.40 (17) | C36—C31—C37 | 118.41 (17) |
C6—C1—C7 | 120.77 (17) | C32—C31—C37 | 120.62 (18) |
C3—C2—C1 | 119.58 (16) | C33—C32—C31 | 118.49 (18) |
C3—C2—C14 | 120.62 (18) | C33—C32—C44 | 121.05 (17) |
C1—C2—C14 | 119.79 (18) | C31—C32—C44 | 120.47 (18) |
C2—C3—C4 | 120.44 (17) | C34—C33—C32 | 121.00 (17) |
C2—C3—C15 | 120.16 (17) | C34—C33—C45 | 117.96 (18) |
C4—C3—C15 | 119.39 (17) | C32—C33—C45 | 121.00 (18) |
C3—C4—C5 | 119.43 (17) | C35—C34—C33 | 119.37 (17) |
C3—C4—C22 | 120.04 (17) | C35—C34—C52 | 120.09 (18) |
C5—C4—C22 | 120.53 (17) | C33—C34—C52 | 120.54 (17) |
C4—C5—C6 | 120.73 (16) | C34—C35—C36 | 120.40 (18) |
C4—C5—C23 | 117.90 (17) | C34—C35—C53 | 119.63 (18) |
C6—C5—C23 | 121.35 (17) | C36—C35—C53 | 119.96 (18) |
C1—C6—C5 | 118.68 (17) | C31—C36—C35 | 119.55 (17) |
C1—C6—C30 | 120.21 (17) | C31—C36—C60 | 119.90 (18) |
C5—C6—C30 | 121.11 (17) | C35—C36—C60 | 120.53 (18) |
O1—C7—C1 | 107.95 (15) | O4—C37—C31 | 108.12 (15) |
O1—C7—H7A | 110.1 | O4—C37—H37A | 110.1 |
C1—C7—H7A | 110.1 | C31—C37—H37A | 110.1 |
O1—C7—H7B | 110.1 | O4—C37—H37B | 110.1 |
C1—C7—H7B | 110.1 | C31—C37—H37B | 110.1 |
H7A—C7—H7B | 108.4 | H37A—C37—H37B | 108.4 |
O1—C8—C9 | 124.38 (17) | O4—C38—C39 | 124.56 (17) |
O1—C8—C13 | 115.43 (17) | O4—C38—C43 | 115.25 (17) |
C9—C8—C13 | 120.18 (18) | C39—C38—C43 | 120.19 (18) |
C8—C9—C10 | 119.09 (18) | C38—C39—C40 | 119.20 (19) |
C8—C9—H9 | 120.5 | C38—C39—H39 | 120.4 |
C10—C9—H9 | 120.5 | C40—C39—H39 | 120.4 |
C11—C10—C9 | 120.65 (19) | C41—C40—C39 | 120.8 (2) |
C11—C10—H10 | 119.7 | C41—C40—H40 | 119.6 |
C9—C10—H10 | 119.7 | C39—C40—H40 | 119.6 |
C10—C11—C12 | 119.69 (19) | C40—C41—C42 | 119.7 (2) |
C10—C11—H11 | 120.2 | C40—C41—H41 | 120.2 |
C12—C11—H11 | 120.2 | C42—C41—H41 | 120.2 |
C13—C12—C11 | 120.61 (19) | C41—C42—C43 | 120.4 (2) |
C13—C12—H12 | 119.7 | C41—C42—H42 | 119.8 |
C11—C12—H12 | 119.7 | C43—C42—H42 | 119.8 |
C12—C13—C8 | 119.75 (19) | C42—C43—C38 | 119.75 (19) |
C12—C13—H13 | 120.1 | C42—C43—H43 | 120.1 |
C8—C13—H13 | 120.1 | C38—C43—H43 | 120.1 |
C2—C14—H14A | 109.5 | C32—C44—H44A | 109.5 |
C2—C14—H14B | 109.5 | C32—C44—H44B | 109.5 |
H14A—C14—H14B | 109.5 | H44A—C44—H44B | 109.5 |
C2—C14—H14C | 109.5 | C32—C44—H44C | 109.5 |
H14A—C14—H14C | 109.5 | H44A—C44—H44C | 109.5 |
H14B—C14—H14C | 109.5 | H44B—C44—H44C | 109.5 |
O2—C15—C3 | 107.45 (15) | O5—C45—C33 | 106.20 (15) |
O2—C15—H15A | 110.2 | O5—C45—H45A | 110.5 |
C3—C15—H15A | 110.2 | C33—C45—H45A | 110.5 |
O2—C15—H15B | 110.2 | O5—C45—H45B | 110.5 |
C3—C15—H15B | 110.2 | C33—C45—H45B | 110.5 |
H15A—C15—H15B | 108.5 | H45A—C45—H45B | 108.7 |
O2—C16—C17 | 124.51 (17) | O5—C46—C47 | 124.34 (19) |
O2—C16—C21 | 114.85 (17) | O5—C46—C51 | 115.23 (18) |
C17—C16—C21 | 120.64 (18) | C47—C46—C51 | 120.42 (19) |
C16—C17—C18 | 118.96 (19) | C46—C47—C48 | 118.7 (2) |
C16—C17—H17 | 120.5 | C46—C47—H47 | 120.7 |
C18—C17—H17 | 120.5 | C48—C47—H47 | 120.7 |
C19—C18—C17 | 120.6 (2) | C49—C48—C47 | 121.2 (2) |
C19—C18—H18 | 119.7 | C49—C48—H48 | 119.4 |
C17—C18—H18 | 119.7 | C47—C48—H48 | 119.4 |
C20—C19—C18 | 120.0 (2) | C48—C49—C50 | 119.9 (2) |
C20—C19—H19 | 120.0 | C48—C49—H49 | 120.1 |
C18—C19—H19 | 120.0 | C50—C49—H49 | 120.1 |
C19—C20—C21 | 120.2 (2) | C49—C50—C51 | 119.8 (2) |
C19—C20—H20 | 119.9 | C49—C50—H50 | 120.1 |
C21—C20—H20 | 119.9 | C51—C50—H50 | 120.1 |
C20—C21—C16 | 119.6 (2) | C50—C51—C46 | 120.0 (2) |
C20—C21—H21 | 120.2 | C50—C51—H51 | 120.0 |
C16—C21—H21 | 120.2 | C46—C51—H51 | 120.0 |
C4—C22—H22A | 109.5 | C34—C52—H52A | 109.5 |
C4—C22—H22B | 109.5 | C34—C52—H52B | 109.5 |
H22A—C22—H22B | 109.5 | H52A—C52—H52B | 109.5 |
C4—C22—H22C | 109.5 | C34—C52—H52C | 109.5 |
H22A—C22—H22C | 109.5 | H52A—C52—H52C | 109.5 |
H22B—C22—H22C | 109.5 | H52B—C52—H52C | 109.5 |
O3—C23—C5 | 106.39 (15) | O6—C53—C35 | 107.42 (15) |
O3—C23—H23A | 110.5 | O6—C53—H53A | 110.2 |
C5—C23—H23A | 110.5 | C35—C53—H53A | 110.2 |
O3—C23—H23B | 110.5 | O6—C53—H53B | 110.2 |
C5—C23—H23B | 110.5 | C35—C53—H53B | 110.2 |
H23A—C23—H23B | 108.6 | H53A—C53—H53B | 108.5 |
O3—C24—C29 | 124.36 (19) | O6—C54—C59 | 124.61 (17) |
O3—C24—C25 | 115.31 (17) | O6—C54—C55 | 115.38 (17) |
C29—C24—C25 | 120.31 (19) | C59—C54—C55 | 120.00 (18) |
C26—C25—C24 | 119.7 (2) | C56—C55—C54 | 120.1 (2) |
C26—C25—H25 | 120.2 | C56—C55—H55 | 120.0 |
C24—C25—H25 | 120.2 | C54—C55—H55 | 120.0 |
C27—C26—C25 | 120.6 (2) | C55—C56—C57 | 120.3 (2) |
C27—C26—H26 | 119.7 | C55—C56—H56 | 119.9 |
C25—C26—H26 | 119.7 | C57—C56—H56 | 119.9 |
C26—C27—C28 | 119.3 (2) | C58—C57—C56 | 119.1 (2) |
C26—C27—H27 | 120.3 | C58—C57—H57 | 120.4 |
C28—C27—H27 | 120.3 | C56—C57—H57 | 120.4 |
C27—C28—C29 | 121.1 (2) | C57—C58—C59 | 121.8 (2) |
C27—C28—H28 | 119.5 | C57—C58—H58 | 119.1 |
C29—C28—H28 | 119.5 | C59—C58—H58 | 119.1 |
C24—C29—C28 | 119.0 (2) | C58—C59—C54 | 118.66 (19) |
C24—C29—H29 | 120.5 | C58—C59—H59 | 120.7 |
C28—C29—H29 | 120.5 | C54—C59—H59 | 120.7 |
C6—C30—H30A | 109.5 | C36—C60—H60A | 109.5 |
C6—C30—H30B | 109.5 | C36—C60—H60B | 109.5 |
H30A—C30—H30B | 109.5 | H60A—C60—H60B | 109.5 |
C6—C30—H30C | 109.5 | C36—C60—H60C | 109.5 |
H30A—C30—H30C | 109.5 | H60A—C60—H60C | 109.5 |
H30B—C30—H30C | 109.5 | H60B—C60—H60C | 109.5 |
C8—O1—C7 | 116.93 (15) | C38—O4—C37 | 117.26 (15) |
C16—O2—C15 | 117.86 (15) | C46—O5—C45 | 117.82 (15) |
C24—O3—C23 | 117.47 (14) | C54—O6—C53 | 117.79 (15) |
C6—C1—C2—C3 | 0.2 (3) | C36—C31—C32—C33 | −4.3 (3) |
C7—C1—C2—C3 | 179.32 (16) | C37—C31—C32—C33 | 174.77 (16) |
C6—C1—C2—C14 | −178.76 (16) | C36—C31—C32—C44 | 175.32 (17) |
C7—C1—C2—C14 | 0.4 (2) | C37—C31—C32—C44 | −5.6 (3) |
C1—C2—C3—C4 | −4.8 (3) | C31—C32—C33—C34 | 3.3 (3) |
C14—C2—C3—C4 | 174.13 (16) | C44—C32—C33—C34 | −176.38 (17) |
C1—C2—C3—C15 | 176.45 (16) | C31—C32—C33—C45 | −179.08 (16) |
C14—C2—C3—C15 | −4.6 (3) | C44—C32—C33—C45 | 1.3 (3) |
C2—C3—C4—C5 | 4.8 (3) | C32—C33—C34—C35 | 0.9 (3) |
C15—C3—C4—C5 | −176.48 (16) | C45—C33—C34—C35 | −176.78 (17) |
C2—C3—C4—C22 | −175.32 (17) | C32—C33—C34—C52 | −179.19 (17) |
C15—C3—C4—C22 | 3.4 (3) | C45—C33—C34—C52 | 3.1 (3) |
C3—C4—C5—C6 | −0.1 (3) | C33—C34—C35—C36 | −4.2 (3) |
C22—C4—C5—C6 | 179.97 (17) | C52—C34—C35—C36 | 175.94 (17) |
C3—C4—C5—C23 | 178.31 (16) | C33—C34—C35—C53 | 176.03 (16) |
C22—C4—C5—C23 | −1.6 (3) | C52—C34—C35—C53 | −3.8 (3) |
C2—C1—C6—C5 | 4.3 (3) | C32—C31—C36—C35 | 1.2 (3) |
C7—C1—C6—C5 | −174.76 (16) | C37—C31—C36—C35 | −177.95 (16) |
C2—C1—C6—C30 | −175.57 (17) | C32—C31—C36—C60 | −179.96 (17) |
C7—C1—C6—C30 | 5.3 (3) | C37—C31—C36—C60 | 0.9 (3) |
C4—C5—C6—C1 | −4.4 (3) | C34—C35—C36—C31 | 3.2 (3) |
C23—C5—C6—C1 | 177.25 (16) | C53—C35—C36—C31 | −177.06 (16) |
C4—C5—C6—C30 | 175.54 (17) | C34—C35—C36—C60 | −175.71 (17) |
C23—C5—C6—C30 | −2.9 (3) | C53—C35—C36—C60 | 4.1 (3) |
C2—C1—C7—O1 | 78.5 (2) | C36—C31—C37—O4 | −80.6 (2) |
C6—C1—C7—O1 | −102.34 (19) | C32—C31—C37—O4 | 100.3 (2) |
O1—C8—C9—C10 | 178.44 (19) | O4—C38—C39—C40 | −177.9 (2) |
C13—C8—C9—C10 | −2.0 (3) | C43—C38—C39—C40 | 1.8 (3) |
C8—C9—C10—C11 | 1.0 (3) | C38—C39—C40—C41 | −1.2 (3) |
C9—C10—C11—C12 | 0.6 (3) | C39—C40—C41—C42 | −0.3 (4) |
C10—C11—C12—C13 | −1.3 (3) | C40—C41—C42—C43 | 1.3 (3) |
C11—C12—C13—C8 | 0.3 (3) | C41—C42—C43—C38 | −0.7 (3) |
O1—C8—C13—C12 | −179.02 (19) | O4—C38—C43—C42 | 178.81 (19) |
C9—C8—C13—C12 | 1.4 (3) | C39—C38—C43—C42 | −0.9 (3) |
C2—C3—C15—O2 | 91.7 (2) | C34—C33—C45—O5 | 66.3 (2) |
C4—C3—C15—O2 | −87.0 (2) | C32—C33—C45—O5 | −111.42 (19) |
O2—C16—C17—C18 | −179.08 (19) | O5—C46—C47—C48 | −179.13 (19) |
C21—C16—C17—C18 | 0.3 (3) | C51—C46—C47—C48 | −0.2 (3) |
C16—C17—C18—C19 | −0.3 (3) | C46—C47—C48—C49 | 0.1 (3) |
C17—C18—C19—C20 | 0.5 (4) | C47—C48—C49—C50 | 0.0 (4) |
C18—C19—C20—C21 | −0.7 (4) | C48—C49—C50—C51 | 0.0 (3) |
C19—C20—C21—C16 | 0.7 (3) | C49—C50—C51—C46 | −0.2 (3) |
O2—C16—C21—C20 | 178.97 (19) | O5—C46—C51—C50 | 179.27 (18) |
C17—C16—C21—C20 | −0.5 (3) | C47—C46—C51—C50 | 0.2 (3) |
C4—C5—C23—O3 | −64.7 (2) | C34—C35—C53—O6 | 88.1 (2) |
C6—C5—C23—O3 | 113.78 (18) | C36—C35—C53—O6 | −91.7 (2) |
O3—C24—C25—C26 | −179.02 (18) | O6—C54—C55—C56 | −178.87 (19) |
C29—C24—C25—C26 | −0.6 (3) | C59—C54—C55—C56 | 0.0 (3) |
C24—C25—C26—C27 | −0.4 (3) | C54—C55—C56—C57 | −0.4 (3) |
C25—C26—C27—C28 | 1.0 (4) | C55—C56—C57—C58 | 0.2 (4) |
C26—C27—C28—C29 | −0.7 (4) | C56—C57—C58—C59 | 0.5 (4) |
O3—C24—C29—C28 | 179.17 (19) | C57—C58—C59—C54 | −0.8 (3) |
C25—C24—C29—C28 | 0.9 (3) | O6—C54—C59—C58 | 179.37 (19) |
C27—C28—C29—C24 | −0.3 (3) | C55—C54—C59—C58 | 0.6 (3) |
C9—C8—O1—C7 | −3.0 (3) | C39—C38—O4—C37 | 2.4 (3) |
C13—C8—O1—C7 | 177.40 (18) | C43—C38—O4—C37 | −177.20 (18) |
C1—C7—O1—C8 | −164.95 (17) | C31—C37—O4—C38 | 165.80 (17) |
C17—C16—O2—C15 | 3.4 (3) | C47—C46—O5—C45 | −24.4 (3) |
C21—C16—O2—C15 | −176.09 (18) | C51—C46—O5—C45 | 156.60 (17) |
C3—C15—O2—C16 | −179.55 (16) | C33—C45—O5—C46 | −160.27 (16) |
C29—C24—O3—C23 | 27.7 (3) | C59—C54—O6—C53 | −5.1 (3) |
C25—C24—O3—C23 | −153.96 (16) | C55—C54—O6—C53 | 173.71 (18) |
C5—C23—O3—C24 | 156.02 (16) | C35—C53—O6—C54 | 179.84 (16) |
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