Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680700640X/pk2002sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680700640X/pk2002Isup2.hkl |
CCDC reference: 640461
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.002 Å
- R factor = 0.043
- wR factor = 0.127
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT410_ALERT_2_C Short Intra H...H Contact H2A .. H36A .. 1.94 Ang. PLAT410_ALERT_2_C Short Intra H...H Contact H14B .. H44A .. 1.92 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL (Sheldrick, 2000); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL (Sheldrick, 2000).
C48H64N4O10 | F(000) = 1840 |
Mr = 857.03 | Dx = 1.292 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9433 reflections |
a = 8.6689 (14) Å | θ = 2.4–27.1° |
b = 17.025 (2) Å | µ = 0.09 mm−1 |
c = 30.072 (4) Å | T = 120 K |
β = 96.779 (5)° | Plate, colorless |
V = 4407.2 (11) Å3 | 0.20 × 0.14 × 0.02 mm |
Z = 4 |
Bruker SMART APEX CCD diffractometer | 8648 independent reflections |
Radiation source: fine-focus sealed tube | 7539 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
ω scans | θmax = 26.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −10→10 |
Tmin = 0.982, Tmax = 0.998 | k = −20→21 |
44693 measured reflections | l = −37→37 |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.127 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.076P)2 + 1.6P] where P = (Fo2 + 2Fc2)/3 |
8648 reflections | (Δ/σ)max = 0.001 |
559 parameters | Δρmax = 0.32 e Å−3 |
0 restraints | Δρmin = −0.17 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
O1 | 0.63563 (12) | 0.78020 (6) | 0.37180 (3) | 0.0262 (2) | |
O2 | 0.56185 (11) | 0.85673 (6) | 0.28159 (3) | 0.0263 (2) | |
O3 | 0.55478 (12) | 0.79098 (6) | 0.19265 (3) | 0.0277 (2) | |
O4 | −0.06881 (12) | 0.33837 (6) | 0.31471 (3) | 0.0269 (2) | |
O5 | −0.06842 (12) | 0.26965 (6) | 0.22518 (3) | 0.0272 (2) | |
O6 | −0.13223 (12) | 0.34288 (6) | 0.13516 (3) | 0.0260 (2) | |
O7 | 0.28390 (11) | 0.60203 (6) | 0.42094 (3) | 0.0248 (2) | |
O8 | −0.05261 (12) | 0.52406 (6) | 0.22569 (3) | 0.0279 (2) | |
O9 | 0.22311 (11) | 0.52418 (5) | 0.08902 (3) | 0.0218 (2) | |
O10 | 0.55090 (12) | 0.59829 (6) | 0.28374 (3) | 0.0286 (2) | |
N1 | 0.61623 (13) | 0.63398 (7) | 0.40492 (4) | 0.0225 (3) | |
N2 | 0.01001 (13) | 0.48319 (7) | 0.34633 (4) | 0.0216 (2) | |
N3 | −0.10904 (13) | 0.49081 (7) | 0.10426 (4) | 0.0231 (3) | |
N4 | 0.49330 (13) | 0.64344 (7) | 0.16384 (4) | 0.0211 (2) | |
C1 | 0.72436 (16) | 0.68750 (8) | 0.42741 (5) | 0.0230 (3) | |
C2 | 0.56126 (16) | 0.56911 (8) | 0.43046 (5) | 0.0240 (3) | |
H2A | 0.6451 | 0.5531 | 0.4539 | 0.029* | |
H2B | 0.5373 | 0.5237 | 0.4103 | 0.029* | |
C3 | 0.41801 (16) | 0.59006 (9) | 0.45229 (4) | 0.0244 (3) | |
H3A | 0.3967 | 0.5474 | 0.4731 | 0.029* | |
H3B | 0.4390 | 0.6385 | 0.4702 | 0.029* | |
C4 | 0.22057 (17) | 0.53086 (8) | 0.40242 (5) | 0.0270 (3) | |
H4A | 0.1874 | 0.4969 | 0.4263 | 0.032* | |
H4B | 0.2990 | 0.5022 | 0.3873 | 0.032* | |
C5 | 0.08235 (16) | 0.55231 (8) | 0.36896 (5) | 0.0233 (3) | |
H5A | 0.0045 | 0.5802 | 0.3847 | 0.028* | |
H5B | 0.1166 | 0.5886 | 0.3463 | 0.028* | |
C6 | −0.07470 (15) | 0.43267 (8) | 0.37222 (5) | 0.0223 (3) | |
C7 | −0.11872 (16) | 0.35782 (8) | 0.35491 (5) | 0.0242 (3) | |
C8 | −0.06245 (19) | 0.25629 (8) | 0.30447 (5) | 0.0288 (3) | |
H8A | −0.1690 | 0.2352 | 0.2977 | 0.035* | |
H8B | −0.0098 | 0.2274 | 0.3305 | 0.035* | |
C9 | 0.02498 (18) | 0.24558 (9) | 0.26492 (5) | 0.0293 (3) | |
H9A | 0.1216 | 0.2771 | 0.2690 | 0.035* | |
H9B | 0.0540 | 0.1897 | 0.2624 | 0.035* | |
C10 | 0.00755 (17) | 0.25465 (9) | 0.18667 (5) | 0.0271 (3) | |
H10A | 0.0531 | 0.2013 | 0.1886 | 0.032* | |
H10B | 0.0928 | 0.2929 | 0.1852 | 0.032* | |
C11 | −0.10668 (18) | 0.26130 (8) | 0.14527 (5) | 0.0268 (3) | |
H11A | −0.0654 | 0.2346 | 0.1199 | 0.032* | |
H11B | −0.2059 | 0.2358 | 0.1502 | 0.032* | |
C12 | −0.22217 (16) | 0.35969 (8) | 0.09559 (5) | 0.0239 (3) | |
C13 | −0.20997 (15) | 0.43715 (8) | 0.07939 (5) | 0.0222 (3) | |
C14 | −0.05359 (16) | 0.55794 (8) | 0.08052 (5) | 0.0241 (3) | |
H14A | −0.0281 | 0.6014 | 0.1020 | 0.029* | |
H14B | −0.1375 | 0.5762 | 0.0577 | 0.029* | |
C15 | 0.08893 (15) | 0.53811 (8) | 0.05787 (4) | 0.0227 (3) | |
H15A | 0.0671 | 0.4907 | 0.0391 | 0.027* | |
H15B | 0.1105 | 0.5820 | 0.0379 | 0.027* | |
C16 | 0.28486 (15) | 0.59466 (8) | 0.10857 (5) | 0.0223 (3) | |
H16A | 0.2057 | 0.6219 | 0.1241 | 0.027* | |
H16B | 0.3168 | 0.6300 | 0.0852 | 0.027* | |
C17 | 0.42390 (15) | 0.57354 (8) | 0.14169 (4) | 0.0213 (3) | |
H17A | 0.3911 | 0.5371 | 0.1644 | 0.026* | |
H17B | 0.5023 | 0.5463 | 0.1258 | 0.026* | |
C18 | 0.57476 (15) | 0.69458 (8) | 0.13735 (4) | 0.0208 (3) | |
C19 | 0.60827 (16) | 0.77157 (8) | 0.15303 (5) | 0.0244 (3) | |
C20 | 0.54589 (19) | 0.87306 (8) | 0.20259 (5) | 0.0289 (3) | |
H20A | 0.4890 | 0.9013 | 0.1769 | 0.035* | |
H20B | 0.6516 | 0.8956 | 0.2085 | 0.035* | |
C21 | 0.46220 (17) | 0.88160 (9) | 0.24315 (5) | 0.0277 (3) | |
H21A | 0.4320 | 0.9371 | 0.2467 | 0.033* | |
H21B | 0.3667 | 0.8492 | 0.2397 | 0.033* | |
C22 | 0.49103 (17) | 0.86850 (9) | 0.32131 (5) | 0.0262 (3) | |
H22A | 0.4087 | 0.8288 | 0.3232 | 0.031* | |
H22B | 0.4425 | 0.9212 | 0.3207 | 0.031* | |
C23 | 0.61074 (18) | 0.86166 (8) | 0.36129 (5) | 0.0266 (3) | |
H23A | 0.7092 | 0.8861 | 0.3548 | 0.032* | |
H23B | 0.5747 | 0.8893 | 0.3871 | 0.032* | |
C24 | 0.73414 (16) | 0.76411 (9) | 0.40969 (5) | 0.0243 (3) | |
C25 | 0.64475 (16) | 0.61406 (8) | 0.35919 (4) | 0.0226 (3) | |
H25A | 0.6823 | 0.5592 | 0.3587 | 0.027* | |
H25B | 0.7280 | 0.6485 | 0.3504 | 0.027* | |
C26 | 0.50253 (16) | 0.62254 (9) | 0.32513 (4) | 0.0244 (3) | |
H26A | 0.4170 | 0.5889 | 0.3332 | 0.029* | |
H26B | 0.4665 | 0.6778 | 0.3234 | 0.029* | |
C27 | 0.46561 (17) | 0.63005 (9) | 0.24473 (5) | 0.0248 (3) | |
H27A | 0.4354 | 0.6851 | 0.2499 | 0.030* | |
H27B | 0.3705 | 0.5989 | 0.2360 | 0.030* | |
C28 | 0.57368 (16) | 0.62610 (8) | 0.20871 (4) | 0.0219 (3) | |
H28A | 0.6593 | 0.6642 | 0.2158 | 0.026* | |
H28B | 0.6199 | 0.5729 | 0.2086 | 0.026* | |
C29 | −0.06989 (15) | 0.50283 (8) | 0.30158 (4) | 0.0221 (3) | |
H29A | −0.1085 | 0.5575 | 0.3019 | 0.027* | |
H29B | −0.1609 | 0.4678 | 0.2948 | 0.027* | |
C30 | 0.03467 (16) | 0.49457 (9) | 0.26502 (5) | 0.0245 (3) | |
H30A | 0.1313 | 0.5253 | 0.2724 | 0.029* | |
H30B | 0.0625 | 0.4388 | 0.2611 | 0.029* | |
C31 | −0.00128 (16) | 0.50022 (9) | 0.18460 (5) | 0.0246 (3) | |
H31A | 0.0364 | 0.4453 | 0.1866 | 0.030* | |
H31B | 0.0839 | 0.5345 | 0.1769 | 0.030* | |
C32 | −0.14194 (16) | 0.50760 (8) | 0.14990 (4) | 0.0231 (3) | |
H32A | −0.2233 | 0.4710 | 0.1577 | 0.028* | |
H32B | −0.1836 | 0.5616 | 0.1509 | 0.028* | |
C33 | 0.84027 (18) | 0.81814 (9) | 0.42989 (5) | 0.0295 (3) | |
H33A | 0.8455 | 0.8694 | 0.4177 | 0.035* | |
C34 | 0.93858 (18) | 0.79741 (10) | 0.46784 (5) | 0.0317 (3) | |
H34A | 1.0126 | 0.8341 | 0.4812 | 0.038* | |
C35 | 0.92908 (18) | 0.72372 (10) | 0.48624 (5) | 0.0325 (3) | |
H35A | 0.9951 | 0.7099 | 0.5126 | 0.039* | |
C36 | 0.82243 (17) | 0.66950 (9) | 0.46613 (5) | 0.0284 (3) | |
H36A | 0.8164 | 0.6189 | 0.4792 | 0.034* | |
C37 | −0.11267 (16) | 0.45150 (9) | 0.41451 (5) | 0.0262 (3) | |
H37A | −0.0806 | 0.5006 | 0.4274 | 0.031* | |
C38 | −0.19695 (18) | 0.39994 (9) | 0.43852 (5) | 0.0314 (3) | |
H38A | −0.2188 | 0.4135 | 0.4678 | 0.038* | |
C39 | −0.24832 (18) | 0.32949 (9) | 0.41983 (5) | 0.0319 (3) | |
H39A | −0.3103 | 0.2955 | 0.4354 | 0.038* | |
C40 | −0.20897 (17) | 0.30832 (9) | 0.37799 (5) | 0.0289 (3) | |
H40A | −0.2440 | 0.2596 | 0.3651 | 0.035* | |
C41 | −0.31820 (17) | 0.30490 (9) | 0.07195 (5) | 0.0280 (3) | |
H41A | −0.3263 | 0.2533 | 0.0835 | 0.034* | |
C42 | −0.40249 (18) | 0.32549 (9) | 0.03139 (5) | 0.0308 (3) | |
H42A | −0.4687 | 0.2881 | 0.0153 | 0.037* | |
C43 | −0.38969 (18) | 0.40008 (10) | 0.01462 (5) | 0.0311 (3) | |
H43A | −0.4459 | 0.4139 | −0.0133 | 0.037* | |
C44 | −0.29463 (17) | 0.45540 (9) | 0.03843 (5) | 0.0272 (3) | |
H44A | −0.2874 | 0.5067 | 0.0265 | 0.033* | |
C45 | 0.61763 (16) | 0.67417 (8) | 0.09584 (5) | 0.0233 (3) | |
H45A | 0.5934 | 0.6232 | 0.0842 | 0.028* | |
C46 | 0.69529 (16) | 0.72671 (9) | 0.07076 (5) | 0.0269 (3) | |
H46A | 0.7212 | 0.7119 | 0.0421 | 0.032* | |
C47 | 0.73448 (18) | 0.80044 (9) | 0.08766 (5) | 0.0298 (3) | |
H47A | 0.7905 | 0.8358 | 0.0711 | 0.036* | |
C48 | 0.69165 (18) | 0.82254 (9) | 0.12889 (5) | 0.0298 (3) | |
H48A | 0.7197 | 0.8730 | 0.1407 | 0.036* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.0304 (5) | 0.0212 (5) | 0.0264 (5) | −0.0040 (4) | 0.0007 (4) | −0.0005 (4) |
O2 | 0.0248 (5) | 0.0278 (5) | 0.0261 (5) | 0.0063 (4) | 0.0021 (4) | −0.0012 (4) |
O3 | 0.0377 (6) | 0.0189 (5) | 0.0266 (5) | −0.0031 (4) | 0.0046 (4) | −0.0013 (4) |
O4 | 0.0341 (6) | 0.0192 (5) | 0.0274 (5) | −0.0025 (4) | 0.0037 (4) | 0.0013 (4) |
O5 | 0.0269 (5) | 0.0263 (5) | 0.0281 (5) | 0.0054 (4) | 0.0017 (4) | 0.0007 (4) |
O6 | 0.0298 (5) | 0.0206 (5) | 0.0272 (5) | −0.0022 (4) | 0.0012 (4) | 0.0007 (4) |
O7 | 0.0213 (5) | 0.0217 (5) | 0.0309 (5) | −0.0006 (4) | 0.0006 (4) | −0.0021 (4) |
O8 | 0.0340 (6) | 0.0262 (5) | 0.0236 (5) | 0.0096 (4) | 0.0038 (4) | 0.0022 (4) |
O9 | 0.0193 (5) | 0.0197 (5) | 0.0257 (5) | −0.0011 (4) | −0.0006 (4) | −0.0011 (4) |
O10 | 0.0357 (6) | 0.0292 (6) | 0.0207 (5) | 0.0106 (4) | 0.0027 (4) | 0.0006 (4) |
N1 | 0.0224 (6) | 0.0236 (6) | 0.0218 (6) | −0.0025 (5) | 0.0037 (5) | −0.0009 (5) |
N2 | 0.0214 (6) | 0.0185 (6) | 0.0246 (6) | −0.0020 (4) | 0.0010 (5) | 0.0023 (4) |
N3 | 0.0215 (6) | 0.0230 (6) | 0.0255 (6) | −0.0026 (5) | 0.0055 (5) | −0.0002 (5) |
N4 | 0.0212 (6) | 0.0197 (6) | 0.0219 (6) | −0.0037 (4) | 0.0004 (4) | 0.0013 (4) |
C1 | 0.0193 (7) | 0.0262 (7) | 0.0243 (7) | −0.0004 (5) | 0.0063 (5) | −0.0050 (5) |
C2 | 0.0221 (7) | 0.0225 (7) | 0.0269 (7) | 0.0002 (5) | 0.0014 (5) | 0.0024 (5) |
C3 | 0.0248 (7) | 0.0264 (7) | 0.0218 (7) | −0.0023 (6) | 0.0026 (5) | 0.0013 (5) |
C4 | 0.0248 (7) | 0.0204 (7) | 0.0346 (8) | −0.0013 (6) | −0.0010 (6) | −0.0011 (6) |
C5 | 0.0224 (7) | 0.0186 (7) | 0.0290 (7) | −0.0009 (5) | 0.0031 (5) | 0.0019 (5) |
C6 | 0.0174 (6) | 0.0211 (7) | 0.0279 (7) | 0.0018 (5) | 0.0010 (5) | 0.0049 (5) |
C7 | 0.0223 (7) | 0.0231 (7) | 0.0264 (7) | 0.0013 (5) | −0.0009 (5) | 0.0041 (5) |
C8 | 0.0371 (8) | 0.0177 (7) | 0.0304 (8) | −0.0020 (6) | −0.0006 (6) | 0.0013 (6) |
C9 | 0.0303 (8) | 0.0233 (7) | 0.0327 (8) | 0.0038 (6) | −0.0025 (6) | 0.0011 (6) |
C10 | 0.0275 (7) | 0.0209 (7) | 0.0336 (8) | 0.0020 (6) | 0.0070 (6) | −0.0011 (6) |
C11 | 0.0307 (8) | 0.0187 (7) | 0.0317 (8) | −0.0017 (6) | 0.0071 (6) | −0.0011 (6) |
C12 | 0.0214 (7) | 0.0263 (7) | 0.0248 (7) | −0.0005 (5) | 0.0063 (5) | −0.0008 (5) |
C13 | 0.0170 (6) | 0.0249 (7) | 0.0256 (7) | −0.0001 (5) | 0.0065 (5) | −0.0028 (5) |
C14 | 0.0194 (7) | 0.0228 (7) | 0.0299 (7) | −0.0003 (5) | 0.0015 (5) | 0.0028 (6) |
C15 | 0.0206 (7) | 0.0256 (7) | 0.0214 (6) | −0.0025 (5) | 0.0005 (5) | 0.0025 (5) |
C16 | 0.0202 (7) | 0.0186 (7) | 0.0279 (7) | −0.0011 (5) | 0.0017 (5) | −0.0004 (5) |
C17 | 0.0210 (7) | 0.0181 (6) | 0.0247 (7) | −0.0022 (5) | 0.0023 (5) | 0.0002 (5) |
C18 | 0.0166 (6) | 0.0201 (7) | 0.0248 (7) | −0.0013 (5) | −0.0011 (5) | 0.0033 (5) |
C19 | 0.0253 (7) | 0.0231 (7) | 0.0239 (7) | −0.0018 (6) | −0.0005 (5) | 0.0013 (5) |
C20 | 0.0366 (8) | 0.0185 (7) | 0.0306 (8) | −0.0026 (6) | −0.0005 (6) | −0.0007 (6) |
C21 | 0.0281 (7) | 0.0210 (7) | 0.0324 (8) | 0.0038 (6) | −0.0035 (6) | −0.0023 (6) |
C22 | 0.0253 (7) | 0.0222 (7) | 0.0323 (8) | 0.0008 (6) | 0.0078 (6) | −0.0023 (6) |
C23 | 0.0322 (8) | 0.0193 (7) | 0.0293 (7) | −0.0023 (6) | 0.0071 (6) | −0.0030 (6) |
C24 | 0.0218 (7) | 0.0286 (8) | 0.0232 (7) | −0.0020 (6) | 0.0052 (5) | −0.0038 (6) |
C25 | 0.0211 (7) | 0.0234 (7) | 0.0240 (7) | −0.0002 (5) | 0.0053 (5) | −0.0028 (5) |
C26 | 0.0230 (7) | 0.0278 (7) | 0.0228 (7) | −0.0001 (6) | 0.0048 (5) | −0.0010 (5) |
C27 | 0.0246 (7) | 0.0260 (7) | 0.0235 (7) | 0.0012 (6) | 0.0011 (6) | 0.0007 (5) |
C28 | 0.0206 (7) | 0.0213 (7) | 0.0232 (7) | −0.0017 (5) | −0.0003 (5) | 0.0009 (5) |
C29 | 0.0202 (7) | 0.0198 (7) | 0.0262 (7) | 0.0002 (5) | 0.0018 (5) | 0.0027 (5) |
C30 | 0.0223 (7) | 0.0247 (7) | 0.0261 (7) | 0.0012 (6) | 0.0018 (5) | 0.0025 (6) |
C31 | 0.0228 (7) | 0.0260 (7) | 0.0257 (7) | 0.0000 (6) | 0.0055 (5) | 0.0011 (6) |
C32 | 0.0209 (7) | 0.0229 (7) | 0.0261 (7) | 0.0001 (5) | 0.0056 (5) | −0.0016 (5) |
C33 | 0.0317 (8) | 0.0296 (8) | 0.0279 (7) | −0.0072 (6) | 0.0066 (6) | −0.0044 (6) |
C34 | 0.0280 (8) | 0.0397 (9) | 0.0278 (7) | −0.0096 (7) | 0.0048 (6) | −0.0106 (6) |
C35 | 0.0272 (8) | 0.0432 (9) | 0.0261 (7) | 0.0022 (7) | −0.0011 (6) | −0.0062 (6) |
C36 | 0.0289 (8) | 0.0293 (8) | 0.0269 (7) | 0.0033 (6) | 0.0030 (6) | −0.0015 (6) |
C37 | 0.0247 (7) | 0.0231 (7) | 0.0309 (7) | 0.0028 (6) | 0.0033 (6) | 0.0023 (6) |
C38 | 0.0324 (8) | 0.0310 (8) | 0.0326 (8) | 0.0059 (6) | 0.0112 (6) | 0.0061 (6) |
C39 | 0.0277 (8) | 0.0281 (8) | 0.0408 (9) | −0.0007 (6) | 0.0083 (6) | 0.0114 (6) |
C40 | 0.0263 (7) | 0.0232 (7) | 0.0364 (8) | −0.0030 (6) | 0.0000 (6) | 0.0065 (6) |
C41 | 0.0286 (8) | 0.0254 (8) | 0.0306 (8) | −0.0042 (6) | 0.0061 (6) | −0.0028 (6) |
C42 | 0.0272 (8) | 0.0338 (8) | 0.0311 (8) | −0.0042 (6) | 0.0021 (6) | −0.0061 (6) |
C43 | 0.0282 (8) | 0.0370 (9) | 0.0270 (7) | 0.0017 (6) | −0.0012 (6) | −0.0026 (6) |
C44 | 0.0266 (7) | 0.0275 (8) | 0.0281 (7) | 0.0018 (6) | 0.0057 (6) | 0.0013 (6) |
C45 | 0.0206 (7) | 0.0217 (7) | 0.0270 (7) | −0.0012 (5) | 0.0008 (5) | 0.0008 (5) |
C46 | 0.0247 (7) | 0.0295 (8) | 0.0265 (7) | −0.0007 (6) | 0.0037 (6) | 0.0022 (6) |
C47 | 0.0291 (8) | 0.0271 (8) | 0.0332 (8) | −0.0054 (6) | 0.0043 (6) | 0.0075 (6) |
C48 | 0.0346 (8) | 0.0220 (7) | 0.0318 (8) | −0.0070 (6) | −0.0002 (6) | 0.0021 (6) |
O1—C24 | 1.3687 (17) | C16—H16A | 0.9900 |
O1—C23 | 1.4330 (17) | C16—H16B | 0.9900 |
O2—C22 | 1.4202 (17) | C17—H17A | 0.9900 |
O2—C21 | 1.4234 (17) | C17—H17B | 0.9900 |
O3—C19 | 1.3688 (17) | C18—C45 | 1.388 (2) |
O3—C20 | 1.4331 (17) | C18—C19 | 1.4116 (19) |
O4—C7 | 1.3718 (17) | C19—C48 | 1.388 (2) |
O4—C8 | 1.4333 (17) | C20—C21 | 1.498 (2) |
O5—C10 | 1.4214 (17) | C20—H20A | 0.9900 |
O5—C9 | 1.4223 (17) | C20—H20B | 0.9900 |
O6—C12 | 1.3736 (17) | C21—H21A | 0.9900 |
O6—C11 | 1.4335 (17) | C21—H21B | 0.9900 |
O7—C4 | 1.4169 (17) | C22—C23 | 1.497 (2) |
O7—C3 | 1.4224 (16) | C22—H22A | 0.9900 |
O8—C30 | 1.4186 (16) | C22—H22B | 0.9900 |
O8—C31 | 1.4210 (16) | C23—H23A | 0.9900 |
O9—C16 | 1.4134 (16) | C23—H23B | 0.9900 |
O9—C15 | 1.4247 (16) | C24—C33 | 1.389 (2) |
O10—C27 | 1.4178 (16) | C25—C26 | 1.5138 (19) |
O10—C26 | 1.4210 (16) | C25—H25A | 0.9900 |
N1—C1 | 1.4201 (18) | C25—H25B | 0.9900 |
N1—C2 | 1.4570 (17) | C26—H26A | 0.9900 |
N1—C25 | 1.4655 (17) | C26—H26B | 0.9900 |
N2—C6 | 1.4213 (17) | C27—C28 | 1.5150 (19) |
N2—C5 | 1.4631 (17) | C27—H27A | 0.9900 |
N2—C29 | 1.4773 (17) | C27—H27B | 0.9900 |
N3—C13 | 1.4159 (18) | C28—H28A | 0.9900 |
N3—C14 | 1.4587 (18) | C28—H28B | 0.9900 |
N3—C32 | 1.4626 (17) | C29—C30 | 1.5117 (19) |
N4—C18 | 1.4227 (17) | C29—H29A | 0.9900 |
N4—C17 | 1.4585 (17) | C29—H29B | 0.9900 |
N4—C28 | 1.4735 (17) | C30—H30A | 0.9900 |
C1—C36 | 1.392 (2) | C30—H30B | 0.9900 |
C1—C24 | 1.415 (2) | C31—C32 | 1.5138 (19) |
C2—C3 | 1.5141 (19) | C31—H31A | 0.9900 |
C2—H2A | 0.9900 | C31—H31B | 0.9900 |
C2—H2B | 0.9900 | C32—H32A | 0.9900 |
C3—H3A | 0.9900 | C32—H32B | 0.9900 |
C3—H3B | 0.9900 | C33—C34 | 1.387 (2) |
C4—C5 | 1.5155 (19) | C33—H33A | 0.9500 |
C4—H4A | 0.9900 | C34—C35 | 1.378 (2) |
C4—H4B | 0.9900 | C34—H34A | 0.9500 |
C5—H5A | 0.9900 | C35—C36 | 1.393 (2) |
C5—H5B | 0.9900 | C35—H35A | 0.9500 |
C6—C37 | 1.388 (2) | C36—H36A | 0.9500 |
C6—C7 | 1.412 (2) | C37—C38 | 1.397 (2) |
C7—C40 | 1.390 (2) | C37—H37A | 0.9500 |
C8—C9 | 1.495 (2) | C38—C39 | 1.376 (2) |
C8—H8A | 0.9900 | C38—H38A | 0.9500 |
C8—H8B | 0.9900 | C39—C40 | 1.389 (2) |
C9—H9A | 0.9900 | C39—H39A | 0.9500 |
C9—H9B | 0.9900 | C40—H40A | 0.9500 |
C10—C11 | 1.501 (2) | C41—C42 | 1.391 (2) |
C10—H10A | 0.9900 | C41—H41A | 0.9500 |
C10—H10B | 0.9900 | C42—C43 | 1.376 (2) |
C11—H11A | 0.9900 | C42—H42A | 0.9500 |
C11—H11B | 0.9900 | C43—C44 | 1.393 (2) |
C12—C41 | 1.389 (2) | C43—H43A | 0.9500 |
C12—C13 | 1.414 (2) | C44—H44A | 0.9500 |
C13—C44 | 1.392 (2) | C45—C46 | 1.394 (2) |
C14—C15 | 1.5177 (19) | C45—H45A | 0.9500 |
C14—H14A | 0.9900 | C46—C47 | 1.382 (2) |
C14—H14B | 0.9900 | C46—H46A | 0.9500 |
C15—H15A | 0.9900 | C47—C48 | 1.388 (2) |
C15—H15B | 0.9900 | C47—H47A | 0.9500 |
C16—C17 | 1.5134 (18) | C48—H48A | 0.9500 |
C24—O1—C23 | 116.12 (11) | C21—C20—H20B | 110.1 |
C22—O2—C21 | 111.09 (11) | H20A—C20—H20B | 108.4 |
C19—O3—C20 | 116.69 (11) | O2—C21—C20 | 109.06 (12) |
C7—O4—C8 | 116.66 (11) | O2—C21—H21A | 109.9 |
C10—O5—C9 | 111.11 (11) | C20—C21—H21A | 109.9 |
C12—O6—C11 | 116.32 (11) | O2—C21—H21B | 109.9 |
C4—O7—C3 | 112.74 (11) | C20—C21—H21B | 109.9 |
C30—O8—C31 | 115.65 (10) | H21A—C21—H21B | 108.3 |
C16—O9—C15 | 111.84 (10) | O2—C22—C23 | 109.69 (12) |
C27—O10—C26 | 115.78 (11) | O2—C22—H22A | 109.7 |
C1—N1—C2 | 118.29 (11) | C23—C22—H22A | 109.7 |
C1—N1—C25 | 114.86 (11) | O2—C22—H22B | 109.7 |
C2—N1—C25 | 114.91 (11) | C23—C22—H22B | 109.7 |
C6—N2—C5 | 116.92 (11) | H22A—C22—H22B | 108.2 |
C6—N2—C29 | 114.76 (11) | O1—C23—C22 | 108.93 (11) |
C5—N2—C29 | 111.77 (11) | O1—C23—H23A | 109.9 |
C13—N3—C14 | 117.77 (11) | C22—C23—H23A | 109.9 |
C13—N3—C32 | 116.41 (11) | O1—C23—H23B | 109.9 |
C14—N3—C32 | 114.71 (11) | C22—C23—H23B | 109.9 |
C18—N4—C17 | 116.67 (11) | H23A—C23—H23B | 108.3 |
C18—N4—C28 | 115.02 (10) | O1—C24—C33 | 123.19 (13) |
C17—N4—C28 | 112.33 (10) | O1—C24—C1 | 116.02 (12) |
C36—C1—C24 | 117.38 (13) | C33—C24—C1 | 120.78 (13) |
C36—C1—N1 | 124.09 (13) | N1—C25—C26 | 113.49 (11) |
C24—C1—N1 | 118.53 (12) | N1—C25—H25A | 108.9 |
N1—C2—C3 | 112.71 (11) | C26—C25—H25A | 108.9 |
N1—C2—H2A | 109.1 | N1—C25—H25B | 108.9 |
C3—C2—H2A | 109.1 | C26—C25—H25B | 108.9 |
N1—C2—H2B | 109.1 | H25A—C25—H25B | 107.7 |
C3—C2—H2B | 109.1 | O10—C26—C25 | 105.30 (11) |
H2A—C2—H2B | 107.8 | O10—C26—H26A | 110.7 |
O7—C3—C2 | 113.23 (11) | C25—C26—H26A | 110.7 |
O7—C3—H3A | 108.9 | O10—C26—H26B | 110.7 |
C2—C3—H3A | 108.9 | C25—C26—H26B | 110.7 |
O7—C3—H3B | 108.9 | H26A—C26—H26B | 108.8 |
C2—C3—H3B | 108.9 | O10—C27—C28 | 105.58 (11) |
H3A—C3—H3B | 107.7 | O10—C27—H27A | 110.6 |
O7—C4—C5 | 107.11 (11) | C28—C27—H27A | 110.6 |
O7—C4—H4A | 110.3 | O10—C27—H27B | 110.6 |
C5—C4—H4A | 110.3 | C28—C27—H27B | 110.6 |
O7—C4—H4B | 110.3 | H27A—C27—H27B | 108.8 |
C5—C4—H4B | 110.3 | N4—C28—C27 | 112.35 (11) |
H4A—C4—H4B | 108.5 | N4—C28—H28A | 109.1 |
N2—C5—C4 | 112.14 (11) | C27—C28—H28A | 109.1 |
N2—C5—H5A | 109.2 | N4—C28—H28B | 109.1 |
C4—C5—H5A | 109.2 | C27—C28—H28B | 109.1 |
N2—C5—H5B | 109.2 | H28A—C28—H28B | 107.9 |
C4—C5—H5B | 109.2 | N2—C29—C30 | 112.61 (11) |
H5A—C5—H5B | 107.9 | N2—C29—H29A | 109.1 |
C37—C6—C7 | 117.58 (13) | C30—C29—H29A | 109.1 |
C37—C6—N2 | 123.77 (13) | N2—C29—H29B | 109.1 |
C7—C6—N2 | 118.61 (12) | C30—C29—H29B | 109.1 |
O4—C7—C40 | 123.25 (13) | H29A—C29—H29B | 107.8 |
O4—C7—C6 | 116.30 (12) | O8—C30—C29 | 105.48 (11) |
C40—C7—C6 | 120.44 (14) | O8—C30—H30A | 110.6 |
O4—C8—C9 | 109.01 (12) | C29—C30—H30A | 110.6 |
O4—C8—H8A | 109.9 | O8—C30—H30B | 110.6 |
C9—C8—H8A | 109.9 | C29—C30—H30B | 110.6 |
O4—C8—H8B | 109.9 | H30A—C30—H30B | 108.8 |
C9—C8—H8B | 109.9 | O8—C31—C32 | 105.44 (11) |
H8A—C8—H8B | 108.3 | O8—C31—H31A | 110.7 |
O5—C9—C8 | 109.97 (12) | C32—C31—H31A | 110.7 |
O5—C9—H9A | 109.7 | O8—C31—H31B | 110.7 |
C8—C9—H9A | 109.7 | C32—C31—H31B | 110.7 |
O5—C9—H9B | 109.7 | H31A—C31—H31B | 108.8 |
C8—C9—H9B | 109.7 | N3—C32—C31 | 113.60 (11) |
H9A—C9—H9B | 108.2 | N3—C32—H32A | 108.8 |
O5—C10—C11 | 109.79 (12) | C31—C32—H32A | 108.8 |
O5—C10—H10A | 109.7 | N3—C32—H32B | 108.8 |
C11—C10—H10A | 109.7 | C31—C32—H32B | 108.8 |
O5—C10—H10B | 109.7 | H32A—C32—H32B | 107.7 |
C11—C10—H10B | 109.7 | C34—C33—C24 | 120.15 (15) |
H10A—C10—H10B | 108.2 | C34—C33—H33A | 119.9 |
O6—C11—C10 | 108.63 (11) | C24—C33—H33A | 119.9 |
O6—C11—H11A | 110.0 | C35—C34—C33 | 120.14 (14) |
C10—C11—H11A | 110.0 | C35—C34—H34A | 119.9 |
O6—C11—H11B | 110.0 | C33—C34—H34A | 119.9 |
C10—C11—H11B | 110.0 | C34—C35—C36 | 119.82 (14) |
H11A—C11—H11B | 108.3 | C34—C35—H35A | 120.1 |
O6—C12—C41 | 123.24 (13) | C36—C35—H35A | 120.1 |
O6—C12—C13 | 115.77 (12) | C1—C36—C35 | 121.71 (15) |
C41—C12—C13 | 120.98 (13) | C1—C36—H36A | 119.1 |
C44—C13—C12 | 117.37 (13) | C35—C36—H36A | 119.1 |
C44—C13—N3 | 123.46 (13) | C6—C37—C38 | 121.58 (14) |
C12—C13—N3 | 119.12 (12) | C6—C37—H37A | 119.2 |
N3—C14—C15 | 112.21 (11) | C38—C37—H37A | 119.2 |
N3—C14—H14A | 109.2 | C39—C38—C37 | 120.03 (14) |
C15—C14—H14A | 109.2 | C39—C38—H38A | 120.0 |
N3—C14—H14B | 109.2 | C37—C38—H38A | 120.0 |
C15—C14—H14B | 109.2 | C38—C39—C40 | 119.59 (14) |
H14A—C14—H14B | 107.9 | C38—C39—H39A | 120.2 |
O9—C15—C14 | 112.74 (11) | C40—C39—H39A | 120.2 |
O9—C15—H15A | 109.0 | C39—C40—C7 | 120.51 (14) |
C14—C15—H15A | 109.0 | C39—C40—H40A | 119.7 |
O9—C15—H15B | 109.0 | C7—C40—H40A | 119.7 |
C14—C15—H15B | 109.0 | C12—C41—C42 | 120.05 (14) |
H15A—C15—H15B | 107.8 | C12—C41—H41A | 120.0 |
O9—C16—C17 | 107.77 (11) | C42—C41—H41A | 120.0 |
O9—C16—H16A | 110.2 | C43—C42—C41 | 119.82 (14) |
C17—C16—H16A | 110.2 | C43—C42—H42A | 120.1 |
O9—C16—H16B | 110.2 | C41—C42—H42A | 120.1 |
C17—C16—H16B | 110.2 | C42—C43—C44 | 120.29 (14) |
H16A—C16—H16B | 108.5 | C42—C43—H43A | 119.9 |
N4—C17—C16 | 111.12 (11) | C44—C43—H43A | 119.9 |
N4—C17—H17A | 109.4 | C13—C44—C43 | 121.46 (14) |
C16—C17—H17A | 109.4 | C13—C44—H44A | 119.3 |
N4—C17—H17B | 109.4 | C43—C44—H44A | 119.3 |
C16—C17—H17B | 109.4 | C18—C45—C46 | 121.59 (13) |
H17A—C17—H17B | 108.0 | C18—C45—H45A | 119.2 |
C45—C18—C19 | 117.80 (12) | C46—C45—H45A | 119.2 |
C45—C18—N4 | 123.61 (12) | C47—C46—C45 | 119.84 (14) |
C19—C18—N4 | 118.52 (12) | C47—C46—H46A | 120.1 |
O3—C19—C48 | 123.72 (13) | C45—C46—H46A | 120.1 |
O3—C19—C18 | 115.94 (12) | C46—C47—C48 | 119.67 (14) |
C48—C19—C18 | 120.34 (13) | C46—C47—H47A | 120.2 |
O3—C20—C21 | 107.92 (12) | C48—C47—H47A | 120.2 |
O3—C20—H20A | 110.1 | C47—C48—C19 | 120.57 (14) |
C21—C20—H20A | 110.1 | C47—C48—H48A | 119.7 |
O3—C20—H20B | 110.1 | C19—C48—H48A | 119.7 |
C2—N1—C1—C36 | 23.67 (19) | C19—O3—C20—C21 | 171.23 (11) |
C25—N1—C1—C36 | −117.26 (15) | C22—O2—C21—C20 | 176.25 (11) |
C2—N1—C1—C24 | −156.31 (12) | O3—C20—C21—O2 | 72.96 (14) |
C25—N1—C1—C24 | 62.75 (16) | C21—O2—C22—C23 | −165.57 (11) |
C1—N1—C2—C3 | 89.19 (14) | C24—O1—C23—C22 | −175.43 (11) |
C25—N1—C2—C3 | −129.89 (12) | O2—C22—C23—O1 | −81.66 (14) |
C4—O7—C3—C2 | 74.62 (15) | C23—O1—C24—C33 | −18.93 (19) |
N1—C2—C3—O7 | 68.00 (15) | C23—O1—C24—C1 | 162.06 (12) |
C3—O7—C4—C5 | −178.46 (11) | C36—C1—C24—O1 | −179.59 (12) |
C6—N2—C5—C4 | 71.58 (15) | N1—C1—C24—O1 | 0.40 (18) |
C29—N2—C5—C4 | −153.30 (12) | C36—C1—C24—C33 | 1.4 (2) |
O7—C4—C5—N2 | 178.02 (11) | N1—C1—C24—C33 | −178.64 (13) |
C5—N2—C6—C37 | 10.64 (19) | C1—N1—C25—C26 | −129.78 (13) |
C29—N2—C6—C37 | −123.17 (14) | C2—N1—C25—C26 | 87.94 (15) |
C5—N2—C6—C7 | −167.09 (12) | C27—O10—C26—C25 | −154.64 (12) |
C29—N2—C6—C7 | 59.10 (16) | N1—C25—C26—O10 | −177.96 (11) |
C8—O4—C7—C40 | −22.25 (19) | C26—O10—C27—C28 | 156.23 (12) |
C8—O4—C7—C6 | 158.36 (12) | C18—N4—C28—C27 | 135.92 (12) |
C37—C6—C7—O4 | −174.89 (12) | C17—N4—C28—C27 | −87.44 (14) |
N2—C6—C7—O4 | 2.97 (18) | O10—C27—C28—N4 | 169.47 (11) |
C37—C6—C7—C40 | 5.7 (2) | C6—N2—C29—C30 | −133.21 (12) |
N2—C6—C7—C40 | −176.43 (12) | C5—N2—C29—C30 | 90.65 (14) |
C7—O4—C8—C9 | −168.05 (11) | C31—O8—C30—C29 | −160.63 (11) |
C10—O5—C9—C8 | −175.67 (12) | N2—C29—C30—O8 | −173.31 (11) |
O4—C8—C9—O5 | −74.05 (15) | C30—O8—C31—C32 | 156.35 (11) |
C9—O5—C10—C11 | 165.85 (12) | C13—N3—C32—C31 | 130.20 (13) |
C12—O6—C11—C10 | 173.68 (11) | C14—N3—C32—C31 | −86.55 (14) |
O5—C10—C11—O6 | 78.07 (14) | O8—C31—C32—N3 | 175.81 (11) |
C11—O6—C12—C41 | 17.00 (19) | O1—C24—C33—C34 | −178.87 (13) |
C11—O6—C12—C13 | −162.07 (12) | C1—C24—C33—C34 | 0.1 (2) |
O6—C12—C13—C44 | 177.45 (12) | C24—C33—C34—C35 | −1.4 (2) |
C41—C12—C13—C44 | −1.6 (2) | C33—C34—C35—C36 | 1.2 (2) |
O6—C12—C13—N3 | −0.05 (18) | C24—C1—C36—C35 | −1.6 (2) |
C41—C12—C13—N3 | −179.14 (12) | N1—C1—C36—C35 | 178.42 (13) |
C14—N3—C13—C44 | −19.70 (19) | C34—C35—C36—C1 | 0.3 (2) |
C32—N3—C13—C44 | 122.40 (14) | C7—C6—C37—C38 | −2.6 (2) |
C14—N3—C13—C12 | 157.64 (12) | N2—C6—C37—C38 | 179.65 (13) |
C32—N3—C13—C12 | −60.26 (17) | C6—C37—C38—C39 | −1.9 (2) |
C13—N3—C14—C15 | −84.97 (14) | C37—C38—C39—C40 | 3.3 (2) |
C32—N3—C14—C15 | 132.30 (12) | C38—C39—C40—C7 | −0.2 (2) |
C16—O9—C15—C14 | −74.34 (14) | O4—C7—C40—C39 | 176.24 (13) |
N3—C14—C15—O9 | −68.88 (15) | C6—C7—C40—C39 | −4.4 (2) |
C15—O9—C16—C17 | 178.75 (10) | O6—C12—C41—C42 | −178.08 (13) |
C18—N4—C17—C16 | −71.38 (14) | C13—C12—C41—C42 | 0.9 (2) |
C28—N4—C17—C16 | 152.74 (11) | C12—C41—C42—C43 | 0.4 (2) |
O9—C16—C17—N4 | −179.24 (10) | C41—C42—C43—C44 | −1.0 (2) |
C17—N4—C18—C45 | −13.47 (18) | C12—C13—C44—C43 | 1.0 (2) |
C28—N4—C18—C45 | 121.24 (14) | N3—C13—C44—C43 | 178.42 (13) |
C17—N4—C18—C19 | 163.65 (12) | C42—C43—C44—C13 | 0.3 (2) |
C28—N4—C18—C19 | −61.63 (16) | C19—C18—C45—C46 | 1.8 (2) |
C20—O3—C19—C48 | 18.3 (2) | N4—C18—C45—C46 | 178.99 (12) |
C20—O3—C19—C18 | −162.15 (12) | C18—C45—C46—C47 | 1.5 (2) |
C45—C18—C19—O3 | 175.73 (12) | C45—C46—C47—C48 | −2.1 (2) |
N4—C18—C19—O3 | −1.57 (18) | C46—C47—C48—C19 | −0.8 (2) |
C45—C18—C19—C48 | −4.7 (2) | O3—C19—C48—C47 | −176.23 (13) |
N4—C18—C19—C48 | 178.02 (12) | C18—C19—C48—C47 | 4.2 (2) |
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