Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802009352/ya6099sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802009352/ya6099Isup2.hkl |
CCDC reference: 189858
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.033
- wR factor = 0.072
- Data-to-parameter ratio = 13.7
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CAD-4 Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1999); software used to prepare material for publication: SHELXL97.
[UO2(C15H11O2)2(H2O)]·C14H20O5 | Z = 2 |
Mr = 1002.82 | F(000) = 992 |
Triclinic, P1 | Dx = 1.633 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.210 (2) Å | Cell parameters from 25 reflections |
b = 12.121 (2) Å | θ = 7–14° |
c = 19.374 (9) Å | µ = 4.04 mm−1 |
α = 73.59 (2)° | T = 293 K |
β = 81.20 (2)° | Needle, orange |
γ = 81.89 (1)° | 0.18 × 0.12 × 0.09 mm |
V = 2039.5 (11) Å3 |
Enraf-Nonius CAD-4 diffractometer | 5830 reflections with I > 2σ(I)' |
Radiation source: fine-focus sealed tube | Rint = 0.032 |
Graphite monochromator | θmax = 25.0°, θmin = 2.2° |
ω–2θ scans | h = 0→10 |
Absorption correction: ψ scan (North et al., 1968) | k = −14→14 |
Tmin = 0.56, Tmax = 0.69 | l = −22→23 |
7623 measured reflections | 2 standard reflections every 100 reflections |
7136 independent reflections | intensity decay: none |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0215P)2 + 3.7856P] where P = (Fo2 + 2Fc2)/3 |
7136 reflections | (Δ/σ)max = 0.002 |
522 parameters | Δρmax = 1.12 e Å−3 |
0 restraints | Δρmin = −1.33 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 | ||
U | 0.13137 (2) | 0.016443 (18) | 0.770235 (11) | 0.03852 (7) | |
O1 | 0.0693 (4) | −0.0358 (3) | 0.70405 (19) | 0.0505 (9) | |
O2 | 0.1882 (4) | 0.0682 (4) | 0.8364 (2) | 0.0587 (11) | |
O3 | −0.1144 (4) | 0.0436 (3) | 0.8190 (2) | 0.0532 (10) | |
O4 | 0.0732 (4) | −0.1462 (3) | 0.86641 (19) | 0.0522 (10) | |
O5 | 0.3211 (4) | 0.1157 (3) | 0.6889 (2) | 0.0517 (10) | |
O6 | 0.0368 (4) | 0.1982 (4) | 0.7108 (3) | 0.0732 (13) | |
O7 | 0.5382 (4) | 0.1566 (4) | 0.3881 (2) | 0.0550 (10) | |
O8 | 0.3506 (4) | 0.1423 (3) | 0.30590 (18) | 0.0463 (9) | |
O9 | 0.3764 (5) | 0.3122 (4) | 0.1744 (2) | 0.0749 (13) | |
O10 | 0.6531 (5) | 0.3811 (4) | 0.1763 (2) | 0.0708 (12) | |
O11 | 0.7019 (5) | 0.3461 (4) | 0.3208 (3) | 0.0764 (13) | |
O12 | 0.3439 (4) | −0.1355 (3) | 0.76465 (19) | 0.0483 (9) | |
C1 | 0.6092 (6) | 0.1577 (5) | 0.6413 (3) | 0.0509 (14) | |
H1 | 0.5886 | 0.0852 | 0.6707 | 0.061* | |
C2 | 0.7537 (6) | 0.1770 (6) | 0.6119 (3) | 0.0597 (16) | |
H2 | 0.8295 | 0.1177 | 0.6224 | 0.072* | |
C3 | 0.7850 (6) | 0.2827 (6) | 0.5677 (3) | 0.0566 (16) | |
H3 | 0.8816 | 0.2954 | 0.5478 | 0.068* | |
C4 | 0.6741 (7) | 0.3689 (6) | 0.5531 (3) | 0.0629 (17) | |
H4 | 0.6953 | 0.4406 | 0.5227 | 0.075* | |
C5 | 0.5307 (6) | 0.3522 (5) | 0.5825 (3) | 0.0612 (16) | |
H5 | 0.4565 | 0.4129 | 0.5725 | 0.073* | |
C6 | 0.4958 (6) | 0.2457 (5) | 0.6269 (3) | 0.0425 (12) | |
C7 | 0.3411 (6) | 0.2209 (5) | 0.6597 (3) | 0.0437 (13) | |
C8 | 0.2276 (6) | 0.3111 (5) | 0.6559 (3) | 0.0536 (15) | |
H8 | 0.2523 | 0.3863 | 0.6356 | 0.064* | |
C9 | 0.0813 (6) | 0.2959 (5) | 0.6803 (3) | 0.0477 (13) | |
C10 | −0.0382 (6) | 0.3939 (5) | 0.6698 (3) | 0.0462 (13) | |
C11 | −0.0237 (7) | 0.4975 (5) | 0.6185 (4) | 0.0691 (19) | |
H11 | 0.0649 | 0.5102 | 0.5887 | 0.083* | |
C12 | −0.1422 (9) | 0.5839 (6) | 0.6112 (5) | 0.095 (3) | |
H12 | −0.1333 | 0.6537 | 0.5759 | 0.114* | |
C13 | −0.2724 (8) | 0.5653 (7) | 0.6563 (5) | 0.092 (3) | |
H13 | −0.3504 | 0.6237 | 0.6525 | 0.110* | |
C14 | −0.2875 (8) | 0.4633 (7) | 0.7060 (4) | 0.080 (2) | |
H14 | −0.3762 | 0.4510 | 0.7359 | 0.096* | |
C15 | −0.1724 (7) | 0.3772 (5) | 0.7128 (3) | 0.0586 (16) | |
H15 | −0.1846 | 0.3065 | 0.7467 | 0.070* | |
C16 | −0.3975 (6) | 0.1447 (5) | 0.8422 (4) | 0.0618 (17) | |
H16 | −0.3626 | 0.1363 | 0.7962 | 0.074* | |
C17 | −0.5318 (7) | 0.2101 (6) | 0.8530 (5) | 0.080 (2) | |
H17 | −0.5864 | 0.2441 | 0.8144 | 0.097* | |
C18 | −0.5833 (8) | 0.2242 (6) | 0.9199 (5) | 0.081 (2) | |
H18 | −0.6724 | 0.2687 | 0.9269 | 0.097* | |
C19 | −0.5046 (8) | 0.1731 (6) | 0.9766 (4) | 0.079 (2) | |
H19 | −0.5412 | 0.1822 | 1.0223 | 0.095* | |
C20 | −0.3701 (7) | 0.1073 (6) | 0.9673 (4) | 0.0666 (18) | |
H20 | −0.3168 | 0.0736 | 1.0064 | 0.080* | |
C21 | −0.3156 (6) | 0.0924 (5) | 0.8988 (3) | 0.0465 (13) | |
C22 | −0.1742 (5) | 0.0225 (5) | 0.8848 (3) | 0.0435 (13) | |
C23 | −0.1158 (6) | −0.0648 (5) | 0.9396 (3) | 0.0495 (14) | |
H23 | −0.1570 | −0.0684 | 0.9870 | 0.059* | |
C24 | −0.0005 (6) | −0.1472 (5) | 0.9289 (3) | 0.0448 (13) | |
C25 | 0.0378 (6) | −0.2472 (5) | 0.9897 (3) | 0.0458 (13) | |
C26 | 0.0049 (7) | −0.2421 (6) | 1.0615 (3) | 0.0638 (17) | |
H26 | −0.0419 | −0.1744 | 1.0717 | 0.077* | |
C27 | 0.0407 (9) | −0.3357 (8) | 1.1170 (4) | 0.086 (2) | |
H27 | 0.0156 | −0.3315 | 1.1646 | 0.104* | |
C28 | 0.1121 (9) | −0.4343 (8) | 1.1036 (4) | 0.101 (3) | |
H28 | 0.1415 | −0.4957 | 1.1416 | 0.121* | |
C29 | 0.1410 (10) | −0.4436 (7) | 1.0337 (4) | 0.115 (3) | |
H29 | 0.1838 | −0.5130 | 1.0245 | 0.138* | |
C30 | 0.1058 (8) | −0.3483 (6) | 0.9767 (4) | 0.088 (2) | |
H30 | 0.1288 | −0.3535 | 0.9292 | 0.105* | |
C31 | 0.3990 (6) | 0.1376 (5) | 0.4219 (3) | 0.0459 (13) | |
C32 | 0.3533 (8) | 0.1267 (6) | 0.4949 (3) | 0.0647 (17) | |
H32 | 0.4212 | 0.1286 | 0.5254 | 0.078* | |
C33 | 0.2075 (8) | 0.1131 (6) | 0.5227 (3) | 0.0687 (19) | |
H33 | 0.1774 | 0.1075 | 0.5715 | 0.082* | |
C34 | 0.1090 (7) | 0.1078 (5) | 0.4793 (3) | 0.0623 (17) | |
H34 | 0.0109 | 0.0994 | 0.4982 | 0.075* | |
C35 | 0.1531 (6) | 0.1149 (5) | 0.4063 (3) | 0.0542 (15) | |
H35 | 0.0848 | 0.1090 | 0.3771 | 0.065* | |
C36 | 0.2966 (6) | 0.1305 (4) | 0.3772 (3) | 0.0422 (12) | |
C37 | 0.2431 (7) | 0.1675 (6) | 0.2550 (3) | 0.0636 (17) | |
H37A | 0.1690 | 0.2287 | 0.2640 | 0.076* | |
H37B | 0.1942 | 0.0993 | 0.2602 | 0.076* | |
C38 | 0.3233 (7) | 0.2044 (6) | 0.1804 (3) | 0.0712 (19) | |
H38A | 0.4051 | 0.1472 | 0.1733 | 0.085* | |
H38B | 0.2572 | 0.2132 | 0.1443 | 0.085* | |
C39 | 0.4748 (8) | 0.3507 (7) | 0.1124 (4) | 0.081 (2) | |
H39A | 0.4214 | 0.3837 | 0.0706 | 0.098* | |
H39B | 0.5439 | 0.2868 | 0.1033 | 0.098* | |
C40 | 0.5540 (8) | 0.4385 (6) | 0.1253 (4) | 0.075 (2) | |
H40A | 0.6079 | 0.4793 | 0.0804 | 0.090* | |
H40B | 0.4848 | 0.4943 | 0.1440 | 0.090* | |
C41 | 0.7265 (8) | 0.4562 (6) | 0.2000 (4) | 0.078 (2) | |
H41A | 0.6556 | 0.5135 | 0.2163 | 0.093* | |
H41B | 0.7947 | 0.4962 | 0.1606 | 0.093* | |
C42 | 0.8072 (8) | 0.3853 (7) | 0.2599 (4) | 0.081 (2) | |
H42A | 0.8650 | 0.3198 | 0.2462 | 0.097* | |
H42B | 0.8738 | 0.4307 | 0.2717 | 0.097* | |
C43 | 0.7547 (7) | 0.2483 (6) | 0.3732 (4) | 0.0687 (19) | |
H43A | 0.8255 | 0.2695 | 0.3982 | 0.082* | |
H43B | 0.8043 | 0.1900 | 0.3497 | 0.082* | |
C44 | 0.6300 (7) | 0.2012 (6) | 0.4257 (4) | 0.0661 (18) | |
H44A | 0.6665 | 0.1399 | 0.4653 | 0.079* | |
H44B | 0.5735 | 0.2615 | 0.4454 | 0.079* | |
H12A | 0.4109 | −0.1316 | 0.7288 | 0.050* | |
H12B | 0.3363 | −0.2067 | 0.7854 | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
U | 0.03745 (11) | 0.03936 (11) | 0.03806 (11) | −0.00347 (7) | −0.00396 (7) | −0.00973 (8) |
O1 | 0.049 (2) | 0.063 (3) | 0.045 (2) | −0.0048 (19) | −0.0137 (17) | −0.0204 (19) |
O2 | 0.060 (2) | 0.067 (3) | 0.064 (3) | −0.010 (2) | −0.007 (2) | −0.040 (2) |
O3 | 0.044 (2) | 0.062 (2) | 0.049 (2) | 0.0015 (18) | 0.0000 (17) | −0.0123 (19) |
O4 | 0.056 (2) | 0.050 (2) | 0.044 (2) | −0.0030 (18) | 0.0040 (18) | −0.0082 (18) |
O5 | 0.045 (2) | 0.043 (2) | 0.059 (2) | −0.0054 (17) | −0.0038 (18) | −0.0017 (18) |
O6 | 0.045 (2) | 0.055 (3) | 0.095 (3) | 0.000 (2) | 0.000 (2) | 0.013 (2) |
O7 | 0.048 (2) | 0.072 (3) | 0.054 (2) | −0.009 (2) | −0.0158 (18) | −0.026 (2) |
O8 | 0.041 (2) | 0.063 (2) | 0.043 (2) | −0.0083 (18) | −0.0079 (16) | −0.0237 (18) |
O9 | 0.080 (3) | 0.079 (3) | 0.068 (3) | −0.016 (3) | −0.006 (2) | −0.019 (3) |
O10 | 0.084 (3) | 0.057 (3) | 0.074 (3) | −0.012 (2) | −0.017 (3) | −0.015 (2) |
O11 | 0.063 (3) | 0.085 (3) | 0.081 (3) | −0.004 (3) | −0.007 (3) | −0.024 (3) |
O12 | 0.040 (2) | 0.054 (2) | 0.052 (2) | −0.0020 (17) | −0.0055 (17) | −0.0160 (18) |
C1 | 0.048 (3) | 0.043 (3) | 0.062 (4) | −0.005 (3) | −0.003 (3) | −0.016 (3) |
C2 | 0.044 (3) | 0.066 (4) | 0.076 (4) | −0.007 (3) | −0.008 (3) | −0.029 (4) |
C3 | 0.046 (3) | 0.078 (5) | 0.056 (4) | −0.024 (3) | 0.000 (3) | −0.029 (3) |
C4 | 0.058 (4) | 0.060 (4) | 0.064 (4) | −0.019 (3) | −0.004 (3) | −0.001 (3) |
C5 | 0.048 (3) | 0.056 (4) | 0.073 (4) | −0.009 (3) | −0.008 (3) | −0.005 (3) |
C6 | 0.048 (3) | 0.045 (3) | 0.037 (3) | −0.011 (3) | −0.005 (2) | −0.012 (2) |
C7 | 0.048 (3) | 0.046 (3) | 0.040 (3) | −0.012 (3) | −0.008 (2) | −0.012 (3) |
C8 | 0.049 (3) | 0.042 (3) | 0.068 (4) | −0.010 (3) | −0.005 (3) | −0.010 (3) |
C9 | 0.055 (3) | 0.042 (3) | 0.045 (3) | −0.004 (3) | −0.009 (3) | −0.009 (3) |
C10 | 0.049 (3) | 0.044 (3) | 0.054 (3) | −0.005 (3) | −0.014 (3) | −0.021 (3) |
C11 | 0.064 (4) | 0.042 (4) | 0.098 (5) | −0.006 (3) | −0.016 (4) | −0.010 (3) |
C12 | 0.090 (6) | 0.037 (4) | 0.149 (8) | 0.000 (4) | −0.027 (5) | −0.008 (4) |
C13 | 0.066 (5) | 0.057 (5) | 0.159 (8) | 0.011 (4) | −0.026 (5) | −0.043 (5) |
C14 | 0.067 (5) | 0.086 (6) | 0.095 (6) | 0.014 (4) | −0.011 (4) | −0.045 (5) |
C15 | 0.063 (4) | 0.060 (4) | 0.056 (4) | 0.004 (3) | −0.012 (3) | −0.022 (3) |
C16 | 0.050 (4) | 0.063 (4) | 0.076 (4) | −0.001 (3) | −0.009 (3) | −0.026 (3) |
C17 | 0.054 (4) | 0.078 (5) | 0.110 (6) | 0.009 (4) | −0.020 (4) | −0.028 (5) |
C18 | 0.052 (4) | 0.059 (4) | 0.134 (7) | −0.005 (3) | 0.009 (5) | −0.038 (5) |
C19 | 0.077 (5) | 0.074 (5) | 0.088 (5) | −0.004 (4) | 0.021 (4) | −0.041 (4) |
C20 | 0.066 (4) | 0.069 (4) | 0.066 (4) | −0.005 (3) | 0.005 (3) | −0.029 (3) |
C21 | 0.036 (3) | 0.048 (3) | 0.059 (4) | −0.012 (2) | 0.000 (3) | −0.019 (3) |
C22 | 0.037 (3) | 0.046 (3) | 0.053 (3) | −0.010 (2) | −0.001 (2) | −0.022 (3) |
C23 | 0.049 (3) | 0.059 (4) | 0.040 (3) | −0.008 (3) | 0.003 (2) | −0.016 (3) |
C24 | 0.044 (3) | 0.055 (3) | 0.038 (3) | −0.018 (3) | −0.001 (2) | −0.012 (3) |
C25 | 0.040 (3) | 0.053 (3) | 0.042 (3) | −0.010 (3) | −0.003 (2) | −0.008 (3) |
C26 | 0.073 (4) | 0.070 (4) | 0.052 (4) | −0.009 (3) | −0.017 (3) | −0.016 (3) |
C27 | 0.088 (6) | 0.112 (7) | 0.052 (4) | −0.003 (5) | −0.023 (4) | −0.007 (4) |
C28 | 0.084 (6) | 0.114 (7) | 0.070 (5) | 0.007 (5) | −0.014 (4) | 0.027 (5) |
C29 | 0.139 (8) | 0.087 (6) | 0.075 (6) | 0.039 (5) | 0.009 (5) | 0.012 (5) |
C30 | 0.105 (6) | 0.081 (5) | 0.050 (4) | 0.026 (4) | 0.008 (4) | 0.000 (4) |
C31 | 0.053 (3) | 0.045 (3) | 0.041 (3) | −0.008 (3) | −0.010 (3) | −0.010 (2) |
C32 | 0.081 (5) | 0.067 (4) | 0.050 (4) | −0.006 (4) | −0.019 (3) | −0.015 (3) |
C33 | 0.088 (5) | 0.070 (4) | 0.046 (4) | −0.020 (4) | 0.008 (4) | −0.015 (3) |
C34 | 0.069 (4) | 0.050 (4) | 0.067 (4) | −0.018 (3) | 0.020 (3) | −0.024 (3) |
C35 | 0.051 (3) | 0.054 (4) | 0.067 (4) | −0.013 (3) | −0.004 (3) | −0.029 (3) |
C36 | 0.052 (3) | 0.038 (3) | 0.041 (3) | −0.005 (2) | −0.007 (2) | −0.016 (2) |
C37 | 0.056 (4) | 0.089 (5) | 0.055 (4) | −0.020 (3) | −0.016 (3) | −0.024 (3) |
C38 | 0.070 (4) | 0.096 (6) | 0.056 (4) | −0.011 (4) | −0.025 (3) | −0.023 (4) |
C39 | 0.088 (5) | 0.088 (6) | 0.061 (4) | −0.001 (4) | −0.022 (4) | −0.005 (4) |
C40 | 0.086 (5) | 0.061 (4) | 0.068 (4) | −0.003 (4) | −0.004 (4) | −0.005 (4) |
C41 | 0.079 (5) | 0.067 (5) | 0.088 (5) | −0.022 (4) | 0.001 (4) | −0.023 (4) |
C42 | 0.060 (4) | 0.098 (6) | 0.100 (6) | −0.032 (4) | −0.001 (4) | −0.045 (5) |
C43 | 0.053 (4) | 0.082 (5) | 0.090 (5) | −0.005 (4) | −0.023 (4) | −0.048 (4) |
C44 | 0.063 (4) | 0.080 (5) | 0.070 (4) | −0.009 (4) | −0.027 (3) | −0.032 (4) |
U—O2 | 1.751 (4) | C17—H17 | 0.9300 |
U—O1 | 1.777 (4) | C18—C19 | 1.359 (10) |
U—O6 | 2.295 (4) | C18—H18 | 0.9300 |
U—O3 | 2.332 (4) | C19—C20 | 1.392 (9) |
U—O4 | 2.359 (4) | C19—H19 | 0.9300 |
U—O5 | 2.380 (3) | C20—C21 | 1.397 (8) |
U—O12 | 2.504 (3) | C20—H20 | 0.9300 |
O3—C22 | 1.277 (6) | C21—C22 | 1.482 (7) |
O4—C24 | 1.292 (6) | C22—C23 | 1.384 (7) |
O5—C7 | 1.268 (6) | C23—C24 | 1.385 (7) |
O6—C9 | 1.260 (6) | C23—H23 | 0.9300 |
O7—C31 | 1.366 (6) | C24—C25 | 1.477 (7) |
O7—C44 | 1.440 (7) | C25—C30 | 1.366 (9) |
O8—C36 | 1.368 (6) | C25—C26 | 1.395 (8) |
O8—C37 | 1.445 (6) | C26—C27 | 1.365 (9) |
O9—C39 | 1.397 (8) | C26—H26 | 0.9300 |
O9—C38 | 1.427 (8) | C27—C28 | 1.353 (11) |
O10—C40 | 1.415 (8) | C27—H27 | 0.9300 |
O10—C41 | 1.415 (8) | C28—C29 | 1.372 (11) |
O11—C43 | 1.407 (8) | C28—H28 | 0.9300 |
O11—C42 | 1.422 (8) | C29—C30 | 1.394 (9) |
O12—H12A | 0.850 | C29—H29 | 0.9300 |
O12—H12B | 0.850 | C30—H30 | 0.9300 |
C1—C6 | 1.382 (7) | C31—C32 | 1.387 (8) |
C1—C2 | 1.389 (7) | C31—C36 | 1.401 (7) |
C1—H1 | 0.9300 | C32—C33 | 1.382 (9) |
C2—C3 | 1.366 (8) | C32—H32 | 0.9300 |
C2—H2 | 0.9300 | C33—C34 | 1.348 (9) |
C3—C4 | 1.355 (8) | C33—H33 | 0.9300 |
C3—H3 | 0.9300 | C34—C35 | 1.391 (8) |
C4—C5 | 1.375 (8) | C34—H34 | 0.9300 |
C4—H4 | 0.9300 | C35—C36 | 1.373 (7) |
C5—C6 | 1.383 (7) | C35—H35 | 0.9300 |
C5—H5 | 0.9300 | C37—C38 | 1.495 (8) |
C6—C7 | 1.504 (7) | C37—H37A | 0.9700 |
C7—C8 | 1.396 (7) | C37—H37B | 0.9700 |
C8—C9 | 1.378 (7) | C38—H38A | 0.9700 |
C8—H8 | 0.9300 | C38—H38B | 0.9700 |
C9—C10 | 1.492 (7) | C39—C40 | 1.468 (10) |
C10—C11 | 1.373 (8) | C39—H39A | 0.9700 |
C10—C15 | 1.386 (8) | C39—H39B | 0.9700 |
C11—C12 | 1.396 (9) | C40—H40A | 0.9700 |
C11—H11 | 0.9300 | C40—H40B | 0.9700 |
C12—C13 | 1.378 (10) | C41—C42 | 1.470 (10) |
C12—H12 | 0.9300 | C41—H41A | 0.9700 |
C13—C14 | 1.346 (10) | C41—H41B | 0.9700 |
C13—H13 | 0.9300 | C42—H42A | 0.9700 |
C14—C15 | 1.372 (8) | C42—H42B | 0.9700 |
C14—H14 | 0.9300 | C43—C44 | 1.477 (9) |
C15—H15 | 0.9300 | C43—H43A | 0.9700 |
C16—C21 | 1.377 (8) | C43—H43B | 0.9700 |
C16—C17 | 1.393 (8) | C44—H44A | 0.9700 |
C16—H16 | 0.9300 | C44—H44B | 0.9700 |
C17—C18 | 1.359 (10) | ||
O2—U—O1 | 178.63 (17) | C20—C21—C22 | 122.8 (5) |
O2—U—O6 | 91.89 (19) | O3—C22—C23 | 122.4 (5) |
O1—U—O6 | 87.78 (18) | O3—C22—C21 | 116.2 (5) |
O2—U—O3 | 90.33 (16) | C23—C22—C21 | 121.3 (5) |
O1—U—O3 | 88.31 (15) | C22—C23—C24 | 124.7 (5) |
O6—U—O3 | 72.40 (14) | C22—C23—H23 | 117.7 |
O2—U—O4 | 85.29 (17) | C24—C23—H23 | 117.7 |
O1—U—O4 | 94.17 (16) | O4—C24—C23 | 123.5 (5) |
O6—U—O4 | 142.56 (13) | O4—C24—C25 | 116.2 (5) |
O3—U—O4 | 70.30 (13) | C23—C24—C25 | 120.2 (5) |
O2—U—O5 | 86.33 (16) | C30—C25—C26 | 118.2 (6) |
O1—U—O5 | 94.79 (15) | C30—C25—C24 | 120.3 (5) |
O6—U—O5 | 70.02 (13) | C26—C25—C24 | 121.5 (5) |
O3—U—O5 | 142.11 (13) | C27—C26—C25 | 120.6 (7) |
O4—U—O5 | 146.53 (13) | C27—C26—H26 | 119.7 |
O2—U—O12 | 97.13 (16) | C25—C26—H26 | 119.7 |
O1—U—O12 | 83.92 (14) | C28—C27—C26 | 120.9 (7) |
O6—U—O12 | 143.21 (13) | C28—C27—H27 | 119.6 |
O3—U—O12 | 142.68 (13) | C26—C27—H27 | 119.6 |
O4—U—O12 | 73.94 (12) | C27—C28—C29 | 119.9 (7) |
O5—U—O12 | 75.05 (12) | C27—C28—H28 | 120.1 |
C22—O3—U | 130.9 (3) | C29—C28—H28 | 120.1 |
C24—O4—U | 127.6 (3) | C28—C29—C30 | 119.5 (8) |
C7—O5—U | 135.1 (3) | C28—C29—H29 | 120.2 |
C9—O6—U | 138.6 (4) | C30—C29—H29 | 120.2 |
C31—O7—C44 | 116.1 (4) | C25—C30—C29 | 120.8 (7) |
C36—O8—C37 | 116.7 (4) | C25—C30—H30 | 119.6 |
C39—O9—C38 | 114.6 (5) | C29—C30—H30 | 119.6 |
C40—O10—C41 | 114.1 (5) | O7—C31—C32 | 125.3 (5) |
C43—O11—C42 | 114.3 (5) | O7—C31—C36 | 115.5 (5) |
U—O12—H12A | 123.9 | C32—C31—C36 | 119.1 (5) |
U—O12—H12B | 121.9 | C33—C32—C31 | 120.5 (6) |
H12A—O12—H12B | 107.7 | C33—C32—H32 | 119.8 |
C6—C1—C2 | 120.4 (5) | C31—C32—H32 | 119.8 |
C6—C1—H1 | 119.8 | C34—C33—C32 | 120.2 (6) |
C2—C1—H1 | 119.8 | C34—C33—H33 | 119.9 |
C3—C2—C1 | 120.3 (6) | C32—C33—H33 | 119.9 |
C3—C2—H2 | 119.8 | C33—C34—C35 | 120.5 (6) |
C1—C2—H2 | 119.8 | C33—C34—H34 | 119.8 |
C4—C3—C2 | 119.5 (5) | C35—C34—H34 | 119.8 |
C4—C3—H3 | 120.3 | C36—C35—C34 | 120.4 (6) |
C2—C3—H3 | 120.3 | C36—C35—H35 | 119.8 |
C3—C4—C5 | 121.2 (6) | C34—C35—H35 | 119.8 |
C3—C4—H4 | 119.4 | O8—C36—C35 | 125.3 (5) |
C5—C4—H4 | 119.4 | O8—C36—C31 | 115.4 (5) |
C4—C5—C6 | 120.5 (6) | C35—C36—C31 | 119.3 (5) |
C4—C5—H5 | 119.7 | O8—C37—C38 | 107.7 (5) |
C6—C5—H5 | 119.7 | O8—C37—H37A | 110.2 |
C1—C6—C5 | 118.1 (5) | C38—C37—H37A | 110.2 |
C1—C6—C7 | 118.6 (5) | O8—C37—H37B | 110.2 |
C5—C6—C7 | 123.3 (5) | C38—C37—H37B | 110.2 |
O5—C7—C8 | 123.3 (5) | H37A—C37—H37B | 108.5 |
O5—C7—C6 | 116.5 (5) | O9—C38—C37 | 106.7 (5) |
C8—C7—C6 | 120.2 (5) | O9—C38—H38A | 110.4 |
C9—C8—C7 | 124.1 (5) | C37—C38—H38A | 110.4 |
C9—C8—H8 | 117.9 | O9—C38—H38B | 110.4 |
C7—C8—H8 | 117.9 | C37—C38—H38B | 110.4 |
O6—C9—C8 | 123.0 (5) | H38A—C38—H38B | 108.6 |
O6—C9—C10 | 114.6 (5) | O9—C39—C40 | 107.5 (6) |
C8—C9—C10 | 122.4 (5) | O9—C39—H39A | 110.2 |
C11—C10—C15 | 118.6 (6) | C40—C39—H39A | 110.2 |
C11—C10—C9 | 123.5 (5) | O9—C39—H39B | 110.2 |
C15—C10—C9 | 117.8 (5) | C40—C39—H39B | 110.2 |
C10—C11—C12 | 119.9 (7) | H39A—C39—H39B | 108.5 |
C10—C11—H11 | 120.0 | O10—C40—C39 | 107.7 (6) |
C12—C11—H11 | 120.0 | O10—C40—H40A | 110.2 |
C13—C12—C11 | 119.7 (7) | C39—C40—H40A | 110.2 |
C13—C12—H12 | 120.1 | O10—C40—H40B | 110.2 |
C11—C12—H12 | 120.1 | C39—C40—H40B | 110.2 |
C14—C13—C12 | 120.4 (7) | H40A—C40—H40B | 108.5 |
C14—C13—H13 | 119.8 | O10—C41—C42 | 107.5 (6) |
C12—C13—H13 | 119.8 | O10—C41—H41A | 110.2 |
C13—C14—C15 | 120.2 (7) | C42—C41—H41A | 110.2 |
C13—C14—H14 | 119.9 | O10—C41—H41B | 110.2 |
C15—C14—H14 | 119.9 | C42—C41—H41B | 110.2 |
C14—C15—C10 | 121.0 (6) | H41A—C41—H41B | 108.5 |
C14—C15—H15 | 119.5 | O11—C42—C41 | 108.0 (6) |
C10—C15—H15 | 119.5 | O11—C42—H42A | 110.1 |
C21—C16—C17 | 121.0 (6) | C41—C42—H42A | 110.1 |
C21—C16—H16 | 119.5 | O11—C42—H42B | 110.1 |
C17—C16—H16 | 119.5 | C41—C42—H42B | 110.1 |
C18—C17—C16 | 120.1 (7) | H42A—C42—H42B | 108.4 |
C18—C17—H17 | 119.9 | O11—C43—C44 | 109.6 (5) |
C16—C17—H17 | 119.9 | O11—C43—H43A | 109.8 |
C17—C18—C19 | 119.9 (7) | C44—C43—H43A | 109.8 |
C17—C18—H18 | 120.0 | O11—C43—H43B | 109.8 |
C19—C18—H18 | 120.0 | C44—C43—H43B | 109.8 |
C18—C19—C20 | 121.1 (7) | H43A—C43—H43B | 108.2 |
C18—C19—H19 | 119.4 | O7—C44—C43 | 107.9 (5) |
C20—C19—H19 | 119.4 | O7—C44—H44A | 110.1 |
C19—C20—C21 | 119.6 (7) | C43—C44—H44A | 110.1 |
C19—C20—H20 | 120.2 | O7—C44—H44B | 110.1 |
C21—C20—H20 | 120.2 | C43—C44—H44B | 110.1 |
C16—C21—C20 | 118.3 (5) | H44A—C44—H44B | 108.4 |
C16—C21—C22 | 119.0 (5) | ||
O2—U—O3—C22 | −42.2 (5) | C17—C18—C19—C20 | 0.9 (12) |
O1—U—O3—C22 | 137.8 (5) | C18—C19—C20—C21 | −0.7 (11) |
O6—U—O3—C22 | −134.0 (5) | C17—C16—C21—C20 | −0.5 (9) |
O4—U—O3—C22 | 42.7 (5) | C17—C16—C21—C22 | 179.2 (6) |
O5—U—O3—C22 | −126.6 (4) | C19—C20—C21—C16 | 0.5 (9) |
O12—U—O3—C22 | 60.1 (5) | C19—C20—C21—C22 | −179.3 (6) |
O2—U—O4—C24 | 48.2 (4) | U—O3—C22—C23 | −28.7 (8) |
O1—U—O4—C24 | −130.5 (4) | U—O3—C22—C21 | 154.9 (4) |
O6—U—O4—C24 | −38.7 (6) | C16—C21—C22—O3 | 21.2 (8) |
O3—U—O4—C24 | −43.8 (4) | C20—C21—C22—O3 | −159.0 (5) |
O5—U—O4—C24 | 124.3 (4) | C16—C21—C22—C23 | −155.3 (6) |
O12—U—O4—C24 | 147.0 (5) | C20—C21—C22—C23 | 24.5 (8) |
O2—U—O5—C7 | −70.1 (5) | O3—C22—C23—C24 | −8.7 (9) |
O1—U—O5—C7 | 109.1 (5) | C21—C22—C23—C24 | 167.6 (5) |
O6—U—O5—C7 | 23.3 (5) | U—O4—C24—C23 | 33.3 (7) |
O3—U—O5—C7 | 15.7 (6) | U—O4—C24—C25 | −150.8 (4) |
O4—U—O5—C7 | −145.8 (4) | C22—C23—C24—O4 | 5.4 (9) |
O12—U—O5—C7 | −168.5 (5) | C22—C23—C24—C25 | −170.3 (5) |
O2—U—O6—C9 | 59.8 (6) | O4—C24—C25—C30 | −21.9 (8) |
O1—U—O6—C9 | −121.5 (6) | C23—C24—C25—C30 | 154.1 (6) |
O3—U—O6—C9 | 149.5 (7) | O4—C24—C25—C26 | 158.7 (5) |
O4—U—O6—C9 | 144.5 (5) | C23—C24—C25—C26 | −25.2 (8) |
O5—U—O6—C9 | −25.6 (6) | C30—C25—C26—C27 | 0.4 (10) |
O12—U—O6—C9 | −44.8 (8) | C24—C25—C26—C27 | 179.7 (6) |
C6—C1—C2—C3 | −0.9 (9) | C25—C26—C27—C28 | 1.7 (12) |
C1—C2—C3—C4 | 0.5 (9) | C26—C27—C28—C29 | −4.1 (14) |
C2—C3—C4—C5 | 0.6 (10) | C27—C28—C29—C30 | 4.5 (15) |
C3—C4—C5—C6 | −1.2 (10) | C26—C25—C30—C29 | 0.0 (11) |
C2—C1—C6—C5 | 0.3 (8) | C24—C25—C30—C29 | −179.3 (7) |
C2—C1—C6—C7 | 179.9 (5) | C28—C29—C30—C25 | −2.5 (14) |
C4—C5—C6—C1 | 0.7 (9) | C44—O7—C31—C32 | −18.7 (8) |
C4—C5—C6—C7 | −178.8 (6) | C44—O7—C31—C36 | 160.4 (5) |
U—O5—C7—C8 | −17.0 (8) | O7—C31—C32—C33 | 176.9 (6) |
U—O5—C7—C6 | 164.2 (3) | C36—C31—C32—C33 | −2.2 (9) |
C1—C6—C7—O5 | −11.1 (7) | C31—C32—C33—C34 | 1.4 (10) |
C5—C6—C7—O5 | 168.4 (5) | C32—C33—C34—C35 | 0.6 (10) |
C1—C6—C7—C8 | 170.1 (5) | C33—C34—C35—C36 | −1.8 (9) |
C5—C6—C7—C8 | −10.4 (8) | C37—O8—C36—C35 | 15.4 (8) |
O5—C7—C8—C9 | −3.0 (9) | C37—O8—C36—C31 | −163.4 (5) |
C6—C7—C8—C9 | 175.8 (5) | C34—C35—C36—O8 | −177.8 (5) |
U—O6—C9—C8 | 20.2 (10) | C34—C35—C36—C31 | 1.0 (8) |
U—O6—C9—C10 | −162.1 (4) | O7—C31—C36—O8 | 0.7 (7) |
C7—C8—C9—O6 | 2.5 (10) | C32—C31—C36—O8 | 179.9 (5) |
C7—C8—C9—C10 | −175.0 (5) | O7—C31—C36—C35 | −178.1 (5) |
O6—C9—C10—C11 | −157.5 (6) | C32—C31—C36—C35 | 1.0 (8) |
C8—C9—C10—C11 | 20.2 (9) | C36—O8—C37—C38 | 166.7 (5) |
O6—C9—C10—C15 | 20.2 (8) | C39—O9—C38—C37 | 170.0 (5) |
C8—C9—C10—C15 | −162.1 (6) | O8—C37—C38—O9 | −66.8 (7) |
C15—C10—C11—C12 | 0.9 (10) | C38—O9—C39—C40 | −161.9 (6) |
C9—C10—C11—C12 | 178.5 (6) | C41—O10—C40—C39 | −173.7 (6) |
C10—C11—C12—C13 | 1.0 (12) | O9—C39—C40—O10 | 71.9 (7) |
C11—C12—C13—C14 | −1.9 (13) | C40—O10—C41—C42 | 171.7 (6) |
C12—C13—C14—C15 | 0.8 (13) | C43—O11—C42—C41 | 159.5 (6) |
C13—C14—C15—C10 | 1.1 (11) | O10—C41—C42—O11 | −70.5 (7) |
C11—C10—C15—C14 | −2.0 (9) | C42—O11—C43—C44 | −168.4 (5) |
C9—C10—C15—C14 | −179.8 (6) | C31—O7—C44—C43 | −163.3 (5) |
C21—C16—C17—C18 | 0.7 (11) | O11—C43—C44—O7 | 67.0 (7) |
C16—C17—C18—C19 | −0.9 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
O12—H12A···O8i | 0.85 | 2.19 | 2.934 (5) | 145.6 |
O12—H12A···O7i | 0.85 | 2.34 | 3.061 (5) | 143.1 |
O12—H12B···O10i | 0.85 | 2.03 | 2.869 (6) | 170.7 |
Symmetry code: (i) −x+1, −y, −z+1. |
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