Bis­[aqua­bis(1,3-di­phenyl­propane-1,3-dionato-κ2O,O′)­dioxouranium(VI)] di­cyclo­hexyl-18-crown-6-ether chloro­form disolvate

Fun, H.-K.; Kannan, S.; Chantrapromma, S.; Razak, I.A.; Usman, A.

doi:10.1107/S160053680201320X

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Bis[aquabis(1,3-diphenylpropane-1,3-dionato-κ²O,O′)dioxouranium(VI)] dicyclohexyl-18-crown-6-ether chloroform disolvate

H.-K. Fun, S. Kannan, S. Chantrapromma, I. A. Razak and A. Usman

In the title compound, [UO₂(DBM)₂(H₂O)]₂.(dicyclohexyl-18-crown-6)·2CHCl₃ or [UO₂(C₃₀H₂₂O₄)₂(H₂O)]₂·C₂₀H₃₆O₆·2CHCl₃, where DBM is 1,3-diphenylpropane-1,3-dionate, the U^VI atom is coordinated by seven O atoms to give a distorted pentagonal bipyramidal geometry. The structure is centrosymmetric. The 18-crown-6 molecule is hydrogen bonded (O—H

O) by the water molecule of [UO₂(DBM)₂(H₂O)], and these binuclear units are interconnected by C—H

O interactions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201320X/ci6125sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680201320X/ci6125Isup2.hkl Contains datablock I

CCDC reference: 193725

checkCIF report

Key indicators

Single-crystal X-ray study
T = 183 K
Mean (C-C) = 0.010 Å
R factor = 0.046
wR factor = 0.116
Data-to-parameter ratio = 21.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level B:



PLAT_601  Alert B Structure Contains Solvent Accessible VOIDS of     200.00 A   3


 Alert Level C:



PLAT_213  Alert C Atom C18     has ADP max/min Ratio ...........       3.20 oblate

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and _chemical_formula_moiety. This is
          usually due to the moiety formula being in the wrong format.
          Atom count from _chemical_formula_sum:   C82 H86 Cl6 O20 U2
          Atom count from _chemical_formula_moiety:C22 H38 Cl6 O6


 0 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 1 Alert Level C = Please check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990).

(I) top

Crystal data top

[UO₂(C₃₀H₂₂O₄)₂(H₂O)]·C₂₀H₃₆O₆·2CHCl₃	F(000) = 2048
M_r = 2080.27	D_x = 1.572 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 8192 reflections
a = 15.5427 (1) Å	θ = 2.6–28.3°
b = 15.2483 (1) Å	µ = 3.93 mm⁻¹
c = 19.4582 (2) Å	T = 183 K
β = 107.643 (1)°	Block, orange
V = 4394.67 (6) Å³	0.12 × 0.10 × 0.08 mm
Z = 2

Data collection top

Siemens SMART CCD area-detector diffractometer	10599 independent reflections
Radiation source: fine-focus sealed tube	7581 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.096
Detector resolution: 8.33 pixels mm^-1	θ_max = 28.3°, θ_min = 2.6°
ω scans	h = −20→20
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996)	k = −20→16
T_min = 0.650, T_max = 0.744	l = −25→21
26358 measured reflections

Refinement top

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.116	H-atom parameters constrained
S = 0.95	w = 1/[σ²(F_o²) + (0.0272P)²] where P = (F_o² + 2F_c²)/3
10599 reflections	(Δ/σ)_max < 0.001
496 parameters	Δρ_max = 1.57 e Å⁻³
0 restraints	Δρ_min = −4.23 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq
U1	0.229240 (12)	0.448563 (12)	0.411375 (10)	0.01317 (7)
O1	0.3102 (3)	0.4440 (2)	0.5342 (2)	0.0195 (8)
O2	0.3423 (3)	0.3446 (2)	0.4295 (2)	0.0215 (9)
O3	0.2261 (3)	0.3971 (3)	0.2965 (2)	0.0253 (9)
O4	0.1132 (3)	0.5191 (3)	0.32241 (19)	0.0207 (8)
O1W	0.1579 (3)	0.5509 (2)	0.4758 (2)	0.0230 (9)
H1W	0.1122	0.5737	0.4485	0.034*
H2W	0.1471	0.5381	0.5142	0.034*
O5	0.1540 (3)	0.3651 (2)	0.4188 (2)	0.0226 (9)
O6	0.3056 (3)	0.5319 (2)	0.4045 (2)	0.0186 (8)
C1	0.3753 (4)	0.4838 (4)	0.6810 (3)	0.0252 (13)
H1	0.3145	0.4695	0.6618	0.030*
C2	0.4066 (5)	0.5150 (5)	0.7500 (3)	0.0349 (16)
H2	0.3677	0.5203	0.7779	0.042*
C3	0.4951 (5)	0.5381 (4)	0.7776 (4)	0.0380 (17)
H3	0.5162	0.5608	0.8240	0.046*
C4	0.5539 (5)	0.5282 (5)	0.7370 (4)	0.0423 (19)
H4	0.6145	0.5430	0.7566	0.051*
C5	0.5229 (4)	0.4969 (4)	0.6687 (3)	0.0295 (14)
H5	0.5626	0.4912	0.6416	0.035*
C6	0.4333 (4)	0.4731 (3)	0.6385 (3)	0.0188 (12)
C7	0.3963 (4)	0.4390 (3)	0.5631 (3)	0.0182 (11)
C8	0.4547 (4)	0.4006 (4)	0.5299 (3)	0.0213 (12)
H8	0.5165	0.4075	0.5514	0.026*
C9	0.4256 (4)	0.3525 (4)	0.4660 (3)	0.0198 (12)
C10	0.4915 (4)	0.3042 (4)	0.4382 (3)	0.0229 (13)
C11	0.4589 (5)	0.2385 (5)	0.3870 (4)	0.0396 (17)
H11	0.3976	0.2254	0.3719	0.048*
C12	0.5167 (6)	0.1928 (5)	0.3585 (5)	0.057 (2)
H12	0.4944	0.1487	0.3247	0.069*
C13	0.6083 (6)	0.2128 (6)	0.3803 (5)	0.065 (3)
H13	0.6473	0.1814	0.3614	0.078*
C14	0.6427 (5)	0.2800 (5)	0.4305 (4)	0.047 (2)
H14	0.7036	0.2946	0.4441	0.057*
C15	0.5825 (4)	0.3247 (4)	0.4595 (4)	0.0303 (15)
H15	0.6042	0.3687	0.4935	0.036*
C16	0.2800 (5)	0.2966 (4)	0.2009 (4)	0.0325 (15)
H16	0.3009	0.2832	0.2498	0.039*
C17	0.3157 (5)	0.2532 (5)	0.1529 (4)	0.0439 (19)
H17	0.3592	0.2100	0.1696	0.053*
C18	0.2870 (5)	0.2739 (4)	0.0819 (4)	0.0391 (18)
H18	0.3120	0.2458	0.0500	0.047*
C19	0.2211 (5)	0.3365 (4)	0.0568 (4)	0.0382 (17)
H19	0.2006	0.3501	0.0080	0.046*
C20	0.1859 (4)	0.3784 (4)	0.1043 (3)	0.0273 (14)
H20	0.1419	0.4211	0.0871	0.033*
C21	0.2137 (4)	0.3595 (3)	0.1767 (3)	0.0186 (11)
C22	0.1790 (4)	0.4053 (3)	0.2311 (3)	0.0159 (11)
C23	0.1005 (4)	0.4541 (4)	0.2099 (3)	0.0199 (11)
H23	0.0649	0.4500	0.1620	0.024*
C24	0.0710 (3)	0.5092 (3)	0.2555 (3)	0.0149 (11)
C25	−0.0107 (4)	0.5650 (4)	0.2263 (3)	0.0193 (12)
C26	−0.0886 (4)	0.5310 (4)	0.1765 (3)	0.0272 (14)
H26	−0.0903	0.4729	0.1614	0.033*
C27	−0.1644 (5)	0.5858 (5)	0.1496 (4)	0.0386 (17)
H27	−0.2170	0.5631	0.1178	0.046*
C28	−0.1613 (5)	0.6724 (5)	0.1700 (4)	0.0408 (18)
H28	−0.2111	0.7085	0.1510	0.049*
C29	−0.0856 (5)	0.7046 (4)	0.2176 (4)	0.0386 (18)
H29	−0.0837	0.7634	0.2307	0.046*
C30	−0.0093 (4)	0.6514 (4)	0.2480 (3)	0.0256 (13)
H30	0.0413	0.6742	0.2822	0.031*
O8	−0.0071 (3)	0.3381 (2)	0.5736 (2)	0.0201 (8)
O9	0.1541 (3)	0.5147 (2)	0.6146 (2)	0.0204 (8)
O10	−0.0961 (3)	0.3145 (2)	0.4295 (2)	0.0212 (9)
C31	−0.0250 (4)	0.2540 (4)	0.4624 (3)	0.0220 (12)
H31	0.0316	0.2752	0.4561	0.026*
C32	−0.0455 (5)	0.1645 (4)	0.4301 (4)	0.0334 (16)
H32A	0.0044	0.1254	0.4524	0.040*
H32B	−0.0522	0.1674	0.3789	0.040*
C33	−0.1308 (5)	0.1284 (4)	0.4407 (4)	0.0398 (18)
H33A	−0.1423	0.0702	0.4197	0.048*
H33B	−0.1813	0.1657	0.4163	0.048*
C34	−0.1223 (5)	0.1236 (4)	0.5199 (4)	0.0420 (19)
H34A	−0.0763	0.0810	0.5431	0.050*
H34B	−0.1792	0.1038	0.5256	0.050*
C35	−0.0974 (5)	0.2132 (4)	0.5572 (3)	0.0295 (14)
H35A	−0.1482	0.2528	0.5403	0.035*
H35B	−0.0849	0.2060	0.6089	0.035*
C36	−0.0166 (4)	0.2525 (4)	0.5424 (3)	0.0222 (12)
H36	0.0367	0.2178	0.5676	0.027*
C37	0.0751 (4)	0.3804 (4)	0.5762 (4)	0.0275 (14)
H37A	0.0762	0.3940	0.5278	0.033*
H37B	0.1258	0.3424	0.5988	0.033*
C38	0.0811 (5)	0.4618 (4)	0.6184 (4)	0.0423 (19)
H38A	0.0253	0.4945	0.6001	0.051*
H38B	0.0885	0.4471	0.6683	0.051*
C39	0.1691 (4)	0.5889 (4)	0.6630 (3)	0.0260 (13)
H39A	0.2271	0.6149	0.6661	0.031*
H39B	0.1716	0.5684	0.7108	0.031*
C40	−0.0971 (4)	0.3419 (4)	0.3602 (3)	0.0237 (13)
H40A	−0.1107	0.2929	0.3269	0.028*
H40B	−0.0388	0.3658	0.3615	0.028*
Cl1	0.25033 (15)	0.65164 (18)	0.24715 (13)	0.0747 (8)
Cl2	0.41462 (17)	0.74811 (17)	0.31251 (17)	0.0842 (8)
Cl3	0.2533 (2)	0.7961 (3)	0.34343 (18)	0.1238 (13)
C41	0.3153 (6)	0.7091 (6)	0.3237 (5)	0.062 (3)
H41	0.3307	0.6687	0.3648	0.075*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.01321 (10)	0.01625 (11)	0.01280 (10)	0.00026 (8)	0.00805 (7)	−0.00090 (8)
O1	0.0176 (19)	0.026 (2)	0.0160 (19)	0.0050 (17)	0.0074 (15)	0.0027 (16)
O2	0.019 (2)	0.019 (2)	0.025 (2)	0.0017 (17)	0.0044 (16)	−0.0039 (17)
O3	0.028 (2)	0.034 (2)	0.014 (2)	0.0132 (19)	0.0075 (17)	−0.0070 (17)
O4	0.026 (2)	0.026 (2)	0.0121 (19)	0.0070 (17)	0.0086 (16)	−0.0024 (15)
O1W	0.025 (2)	0.030 (2)	0.017 (2)	0.0075 (18)	0.0113 (16)	−0.0017 (17)
O5	0.024 (2)	0.022 (2)	0.027 (2)	−0.0037 (17)	0.0142 (18)	−0.0047 (16)
O6	0.026 (2)	0.019 (2)	0.016 (2)	−0.0021 (16)	0.0129 (16)	−0.0013 (15)
C1	0.020 (3)	0.036 (3)	0.021 (3)	0.004 (3)	0.009 (2)	−0.001 (3)
C2	0.038 (4)	0.048 (4)	0.022 (3)	0.008 (3)	0.015 (3)	−0.007 (3)
C3	0.044 (4)	0.037 (4)	0.027 (4)	0.002 (3)	0.002 (3)	−0.013 (3)
C4	0.027 (4)	0.053 (5)	0.043 (4)	−0.011 (3)	0.005 (3)	−0.019 (3)
C5	0.027 (3)	0.031 (4)	0.034 (4)	−0.008 (3)	0.013 (3)	−0.007 (3)
C6	0.023 (3)	0.014 (3)	0.021 (3)	0.004 (2)	0.010 (2)	0.003 (2)
C7	0.022 (3)	0.016 (3)	0.018 (3)	0.003 (2)	0.010 (2)	0.005 (2)
C8	0.015 (3)	0.032 (3)	0.017 (3)	0.006 (2)	0.005 (2)	−0.001 (2)
C9	0.020 (3)	0.021 (3)	0.021 (3)	0.004 (2)	0.010 (2)	0.005 (2)
C10	0.024 (3)	0.024 (3)	0.024 (3)	0.006 (2)	0.010 (2)	−0.001 (2)
C11	0.032 (4)	0.046 (4)	0.045 (5)	0.006 (3)	0.017 (3)	−0.013 (3)
C12	0.050 (5)	0.059 (5)	0.063 (6)	0.012 (4)	0.017 (4)	−0.034 (4)
C13	0.047 (5)	0.085 (7)	0.069 (6)	0.033 (5)	0.027 (5)	−0.018 (5)
C14	0.033 (4)	0.073 (6)	0.039 (4)	0.007 (4)	0.016 (3)	−0.010 (4)
C15	0.024 (3)	0.041 (4)	0.030 (4)	0.005 (3)	0.014 (3)	−0.004 (3)
C16	0.040 (4)	0.035 (4)	0.029 (4)	0.010 (3)	0.020 (3)	−0.005 (3)
C17	0.056 (5)	0.037 (4)	0.049 (5)	0.021 (4)	0.032 (4)	−0.005 (3)
C18	0.056 (5)	0.031 (4)	0.044 (4)	−0.001 (3)	0.037 (4)	−0.018 (3)
C19	0.059 (5)	0.040 (4)	0.027 (4)	−0.004 (4)	0.030 (3)	−0.013 (3)
C20	0.036 (4)	0.026 (3)	0.026 (3)	−0.002 (3)	0.020 (3)	−0.007 (3)
C21	0.021 (3)	0.018 (3)	0.023 (3)	−0.004 (2)	0.016 (2)	−0.004 (2)
C22	0.020 (3)	0.015 (3)	0.015 (3)	−0.003 (2)	0.010 (2)	−0.004 (2)
C23	0.023 (3)	0.027 (3)	0.013 (3)	0.000 (2)	0.011 (2)	−0.005 (2)
C24	0.016 (3)	0.016 (3)	0.015 (3)	0.000 (2)	0.009 (2)	0.001 (2)
C25	0.022 (3)	0.027 (3)	0.013 (3)	0.008 (2)	0.011 (2)	0.005 (2)
C26	0.030 (3)	0.035 (4)	0.021 (3)	0.006 (3)	0.013 (3)	−0.001 (2)
C27	0.026 (4)	0.067 (5)	0.020 (3)	0.015 (3)	0.003 (3)	0.012 (3)
C28	0.037 (4)	0.049 (5)	0.038 (4)	0.026 (3)	0.016 (3)	0.015 (3)
C29	0.050 (5)	0.030 (4)	0.044 (4)	0.023 (3)	0.026 (4)	0.011 (3)
C30	0.036 (4)	0.021 (3)	0.026 (3)	0.009 (3)	0.017 (3)	0.003 (2)
O8	0.020 (2)	0.020 (2)	0.023 (2)	−0.0012 (16)	0.0106 (16)	−0.0058 (16)
O9	0.018 (2)	0.025 (2)	0.022 (2)	0.0001 (17)	0.0118 (16)	−0.0021 (16)
O10	0.030 (2)	0.021 (2)	0.018 (2)	0.0045 (17)	0.0160 (17)	0.0006 (15)
C31	0.026 (3)	0.018 (3)	0.026 (3)	0.005 (2)	0.014 (3)	0.000 (2)
C32	0.048 (4)	0.022 (3)	0.033 (4)	0.010 (3)	0.017 (3)	−0.003 (3)
C33	0.065 (5)	0.021 (3)	0.034 (4)	−0.011 (3)	0.016 (4)	−0.007 (3)
C34	0.064 (5)	0.024 (4)	0.039 (4)	−0.010 (3)	0.017 (4)	0.005 (3)
C35	0.043 (4)	0.025 (3)	0.026 (3)	−0.005 (3)	0.018 (3)	0.001 (3)
C36	0.027 (3)	0.022 (3)	0.021 (3)	0.006 (2)	0.012 (2)	0.004 (2)
C37	0.022 (3)	0.024 (3)	0.041 (4)	−0.001 (3)	0.016 (3)	−0.003 (3)
C38	0.043 (4)	0.046 (4)	0.054 (5)	−0.024 (3)	0.038 (4)	−0.025 (3)
C39	0.031 (3)	0.033 (3)	0.014 (3)	−0.004 (3)	0.008 (2)	−0.006 (2)
C40	0.034 (3)	0.026 (3)	0.015 (3)	−0.002 (3)	0.013 (2)	−0.004 (2)
Cl1	0.0512 (13)	0.108 (2)	0.0597 (15)	−0.0202 (14)	0.0083 (11)	0.0303 (14)
Cl2	0.0661 (16)	0.0668 (16)	0.135 (3)	−0.0214 (13)	0.0539 (16)	−0.0077 (15)
Cl3	0.092 (2)	0.217 (4)	0.079 (2)	0.042 (2)	0.0504 (18)	0.002 (2)
C41	0.052 (5)	0.072 (6)	0.060 (6)	−0.007 (4)	0.011 (4)	0.044 (5)

Geometric parameters (Å, º) top

U1—O5	1.764 (4)	C22—C23	1.381 (8)
U1—O6	1.771 (4)	C23—C24	1.397 (7)
U1—O2	2.312 (4)	C23—H23	0.93
U1—O1	2.340 (4)	C24—C25	1.490 (7)
U1—O4	2.348 (4)	C25—C30	1.382 (8)
U1—O3	2.356 (4)	C25—C26	1.401 (8)
U1—O1W	2.465 (4)	C26—C27	1.409 (9)
O1—C7	1.288 (7)	C26—H26	0.93
O2—C9	1.280 (6)	C27—C28	1.375 (10)
O3—C22	1.267 (6)	C27—H27	0.93
O4—C24	1.277 (6)	C28—C29	1.351 (10)
O1W—H1W	0.82	C28—H28	0.93
O1W—H2W	0.84	C29—C30	1.409 (8)
C1—C2	1.367 (8)	C29—H29	0.93
C1—C6	1.406 (8)	C30—H30	0.93
C1—H1	0.93	O8—C37	1.419 (7)
C2—C3	1.364 (10)	O8—C36	1.427 (7)
C2—H2	0.93	O9—C38	1.412 (7)
C3—C4	1.385 (10)	O9—C39	1.445 (7)
C3—H3	0.93	O10—C40	1.406 (6)
C4—C5	1.355 (9)	O10—C31	1.432 (6)
C4—H4	0.93	C31—C32	1.497 (8)
C5—C6	1.386 (8)	C31—C36	1.522 (8)
C5—H5	0.93	C31—H31	0.98
C6—C7	1.496 (8)	C32—C33	1.506 (10)
C7—C8	1.394 (8)	C32—H32A	0.97
C8—C9	1.394 (8)	C32—H32B	0.97
C8—H8	0.93	C33—C34	1.509 (9)
C9—C10	1.490 (8)	C33—H33A	0.97
C10—C15	1.385 (8)	C33—H33B	0.97
C10—C11	1.396 (8)	C34—C35	1.541 (8)
C11—C12	1.380 (9)	C34—H34A	0.97
C11—H11	0.93	C34—H34B	0.97
C12—C13	1.392 (11)	C35—C36	1.496 (8)
C12—H12	0.93	C35—H35A	0.97
C13—C14	1.405 (11)	C35—H35B	0.97
C13—H13	0.93	C36—H36	0.98
C14—C15	1.406 (9)	C37—C38	1.475 (8)
C14—H14	0.93	C37—H37A	0.97
C15—H15	0.93	C37—H37B	0.97
C16—C21	1.381 (8)	C38—H38A	0.97
C16—C17	1.390 (9)	C38—H38B	0.97
C16—H16	0.93	C39—C40ⁱ	1.504 (8)
C17—C18	1.355 (9)	C39—H39A	0.97
C17—H17	0.93	C39—H39B	0.97
C18—C19	1.377 (10)	C40—C39ⁱ	1.504 (8)
C18—H18	0.93	C40—H40A	0.97
C19—C20	1.366 (8)	C40—H40B	0.97
C19—H19	0.93	Cl1—C41	1.759 (9)
C20—C21	1.374 (8)	Cl2—C41	1.729 (8)
C20—H20	0.93	Cl3—C41	1.749 (11)
C21—C22	1.499 (7)	C41—H41	0.98

O5—U1—O6	179.44 (19)	C22—C23—C24	124.3 (5)
O5—U1—O2	89.11 (16)	C22—C23—H23	117.8
O6—U1—O2	90.43 (16)	C24—C23—H23	117.8
O5—U1—O1	93.38 (16)	O4—C24—C23	123.6 (5)
O6—U1—O1	86.16 (15)	O4—C24—C25	115.9 (5)
O2—U1—O1	71.09 (13)	C23—C24—C25	120.4 (5)
O5—U1—O4	90.64 (16)	C30—C25—C26	119.6 (5)
O6—U1—O4	89.93 (16)	C30—C25—C24	119.7 (5)
O2—U1—O4	143.55 (13)	C26—C25—C24	120.6 (5)
O1—U1—O4	145.24 (13)	C25—C26—C27	119.2 (6)
O5—U1—O3	90.83 (17)	C25—C26—H26	120.4
O6—U1—O3	89.34 (16)	C27—C26—H26	120.4
O2—U1—O3	73.28 (13)	C28—C27—C26	120.7 (7)
O1—U1—O3	144.03 (13)	C28—C27—H27	119.7
O4—U1—O3	70.28 (13)	C26—C27—H27	119.7
O5—U1—O1W	90.22 (16)	C29—C28—C27	119.6 (6)
O6—U1—O1W	89.95 (15)	C29—C28—H28	120.2
O2—U1—O1W	142.61 (13)	C27—C28—H28	120.2
O1—U1—O1W	71.64 (13)	C28—C29—C30	121.7 (6)
O4—U1—O1W	73.84 (13)	C28—C29—H29	119.1
O3—U1—O1W	144.11 (13)	C30—C29—H29	119.1
C7—O1—U1	127.9 (4)	C25—C30—C29	119.2 (6)
C9—O2—U1	127.8 (3)	C25—C30—H30	120.4
C22—O3—U1	139.4 (3)	C29—C30—H30	120.4
C24—O4—U1	137.8 (3)	C37—O8—C36	114.0 (4)
U1—O1W—H1W	111.8	C38—O9—C39	112.8 (5)
U1—O1W—H2W	123.3	C40—O10—C31	113.8 (4)
H1W—O1W—H2W	107.9	O10—C31—C32	111.2 (5)
C2—C1—C6	121.2 (6)	O10—C31—C36	106.5 (4)
C2—C1—H1	119.4	C32—C31—C36	110.9 (5)
C6—C1—H1	119.4	O10—C31—H31	109.4
C3—C2—C1	119.5 (7)	C32—C31—H31	109.4
C3—C2—H2	120.2	C36—C31—H31	109.4
C1—C2—H2	120.2	C31—C32—C33	111.1 (5)
C2—C3—C4	120.6 (6)	C31—C32—H32A	109.4
C2—C3—H3	119.7	C33—C32—H32A	109.4
C4—C3—H3	119.7	C31—C32—H32B	109.4
C5—C4—C3	119.8 (6)	C33—C32—H32B	109.4
C5—C4—H4	120.1	H32A—C32—H32B	108.0
C3—C4—H4	120.1	C32—C33—C34	110.5 (6)
C4—C5—C6	121.4 (6)	C32—C33—H33A	109.5
C4—C5—H5	119.3	C34—C33—H33A	109.5
C6—C5—H5	119.3	C32—C33—H33B	109.5
C5—C6—C1	117.5 (5)	C34—C33—H33B	109.5
C5—C6—C7	123.0 (5)	H33A—C33—H33B	108.1
C1—C6—C7	119.5 (5)	C33—C34—C35	111.7 (5)
O1—C7—C8	124.0 (5)	C33—C34—H34A	109.3
O1—C7—C6	116.6 (5)	C35—C34—H34A	109.3
C8—C7—C6	119.4 (5)	C33—C34—H34B	109.3
C7—C8—C9	123.6 (5)	C35—C34—H34B	109.3
C7—C8—H8	118.2	H34A—C34—H34B	107.9
C9—C8—H8	118.2	C36—C35—C34	111.8 (6)
O2—C9—C8	123.1 (5)	C36—C35—H35A	109.3
O2—C9—C10	116.2 (5)	C34—C35—H35A	109.3
C8—C9—C10	120.6 (5)	C36—C35—H35B	109.3
C15—C10—C11	119.5 (6)	C34—C35—H35B	109.3
C15—C10—C9	122.2 (5)	H35A—C35—H35B	107.9
C11—C10—C9	118.3 (5)	O8—C36—C35	105.6 (5)
C12—C11—C10	120.7 (7)	O8—C36—C31	112.8 (4)
C12—C11—H11	119.6	C35—C36—C31	112.7 (5)
C10—C11—H11	119.6	O8—C36—H36	108.5
C11—C12—C13	119.8 (7)	C35—C36—H36	108.5
C11—C12—H12	120.1	C31—C36—H36	108.5
C13—C12—H12	120.1	O8—C37—C38	107.9 (5)
C12—C13—C14	120.7 (7)	O8—C37—H37A	110.1
C12—C13—H13	119.7	C38—C37—H37A	110.1
C14—C13—H13	119.7	O8—C37—H37B	110.1
C13—C14—C15	118.3 (7)	C38—C37—H37B	110.1
C13—C14—H14	120.8	H37A—C37—H37B	108.4
C15—C14—H14	120.8	O9—C38—C37	111.6 (5)
C10—C15—C14	121.0 (6)	O9—C38—H38A	109.3
C10—C15—H15	119.5	C37—C38—H38A	109.3
C14—C15—H15	119.5	O9—C38—H38B	109.3
C21—C16—C17	120.6 (6)	C37—C38—H38B	109.3
C21—C16—H16	119.7	H38A—C38—H38B	108.0
C17—C16—H16	119.7	O9—C39—C40ⁱ	113.3 (5)
C18—C17—C16	120.0 (7)	O9—C39—H39A	108.9
C18—C17—H17	120.0	C40ⁱ—C39—H39A	108.9
C16—C17—H17	120.0	O9—C39—H39B	108.9
C17—C18—C19	120.1 (6)	C40ⁱ—C39—H39B	108.9
C17—C18—H18	120.0	H39A—C39—H39B	107.7
C19—C18—H18	120.0	O10—C40—C39ⁱ	106.7 (5)
C20—C19—C18	119.5 (6)	O10—C40—H40A	110.4
C20—C19—H19	120.3	C39ⁱ—C40—H40A	110.4
C18—C19—H19	120.3	O10—C40—H40B	110.4
C19—C20—C21	122.0 (6)	C39ⁱ—C40—H40B	110.4
C19—C20—H20	119.0	H40A—C40—H40B	108.6
C21—C20—H20	119.0	Cl2—C41—Cl3	109.8 (5)
C20—C21—C16	117.8 (5)	Cl2—C41—Cl1	111.7 (5)
C20—C21—C22	123.9 (5)	Cl3—C41—Cl1	110.5 (5)
C16—C21—C22	118.3 (5)	Cl2—C41—H41	108.2
O3—C22—C23	122.9 (5)	Cl3—C41—H41	108.2
O3—C22—C21	116.1 (5)	Cl1—C41—H41	108.2
C23—C22—C21	120.9 (5)

O5—U1—O1—C7	130.5 (4)	C9—C10—C15—C14	−177.8 (6)
O6—U1—O1—C7	−49.1 (4)	C13—C14—C15—C10	−1.2 (12)
O2—U1—O1—C7	42.6 (4)	C21—C16—C17—C18	1.6 (11)
O4—U1—O1—C7	−133.5 (4)	C16—C17—C18—C19	−1.5 (11)
O3—U1—O1—C7	34.4 (5)	C17—C18—C19—C20	1.1 (11)
O1W—U1—O1—C7	−140.4 (4)	C18—C19—C20—C21	−0.7 (10)
O5—U1—O2—C9	−141.2 (5)	C19—C20—C21—C16	0.7 (9)
O6—U1—O2—C9	38.5 (5)	C19—C20—C21—C22	178.3 (6)
O1—U1—O2—C9	−47.3 (4)	C17—C16—C21—C20	−1.2 (10)
O4—U1—O2—C9	128.9 (4)	C17—C16—C21—C22	−178.9 (6)
O3—U1—O2—C9	127.6 (5)	U1—O3—C22—C23	−3.5 (9)
O1W—U1—O2—C9	−52.0 (5)	U1—O3—C22—C21	175.8 (4)
O5—U1—O3—C22	85.3 (6)	C20—C21—C22—O3	−162.7 (5)
O6—U1—O3—C22	−95.3 (6)	C16—C21—C22—O3	14.9 (8)
O2—U1—O3—C22	174.1 (6)	C20—C21—C22—C23	16.6 (8)
O1—U1—O3—C22	−177.8 (5)	C16—C21—C22—C23	−165.8 (6)
O4—U1—O3—C22	−5.1 (5)	O3—C22—C23—C24	9.4 (9)
O1W—U1—O3—C22	−6.2 (7)	C21—C22—C23—C24	−169.8 (5)
O5—U1—O4—C24	−76.4 (5)	U1—O4—C24—C23	−14.4 (9)
O6—U1—O4—C24	103.6 (5)	U1—O4—C24—C25	169.4 (4)
O2—U1—O4—C24	13.0 (6)	C22—C23—C24—O4	−1.2 (9)
O1—U1—O4—C24	−173.3 (5)	C22—C23—C24—C25	174.8 (5)
O3—U1—O4—C24	14.3 (5)	O4—C24—C25—C30	40.3 (7)
O1W—U1—O4—C24	−166.4 (5)	C23—C24—C25—C30	−136.0 (6)
C6—C1—C2—C3	1.7 (10)	O4—C24—C25—C26	−140.3 (5)
C1—C2—C3—C4	−1.8 (11)	C23—C24—C25—C26	43.4 (8)
C2—C3—C4—C5	1.4 (11)	C30—C25—C26—C27	−0.1 (9)
C3—C4—C5—C6	−0.9 (11)	C24—C25—C26—C27	−179.6 (5)
C4—C5—C6—C1	0.8 (9)	C25—C26—C27—C28	2.1 (10)
C4—C5—C6—C7	179.5 (6)	C26—C27—C28—C29	−1.7 (11)
C2—C1—C6—C5	−1.2 (9)	C27—C28—C29—C30	−0.7 (11)
C2—C1—C6—C7	−179.9 (6)	C26—C25—C30—C29	−2.2 (9)
U1—O1—C7—C8	−27.3 (7)	C24—C25—C30—C29	177.3 (5)
U1—O1—C7—C6	155.7 (3)	C28—C29—C30—C25	2.7 (10)
C5—C6—C7—O1	−159.9 (5)	C40—O10—C31—C32	−75.3 (6)
C1—C6—C7—O1	18.7 (7)	C40—O10—C31—C36	163.8 (5)
C5—C6—C7—C8	23.0 (8)	O10—C31—C32—C33	−60.8 (7)
C1—C6—C7—C8	−158.4 (5)	C36—C31—C32—C33	57.5 (7)
O1—C7—C8—C9	−9.4 (9)	C31—C32—C33—C34	−58.8 (7)
C6—C7—C8—C9	167.5 (5)	C32—C33—C34—C35	55.3 (8)
U1—O2—C9—C8	36.3 (8)	C33—C34—C35—C36	−51.6 (8)
U1—O2—C9—C10	−145.9 (4)	C37—O8—C36—C35	169.6 (5)
C7—C8—C9—O2	5.2 (9)	C37—O8—C36—C31	−66.9 (6)
C7—C8—C9—C10	−172.5 (5)	C34—C35—C36—O8	174.2 (5)
O2—C9—C10—C15	162.0 (6)	C34—C35—C36—C31	50.7 (7)
C8—C9—C10—C15	−20.2 (9)	O10—C31—C36—O8	−52.3 (6)
O2—C9—C10—C11	−15.5 (8)	C32—C31—C36—O8	−173.4 (5)
C8—C9—C10—C11	162.3 (6)	O10—C31—C36—C35	67.2 (6)
C15—C10—C11—C12	1.2 (11)	C32—C31—C36—C35	−54.0 (7)
C9—C10—C11—C12	178.8 (7)	C36—O8—C37—C38	−172.3 (5)
C10—C11—C12—C13	−0.7 (13)	C39—O9—C38—C37	−172.1 (6)
C11—C12—C13—C14	−0.8 (15)	O8—C37—C38—O9	−171.1 (5)
C12—C13—C14—C15	1.7 (14)	C38—O9—C39—C40ⁱ	−71.2 (7)
C11—C10—C15—C14	−0.3 (10)	C31—O10—C40—C39ⁱ	−174.5 (4)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O8ⁱ	0.82	2.06	2.814 (6)	152
O1W—H2W···O9	0.84	1.96	2.775 (5)	166
C1—H1···O9	0.93	2.48	3.319 (8)	150
C5—H5···O6ⁱⁱ	0.93	2.50	3.410 (8)	167
C15—H15···O6ⁱⁱ	0.93	2.55	3.467 (8)	167
C41—H41···O6	0.98	2.30	3.153 (10)	145

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1.

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