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
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.007 Å
- R factor = 0.033
- wR factor = 0.065
- Data-to-parameter ratio = 16.1
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.527 0.863 Tmin(prime) and Tmax expected: 0.590 0.863 RR(prime) = 0.894 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.87 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.04 Ratio PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C46 PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1B ... ? PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 41.90 Deg. O3 -C14 -U 1.555 1.555 1.555
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.68 From the CIF: _reflns_number_total 8750 Count of symmetry unique reflns 4971 Completeness (_total/calc) 176.02% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3779 Fraction of Friedel pairs measured 0.760 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 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 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
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 |