Supporting information
Portable Document Format (PDF) file https://doi.org/10.1107/S0907444908040602/dz5137sup3.pdf | |
Crystallographic Information File (CIF) https://doi.org/10.1107/S0907444908040602/dz5137sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0907444908040602/dz5137CYCLOsup2.hkl |
CCDC reference: 725429
Program(s) used to refine structure: Volkov et al., (2006); molecular graphics: Volkov et al., (2006); software used to prepare material for publication: Volkov et al., (2006).
C62H111N11O12·0.754(H2O) | Dx = 1.159 Mg m−3 |
Mr = 1216.21 | Melting point: 150 K |
Orthorhombic, P212121 | Monochromated synchrotron radiation radiation, λ = 0.6261 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 19564 reflections |
a = 12.4960 (15) Å | θ = 10–34.7° |
b = 15.6450 (14) Å | µ = 0.81 mm−1 |
c = 35.653 (3) Å | T = 5 K |
V = 6970.2 (12) Å3 | Rectangle, colorless |
Z = 4 | 0.5 × 0.3 × 0.3 mm |
F(000) = 2654.2 |
Diffractometer X10SA beamline at the SLS | Rint = 0.008 |
Radiation source: Synchrotron | θmax = 34.7° |
φ scans | h = −22→22 |
246948 measured reflections | k = 0→26 |
40848 independent reflections | l = 0→63 |
40377 reflections with F2 > 3σ F2 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.025 | w2 = 1/[s2(Fo2)] |
wR(F2) = 0.057 | (Δ/σ)max < 0.001 |
S = 3.70 | Δρmax = 0.26 e Å−3 |
40377 reflections | Δρmin = −0.25 e Å−3 |
1279 parameters |
Experimental. A helium gas-flow low temperature device was used. |
Refinement. A rotationally disordered methyl group was modeled with an alternative position for all three hydrogen atoms. Friedel pairs were not merged, as the molecule is chiral and the accuracy of the measurement (Rint = 0.8%) suggested that anomalous dispersion might otherwise cause a small effect. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
O(10) | 0.71584 (3) | 0.45769 (2) | 0.159103 (9) | 0.015 | |
O(20) | 0.46835 (3) | 0.33545 (2) | 0.210138 (10) | 0.015 | |
O(30) | 0.47100 (3) | 0.31127 (2) | 0.082536 (9) | 0.015 | |
O(40) | 0.57974 (3) | 0.04789 (2) | 0.083755 (9) | 0.014 | |
O(50) | 0.50842 (3) | −0.00420 (2) | −0.039859 (9) | 0.017 | |
O(60) | 0.72506 (3) | −0.21223 (3) | 0.022315 (9) | 0.018 | |
O(70) | 0.51275 (3) | −0.18019 (2) | 0.081466 (9) | 0.015 | |
O(80) | 0.85154 (3) | −0.14240 (2) | 0.136386 (10) | 0.018 | |
O(83) | 0.13203 (4) | 0.12882 (3) | 0.15930 (2) | 0.016 | 0.7535 |
O(90) | 0.70443 (3) | 0.12044 (2) | 0.158550 (9) | 0.014 | |
O(100) | 0.98466 (3) | 0.21649 (2) | 0.214158 (9) | 0.014 | |
O(112) | 0.78463 (9) | 0.47479 (7) | 0.29324 (6) | 0.028 | |
O(82) | 0.98512 (4) | 0.09172 (4) | 0.098737 (16) | 0.017 | |
N(1) | 0.66662 (4) | 0.49925 (2) | 0.217935 (13) | 0.013 | |
N(2) | 0.49587 (3) | 0.39590 (3) | 0.153107 (11) | 0.013 | |
N(3) | 0.52331 (3) | 0.22102 (3) | 0.128792 (10) | 0.011 | |
N(4) | 0.55815 (3) | 0.15633 (3) | 0.042278 (10) | 0.012 | |
N(5) | 0.50350 (3) | −0.05472 (3) | 0.019874 (11) | 0.012 | |
N(6) | 0.56012 (3) | −0.21472 (3) | −0.004558 (10) | 0.013 | |
N(7) | 0.63821 (3) | −0.28292 (3) | 0.086176 (11) | 0.014 | |
N(8) | 0.68459 (3) | −0.09033 (3) | 0.124308 (10) | 0.013 | |
N(9) | 0.85700 (3) | 0.04122 (3) | 0.160384 (13) | 0.013 | |
N(10) | 0.80291 (3) | 0.21968 (3) | 0.216361 (9) | 0.011 | |
N(11) | 0.86538 (3) | 0.38341 (3) | 0.254319 (13) | 0.011 | |
C(10) | 0.64513 (3) | 0.47638 (3) | 0.181699 (11) | 0.012 | |
C(11) | 0.52775 (3) | 0.47818 (3) | 0.168235 (12) | 0.014 | |
C(12) | 0.51840 (4) | 0.54566 (3) | 0.137448 (15) | 0.022 | |
C(20) | 0.46899 (3) | 0.32994 (3) | 0.175737 (11) | 0.011 | |
C(21) | 0.43857 (3) | 0.24726 (3) | 0.154615 (11) | 0.011 | |
C(22) | 0.41280 (3) | 0.17486 (3) | 0.181477 (12) | 0.016 | |
C(30) | 0.53030 (3) | 0.25354 (3) | 0.093978 (10) | 0.011 | |
C(31) | 0.61554 (3) | 0.21390 (3) | 0.068453 (10) | 0.011 | |
C(32) | 0.68019 (3) | 0.28506 (3) | 0.049891 (11) | 0.014 | |
C(33) | 0.74094 (3) | 0.33789 (3) | 0.079485 (11) | 0.014 | |
C(34) | 0.83741 (4) | 0.28963 (4) | 0.095300 (16) | 0.024 | |
C(35) | 0.77454 (4) | 0.42377 (3) | 0.063075 (14) | 0.02 | |
C(40) | 0.53671 (3) | 0.07668 (3) | 0.055106 (10) | 0.011 | |
C(41) | 0.45293 (3) | 0.02149 (3) | 0.034963 (11) | 0.012 | |
C(42) | 0.36347 (3) | −0.00011 (3) | 0.063244 (13) | 0.016 | |
C(43) | 0.28185 (4) | −0.06076 (4) | 0.045810 (16) | 0.022 | |
C(44) | 0.30894 (4) | 0.08230 (4) | 0.076526 (15) | 0.022 | |
C(50) | 0.52752 (3) | −0.06097 (3) | −0.017065 (11) | 0.012 | |
C(51) | 0.58811 (3) | −0.14227 (3) | −0.028767 (10) | 0.012 | |
C(52) | 0.57661 (3) | −0.16320 (3) | −0.070463 (11) | 0.015 | |
C(53) | 0.66077 (4) | −0.22789 (3) | −0.083662 (12) | 0.017 | |
C(54) | 0.63000 (5) | −0.26572 (4) | −0.121691 (13) | 0.024 | |
C(55) | 0.77243 (4) | −0.18782 (4) | −0.085714 (13) | 0.025 | |
C(60) | 0.63397 (3) | −0.24200 (3) | 0.020608 (11) | 0.013 | |
C(61) | 0.60256 (4) | −0.31108 (4) | 0.048982 (14) | 0.015 | |
C(70) | 0.58864 (3) | −0.21188 (3) | 0.099053 (11) | 0.013 | |
C(71) | 0.62660 (3) | −0.16760 (3) | 0.135102 (11) | 0.014 | |
C(72) | 0.53095 (4) | −0.14225 (4) | 0.159740 (12) | 0.018 | |
C(73) | 0.46817 (4) | −0.21852 (4) | 0.174821 (14) | 0.025 | |
C(80) | 0.79182 (3) | −0.08296 (3) | 0.127391 (10) | 0.012 | |
C(81) | 0.83493 (3) | 0.00821 (3) | 0.122307 (10) | 0.011 | |
C(82) | 0.93361 (3) | 0.01112 (3) | 0.096541 (12) | 0.012 | |
C(83) | 0.90050 (3) | −0.00582 (3) | 0.055479 (11) | 0.014 | |
C(84) | 0.99937 (4) | −0.02497 (4) | 0.031706 (13) | 0.02 | |
C(85) | 0.83840 (3) | 0.07067 (3) | 0.039014 (11) | 0.015 | |
C(86) | 0.78517 (4) | 0.05137 (4) | 0.002412 (15) | 0.017 | |
C(87) | 0.80823 (5) | 0.09019 (5) | −0.029835 (16) | 0.021 | |
C(88) | 0.75411 (5) | 0.07418 (5) | −0.066681 (13) | 0.027 | |
C(90) | 0.78429 (3) | 0.09502 (3) | 0.175743 (12) | 0.011 | |
C(91) | 0.80054 (3) | 0.12539 (3) | 0.216315 (10) | 0.011 | |
C(92) | 0.71360 (3) | 0.08651 (3) | 0.241846 (11) | 0.012 | |
C(93) | 0.72558 (4) | 0.11886 (3) | 0.282125 (12) | 0.017 | |
C(94) | 0.72085 (3) | −0.01135 (3) | 0.240461 (12) | 0.015 | |
C(100) | 0.90038 (3) | 0.25782 (3) | 0.215157 (10) | 0.01 | |
C(101) | 0.90243 (3) | 0.35677 (3) | 0.216712 (10) | 0.01 | |
C(1E) | 1.01516 (3) | 0.39128 (3) | 0.208961 (10) | 0.011 | |
C(1F) | 1.05531 (3) | 0.37922 (3) | 0.168479 (10) | 0.012 | |
C(1G) | 1.17765 (3) | 0.37478 (4) | 0.167837 (12) | 0.019 | |
C(1H) | 1.01475 (3) | 0.45108 (3) | 0.142930 (11) | 0.015 | |
C(110) | 0.80936 (11) | 0.45521 (13) | 0.26114 (6) | 0.015 | |
C(111) | 0.77855 (4) | 0.51478 (3) | 0.228948 (13) | 0.011 | |
C(1I) | 0.79521 (3) | 0.60766 (3) | 0.240856 (11) | 0.012 | |
C(1J) | 0.79179 (3) | 0.67188 (3) | 0.208441 (11) | 0.012 | |
C(1K) | 0.77918 (4) | 0.76220 (3) | 0.224407 (12) | 0.016 | |
C(1L) | 0.89301 (4) | 0.66501 (3) | 0.184305 (12) | 0.016 | |
C(19) | 0.58265 (4) | 0.51434 (4) | 0.245851 (13) | 0.02 | |
C(49) | 0.51246 (5) | 0.19114 (3) | 0.007706 (13) | 0.021 | |
C(69) | 0.44913 (3) | −0.24466 (3) | −0.005451 (13) | 0.017 | |
C(79) | 0.73965 (4) | −0.31743 (3) | 0.100163 (13) | 0.017 | |
C(99) | 0.94614 (12) | 0.00409 (9) | 0.18099 (3) | 0.025 | |
C(98) | 0.70301 (3) | 0.26801 (3) | 0.212472 (12) | 0.013 | |
C(97) | 0.90127 (3) | 0.33210 (3) | 0.286270 (11) | 0.014 | |
H(83A) | 0.161374 | 0.080824 | 0.172944 | 0.043 (5) | 0.7535 |
H(83B) | 0.094147 | 0.165724 | 0.176531 | 0.053 (5) | 0.7535 |
H(82A) | 1.026496 | 0.095024 | 0.121544 | 0.049 (6) | |
H(2) | 0.493764 | 0.387578 | 0.125052 | 0.038 (3) | |
H(3) | 0.577937 | 0.177589 | 0.137225 | 0.042 (3) | |
H(5) | 0.521113 | −0.103907 | 0.037108 | 0.031 (3) | |
H(8) | 0.642675 | −0.040339 | 0.114118 | 0.039 (3) | |
H(11) | 0.475082 | 0.495478 | 0.191727 | 0.034 (2) | |
H(12A) | 0.542794 | 0.60593 | 0.147925 | 0.052 (2) | |
H(12B) | 0.438017 | 0.549422 | 0.128186 | 0.062 (3) | |
H(12C) | 0.56814 | 0.528356 | 0.11463 | 0.053 (3) | |
H(21) | 0.36624 | 0.260678 | 0.138095 | 0.037 (2) | |
H(22A) | 0.384014 | 0.121566 | 0.166196 | 0.044 (2) | |
H(22B) | 0.353449 | 0.195302 | 0.200689 | 0.062 (3) | |
H(22C) | 0.482931 | 0.157339 | 0.196275 | 0.060 (3) | |
H(31) | 0.669922 | 0.17533 | 0.085787 | 0.023 (2) | |
H(32A) | 0.626382 | 0.32683 | 0.03419 | 0.041 (2) | |
H(32B) | 0.737323 | 0.256962 | 0.030269 | 0.056 (3) | |
H(33) | 0.685585 | 0.350623 | 0.102776 | 0.038 (3) | |
H(34A) | 0.874184 | 0.326864 | 0.116495 | 0.041 (2) | |
H(34B) | 0.893309 | 0.277745 | 0.073592 | 0.062 (3) | |
H(34C) | 0.811609 | 0.230749 | 0.106827 | 0.056 (3) | |
H(35A) | 0.827679 | 0.41372 | 0.040359 | 0.060 (3) | |
H(35B) | 0.813427 | 0.460572 | 0.083949 | 0.051 (2) | |
H(35C) | 0.705944 | 0.457114 | 0.053582 | 0.049 (2) | |
H(41) | 0.418184 | 0.058703 | 0.01183 | 0.029 (2) | |
H(42) | 0.399632 | −0.031951 | 0.087623 | 0.033 (2) | |
H(43A) | 0.318502 | −0.120417 | 0.040157 | 0.067 (3) | |
H(43B) | 0.252663 | −0.034055 | 0.020506 | 0.054 (3) | |
H(43C) | 0.217159 | −0.069932 | 0.064571 | 0.057 (3) | |
H(44A) | 0.247838 | 0.067256 | 0.096022 | 0.050 (2) | |
H(44B) | 0.274859 | 0.114238 | 0.053219 | 0.058 (3) | |
H(44C) | 0.366278 | 0.122677 | 0.089349 | 0.052 (2) | |
H(51) | 0.673413 | −0.12917 | −0.023949 | 0.034 (2) | |
H(52A) | 0.496876 | −0.189219 | −0.075648 | 0.045 (3) | |
H(52B) | 0.584752 | −0.104478 | −0.086771 | 0.038 (2) | |
H(53) | 0.663552 | −0.280353 | −0.063187 | 0.039 (3) | |
H(54A) | 0.626692 | −0.21625 | −0.141935 | 0.044 (2) | |
H(54B) | 0.553921 | −0.295194 | −0.1197 | 0.051 (2) | |
H(54C) | 0.68752 | −0.311778 | −0.12989 | 0.066 (3) | |
H(55A) | 0.829313 | −0.23556 | −0.092482 | 0.067 (3) | |
H(55B) | 0.792024 | −0.160037 | −0.059513 | 0.061 (3) | |
H(55C) | 0.773107 | −0.139862 | −0.106677 | 0.054 (3) | |
H(61A) | 0.515931 | −0.320247 | 0.048745 | 0.020 (3) | |
H(61B) | 0.640476 | −0.371699 | 0.041646 | 0.033 (3) | |
H(71) | 0.679785 | −0.210687 | 0.150765 | 0.023 (2) | |
H(72A) | 0.559983 | −0.104089 | 0.183282 | 0.040 (2) | |
H(72B) | 0.477014 | −0.101938 | 0.143373 | 0.051 (3) | |
H(73A) | 0.43655 | −0.25429 | 0.152172 | 0.049 (2) | |
H(73B) | 0.404707 | −0.196683 | 0.192017 | 0.074 (3) | |
H(73C) | 0.51987 | −0.258069 | 0.190717 | 0.049 (2) | |
H(81) | 0.771443 | 0.047405 | 0.109686 | 0.031 (2) | |
H(82) | 0.990209 | −0.03887 | 0.105234 | 0.026 (3) | |
H(83) | 0.848001 | −0.062162 | 0.054888 | 0.035 (3) | |
H(84A) | 1.038102 | −0.080297 | 0.042122 | 0.046 (2) | |
H(84B) | 1.052683 | 0.027579 | 0.032922 | 0.049 (2) | |
H(84C) | 0.975925 | −0.035479 | 0.003538 | 0.053 (3) | |
H(85A) | 0.777372 | 0.090686 | 0.059101 | 0.039 (2) | |
H(85B) | 0.893752 | 0.123963 | 0.035166 | 0.052 (3) | |
H(86) | 0.723873 | 0.002989 | 0.001916 | 0.046 (6) | |
H(87) | 0.871696 | 0.13676 | −0.029361 | 0.062 (6) | |
H(88A) | 0.811105 | 0.052256 | −0.086446 | 0.073 (3) | |
H(88B) | 0.719579 | 0.131902 | −0.076387 | 0.074 (3) | |
H(88C) | 0.693293 | 0.027671 | −0.063301 | 0.064 (3) | |
H(91) | 0.878796 | 0.102058 | 0.225963 | 0.028 (2) | |
H(92) | 0.634724 | 0.106084 | 0.231261 | 0.029 (2) | |
H(93A) | 0.71512 | 0.186013 | 0.28277 | 0.045 (2) | |
H(93B) | 0.802822 | 0.103179 | 0.292227 | 0.052 (2) | |
H(93C) | 0.667058 | 0.089347 | 0.299267 | 0.048 (2) | |
H(94A) | 0.661243 | −0.038161 | 0.257994 | 0.043 (2) | |
H(94B) | 0.797342 | −0.031132 | 0.249847 | 0.043 (2) | |
H(94C) | 0.70892 | −0.03267 | 0.212582 | 0.048 (2) | |
H(101) | 0.847102 | 0.382076 | 0.195478 | 0.0223 (19) | |
H(11E) | 1.071224 | 0.359612 | 0.227905 | 0.035 (2) | |
H(12E) | 1.016231 | 0.45945 | 0.215519 | 0.034 (2) | |
H(1F) | 1.023924 | 0.318256 | 0.157824 | 0.034 (2) | |
H(11G) | 1.204444 | 0.364472 | 0.140023 | 0.052 (2) | |
H(12G) | 1.20384 | 0.323901 | 0.185144 | 0.057 (3) | |
H(13G) | 1.209485 | 0.43313 | 0.177942 | 0.055 (3) | |
H(11H) | 1.05034 | 0.509652 | 0.151058 | 0.037 (2) | |
H(12H) | 0.930501 | 0.45595 | 0.145331 | 0.048 (2) | |
H(13H) | 1.035517 | 0.437253 | 0.114779 | 0.048 (2) | |
H(111) | 0.826469 | 0.502011 | 0.207196 | 0.028 (4) | |
H(11I) | 0.872607 | 0.61298 | 0.254882 | 0.037 (2) | |
H(12I) | 0.733251 | 0.624693 | 0.261122 | 0.033 (2) | |
H(1J) | 0.721794 | 0.657548 | 0.190871 | 0.031 (2) | |
H(11K) | 0.703159 | 0.768101 | 0.237277 | 0.059 (3) | |
H(12K) | 0.785729 | 0.807498 | 0.202456 | 0.042 (2) | |
H(13K) | 0.839999 | 0.773652 | 0.244472 | 0.050 (2) | |
H(11L) | 0.895113 | 0.716324 | 0.164949 | 0.049 (2) | |
H(12L) | 0.892538 | 0.606195 | 0.169602 | 0.047 (2) | |
H(13L) | 0.961612 | 0.667885 | 0.201699 | 0.035 (2) | |
H(19A) | 0.541787 | 0.572399 | 0.239539 | 0.040 (2) | |
H(19B) | 0.617814 | 0.519151 | 0.27301 | 0.048 (3) | |
H(19C) | 0.526751 | 0.462871 | 0.245555 | 0.038 (2) | |
H(49A) | 0.50653 | 0.14164 | −0.012737 | 0.035 (2) | |
H(49B) | 0.562607 | 0.240843 | −0.002749 | 0.069 (3) | |
H(49C) | 0.434688 | 0.216216 | 0.013171 | 0.056 (3) | |
H(69A) | 0.446894 | −0.309382 | −0.014767 | 0.053 (3) | |
H(69B) | 0.403505 | −0.205899 | −0.024129 | 0.039 (2) | |
H(69C) | 0.415361 | −0.240796 | 0.021953 | 0.048 (3) | |
H(79A) | 0.791735 | −0.330225 | 0.077159 | 0.078 (6) | 0.7172 |
H(79B) | 0.724617 | −0.375274 | 0.115061 | 0.050 (5) | 0.7172 |
H(79C) | 0.77607 | −0.272084 | 0.118468 | 0.058 (5) | 0.7172 |
H(79D) | 0.736534 | −0.321629 | 0.129986 | 0.092 (18) | 0.2828 |
H(79E) | 0.798358 | −0.27976 | 0.092735 | 0.10 (2) | 0.2828 |
H(79F) | 0.752106 | −0.379605 | 0.088737 | 0.092 (18) | 0.2828 |
H(99A) | 0.97776 | 0.044696 | 0.202284 | 0.078 (4) | |
H(99B) | 1.001017 | −0.030407 | 0.163814 | 0.058 (4) | |
H(99C) | 0.908232 | −0.045557 | 0.19657 | 0.060 (4) | |
H(98A) | 0.698457 | 0.315242 | 0.233962 | 0.048 (3) | |
H(98B) | 0.63654 | 0.225651 | 0.214864 | 0.042 (2) | |
H(98C) | 0.701045 | 0.298682 | 0.185782 | 0.053 (3) | |
H(97A) | 0.891666 | 0.367868 | 0.311495 | 0.041 (2) | |
H(97B) | 0.98347 | 0.315697 | 0.28278 | 0.049 (3) | |
H(97C) | 0.854853 | 0.275055 | 0.287897 | 0.045 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
O(10) | 0.01254 (11) | 0.02118 (17) | 0.01157 (11) | 0.00190 (10) | 0.00115 (9) | −0.00154 (11) |
O(20) | 0.01604 (13) | 0.01693 (17) | 0.01332 (12) | 0.00025 (11) | 0.00172 (8) | −0.00133 (10) |
O(30) | 0.01504 (12) | 0.01702 (15) | 0.01305 (12) | 0.00437 (11) | −0.00160 (9) | 0.00261 (11) |
O(40) | 0.01471 (12) | 0.01369 (15) | 0.01439 (11) | −0.00038 (10) | −0.00338 (9) | 0.00135 (10) |
O(50) | 0.01850 (14) | 0.01901 (16) | 0.01439 (12) | 0.00582 (12) | 0.00068 (9) | 0.00212 (12) |
O(60) | 0.01039 (12) | 0.02656 (18) | 0.01746 (13) | −0.00020 (11) | −0.00166 (9) | 0.00645 (13) |
O(70) | 0.01387 (11) | 0.01545 (15) | 0.01467 (11) | 0.00016 (10) | −0.00092 (9) | −0.00102 (11) |
O(80) | 0.01476 (13) | 0.01377 (16) | 0.02580 (16) | 0.00193 (11) | −0.00160 (10) | 0.00419 (12) |
O(83) | 0.0153 (2) | 0.0194 (3) | 0.0137 (3) | 0.0002 (2) | −0.00076 (12) | 0.00039 (15) |
O(90) | 0.01137 (11) | 0.01607 (15) | 0.01418 (11) | 0.00442 (10) | −0.00316 (9) | −0.00150 (11) |
O(100) | 0.00893 (11) | 0.01273 (15) | 0.02141 (14) | 0.00135 (10) | 0.00047 (8) | 0.00243 (11) |
O(112) | 0.0395 (4) | 0.0294 (3) | 0.0158 (3) | 0.0168 (3) | 0.00907 (18) | 0.0058 (2) |
O(82) | 0.01723 (16) | 0.0175 (2) | 0.01523 (17) | −0.00676 (16) | −0.00294 (14) | 0.00289 (16) |
N(1) | 0.01299 (16) | 0.0124 (2) | 0.01266 (16) | −0.00103 (11) | 0.00289 (12) | −0.00336 (12) |
N(2) | 0.01428 (13) | 0.01134 (17) | 0.01399 (14) | −0.00160 (11) | 0.00119 (9) | −0.00042 (12) |
N(3) | 0.01011 (11) | 0.01099 (15) | 0.01056 (12) | 0.00151 (10) | 0.00019 (9) | 0.00134 (10) |
N(4) | 0.01447 (13) | 0.01223 (17) | 0.01056 (12) | −0.00103 (11) | −0.00250 (9) | −0.00039 (11) |
N(5) | 0.01258 (12) | 0.01254 (17) | 0.01204 (13) | 0.00132 (11) | −0.00038 (9) | −0.00141 (12) |
N(6) | 0.01056 (12) | 0.01394 (16) | 0.01311 (12) | 0.00005 (11) | −0.00123 (9) | −0.00104 (12) |
N(7) | 0.01599 (13) | 0.01306 (17) | 0.01334 (13) | −0.00007 (12) | −0.00120 (10) | 0.00041 (12) |
N(8) | 0.01132 (13) | 0.01230 (17) | 0.01566 (14) | −0.00157 (11) | −0.00101 (9) | 0.00187 (12) |
N(9) | 0.01139 (14) | 0.01369 (18) | 0.01277 (15) | 0.00366 (14) | −0.00305 (11) | −0.00326 (14) |
N(10) | 0.00852 (12) | 0.00869 (16) | 0.01438 (13) | 0.00018 (10) | −0.00096 (8) | −0.00022 (10) |
N(11) | 0.01203 (13) | 0.01057 (18) | 0.00989 (16) | 0.00076 (14) | 0.00026 (9) | 0.00091 (13) |
C(10) | 0.01143 (13) | 0.01109 (17) | 0.01274 (14) | 0.00078 (11) | 0.00125 (10) | −0.00102 (12) |
C(11) | 0.01188 (13) | 0.01110 (18) | 0.01933 (16) | 0.00069 (12) | 0.00015 (11) | −0.00160 (13) |
C(12) | 0.02014 (19) | 0.0140 (2) | 0.0311 (2) | −0.00010 (15) | −0.00694 (15) | 0.00550 (17) |
C(20) | 0.01001 (12) | 0.01202 (18) | 0.01215 (14) | −0.00005 (11) | 0.00133 (9) | −0.00063 (12) |
C(21) | 0.00916 (12) | 0.01229 (17) | 0.01234 (13) | −0.00067 (11) | 0.00132 (9) | 0.00045 (11) |
C(22) | 0.01621 (15) | 0.01549 (19) | 0.01670 (15) | −0.00369 (13) | 0.00259 (11) | 0.00338 (14) |
C(30) | 0.01056 (12) | 0.01209 (17) | 0.01014 (13) | 0.00122 (11) | −0.00076 (9) | 0.00109 (11) |
C(31) | 0.01196 (13) | 0.01239 (17) | 0.01003 (12) | −0.00035 (11) | −0.00027 (9) | −0.00084 (11) |
C(32) | 0.01495 (14) | 0.01580 (19) | 0.01118 (14) | −0.00265 (13) | 0.00094 (10) | −0.00047 (12) |
C(33) | 0.01401 (14) | 0.01450 (19) | 0.01360 (14) | −0.00260 (12) | 0.00082 (10) | −0.00106 (12) |
C(34) | 0.01998 (19) | 0.0209 (2) | 0.0314 (2) | −0.00008 (16) | −0.01011 (16) | −0.00305 (19) |
C(35) | 0.02192 (19) | 0.0181 (2) | 0.02149 (18) | −0.00728 (16) | 0.00207 (14) | 0.00186 (16) |
C(40) | 0.01057 (12) | 0.01174 (17) | 0.01124 (13) | 0.00057 (11) | −0.00107 (9) | −0.00087 (12) |
C(41) | 0.00987 (12) | 0.01296 (18) | 0.01380 (14) | 0.00044 (11) | −0.00083 (9) | −0.00196 (12) |
C(42) | 0.01065 (13) | 0.0181 (2) | 0.01917 (16) | −0.00028 (12) | 0.00243 (11) | −0.00276 (15) |
C(43) | 0.01365 (16) | 0.0215 (2) | 0.0322 (2) | −0.00400 (15) | 0.00321 (14) | −0.00586 (19) |
C(44) | 0.01414 (16) | 0.0237 (2) | 0.0290 (2) | 0.00132 (15) | 0.00475 (14) | −0.00897 (19) |
C(50) | 0.01079 (12) | 0.01419 (18) | 0.01177 (14) | 0.00209 (12) | −0.00066 (10) | −0.00043 (12) |
C(51) | 0.01020 (12) | 0.01486 (18) | 0.01124 (13) | 0.00135 (11) | −0.00085 (9) | −0.00154 (12) |
C(52) | 0.01321 (14) | 0.0200 (2) | 0.01166 (13) | 0.00270 (13) | −0.00180 (10) | −0.00253 (13) |
C(53) | 0.01775 (16) | 0.0213 (2) | 0.01236 (14) | 0.00519 (14) | −0.00032 (11) | −0.00332 (14) |
C(54) | 0.0279 (2) | 0.0288 (3) | 0.01571 (17) | 0.00378 (19) | −0.00086 (14) | −0.00822 (18) |
C(55) | 0.01432 (17) | 0.0405 (3) | 0.01939 (17) | 0.00411 (18) | 0.00126 (12) | −0.0061 (2) |
C(60) | 0.01141 (13) | 0.01535 (18) | 0.01248 (14) | 0.00131 (12) | −0.00054 (10) | 0.00049 (13) |
C(61) | 0.01792 (17) | 0.01231 (19) | 0.01517 (16) | −0.00018 (13) | −0.00053 (13) | −0.00118 (14) |
C(70) | 0.01331 (13) | 0.01267 (18) | 0.01246 (13) | −0.00162 (12) | −0.00024 (10) | 0.00027 (12) |
C(71) | 0.01491 (14) | 0.01401 (18) | 0.01331 (14) | −0.00386 (12) | −0.00048 (10) | 0.00119 (13) |
C(72) | 0.01985 (17) | 0.0207 (2) | 0.01490 (15) | −0.00717 (15) | 0.00424 (12) | −0.00278 (14) |
C(73) | 0.0271 (2) | 0.0286 (3) | 0.01875 (18) | −0.0137 (2) | 0.00492 (15) | 0.00075 (18) |
C(80) | 0.01117 (14) | 0.01001 (17) | 0.01459 (14) | 0.00029 (12) | −0.00107 (9) | 0.00106 (12) |
C(81) | 0.00988 (12) | 0.01029 (16) | 0.01214 (13) | 0.00056 (11) | −0.00097 (9) | −0.00064 (11) |
C(82) | 0.00940 (13) | 0.0127 (2) | 0.01484 (15) | 0.00032 (13) | −0.00030 (11) | 0.00006 (13) |
C(83) | 0.01186 (13) | 0.01437 (18) | 0.01435 (14) | −0.00027 (12) | 0.00117 (10) | −0.00158 (12) |
C(84) | 0.01640 (16) | 0.0234 (2) | 0.02060 (17) | 0.00350 (15) | 0.00561 (13) | −0.00300 (16) |
C(85) | 0.01416 (14) | 0.0179 (2) | 0.01274 (14) | 0.00111 (13) | −0.00027 (11) | −0.00001 (13) |
C(86) | 0.01464 (16) | 0.0252 (2) | 0.01227 (19) | −0.00472 (18) | 0.00011 (12) | 0.00133 (17) |
C(87) | 0.02097 (19) | 0.0300 (3) | 0.0124 (2) | −0.0079 (2) | −0.00003 (14) | 0.00199 (19) |
C(88) | 0.0256 (2) | 0.0434 (4) | 0.01309 (16) | −0.0116 (2) | −0.00181 (14) | 0.00152 (19) |
C(90) | 0.00958 (13) | 0.01056 (17) | 0.01172 (14) | 0.00194 (12) | −0.00193 (10) | −0.00084 (12) |
C(91) | 0.00983 (12) | 0.00923 (16) | 0.01246 (13) | 0.00066 (10) | −0.00110 (9) | −0.00026 (11) |
C(92) | 0.01137 (13) | 0.01091 (17) | 0.01467 (14) | −0.00078 (11) | −0.00030 (10) | 0.00076 (12) |
C(93) | 0.01975 (17) | 0.0164 (2) | 0.01452 (15) | −0.00304 (14) | 0.00274 (12) | −0.00148 (14) |
C(94) | 0.01732 (15) | 0.01066 (18) | 0.01757 (15) | −0.00136 (13) | −0.00215 (11) | 0.00135 (13) |
C(100) | 0.00834 (12) | 0.00973 (17) | 0.01335 (13) | 0.00016 (11) | −0.00027 (9) | 0.00065 (11) |
C(101) | 0.00924 (12) | 0.00995 (16) | 0.01053 (12) | −0.00023 (10) | −0.00038 (9) | 0.00048 (11) |
C(1E) | 0.00963 (12) | 0.01300 (17) | 0.01128 (12) | −0.00174 (11) | −0.00031 (9) | 0.00116 (11) |
C(1F) | 0.01080 (12) | 0.01426 (18) | 0.01148 (13) | 0.00044 (11) | 0.00042 (9) | 0.00070 (12) |
C(1G) | 0.01138 (14) | 0.0302 (3) | 0.01599 (15) | 0.00325 (14) | 0.00166 (11) | 0.00245 (16) |
C(1H) | 0.01523 (14) | 0.01590 (19) | 0.01304 (14) | 0.00041 (13) | −0.00036 (10) | 0.00286 (13) |
C(110) | 0.01991 (19) | 0.0150 (2) | 0.01045 (19) | 0.00488 (17) | 0.00466 (14) | 0.00253 (16) |
C(111) | 0.01346 (15) | 0.01023 (19) | 0.01061 (15) | 0.00126 (11) | 0.00106 (12) | 0.00058 (12) |
C(1I) | 0.01391 (14) | 0.01238 (18) | 0.01089 (13) | 0.00056 (12) | −0.00112 (10) | −0.00155 (12) |
C(1J) | 0.01278 (13) | 0.01050 (17) | 0.01264 (13) | −0.00041 (11) | −0.00142 (10) | −0.00098 (11) |
C(1K) | 0.01885 (16) | 0.01092 (19) | 0.01857 (16) | 0.00035 (13) | −0.00139 (12) | −0.00301 (13) |
C(1L) | 0.01624 (15) | 0.01425 (19) | 0.01794 (16) | −0.00036 (13) | 0.00327 (12) | 0.00076 (14) |
C(19) | 0.01522 (16) | 0.0252 (2) | 0.01882 (16) | −0.00240 (15) | 0.00583 (12) | −0.00877 (16) |
C(49) | 0.0319 (2) | 0.0169 (2) | 0.01543 (16) | −0.00389 (17) | −0.01040 (15) | 0.00263 (15) |
C(69) | 0.01236 (14) | 0.0176 (2) | 0.02140 (17) | −0.00262 (13) | −0.00191 (11) | −0.00298 (15) |
C(79) | 0.01858 (18) | 0.0161 (2) | 0.01729 (16) | 0.00205 (15) | −0.00183 (13) | 0.00078 (14) |
C(99) | 0.0211 (2) | 0.0351 (4) | 0.0201 (2) | 0.0174 (2) | −0.00942 (18) | −0.0103 (2) |
C(98) | 0.00914 (12) | 0.01080 (17) | 0.02046 (16) | 0.00102 (11) | −0.00123 (10) | 0.00036 (13) |
C(97) | 0.01665 (15) | 0.01337 (18) | 0.01157 (13) | −0.00087 (12) | −0.00167 (10) | 0.00213 (12) |
O(10)—C(10) | 1.2309 (5) | C(61)—H(61A) | 1.0920 |
O(20)—C(20) | 1.2295 (5) | C(61)—H(61B) | 1.0920 |
O(30)—C(30) | 1.2374 (5) | C(70)—C(71) | 1.5352 (6) |
O(40)—C(40) | 1.2391 (5) | C(71)—C(72) | 1.5355 (6) |
O(50)—C(50) | 1.2273 (6) | C(71)—H(71) | 1.0990 |
O(60)—C(60) | 1.2314 (5) | C(72)—C(73) | 1.5259 (7) |
O(70)—C(70) | 1.2403 (5) | C(72)—H(72A) | 1.0920 |
O(80)—C(80) | 1.2347 (6) | C(72)—H(72B) | 1.0920 |
O(83)—H(83A) | 0.9670 | C(73)—H(73A) | 1.0590 |
O(83)—H(83B) | 0.9670 | C(73)—H(73B) | 1.0590 |
O(90)—C(90) | 1.2368 (5) | C(73)—H(73C) | 1.0590 |
O(100)—C(100) | 1.2363 (5) | C(80)—C(81) | 1.5355 (6) |
O(112)—C(110) | 1.224 (3) | C(81)—C(82) | 1.5384 (6) |
O(82)—C(82) | 1.4179 (8) | C(81)—H(81) | 1.0990 |
O(82)—H(82A) | 0.9650 | C(82)—H(82) | 1.0990 |
N(1)—C(10) | 1.3672 (6) | C(83)—C(84) | 1.5279 (6) |
N(1)—C(19) | 1.4654 (6) | C(83)—H(83) | 1.0990 |
N(2)—C(11) | 1.4515 (6) | C(84)—H(84A) | 1.0590 |
N(2)—C(20) | 1.3523 (6) | C(84)—H(84B) | 1.0590 |
N(2)—H(2) | 1.0090 | C(84)—H(84C) | 1.0590 |
N(3)—C(21) | 1.4620 (5) | C(85)—C(86) | 1.4955 (7) |
N(3)—C(30) | 1.3443 (5) | C(85)—H(85A) | 1.0920 |
N(3)—H(3) | 1.0090 | C(85)—H(85B) | 1.0920 |
N(4)—C(40) | 1.3541 (6) | C(86)—C(87) | 1.3318 (8) |
N(4)—C(49) | 1.4635 (6) | C(86)—H(86) | 1.0770 |
N(5)—C(41) | 1.4527 (6) | C(87)—C(88) | 1.4986 (8) |
N(5)—C(50) | 1.3543 (5) | C(87)—H(87) | 1.0770 |
N(5)—H(5) | 1.0090 | C(88)—H(88A) | 1.0590 |
N(6)—C(51) | 1.4670 (6) | C(88)—H(88B) | 1.0590 |
N(6)—C(60) | 1.3560 (6) | C(88)—H(88C) | 1.0590 |
N(6)—C(69) | 1.4643 (6) | C(90)—C(91) | 1.5360 (6) |
N(7)—C(61) | 1.4666 (7) | C(91)—H(91) | 1.0990 |
N(7)—C(70) | 1.3526 (6) | C(92)—C(93) | 1.5300 (6) |
N(7)—C(79) | 1.4653 (7) | C(92)—C(94) | 1.5344 (6) |
N(8)—C(71) | 1.4611 (6) | C(92)—H(92) | 1.0990 |
N(8)—C(80) | 1.3494 (5) | C(93)—H(93A) | 1.0590 |
N(8)—H(8) | 1.0090 | C(93)—H(93B) | 1.0590 |
N(9)—C(90) | 1.3542 (7) | C(93)—H(93C) | 1.0590 |
N(9)—C(99) | 1.4553 (17) | C(94)—H(94A) | 1.0590 |
N(10)—C(100) | 1.3570 (5) | C(94)—H(94B) | 1.0590 |
N(10)—C(98) | 1.4661 (5) | C(94)—H(94C) | 1.0590 |
N(11)—C(110) | 1.346 (2) | C(101)—C(1E) | 1.5336 (5) |
N(11)—C(97) | 1.4640 (6) | C(101)—H(101) | 1.0990 |
C(11)—C(12) | 1.5274 (7) | C(1E)—C(1F) | 1.5396 (5) |
C(11)—H(11) | 1.0990 | C(1E)—H(11E) | 1.0920 |
C(12)—H(12A) | 1.0590 (5) | C(1E)—H(12E) | 1.0920 |
C(12)—H(12B) | 1.0590 (5) | C(1F)—C(1G) | 1.5305 (6) |
C(12)—H(12C) | 1.0590 (6) | C(1F)—C(1H) | 1.5331 (6) |
C(21)—C(22) | 1.5178 (6) | C(1F)—H(1F) | 1.0990 |
C(21)—H(21) | 1.0990 | C(1G)—H(11G) | 1.0590 |
C(22)—H(22A) | 1.0590 | C(1G)—H(12G) | 1.0590 |
C(22)—H(22B) | 1.0590 | C(1G)—H(13G) | 1.0590 |
C(22)—H(22C) | 1.0590 | C(1H)—H(11H) | 1.0590 |
C(30)—C(31) | 1.5321 (5) | C(1H)—H(12H) | 1.0590 |
C(31)—C(32) | 1.5265 (6) | C(1H)—H(13H) | 1.0590 |
C(31)—H(31) | 1.0990 | C(110)—C(111) | 1.528 (2) |
C(32)—H(32A) | 1.0920 | C(111)—C(1I) | 1.5281 (6) |
C(32)—H(32B) | 1.0920 | C(111)—H(111) | 1.0000 |
C(33)—C(34) | 1.5300 (7) | C(1I)—C(1J) | 1.5320 (6) |
C(33)—C(35) | 1.5245 (7) | C(1I)—H(11I) | 1.0920 |
C(33)—H(33) | 1.0990 | C(1I)—H(12I) | 1.0920 |
C(34)—H(34A) | 1.0590 | C(1J)—C(1K) | 1.5315 (6) |
C(34)—H(34B) | 1.0590 | C(1J)—C(1L) | 1.5336 (6) |
C(34)—H(34C) | 1.0590 | C(1J)—H(1J) | 1.0990 |
C(35)—H(35A) | 1.0590 | C(1K)—H(11K) | 1.0590 |
C(35)—H(35B) | 1.0590 | C(1K)—H(12K) | 1.0590 |
C(35)—H(35C) | 1.0590 | C(1K)—H(13K) | 1.0590 |
C(40)—C(41) | 1.5354 (6) | C(1L)—H(11L) | 1.0590 |
C(41)—H(41) | 1.0990 | C(1L)—H(12L) | 1.0590 |
C(42)—C(43) | 1.5255 (7) | C(1L)—H(13L) | 1.0590 |
C(42)—C(44) | 1.5333 (7) | C(19)—H(19A) | 1.0660 |
C(42)—H(42) | 1.0990 | C(19)—H(19B) | 1.0660 |
C(43)—H(43A) | 1.0590 | C(19)—H(19C) | 1.0660 |
C(43)—H(43B) | 1.0590 | C(49)—H(49A) | 1.0660 |
C(43)—H(43C) | 1.0590 | C(49)—H(49B) | 1.0660 |
C(44)—H(44A) | 1.0590 | C(49)—H(49C) | 1.0660 |
C(44)—H(44B) | 1.0590 | C(69)—H(69A) | 1.0660 |
C(44)—H(44C) | 1.0590 | C(69)—H(69B) | 1.0660 |
C(50)—C(51) | 1.5379 (6) | C(69)—H(69C) | 1.0660 |
C(51)—C(52) | 1.5290 (5) | C(79)—H(79A) | 1.0660 |
C(51)—H(51) | 1.0990 | C(79)—H(79B) | 1.0660 |
C(52)—C(53) | 1.5336 (6) | C(79)—H(79C) | 1.0660 |
C(52)—H(52A) | 1.0920 | C(79)—H(79D) | 1.0660 |
C(52)—H(52B) | 1.0920 | C(79)—H(79E) | 0.9776 |
C(53)—C(54) | 1.5285 (6) | C(79)—H(79F) | 1.0660 |
C(53)—C(55) | 1.5315 (7) | C(99)—H(99A) | 1.0660 |
C(53)—H(53) | 1.0990 | C(99)—H(99B) | 1.0660 |
C(54)—H(54A) | 1.0590 | C(99)—H(99C) | 1.0660 |
C(54)—H(54B) | 1.0590 | C(98)—H(98A) | 1.0660 |
C(54)—H(54C) | 1.0590 | C(98)—H(98B) | 1.0660 |
C(55)—H(55A) | 1.0590 | C(98)—H(98C) | 1.0660 |
C(55)—H(55B) | 1.0590 | C(97)—H(97A) | 1.0660 |
C(55)—H(55C) | 1.0590 | C(97)—H(97B) | 1.0660 |
C(60)—C(61) | 1.5314 (7) | C(97)—H(97C) | 1.0660 |
C(10)—N(1)—C(19) | 122.91 (4) | C(54)—C(53)—C(55) | 110.20 (4) |
C(11)—N(2)—C(20) | 121.55 (4) | O(60)—C(60)—N(6) | 122.86 (4) |
C(21)—N(3)—C(30) | 121.48 (4) | O(60)—C(60)—C(61) | 118.12 (4) |
C(40)—N(4)—C(49) | 123.35 (4) | N(6)—C(60)—C(61) | 119.00 (4) |
C(41)—N(5)—C(50) | 121.05 (4) | N(7)—C(61)—C(60) | 107.91 (4) |
C(51)—N(6)—C(60) | 118.05 (4) | O(70)—C(70)—N(7) | 120.46 (4) |
C(51)—N(6)—C(69) | 117.40 (4) | O(70)—C(70)—C(71) | 118.63 (4) |
C(60)—N(6)—C(69) | 123.94 (4) | N(7)—C(70)—C(71) | 120.89 (4) |
C(61)—N(7)—C(70) | 114.49 (4) | N(8)—C(71)—C(70) | 107.83 (3) |
C(61)—N(7)—C(79) | 117.37 (4) | N(8)—C(71)—C(72) | 108.84 (4) |
C(70)—N(7)—C(79) | 125.69 (4) | C(70)—C(71)—C(72) | 110.80 (3) |
C(71)—N(8)—C(80) | 122.80 (4) | C(71)—C(72)—C(73) | 113.56 (5) |
C(90)—N(9)—C(99) | 123.89 (6) | O(80)—C(80)—N(8) | 123.84 (4) |
C(100)—N(10)—C(98) | 122.31 (4) | O(80)—C(80)—C(81) | 121.22 (4) |
C(110)—N(11)—C(97) | 118.45 (10) | N(8)—C(80)—C(81) | 114.72 (4) |
O(10)—C(10)—N(1) | 122.66 (4) | C(80)—C(81)—C(82) | 112.28 (4) |
N(2)—C(11)—C(12) | 108.97 (4) | O(82)—C(82)—C(81) | 110.93 (4) |
O(20)—C(20)—N(2) | 122.91 (4) | C(85)—C(86)—C(87) | 124.40 (6) |
N(3)—C(21)—C(22) | 109.97 (4) | C(86)—C(87)—C(88) | 125.65 (6) |
O(30)—C(30)—N(3) | 122.80 (4) | O(90)—C(90)—N(9) | 122.74 (4) |
O(30)—C(30)—C(31) | 121.06 (3) | O(90)—C(90)—C(91) | 118.29 (4) |
N(3)—C(30)—C(31) | 116.13 (4) | N(9)—C(90)—C(91) | 118.97 (4) |
C(30)—C(31)—C(32) | 109.28 (4) | C(93)—C(92)—C(94) | 110.76 (3) |
C(34)—C(33)—C(35) | 111.06 (4) | O(100)—C(100)—N(10) | 122.38 (4) |
O(40)—C(40)—N(4) | 121.81 (4) | C(101)—C(1E)—C(1F) | 115.16 (3) |
O(40)—C(40)—C(41) | 118.49 (4) | C(1E)—C(1F)—C(1G) | 110.19 (3) |
N(4)—C(40)—C(41) | 119.63 (3) | C(1E)—C(1F)—C(1H) | 111.06 (3) |
N(5)—C(41)—C(40) | 109.77 (3) | C(1G)—C(1F)—C(1H) | 110.77 (4) |
C(43)—C(42)—C(44) | 110.59 (4) | O(112)—C(110)—N(11) | 120.61 (16) |
O(50)—C(50)—N(5) | 123.27 (4) | O(112)—C(110)—C(111) | 119.07 (16) |
O(50)—C(50)—C(51) | 120.97 (4) | N(11)—C(110)—C(111) | 120.30 (16) |
N(5)—C(50)—C(51) | 115.63 (4) | C(110)—C(111)—C(1I) | 109.70 (8) |
N(6)—C(51)—C(50) | 111.23 (3) | C(110)—C(111)—H(111) | 108.05 (9) |
N(6)—C(51)—C(52) | 112.59 (4) | C(111)—C(1I)—C(1J) | 114.22 (3) |
C(50)—C(51)—C(52) | 113.24 (3) | C(1I)—C(1J)—C(1K) | 109.12 (3) |
C(51)—C(52)—C(53) | 112.04 (3) | C(1I)—C(1J)—C(1L) | 110.75 (3) |
C(52)—C(53)—C(54) | 110.81 (4) | C(1I)—C(1J)—H(1J) | 108.56 (3) |
C(52)—C(53)—C(55) | 111.67 (4) | C(1K)—C(1J)—C(1L) | 110.99 (4) |