Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805031867/dn6262sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805031867/dn6262Isup2.hkl |
CCDC reference: 289717
Data collection: COLLECT (Hooft, 1998); cell refinement: HKL-2000 (Otwinowski & Minor, 1997); data reduction: HKL-2000; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL (Bruker, 1999); PLATON (Spek, 2003).
(C9H14N)[UO2(C36H45O6)]·CHCl3 | F(000) = 2200 |
Mr = 1099.33 | Dx = 1.554 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 82013 reflections |
a = 9.6605 (3) Å | θ = 2.6–25.7° |
b = 21.2825 (10) Å | µ = 3.68 mm−1 |
c = 22.8491 (11) Å | T = 100 K |
V = 4697.8 (3) Å3 | Platelet, translucent dark orange |
Z = 4 | 0.14 × 0.12 × 0.04 mm |
Nonius KappaCCD area-detector diffractometer | 8750 independent reflections |
Radiation source: fine-focus sealed tube | 8052 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
two φ and one ω scans with 2° steps | θmax = 25.7°, θmin = 2.6° |
Absorption correction: part of the refinement model (ΔF) (DELABS in PLATON; Spek, 2003) | h = −11→11 |
Tmin = 0.527, Tmax = 0.863 | k = −25→25 |
82013 measured reflections | l = −25→27 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.065 | w = 1/[σ2(Fo2) + (0.0114P)2 + 4.555P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.003 |
8750 reflections | Δρmax = 0.80 e Å−3 |
543 parameters | Δρmin = −0.83 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 3779 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.010 (5) |
Experimental. crystal-to-detector distance 30 mm |
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 | ||
U | 0.270765 (17) | 0.586874 (8) | 0.744028 (8) | 0.02301 (5) | |
O1 | 0.3555 (3) | 0.49034 (15) | 0.73374 (17) | 0.0270 (9) | |
O2 | 0.3296 (4) | 0.56025 (16) | 0.62763 (17) | 0.0279 (8) | |
O3 | 0.1384 (4) | 0.64170 (17) | 0.68204 (17) | 0.0269 (8) | |
O4 | 0.2648 (4) | 0.71740 (15) | 0.76827 (15) | 0.0292 (8) | |
O5 | 0.2990 (4) | 0.60517 (16) | 0.83913 (15) | 0.0268 (8) | |
O6 | 0.5806 (4) | 0.53292 (17) | 0.82365 (17) | 0.0309 (9) | |
O7 | 0.1103 (3) | 0.55040 (16) | 0.76366 (17) | 0.0280 (9) | |
O8 | 0.4380 (3) | 0.61994 (15) | 0.72896 (15) | 0.0227 (8) | |
C1 | 0.5930 (4) | 0.4623 (2) | 0.7440 (3) | 0.0240 (11) | |
C2 | 0.4776 (6) | 0.4769 (2) | 0.7099 (2) | 0.0258 (12) | |
C3 | 0.4931 (5) | 0.4786 (2) | 0.6488 (2) | 0.0256 (12) | |
C4 | 0.6212 (5) | 0.4651 (2) | 0.6235 (3) | 0.0260 (12) | |
H4 | 0.6296 | 0.4664 | 0.5830 | 0.031* | |
C5 | 0.7372 (6) | 0.4495 (2) | 0.6571 (2) | 0.0254 (11) | |
C6 | 0.7209 (6) | 0.4490 (2) | 0.7174 (2) | 0.0269 (11) | |
H6 | 0.7967 | 0.4396 | 0.7409 | 0.032* | |
C7 | 0.8767 (6) | 0.4370 (2) | 0.6275 (3) | 0.0296 (13) | |
C8 | 0.8606 (6) | 0.3909 (3) | 0.5763 (3) | 0.0362 (14) | |
H8A | 0.8196 | 0.3526 | 0.5902 | 0.054* | |
H8B | 0.9499 | 0.3820 | 0.5599 | 0.054* | |
H8C | 0.8022 | 0.4092 | 0.5469 | 0.054* | |
C9 | 0.9360 (7) | 0.4990 (3) | 0.6032 (4) | 0.052 (2) | |
H9A | 1.0244 | 0.4911 | 0.5855 | 0.079* | |
H9B | 0.9467 | 0.5286 | 0.6345 | 0.079* | |
H9C | 0.8737 | 0.5158 | 0.5744 | 0.079* | |
C10 | 0.9856 (5) | 0.4103 (3) | 0.6698 (2) | 0.0353 (13) | |
H10A | 0.9561 | 0.3698 | 0.6835 | 0.053* | |
H10B | 0.9963 | 0.4382 | 0.7025 | 0.053* | |
H10C | 1.0726 | 0.4061 | 0.6498 | 0.053* | |
C11 | 0.3696 (6) | 0.4964 (2) | 0.6118 (3) | 0.0308 (13) | |
H11A | 0.3935 | 0.4944 | 0.5706 | 0.037* | |
H11B | 0.2936 | 0.4676 | 0.6190 | 0.037* | |
C12 | 0.2606 (5) | 0.5949 (2) | 0.5811 (2) | 0.0285 (11) | |
H12A | 0.1650 | 0.5814 | 0.5777 | 0.034* | |
H12B | 0.3065 | 0.5872 | 0.5440 | 0.034* | |
C13 | 0.2663 (5) | 0.6636 (2) | 0.5958 (2) | 0.0224 (10) | |
C14 | 0.2077 (5) | 0.6831 (2) | 0.6488 (2) | 0.0238 (11) | |
C15 | 0.2317 (6) | 0.7447 (2) | 0.6683 (2) | 0.0261 (12) | |
C16 | 0.3008 (5) | 0.7864 (2) | 0.6322 (2) | 0.0275 (12) | |
H16 | 0.3155 | 0.8272 | 0.6453 | 0.033* | |
C17 | 0.3490 (5) | 0.7696 (3) | 0.5771 (2) | 0.0252 (12) | |
C18 | 0.3331 (5) | 0.7068 (2) | 0.5606 (2) | 0.0220 (11) | |
H18 | 0.3685 | 0.6937 | 0.5247 | 0.026* | |
C19 | 0.4236 (6) | 0.8185 (3) | 0.5385 (2) | 0.0291 (13) | |
C20 | 0.5631 (6) | 0.8360 (3) | 0.5657 (3) | 0.0422 (16) | |
H20A | 0.6054 | 0.8688 | 0.5431 | 0.063* | |
H20B | 0.6224 | 0.7998 | 0.5660 | 0.063* | |
H20C | 0.5490 | 0.8503 | 0.6051 | 0.063* | |
C21 | 0.4494 (6) | 0.7927 (3) | 0.4759 (3) | 0.0330 (13) | |
H21A | 0.4860 | 0.8255 | 0.4516 | 0.049* | |
H21B | 0.3637 | 0.7779 | 0.4597 | 0.049* | |
H21C | 0.5144 | 0.7586 | 0.4777 | 0.049* | |
C22 | 0.3327 (7) | 0.8777 (3) | 0.5334 (3) | 0.0409 (15) | |
H22A | 0.3141 | 0.8940 | 0.5718 | 0.061* | |
H22B | 0.2471 | 0.8671 | 0.5146 | 0.061* | |
H22C | 0.3804 | 0.9089 | 0.5107 | 0.061* | |
C23 | 0.1897 (5) | 0.7600 (2) | 0.7301 (2) | 0.0282 (12) | |
H23A | 0.2128 | 0.8032 | 0.7393 | 0.034* | |
H23B | 0.0908 | 0.7544 | 0.7349 | 0.034* | |
C24 | 0.2588 (6) | 0.7353 (3) | 0.8295 (2) | 0.0299 (13) | |
H24A | 0.1748 | 0.7192 | 0.8473 | 0.036* | |
H24B | 0.2591 | 0.7807 | 0.8332 | 0.036* | |
C25 | 0.3835 (5) | 0.7079 (3) | 0.8591 (2) | 0.0255 (12) | |
C26 | 0.3977 (5) | 0.6421 (2) | 0.8618 (2) | 0.0233 (11) | |
C27 | 0.5194 (6) | 0.6165 (3) | 0.8859 (2) | 0.0244 (12) | |
C28 | 0.6215 (6) | 0.6565 (3) | 0.9075 (2) | 0.0281 (13) | |
H28 | 0.7002 | 0.6390 | 0.9243 | 0.034* | |
C29 | 0.6104 (5) | 0.7220 (3) | 0.9049 (2) | 0.0253 (12) | |
C30 | 0.4899 (5) | 0.7458 (3) | 0.8802 (2) | 0.0298 (13) | |
H30 | 0.4797 | 0.7892 | 0.8777 | 0.036* | |
C31 | 0.7293 (6) | 0.7638 (2) | 0.9267 (2) | 0.0317 (12) | |
C32 | 0.7572 (7) | 0.7514 (3) | 0.9916 (3) | 0.0462 (16) | |
H32A | 0.6772 | 0.7628 | 1.0141 | 0.069* | |
H32B | 0.8351 | 0.7759 | 1.0041 | 0.069* | |
H32C | 0.7768 | 0.7076 | 0.9972 | 0.069* | |
C33 | 0.6949 (6) | 0.8347 (3) | 0.9200 (3) | 0.0368 (14) | |
H33A | 0.6111 | 0.8441 | 0.9408 | 0.055* | |
H33B | 0.6831 | 0.8445 | 0.8793 | 0.055* | |
H33C | 0.7694 | 0.8593 | 0.9357 | 0.055* | |
C34 | 0.8622 (6) | 0.7499 (3) | 0.8909 (3) | 0.0406 (16) | |
H34A | 0.9376 | 0.7744 | 0.9061 | 0.061* | |
H34B | 0.8471 | 0.7608 | 0.8506 | 0.061* | |
H34C | 0.8843 | 0.7061 | 0.8938 | 0.061* | |
C35 | 0.5409 (6) | 0.5474 (3) | 0.8833 (3) | 0.0305 (13) | |
H35A | 0.6133 | 0.5348 | 0.9103 | 0.037* | |
H35B | 0.4564 | 0.5255 | 0.8936 | 0.037* | |
C36 | 0.5785 (6) | 0.4670 (3) | 0.8099 (2) | 0.0287 (13) | |
H36A | 0.4921 | 0.4482 | 0.8226 | 0.034* | |
H36B | 0.6544 | 0.4455 | 0.8291 | 0.034* | |
N1 | 0.7241 (5) | 0.6128 (2) | 0.7176 (2) | 0.0305 (10) | |
H1A | 0.6360 | 0.6173 | 0.7297 | 0.037* | |
H1B | 0.7342 | 0.5730 | 0.7048 | 0.037* | |
C37 | 0.7489 (6) | 0.6569 (2) | 0.6669 (2) | 0.0296 (12) | |
H37 | 0.8420 | 0.6487 | 0.6516 | 0.035* | |
C38 | 0.6448 (6) | 0.6425 (3) | 0.6182 (3) | 0.0344 (15) | |
H38A | 0.5525 | 0.6480 | 0.6328 | 0.041* | |
H38B | 0.6567 | 0.5999 | 0.6053 | 0.041* | |
H38C | 0.6600 | 0.6705 | 0.5859 | 0.041* | |
C39 | 0.8171 (6) | 0.6226 (3) | 0.7681 (3) | 0.0407 (16) | |
H39A | 0.9108 | 0.6262 | 0.7545 | 0.061* | |
H39B | 0.8098 | 0.5875 | 0.7943 | 0.061* | |
H39C | 0.7911 | 0.6604 | 0.7882 | 0.061* | |
C40 | 0.7427 (5) | 0.7246 (2) | 0.6861 (2) | 0.0234 (11) | |
C41 | 0.8540 (5) | 0.7639 (3) | 0.6729 (2) | 0.0269 (12) | |
H41 | 0.9307 | 0.7480 | 0.6532 | 0.032* | |
C42 | 0.8499 (6) | 0.8275 (3) | 0.6892 (3) | 0.0360 (14) | |
H42 | 0.9226 | 0.8540 | 0.6791 | 0.043* | |
C43 | 0.7383 (6) | 0.8509 (2) | 0.7204 (2) | 0.0342 (13) | |
H43 | 0.7370 | 0.8926 | 0.7325 | 0.041* | |
C44 | 0.6294 (6) | 0.8116 (2) | 0.7334 (3) | 0.0336 (14) | |
H44 | 0.5536 | 0.8274 | 0.7537 | 0.040* | |
C45 | 0.6304 (5) | 0.7491 (3) | 0.7170 (3) | 0.0291 (13) | |
H45 | 0.5560 | 0.7233 | 0.7265 | 0.035* | |
C46 | 0.0711 (7) | 0.5242 (3) | 0.9009 (3) | 0.0426 (16) | |
H46 | 0.1105 | 0.5454 | 0.8666 | 0.051* | |
Cl1 | −0.0905 (3) | 0.49365 (17) | 0.88148 (16) | 0.1219 (14) | |
Cl2 | 0.0520 (4) | 0.57911 (13) | 0.95616 (12) | 0.1363 (14) | |
Cl3 | 0.1795 (2) | 0.46306 (10) | 0.92023 (10) | 0.0676 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
U | 0.02195 (8) | 0.02348 (8) | 0.02359 (9) | −0.00157 (7) | 0.00174 (7) | 0.00063 (9) |
O1 | 0.0275 (19) | 0.0228 (18) | 0.031 (2) | 0.0011 (14) | 0.0068 (16) | 0.0008 (16) |
O2 | 0.033 (2) | 0.0210 (18) | 0.029 (2) | 0.0054 (15) | −0.0062 (16) | −0.0030 (16) |
O3 | 0.026 (2) | 0.027 (2) | 0.028 (2) | 0.0000 (16) | −0.0003 (15) | 0.0031 (16) |
O4 | 0.032 (2) | 0.0325 (18) | 0.0235 (19) | 0.0079 (16) | −0.0027 (17) | −0.0015 (14) |
O5 | 0.028 (2) | 0.031 (2) | 0.0218 (19) | −0.0028 (15) | 0.0012 (15) | 0.0015 (14) |
O6 | 0.045 (2) | 0.025 (2) | 0.023 (2) | −0.0010 (17) | 0.0054 (17) | −0.0015 (16) |
O7 | 0.0274 (18) | 0.0277 (19) | 0.029 (2) | 0.0009 (14) | 0.0009 (16) | −0.0011 (17) |
O8 | 0.0220 (18) | 0.0200 (17) | 0.026 (2) | 0.0025 (14) | −0.0017 (14) | 0.0005 (15) |
C1 | 0.026 (2) | 0.019 (2) | 0.027 (3) | −0.0002 (17) | 0.004 (2) | 0.002 (3) |
C2 | 0.030 (3) | 0.017 (3) | 0.031 (3) | 0.000 (2) | 0.007 (2) | −0.001 (2) |
C3 | 0.029 (3) | 0.022 (3) | 0.026 (3) | 0.001 (2) | −0.002 (2) | −0.004 (2) |
C4 | 0.032 (3) | 0.019 (3) | 0.028 (3) | 0.000 (2) | 0.003 (2) | −0.007 (2) |
C5 | 0.027 (3) | 0.014 (2) | 0.035 (3) | −0.001 (2) | 0.002 (2) | −0.001 (2) |
C6 | 0.025 (3) | 0.015 (2) | 0.041 (3) | 0.003 (2) | 0.001 (2) | 0.000 (2) |
C7 | 0.029 (3) | 0.015 (3) | 0.046 (4) | −0.004 (2) | 0.002 (2) | −0.002 (2) |
C8 | 0.033 (3) | 0.043 (4) | 0.032 (4) | 0.007 (3) | −0.001 (2) | −0.002 (3) |
C9 | 0.034 (4) | 0.050 (4) | 0.073 (6) | −0.003 (3) | 0.015 (4) | −0.004 (4) |
C10 | 0.033 (3) | 0.033 (3) | 0.040 (3) | 0.006 (3) | −0.003 (2) | −0.005 (3) |
C11 | 0.033 (3) | 0.022 (3) | 0.038 (4) | −0.001 (2) | 0.002 (2) | −0.004 (2) |
C12 | 0.032 (3) | 0.027 (3) | 0.026 (3) | −0.001 (3) | −0.003 (2) | 0.000 (2) |
C13 | 0.021 (3) | 0.022 (2) | 0.024 (3) | −0.002 (2) | −0.007 (2) | −0.0025 (19) |
C14 | 0.020 (3) | 0.025 (3) | 0.026 (3) | 0.000 (2) | −0.004 (2) | 0.003 (2) |
C15 | 0.026 (3) | 0.028 (3) | 0.024 (3) | 0.002 (3) | 0.000 (2) | −0.002 (2) |
C16 | 0.033 (3) | 0.022 (3) | 0.027 (3) | 0.001 (2) | −0.005 (2) | −0.002 (2) |
C17 | 0.021 (3) | 0.031 (3) | 0.023 (3) | −0.001 (2) | −0.006 (2) | 0.001 (2) |
C18 | 0.020 (3) | 0.027 (3) | 0.019 (3) | 0.002 (2) | 0.000 (2) | −0.002 (2) |
C19 | 0.031 (3) | 0.029 (3) | 0.027 (3) | −0.004 (2) | 0.000 (2) | 0.004 (2) |
C20 | 0.044 (4) | 0.047 (4) | 0.035 (4) | −0.017 (3) | −0.005 (3) | 0.003 (3) |
C21 | 0.035 (3) | 0.032 (3) | 0.032 (4) | −0.004 (3) | −0.001 (2) | 0.004 (3) |
C22 | 0.062 (4) | 0.030 (3) | 0.030 (4) | 0.002 (3) | −0.001 (3) | 0.012 (3) |
C23 | 0.025 (3) | 0.032 (3) | 0.028 (3) | 0.008 (2) | −0.002 (2) | −0.005 (2) |
C24 | 0.036 (4) | 0.031 (3) | 0.022 (3) | 0.003 (3) | −0.001 (2) | −0.005 (2) |
C25 | 0.027 (3) | 0.031 (3) | 0.019 (3) | 0.006 (2) | 0.001 (2) | −0.004 (2) |
C26 | 0.028 (3) | 0.027 (3) | 0.015 (3) | −0.002 (2) | 0.004 (2) | −0.003 (2) |
C27 | 0.028 (3) | 0.028 (3) | 0.017 (3) | −0.004 (2) | −0.002 (2) | 0.005 (2) |
C28 | 0.034 (3) | 0.030 (3) | 0.021 (3) | −0.004 (2) | −0.001 (2) | 0.005 (2) |
C29 | 0.026 (3) | 0.031 (3) | 0.018 (3) | −0.004 (2) | 0.003 (2) | 0.001 (2) |
C30 | 0.033 (3) | 0.029 (3) | 0.027 (3) | 0.003 (2) | 0.002 (2) | −0.001 (2) |
C31 | 0.031 (3) | 0.030 (3) | 0.034 (3) | −0.005 (3) | −0.007 (3) | 0.002 (2) |
C32 | 0.054 (4) | 0.044 (4) | 0.040 (3) | −0.015 (3) | −0.013 (3) | 0.003 (3) |
C33 | 0.038 (4) | 0.034 (3) | 0.039 (4) | −0.004 (3) | −0.006 (3) | −0.002 (3) |
C34 | 0.030 (3) | 0.037 (4) | 0.055 (5) | −0.005 (3) | 0.002 (3) | −0.006 (3) |
C35 | 0.037 (3) | 0.022 (3) | 0.032 (4) | −0.003 (2) | −0.001 (3) | 0.005 (2) |
C36 | 0.034 (3) | 0.024 (3) | 0.027 (3) | 0.001 (2) | 0.001 (2) | 0.006 (2) |
N1 | 0.026 (2) | 0.023 (2) | 0.043 (3) | 0.001 (2) | 0.005 (2) | 0.0066 (18) |
C37 | 0.026 (3) | 0.027 (3) | 0.035 (3) | 0.002 (2) | 0.009 (2) | 0.003 (2) |
C38 | 0.037 (4) | 0.036 (4) | 0.031 (4) | −0.009 (3) | 0.006 (3) | −0.002 (3) |
C39 | 0.029 (3) | 0.047 (4) | 0.046 (4) | 0.002 (3) | −0.003 (3) | 0.017 (3) |
C40 | 0.022 (3) | 0.025 (3) | 0.023 (3) | 0.002 (2) | −0.003 (2) | 0.003 (2) |
C41 | 0.029 (3) | 0.025 (3) | 0.027 (3) | 0.005 (2) | −0.002 (2) | −0.001 (2) |
C42 | 0.036 (4) | 0.028 (3) | 0.043 (4) | −0.007 (3) | −0.010 (3) | 0.002 (3) |
C43 | 0.042 (4) | 0.021 (3) | 0.039 (3) | 0.005 (3) | −0.008 (3) | −0.007 (2) |
C44 | 0.035 (3) | 0.031 (3) | 0.034 (4) | 0.011 (2) | 0.000 (2) | −0.007 (3) |
C45 | 0.024 (3) | 0.026 (3) | 0.037 (4) | 0.001 (2) | 0.004 (2) | 0.002 (2) |
C46 | 0.049 (4) | 0.045 (4) | 0.034 (4) | 0.002 (3) | 0.005 (3) | 0.003 (3) |
Cl1 | 0.0419 (13) | 0.150 (3) | 0.174 (3) | −0.0300 (16) | −0.0248 (15) | 0.088 (2) |
Cl2 | 0.286 (4) | 0.0694 (18) | 0.0534 (16) | 0.029 (2) | 0.036 (2) | −0.0101 (14) |
Cl3 | 0.0557 (11) | 0.0666 (12) | 0.0804 (15) | 0.0139 (10) | 0.0060 (10) | 0.0290 (11) |
U—O1 | 2.224 (3) | C21—H21C | 0.9600 |
U—O2 | 2.778 (4) | C22—H22A | 0.9600 |
U—O3 | 2.237 (4) | C22—H22B | 0.9600 |
U—O4 | 2.833 (3) | C22—H22C | 0.9600 |
U—O5 | 2.224 (4) | C23—H23A | 0.9700 |
U—O7 | 1.791 (3) | C23—H23B | 0.9700 |
U—O8 | 1.795 (3) | C24—C25 | 1.500 (8) |
U—C14 | 3.049 (5) | C24—H24A | 0.9700 |
O1—C2 | 1.331 (6) | C24—H24B | 0.9700 |
O2—C12 | 1.457 (6) | C25—C30 | 1.393 (8) |
O2—C11 | 1.459 (6) | C25—C26 | 1.409 (7) |
O3—C14 | 1.342 (6) | C26—C27 | 1.407 (8) |
O4—C24 | 1.450 (6) | C27—C28 | 1.393 (8) |
O4—C23 | 1.452 (6) | C27—C35 | 1.487 (7) |
O5—C26 | 1.340 (6) | C28—C29 | 1.400 (8) |
O6—C36 | 1.438 (6) | C28—H28 | 0.9300 |
O6—C35 | 1.448 (7) | C29—C30 | 1.389 (7) |
C1—C2 | 1.395 (7) | C29—C31 | 1.536 (7) |
C1—C6 | 1.406 (7) | C30—H30 | 0.9300 |
C1—C36 | 1.515 (8) | C31—C32 | 1.529 (8) |
C2—C3 | 1.403 (8) | C31—C34 | 1.552 (8) |
C3—C4 | 1.396 (7) | C31—C33 | 1.552 (7) |
C3—C11 | 1.511 (8) | C32—H32A | 0.9600 |
C4—C5 | 1.399 (7) | C32—H32B | 0.9600 |
C4—H4 | 0.9300 | C32—H32C | 0.9600 |
C5—C6 | 1.386 (7) | C33—H33A | 0.9600 |
C5—C7 | 1.532 (7) | C33—H33B | 0.9600 |
C6—H6 | 0.9300 | C33—H33C | 0.9600 |
C7—C8 | 1.534 (8) | C34—H34A | 0.9600 |
C7—C10 | 1.538 (8) | C34—H34B | 0.9600 |
C7—C9 | 1.541 (9) | C34—H34C | 0.9600 |
C8—H8A | 0.9600 | C35—H35A | 0.9700 |
C8—H8B | 0.9600 | C35—H35B | 0.9700 |
C8—H8C | 0.9600 | C36—H36A | 0.9700 |
C9—H9A | 0.9600 | C36—H36B | 0.9700 |
C9—H9B | 0.9600 | N1—C39 | 1.477 (7) |
C9—H9C | 0.9600 | N1—C37 | 1.509 (6) |
C10—H10A | 0.9600 | N1—H1A | 0.9000 |
C10—H10B | 0.9600 | N1—H1B | 0.9000 |
C10—H10C | 0.9600 | C37—C40 | 1.509 (7) |
C11—H11A | 0.9700 | C37—C38 | 1.531 (8) |
C11—H11B | 0.9700 | C37—H37 | 0.9800 |
C12—C13 | 1.501 (6) | C38—H38A | 0.9600 |
C12—H12A | 0.9700 | C38—H38B | 0.9600 |
C12—H12B | 0.9700 | C38—H38C | 0.9600 |
C13—C18 | 1.381 (7) | C39—H39A | 0.9600 |
C13—C14 | 1.400 (7) | C39—H39B | 0.9600 |
C14—C15 | 1.405 (7) | C39—H39C | 0.9600 |
C15—C16 | 1.383 (7) | C40—C45 | 1.395 (7) |
C15—C23 | 1.503 (7) | C40—C41 | 1.395 (7) |
C16—C17 | 1.390 (7) | C41—C42 | 1.404 (8) |
C16—H16 | 0.9300 | C41—H41 | 0.9300 |
C17—C18 | 1.397 (7) | C42—C43 | 1.386 (8) |
C17—C19 | 1.543 (7) | C42—H42 | 0.9300 |
C18—H18 | 0.9300 | C43—C44 | 1.376 (8) |
C19—C20 | 1.529 (8) | C43—H43 | 0.9300 |
C19—C22 | 1.540 (8) | C44—C45 | 1.382 (7) |
C19—C21 | 1.553 (8) | C44—H44 | 0.9300 |
C20—H20A | 0.9600 | C45—H45 | 0.9300 |
C20—H20B | 0.9600 | C46—Cl3 | 1.728 (7) |
C20—H20C | 0.9600 | C46—Cl2 | 1.730 (7) |
C21—H21A | 0.9600 | C46—Cl1 | 1.749 (7) |
C21—H21B | 0.9600 | C46—H46 | 0.9800 |
O1—U—O2 | 68.60 (12) | C19—C21—H21B | 109.5 |
O2—U—O3 | 67.48 (12) | H21A—C21—H21B | 109.5 |
O1—U—O3 | 128.72 (14) | C19—C21—H21C | 109.5 |
O3—U—O4 | 66.46 (12) | H21A—C21—H21C | 109.5 |
O4—U—O5 | 68.89 (11) | H21B—C21—H21C | 109.5 |
O3—U—O5 | 126.69 (13) | C19—C22—H22A | 109.5 |
O5—U—O1 | 102.69 (13) | C19—C22—H22B | 109.5 |
O7—U—O8 | 175.44 (16) | H22A—C22—H22B | 109.5 |
O1—U—O7 | 86.83 (14) | C19—C22—H22C | 109.5 |
O1—U—O8 | 90.60 (13) | H22A—C22—H22C | 109.5 |
O2—U—O7 | 109.17 (14) | H22B—C22—H22C | 109.5 |
O2—U—O8 | 73.29 (13) | O4—C23—C15 | 107.1 (4) |
O3—U—O7 | 83.68 (15) | O4—C23—H23A | 110.3 |
O3—U—O8 | 100.86 (14) | C15—C23—H23A | 110.3 |
O4—U—O7 | 111.00 (13) | O4—C23—H23B | 110.3 |
O4—U—O8 | 70.82 (13) | C15—C23—H23B | 110.3 |
O5—U—O7 | 86.40 (15) | H23A—C23—H23B | 108.5 |
O5—U—O8 | 90.48 (14) | O4—C24—C25 | 107.5 (4) |
O1—U—O4 | 159.05 (11) | O4—C24—H24A | 110.2 |
O2—U—O4 | 113.04 (10) | C25—C24—H24A | 110.2 |
O5—U—O2 | 161.07 (12) | O4—C24—H24B | 110.2 |
O7—U—C14 | 107.27 (15) | C25—C24—H24B | 110.2 |
O8—U—C14 | 77.27 (14) | H24A—C24—H24B | 108.5 |
O1—U—C14 | 128.21 (14) | C30—C25—C26 | 119.2 (5) |
O5—U—C14 | 127.16 (13) | C30—C25—C24 | 121.6 (5) |
O3—U—C14 | 23.60 (13) | C26—C25—C24 | 119.0 (5) |
O2—U—C14 | 59.65 (12) | O5—C26—C27 | 121.3 (5) |
O4—U—C14 | 58.47 (12) | O5—C26—C25 | 119.7 (5) |
C2—O1—U | 124.6 (3) | C27—C26—C25 | 118.9 (5) |
C12—O2—C11 | 114.3 (4) | C28—C27—C26 | 119.6 (5) |
C12—O2—U | 120.2 (3) | C28—C27—C35 | 121.3 (5) |
C11—O2—U | 118.8 (3) | C26—C27—C35 | 118.9 (5) |
C14—O3—U | 114.5 (3) | C27—C28—C29 | 122.6 (5) |
C24—O4—C23 | 113.3 (4) | C27—C28—H28 | 118.7 |
C24—O4—U | 116.5 (3) | C29—C28—H28 | 118.7 |
C23—O4—U | 120.3 (3) | C30—C29—C28 | 116.4 (5) |
C26—O5—U | 124.6 (3) | C30—C29—C31 | 123.2 (5) |
C36—O6—C35 | 114.2 (4) | C28—C29—C31 | 120.4 (5) |
C2—C1—C6 | 120.4 (5) | C29—C30—C25 | 123.3 (5) |
C2—C1—C36 | 117.8 (4) | C29—C30—H30 | 118.4 |
C6—C1—C36 | 121.6 (5) | C25—C30—H30 | 118.4 |
O1—C2—C1 | 121.8 (5) | C32—C31—C29 | 110.2 (5) |
O1—C2—C3 | 119.8 (5) | C32—C31—C34 | 109.4 (5) |
C1—C2—C3 | 118.4 (5) | C29—C31—C34 | 109.7 (4) |
C4—C3—C2 | 120.1 (5) | C32—C31—C33 | 107.6 (5) |
C4—C3—C11 | 121.3 (5) | C29—C31—C33 | 111.8 (5) |
C2—C3—C11 | 118.6 (5) | C34—C31—C33 | 108.1 (5) |
C3—C4—C5 | 122.1 (5) | C31—C32—H32A | 109.5 |
C3—C4—H4 | 119.0 | C31—C32—H32B | 109.5 |
C5—C4—H4 | 119.0 | H32A—C32—H32B | 109.5 |
C6—C5—C4 | 117.2 (5) | C31—C32—H32C | 109.5 |
C6—C5—C7 | 122.5 (5) | H32A—C32—H32C | 109.5 |
C4—C5—C7 | 120.2 (5) | H32B—C32—H32C | 109.5 |
C5—C6—C1 | 121.8 (5) | C31—C33—H33A | 109.5 |
C5—C6—H6 | 119.1 | C31—C33—H33B | 109.5 |
C1—C6—H6 | 119.1 | H33A—C33—H33B | 109.5 |
C5—C7—C8 | 111.0 (4) | C31—C33—H33C | 109.5 |
C5—C7—C10 | 112.8 (5) | H33A—C33—H33C | 109.5 |
C8—C7—C10 | 108.2 (5) | H33B—C33—H33C | 109.5 |
C5—C7—C9 | 109.7 (5) | C31—C34—H34A | 109.5 |
C8—C7—C9 | 108.1 (6) | C31—C34—H34B | 109.5 |
C10—C7—C9 | 106.8 (5) | H34A—C34—H34B | 109.5 |
C7—C8—H8A | 109.5 | C31—C34—H34C | 109.5 |
C7—C8—H8B | 109.5 | H34A—C34—H34C | 109.5 |
H8A—C8—H8B | 109.5 | H34B—C34—H34C | 109.5 |
C7—C8—H8C | 109.5 | O6—C35—C27 | 106.6 (5) |
H8A—C8—H8C | 109.5 | O6—C35—H35A | 110.4 |
H8B—C8—H8C | 109.5 | C27—C35—H35A | 110.4 |
C7—C9—H9A | 109.5 | O6—C35—H35B | 110.4 |
C7—C9—H9B | 109.5 | C27—C35—H35B | 110.4 |
H9A—C9—H9B | 109.5 | H35A—C35—H35B | 108.6 |
C7—C9—H9C | 109.5 | O6—C36—C1 | 106.3 (4) |
H9A—C9—H9C | 109.5 | O6—C36—H36A | 110.5 |
H9B—C9—H9C | 109.5 | C1—C36—H36A | 110.5 |
C7—C10—H10A | 109.5 | O6—C36—H36B | 110.5 |
C7—C10—H10B | 109.5 | C1—C36—H36B | 110.5 |
H10A—C10—H10B | 109.5 | H36A—C36—H36B | 108.7 |
C7—C10—H10C | 109.5 | C39—N1—C37 | 114.5 (4) |
H10A—C10—H10C | 109.5 | C39—N1—H1A | 108.6 |
H10B—C10—H10C | 109.5 | C37—N1—H1A | 108.6 |
O2—C11—C3 | 107.7 (4) | C39—N1—H1B | 108.6 |
O2—C11—H11A | 110.2 | C37—N1—H1B | 108.6 |
C3—C11—H11A | 110.2 | H1A—N1—H1B | 107.6 |
O2—C11—H11B | 110.2 | C40—C37—N1 | 111.4 (4) |
C3—C11—H11B | 110.2 | C40—C37—C38 | 112.1 (5) |
H11A—C11—H11B | 108.5 | N1—C37—C38 | 109.2 (4) |
O2—C12—C13 | 108.2 (4) | C40—C37—H37 | 108.0 |
O2—C12—H12A | 110.1 | N1—C37—H37 | 108.0 |
C13—C12—H12A | 110.1 | C38—C37—H37 | 108.0 |
O2—C12—H12B | 110.1 | C37—C38—H38A | 109.5 |
C13—C12—H12B | 110.1 | C37—C38—H38B | 109.5 |
H12A—C12—H12B | 108.4 | H38A—C38—H38B | 109.5 |
C18—C13—C14 | 119.7 (4) | C37—C38—H38C | 109.5 |
C18—C13—C12 | 122.3 (5) | H38A—C38—H38C | 109.5 |
C14—C13—C12 | 117.8 (4) | H38B—C38—H38C | 109.5 |
O3—C14—C13 | 119.8 (4) | N1—C39—H39A | 109.5 |
O3—C14—C15 | 121.0 (5) | N1—C39—H39B | 109.5 |
C13—C14—C15 | 119.0 (5) | H39A—C39—H39B | 109.5 |
O3—C14—U | 41.9 (2) | N1—C39—H39C | 109.5 |
C13—C14—U | 109.8 (3) | H39A—C39—H39C | 109.5 |
C15—C14—U | 111.6 (3) | H39B—C39—H39C | 109.5 |
C16—C15—C14 | 119.3 (5) | C45—C40—C41 | 119.0 (5) |
C16—C15—C23 | 123.5 (5) | C45—C40—C37 | 122.4 (5) |
C14—C15—C23 | 117.1 (5) | C41—C40—C37 | 118.6 (5) |
C15—C16—C17 | 122.5 (5) | C40—C41—C42 | 119.9 (5) |
C15—C16—H16 | 118.8 | C40—C41—H41 | 120.1 |
C17—C16—H16 | 118.8 | C42—C41—H41 | 120.1 |
C16—C17—C18 | 117.1 (5) | C43—C42—C41 | 120.3 (6) |
C16—C17—C19 | 120.0 (5) | C43—C42—H42 | 119.8 |
C18—C17—C19 | 122.8 (5) | C41—C42—H42 | 119.8 |
C13—C18—C17 | 122.0 (5) | C44—C43—C42 | 119.2 (5) |
C13—C18—H18 | 119.0 | C44—C43—H43 | 120.4 |
C17—C18—H18 | 119.0 | C42—C43—H43 | 120.4 |
C20—C19—C22 | 109.5 (5) | C43—C44—C45 | 121.4 (5) |
C20—C19—C17 | 110.1 (5) | C43—C44—H44 | 119.3 |
C22—C19—C17 | 109.2 (5) | C45—C44—H44 | 119.3 |
C20—C19—C21 | 108.6 (5) | C44—C45—C40 | 120.2 (5) |
C22—C19—C21 | 108.1 (5) | C44—C45—H45 | 119.9 |
C17—C19—C21 | 111.3 (4) | C40—C45—H45 | 119.9 |
C19—C20—H20A | 109.5 | Cl3—C46—Cl2 | 112.8 (4) |
C19—C20—H20B | 109.5 | Cl3—C46—Cl1 | 109.0 (4) |
H20A—C20—H20B | 109.5 | Cl2—C46—Cl1 | 110.0 (4) |
C19—C20—H20C | 109.5 | Cl3—C46—H46 | 108.3 |
H20A—C20—H20C | 109.5 | Cl2—C46—H46 | 108.3 |
H20B—C20—H20C | 109.5 | Cl1—C46—H46 | 108.3 |
C19—C21—H21A | 109.5 |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O8 | 0.90 | 1.91 | 2.781 (6) | 161 |
N1—H1B···Cg | 0.90 | 2.68 | 3.460 (4) | 146 |
C46—H46···O5 | 0.98 | 2.31 | 3.132 (7) | 141 |
C46—H46···O7 | 0.98 | 2.36 | 3.208 (8) | 145 |