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In the title compound, (S)-(−)-N,α-dimethyl­benzyl­ammonium dioxo[7,15,23-tri-tert-butyl-3,11,19-trioxatetra­cyclo­[19.3.1.15,9.113,17]hepta­cosa-1(25),5,7,9(27),13,15,17(26),21,23-nona­ene-25,26,27-triolato]uranate(VI) chloroform solvate, (C9H14N)[UO2(C36H45O6)]·CHCl3, the uranyl ion is bound to the three phenoxide groups and two of the ether groups of the deprotonated p-tert-butyl­hexa­homo­tri­oxa­calix[3]arene mol­ecule in a cone conformation, giving a mono-anionic complex. The chiral counter-ion, (S)-(−)-N,α-dimethyl­benzyl­ammonium, is included in the cavity and involved in both a hydrogen bond with the uranyl oxo group directed inwards and an N—H...π inter­action with one of the aromatic rings.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805031867/dn6262sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805031867/dn6262Isup2.hkl
Contains datablock I

CCDC reference: 289717

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](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

Computing details top

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).

(S)-(-)-N,α-dimethylbenzylammonium dioxo[7,15,23-tri-tert-butyl-3,11,19-trioxatetracyclo[19.3.1.15,9.113,17] heptacosa-1(25),5,7,9(27),13,15,17 (26),21,23-nonaene-25,26,27-triolato]uranium trichloromethane solvate top
Crystal data top
(C9H14N)[UO2(C36H45O6)]·CHCl3F(000) = 2200
Mr = 1099.33Dx = 1.554 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 82013 reflections
a = 9.6605 (3) Åθ = 2.6–25.7°
b = 21.2825 (10) ŵ = 3.68 mm1
c = 22.8491 (11) ÅT = 100 K
V = 4697.8 (3) Å3Platelet, translucent dark orange
Z = 40.14 × 0.12 × 0.04 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
8750 independent reflections
Radiation source: fine-focus sealed tube8052 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.062
two φ and one ω scans with 2° stepsθmax = 25.7°, θmin = 2.6°
Absorption correction: part of the refinement model (ΔF)
(DELABS in PLATON; Spek, 2003)
h = 1111
Tmin = 0.527, Tmax = 0.863k = 2525
82013 measured reflectionsl = 2527
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H-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 reflectionsΔρmax = 0.80 e Å3
543 parametersΔρmin = 0.83 e Å3
0 restraintsAbsolute structure: Flack (1983), 3779 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.010 (5)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
U0.270765 (17)0.586874 (8)0.744028 (8)0.02301 (5)
O10.3555 (3)0.49034 (15)0.73374 (17)0.0270 (9)
O20.3296 (4)0.56025 (16)0.62763 (17)0.0279 (8)
O30.1384 (4)0.64170 (17)0.68204 (17)0.0269 (8)
O40.2648 (4)0.71740 (15)0.76827 (15)0.0292 (8)
O50.2990 (4)0.60517 (16)0.83913 (15)0.0268 (8)
O60.5806 (4)0.53292 (17)0.82365 (17)0.0309 (9)
O70.1103 (3)0.55040 (16)0.76366 (17)0.0280 (9)
O80.4380 (3)0.61994 (15)0.72896 (15)0.0227 (8)
C10.5930 (4)0.4623 (2)0.7440 (3)0.0240 (11)
C20.4776 (6)0.4769 (2)0.7099 (2)0.0258 (12)
C30.4931 (5)0.4786 (2)0.6488 (2)0.0256 (12)
C40.6212 (5)0.4651 (2)0.6235 (3)0.0260 (12)
H40.62960.46640.58300.031*
C50.7372 (6)0.4495 (2)0.6571 (2)0.0254 (11)
C60.7209 (6)0.4490 (2)0.7174 (2)0.0269 (11)
H60.79670.43960.74090.032*
C70.8767 (6)0.4370 (2)0.6275 (3)0.0296 (13)
C80.8606 (6)0.3909 (3)0.5763 (3)0.0362 (14)
H8A0.81960.35260.59020.054*
H8B0.94990.38200.55990.054*
H8C0.80220.40920.54690.054*
C90.9360 (7)0.4990 (3)0.6032 (4)0.052 (2)
H9A1.02440.49110.58550.079*
H9B0.94670.52860.63450.079*
H9C0.87370.51580.57440.079*
C100.9856 (5)0.4103 (3)0.6698 (2)0.0353 (13)
H10A0.95610.36980.68350.053*
H10B0.99630.43820.70250.053*
H10C1.07260.40610.64980.053*
C110.3696 (6)0.4964 (2)0.6118 (3)0.0308 (13)
H11A0.39350.49440.57060.037*
H11B0.29360.46760.61900.037*
C120.2606 (5)0.5949 (2)0.5811 (2)0.0285 (11)
H12A0.16500.58140.57770.034*
H12B0.30650.58720.54400.034*
C130.2663 (5)0.6636 (2)0.5958 (2)0.0224 (10)
C140.2077 (5)0.6831 (2)0.6488 (2)0.0238 (11)
C150.2317 (6)0.7447 (2)0.6683 (2)0.0261 (12)
C160.3008 (5)0.7864 (2)0.6322 (2)0.0275 (12)
H160.31550.82720.64530.033*
C170.3490 (5)0.7696 (3)0.5771 (2)0.0252 (12)
C180.3331 (5)0.7068 (2)0.5606 (2)0.0220 (11)
H180.36850.69370.52470.026*
C190.4236 (6)0.8185 (3)0.5385 (2)0.0291 (13)
C200.5631 (6)0.8360 (3)0.5657 (3)0.0422 (16)
H20A0.60540.86880.54310.063*
H20B0.62240.79980.56600.063*
H20C0.54900.85030.60510.063*
C210.4494 (6)0.7927 (3)0.4759 (3)0.0330 (13)
H21A0.48600.82550.45160.049*
H21B0.36370.77790.45970.049*
H21C0.51440.75860.47770.049*
C220.3327 (7)0.8777 (3)0.5334 (3)0.0409 (15)
H22A0.31410.89400.57180.061*
H22B0.24710.86710.51460.061*
H22C0.38040.90890.51070.061*
C230.1897 (5)0.7600 (2)0.7301 (2)0.0282 (12)
H23A0.21280.80320.73930.034*
H23B0.09080.75440.73490.034*
C240.2588 (6)0.7353 (3)0.8295 (2)0.0299 (13)
H24A0.17480.71920.84730.036*
H24B0.25910.78070.83320.036*
C250.3835 (5)0.7079 (3)0.8591 (2)0.0255 (12)
C260.3977 (5)0.6421 (2)0.8618 (2)0.0233 (11)
C270.5194 (6)0.6165 (3)0.8859 (2)0.0244 (12)
C280.6215 (6)0.6565 (3)0.9075 (2)0.0281 (13)
H280.70020.63900.92430.034*
C290.6104 (5)0.7220 (3)0.9049 (2)0.0253 (12)
C300.4899 (5)0.7458 (3)0.8802 (2)0.0298 (13)
H300.47970.78920.87770.036*
C310.7293 (6)0.7638 (2)0.9267 (2)0.0317 (12)
C320.7572 (7)0.7514 (3)0.9916 (3)0.0462 (16)
H32A0.67720.76281.01410.069*
H32B0.83510.77591.00410.069*
H32C0.77680.70760.99720.069*
C330.6949 (6)0.8347 (3)0.9200 (3)0.0368 (14)
H33A0.61110.84410.94080.055*
H33B0.68310.84450.87930.055*
H33C0.76940.85930.93570.055*
C340.8622 (6)0.7499 (3)0.8909 (3)0.0406 (16)
H34A0.93760.77440.90610.061*
H34B0.84710.76080.85060.061*
H34C0.88430.70610.89380.061*
C350.5409 (6)0.5474 (3)0.8833 (3)0.0305 (13)
H35A0.61330.53480.91030.037*
H35B0.45640.52550.89360.037*
C360.5785 (6)0.4670 (3)0.8099 (2)0.0287 (13)
H36A0.49210.44820.82260.034*
H36B0.65440.44550.82910.034*
N10.7241 (5)0.6128 (2)0.7176 (2)0.0305 (10)
H1A0.63600.61730.72970.037*
H1B0.73420.57300.70480.037*
C370.7489 (6)0.6569 (2)0.6669 (2)0.0296 (12)
H370.84200.64870.65160.035*
C380.6448 (6)0.6425 (3)0.6182 (3)0.0344 (15)
H38A0.55250.64800.63280.041*
H38B0.65670.59990.60530.041*
H38C0.66000.67050.58590.041*
C390.8171 (6)0.6226 (3)0.7681 (3)0.0407 (16)
H39A0.91080.62620.75450.061*
H39B0.80980.58750.79430.061*
H39C0.79110.66040.78820.061*
C400.7427 (5)0.7246 (2)0.6861 (2)0.0234 (11)
C410.8540 (5)0.7639 (3)0.6729 (2)0.0269 (12)
H410.93070.74800.65320.032*
C420.8499 (6)0.8275 (3)0.6892 (3)0.0360 (14)
H420.92260.85400.67910.043*
C430.7383 (6)0.8509 (2)0.7204 (2)0.0342 (13)
H430.73700.89260.73250.041*
C440.6294 (6)0.8116 (2)0.7334 (3)0.0336 (14)
H440.55360.82740.75370.040*
C450.6304 (5)0.7491 (3)0.7170 (3)0.0291 (13)
H450.55600.72330.72650.035*
C460.0711 (7)0.5242 (3)0.9009 (3)0.0426 (16)
H460.11050.54540.86660.051*
Cl10.0905 (3)0.49365 (17)0.88148 (16)0.1219 (14)
Cl20.0520 (4)0.57911 (13)0.95616 (12)0.1363 (14)
Cl30.1795 (2)0.46306 (10)0.92023 (10)0.0676 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U0.02195 (8)0.02348 (8)0.02359 (9)0.00157 (7)0.00174 (7)0.00063 (9)
O10.0275 (19)0.0228 (18)0.031 (2)0.0011 (14)0.0068 (16)0.0008 (16)
O20.033 (2)0.0210 (18)0.029 (2)0.0054 (15)0.0062 (16)0.0030 (16)
O30.026 (2)0.027 (2)0.028 (2)0.0000 (16)0.0003 (15)0.0031 (16)
O40.032 (2)0.0325 (18)0.0235 (19)0.0079 (16)0.0027 (17)0.0015 (14)
O50.028 (2)0.031 (2)0.0218 (19)0.0028 (15)0.0012 (15)0.0015 (14)
O60.045 (2)0.025 (2)0.023 (2)0.0010 (17)0.0054 (17)0.0015 (16)
O70.0274 (18)0.0277 (19)0.029 (2)0.0009 (14)0.0009 (16)0.0011 (17)
O80.0220 (18)0.0200 (17)0.026 (2)0.0025 (14)0.0017 (14)0.0005 (15)
C10.026 (2)0.019 (2)0.027 (3)0.0002 (17)0.004 (2)0.002 (3)
C20.030 (3)0.017 (3)0.031 (3)0.000 (2)0.007 (2)0.001 (2)
C30.029 (3)0.022 (3)0.026 (3)0.001 (2)0.002 (2)0.004 (2)
C40.032 (3)0.019 (3)0.028 (3)0.000 (2)0.003 (2)0.007 (2)
C50.027 (3)0.014 (2)0.035 (3)0.001 (2)0.002 (2)0.001 (2)
C60.025 (3)0.015 (2)0.041 (3)0.003 (2)0.001 (2)0.000 (2)
C70.029 (3)0.015 (3)0.046 (4)0.004 (2)0.002 (2)0.002 (2)
C80.033 (3)0.043 (4)0.032 (4)0.007 (3)0.001 (2)0.002 (3)
C90.034 (4)0.050 (4)0.073 (6)0.003 (3)0.015 (4)0.004 (4)
C100.033 (3)0.033 (3)0.040 (3)0.006 (3)0.003 (2)0.005 (3)
C110.033 (3)0.022 (3)0.038 (4)0.001 (2)0.002 (2)0.004 (2)
C120.032 (3)0.027 (3)0.026 (3)0.001 (3)0.003 (2)0.000 (2)
C130.021 (3)0.022 (2)0.024 (3)0.002 (2)0.007 (2)0.0025 (19)
C140.020 (3)0.025 (3)0.026 (3)0.000 (2)0.004 (2)0.003 (2)
C150.026 (3)0.028 (3)0.024 (3)0.002 (3)0.000 (2)0.002 (2)
C160.033 (3)0.022 (3)0.027 (3)0.001 (2)0.005 (2)0.002 (2)
C170.021 (3)0.031 (3)0.023 (3)0.001 (2)0.006 (2)0.001 (2)
C180.020 (3)0.027 (3)0.019 (3)0.002 (2)0.000 (2)0.002 (2)
C190.031 (3)0.029 (3)0.027 (3)0.004 (2)0.000 (2)0.004 (2)
C200.044 (4)0.047 (4)0.035 (4)0.017 (3)0.005 (3)0.003 (3)
C210.035 (3)0.032 (3)0.032 (4)0.004 (3)0.001 (2)0.004 (3)
C220.062 (4)0.030 (3)0.030 (4)0.002 (3)0.001 (3)0.012 (3)
C230.025 (3)0.032 (3)0.028 (3)0.008 (2)0.002 (2)0.005 (2)
C240.036 (4)0.031 (3)0.022 (3)0.003 (3)0.001 (2)0.005 (2)
C250.027 (3)0.031 (3)0.019 (3)0.006 (2)0.001 (2)0.004 (2)
C260.028 (3)0.027 (3)0.015 (3)0.002 (2)0.004 (2)0.003 (2)
C270.028 (3)0.028 (3)0.017 (3)0.004 (2)0.002 (2)0.005 (2)
C280.034 (3)0.030 (3)0.021 (3)0.004 (2)0.001 (2)0.005 (2)
C290.026 (3)0.031 (3)0.018 (3)0.004 (2)0.003 (2)0.001 (2)
C300.033 (3)0.029 (3)0.027 (3)0.003 (2)0.002 (2)0.001 (2)
C310.031 (3)0.030 (3)0.034 (3)0.005 (3)0.007 (3)0.002 (2)
C320.054 (4)0.044 (4)0.040 (3)0.015 (3)0.013 (3)0.003 (3)
C330.038 (4)0.034 (3)0.039 (4)0.004 (3)0.006 (3)0.002 (3)
C340.030 (3)0.037 (4)0.055 (5)0.005 (3)0.002 (3)0.006 (3)
C350.037 (3)0.022 (3)0.032 (4)0.003 (2)0.001 (3)0.005 (2)
C360.034 (3)0.024 (3)0.027 (3)0.001 (2)0.001 (2)0.006 (2)
N10.026 (2)0.023 (2)0.043 (3)0.001 (2)0.005 (2)0.0066 (18)
C370.026 (3)0.027 (3)0.035 (3)0.002 (2)0.009 (2)0.003 (2)
C380.037 (4)0.036 (4)0.031 (4)0.009 (3)0.006 (3)0.002 (3)
C390.029 (3)0.047 (4)0.046 (4)0.002 (3)0.003 (3)0.017 (3)
C400.022 (3)0.025 (3)0.023 (3)0.002 (2)0.003 (2)0.003 (2)
C410.029 (3)0.025 (3)0.027 (3)0.005 (2)0.002 (2)0.001 (2)
C420.036 (4)0.028 (3)0.043 (4)0.007 (3)0.010 (3)0.002 (3)
C430.042 (4)0.021 (3)0.039 (3)0.005 (3)0.008 (3)0.007 (2)
C440.035 (3)0.031 (3)0.034 (4)0.011 (2)0.000 (2)0.007 (3)
C450.024 (3)0.026 (3)0.037 (4)0.001 (2)0.004 (2)0.002 (2)
C460.049 (4)0.045 (4)0.034 (4)0.002 (3)0.005 (3)0.003 (3)
Cl10.0419 (13)0.150 (3)0.174 (3)0.0300 (16)0.0248 (15)0.088 (2)
Cl20.286 (4)0.0694 (18)0.0534 (16)0.029 (2)0.036 (2)0.0101 (14)
Cl30.0557 (11)0.0666 (12)0.0804 (15)0.0139 (10)0.0060 (10)0.0290 (11)
Geometric parameters (Å, º) top
U—O12.224 (3)C21—H21C0.9600
U—O22.778 (4)C22—H22A0.9600
U—O32.237 (4)C22—H22B0.9600
U—O42.833 (3)C22—H22C0.9600
U—O52.224 (4)C23—H23A0.9700
U—O71.791 (3)C23—H23B0.9700
U—O81.795 (3)C24—C251.500 (8)
U—C143.049 (5)C24—H24A0.9700
O1—C21.331 (6)C24—H24B0.9700
O2—C121.457 (6)C25—C301.393 (8)
O2—C111.459 (6)C25—C261.409 (7)
O3—C141.342 (6)C26—C271.407 (8)
O4—C241.450 (6)C27—C281.393 (8)
O4—C231.452 (6)C27—C351.487 (7)
O5—C261.340 (6)C28—C291.400 (8)
O6—C361.438 (6)C28—H280.9300
O6—C351.448 (7)C29—C301.389 (7)
C1—C21.395 (7)C29—C311.536 (7)
C1—C61.406 (7)C30—H300.9300
C1—C361.515 (8)C31—C321.529 (8)
C2—C31.403 (8)C31—C341.552 (8)
C3—C41.396 (7)C31—C331.552 (7)
C3—C111.511 (8)C32—H32A0.9600
C4—C51.399 (7)C32—H32B0.9600
C4—H40.9300C32—H32C0.9600
C5—C61.386 (7)C33—H33A0.9600
C5—C71.532 (7)C33—H33B0.9600
C6—H60.9300C33—H33C0.9600
C7—C81.534 (8)C34—H34A0.9600
C7—C101.538 (8)C34—H34B0.9600
C7—C91.541 (9)C34—H34C0.9600
C8—H8A0.9600C35—H35A0.9700
C8—H8B0.9600C35—H35B0.9700
C8—H8C0.9600C36—H36A0.9700
C9—H9A0.9600C36—H36B0.9700
C9—H9B0.9600N1—C391.477 (7)
C9—H9C0.9600N1—C371.509 (6)
C10—H10A0.9600N1—H1A0.9000
C10—H10B0.9600N1—H1B0.9000
C10—H10C0.9600C37—C401.509 (7)
C11—H11A0.9700C37—C381.531 (8)
C11—H11B0.9700C37—H370.9800
C12—C131.501 (6)C38—H38A0.9600
C12—H12A0.9700C38—H38B0.9600
C12—H12B0.9700C38—H38C0.9600
C13—C181.381 (7)C39—H39A0.9600
C13—C141.400 (7)C39—H39B0.9600
C14—C151.405 (7)C39—H39C0.9600
C15—C161.383 (7)C40—C451.395 (7)
C15—C231.503 (7)C40—C411.395 (7)
C16—C171.390 (7)C41—C421.404 (8)
C16—H160.9300C41—H410.9300
C17—C181.397 (7)C42—C431.386 (8)
C17—C191.543 (7)C42—H420.9300
C18—H180.9300C43—C441.376 (8)
C19—C201.529 (8)C43—H430.9300
C19—C221.540 (8)C44—C451.382 (7)
C19—C211.553 (8)C44—H440.9300
C20—H20A0.9600C45—H450.9300
C20—H20B0.9600C46—Cl31.728 (7)
C20—H20C0.9600C46—Cl21.730 (7)
C21—H21A0.9600C46—Cl11.749 (7)
C21—H21B0.9600C46—H460.9800
O1—U—O268.60 (12)C19—C21—H21B109.5
O2—U—O367.48 (12)H21A—C21—H21B109.5
O1—U—O3128.72 (14)C19—C21—H21C109.5
O3—U—O466.46 (12)H21A—C21—H21C109.5
O4—U—O568.89 (11)H21B—C21—H21C109.5
O3—U—O5126.69 (13)C19—C22—H22A109.5
O5—U—O1102.69 (13)C19—C22—H22B109.5
O7—U—O8175.44 (16)H22A—C22—H22B109.5
O1—U—O786.83 (14)C19—C22—H22C109.5
O1—U—O890.60 (13)H22A—C22—H22C109.5
O2—U—O7109.17 (14)H22B—C22—H22C109.5
O2—U—O873.29 (13)O4—C23—C15107.1 (4)
O3—U—O783.68 (15)O4—C23—H23A110.3
O3—U—O8100.86 (14)C15—C23—H23A110.3
O4—U—O7111.00 (13)O4—C23—H23B110.3
O4—U—O870.82 (13)C15—C23—H23B110.3
O5—U—O786.40 (15)H23A—C23—H23B108.5
O5—U—O890.48 (14)O4—C24—C25107.5 (4)
O1—U—O4159.05 (11)O4—C24—H24A110.2
O2—U—O4113.04 (10)C25—C24—H24A110.2
O5—U—O2161.07 (12)O4—C24—H24B110.2
O7—U—C14107.27 (15)C25—C24—H24B110.2
O8—U—C1477.27 (14)H24A—C24—H24B108.5
O1—U—C14128.21 (14)C30—C25—C26119.2 (5)
O5—U—C14127.16 (13)C30—C25—C24121.6 (5)
O3—U—C1423.60 (13)C26—C25—C24119.0 (5)
O2—U—C1459.65 (12)O5—C26—C27121.3 (5)
O4—U—C1458.47 (12)O5—C26—C25119.7 (5)
C2—O1—U124.6 (3)C27—C26—C25118.9 (5)
C12—O2—C11114.3 (4)C28—C27—C26119.6 (5)
C12—O2—U120.2 (3)C28—C27—C35121.3 (5)
C11—O2—U118.8 (3)C26—C27—C35118.9 (5)
C14—O3—U114.5 (3)C27—C28—C29122.6 (5)
C24—O4—C23113.3 (4)C27—C28—H28118.7
C24—O4—U116.5 (3)C29—C28—H28118.7
C23—O4—U120.3 (3)C30—C29—C28116.4 (5)
C26—O5—U124.6 (3)C30—C29—C31123.2 (5)
C36—O6—C35114.2 (4)C28—C29—C31120.4 (5)
C2—C1—C6120.4 (5)C29—C30—C25123.3 (5)
C2—C1—C36117.8 (4)C29—C30—H30118.4
C6—C1—C36121.6 (5)C25—C30—H30118.4
O1—C2—C1121.8 (5)C32—C31—C29110.2 (5)
O1—C2—C3119.8 (5)C32—C31—C34109.4 (5)
C1—C2—C3118.4 (5)C29—C31—C34109.7 (4)
C4—C3—C2120.1 (5)C32—C31—C33107.6 (5)
C4—C3—C11121.3 (5)C29—C31—C33111.8 (5)
C2—C3—C11118.6 (5)C34—C31—C33108.1 (5)
C3—C4—C5122.1 (5)C31—C32—H32A109.5
C3—C4—H4119.0C31—C32—H32B109.5
C5—C4—H4119.0H32A—C32—H32B109.5
C6—C5—C4117.2 (5)C31—C32—H32C109.5
C6—C5—C7122.5 (5)H32A—C32—H32C109.5
C4—C5—C7120.2 (5)H32B—C32—H32C109.5
C5—C6—C1121.8 (5)C31—C33—H33A109.5
C5—C6—H6119.1C31—C33—H33B109.5
C1—C6—H6119.1H33A—C33—H33B109.5
C5—C7—C8111.0 (4)C31—C33—H33C109.5
C5—C7—C10112.8 (5)H33A—C33—H33C109.5
C8—C7—C10108.2 (5)H33B—C33—H33C109.5
C5—C7—C9109.7 (5)C31—C34—H34A109.5
C8—C7—C9108.1 (6)C31—C34—H34B109.5
C10—C7—C9106.8 (5)H34A—C34—H34B109.5
C7—C8—H8A109.5C31—C34—H34C109.5
C7—C8—H8B109.5H34A—C34—H34C109.5
H8A—C8—H8B109.5H34B—C34—H34C109.5
C7—C8—H8C109.5O6—C35—C27106.6 (5)
H8A—C8—H8C109.5O6—C35—H35A110.4
H8B—C8—H8C109.5C27—C35—H35A110.4
C7—C9—H9A109.5O6—C35—H35B110.4
C7—C9—H9B109.5C27—C35—H35B110.4
H9A—C9—H9B109.5H35A—C35—H35B108.6
C7—C9—H9C109.5O6—C36—C1106.3 (4)
H9A—C9—H9C109.5O6—C36—H36A110.5
H9B—C9—H9C109.5C1—C36—H36A110.5
C7—C10—H10A109.5O6—C36—H36B110.5
C7—C10—H10B109.5C1—C36—H36B110.5
H10A—C10—H10B109.5H36A—C36—H36B108.7
C7—C10—H10C109.5C39—N1—C37114.5 (4)
H10A—C10—H10C109.5C39—N1—H1A108.6
H10B—C10—H10C109.5C37—N1—H1A108.6
O2—C11—C3107.7 (4)C39—N1—H1B108.6
O2—C11—H11A110.2C37—N1—H1B108.6
C3—C11—H11A110.2H1A—N1—H1B107.6
O2—C11—H11B110.2C40—C37—N1111.4 (4)
C3—C11—H11B110.2C40—C37—C38112.1 (5)
H11A—C11—H11B108.5N1—C37—C38109.2 (4)
O2—C12—C13108.2 (4)C40—C37—H37108.0
O2—C12—H12A110.1N1—C37—H37108.0
C13—C12—H12A110.1C38—C37—H37108.0
O2—C12—H12B110.1C37—C38—H38A109.5
C13—C12—H12B110.1C37—C38—H38B109.5
H12A—C12—H12B108.4H38A—C38—H38B109.5
C18—C13—C14119.7 (4)C37—C38—H38C109.5
C18—C13—C12122.3 (5)H38A—C38—H38C109.5
C14—C13—C12117.8 (4)H38B—C38—H38C109.5
O3—C14—C13119.8 (4)N1—C39—H39A109.5
O3—C14—C15121.0 (5)N1—C39—H39B109.5
C13—C14—C15119.0 (5)H39A—C39—H39B109.5
O3—C14—U41.9 (2)N1—C39—H39C109.5
C13—C14—U109.8 (3)H39A—C39—H39C109.5
C15—C14—U111.6 (3)H39B—C39—H39C109.5
C16—C15—C14119.3 (5)C45—C40—C41119.0 (5)
C16—C15—C23123.5 (5)C45—C40—C37122.4 (5)
C14—C15—C23117.1 (5)C41—C40—C37118.6 (5)
C15—C16—C17122.5 (5)C40—C41—C42119.9 (5)
C15—C16—H16118.8C40—C41—H41120.1
C17—C16—H16118.8C42—C41—H41120.1
C16—C17—C18117.1 (5)C43—C42—C41120.3 (6)
C16—C17—C19120.0 (5)C43—C42—H42119.8
C18—C17—C19122.8 (5)C41—C42—H42119.8
C13—C18—C17122.0 (5)C44—C43—C42119.2 (5)
C13—C18—H18119.0C44—C43—H43120.4
C17—C18—H18119.0C42—C43—H43120.4
C20—C19—C22109.5 (5)C43—C44—C45121.4 (5)
C20—C19—C17110.1 (5)C43—C44—H44119.3
C22—C19—C17109.2 (5)C45—C44—H44119.3
C20—C19—C21108.6 (5)C44—C45—C40120.2 (5)
C22—C19—C21108.1 (5)C44—C45—H45119.9
C17—C19—C21111.3 (4)C40—C45—H45119.9
C19—C20—H20A109.5Cl3—C46—Cl2112.8 (4)
C19—C20—H20B109.5Cl3—C46—Cl1109.0 (4)
H20A—C20—H20B109.5Cl2—C46—Cl1110.0 (4)
C19—C20—H20C109.5Cl3—C46—H46108.3
H20A—C20—H20C109.5Cl2—C46—H46108.3
H20B—C20—H20C109.5Cl1—C46—H46108.3
C19—C21—H21A109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O80.901.912.781 (6)161
N1—H1B···Cg0.902.683.460 (4)146
C46—H46···O50.982.313.132 (7)141
C46—H46···O70.982.363.208 (8)145
 

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