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In the title compound, [UO2(C15H11O2)2(C18H15OP)] or [UO2(DBM)2(Ph3PO)], where DBM is di­benzoyl methanate, the UVI atom is coordinated by seven O atoms in a distorted pentagonal–bipyramidal geometry. The di­phenyl­propane-1,3-dionate system acts as a chelating ligand and coordinates through both of its ketonate O atoms and the tri­phenyl phosphine oxide ligand coordinates through the O atom. The U—O distances range from 1.759 (4) to 2.385 (4) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803012923/ci6234sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803012923/ci6234Isup2.hkl
Contains datablock I

CCDC reference: 217392

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.036
  • wR factor = 0.084
  • Data-to-parameter ratio = 14.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_213 Alert C Atom has ADP max/min Ratio ............. 3.10 C18
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

The compounds of uranyl bis(β-diketonates) with neutral donor ligands are of importance to understand the nature of the species extracted during the solvent-extraction separation of the uranyl ion using mixtures of β-diketones and neutral ligands (Ramakrishna & Patil, 1984). An increase (or synergism) in solvent extraction separation of uranyl ion from nitric acid medium by using mixtures of β-diketones and phosphine oxides or phosphate have been reported (Irving & Edgington, 1960; Healy, 1961; Akiba, 1977). The species responsible for the extraction have been isolated in solid state for some of the systems and characterized by IR (Ferraro & Healy, 1962), 1H, 19F NMR (Subramanian & Viswanatha, 1969) spectroscopic and elemental analyses methods. In few of the cases it has been characterized using single-crystal X-ray diffraction methods (Taylor & McLaren, 1979; Lu et al., 1977; Taylor & Waugh, 1977a,b; Kannan et al., 2001a). In continuation of our work on uranyl bis(/b-diketones) with neutral donor ligands (Kannan & Venugopal, 1995; Kannan, Venugopal, Pillai, Droege & Barnes, 1996; Kannan, Venugopal, Pillai, Droege, Barnes & Schlmber, 1996; Kannan et al., 1997, 2001a,b; Kannan & Ferguson, 1997; Kannan, 2000; Fun et al., 2002; Rajagopal et al., 2002), we report here the structure of [UO2(DBM)2(Ph3PO)], (I), where DBM is dibenzoyl methanate.

The structure of (I) is shown in Fig. 1. Selected bond distances and angles are listed in Table 1. The structure of the molecule shows that the U atom is surrounded by seven O atoms in a pentagonal–bipyramidal geometry. Four O atoms of the DBM and one O atom of phosphine oxide form a planar pentagon and two uranyl O atoms occupy the apices. The average of U—Ouranyl [1.767 (4) Å], U—ODBM [2.365 (4) Å] distances are within the accepted ranges (Taylor & McLaren, 1979; Kannan, Venugopal, Pillai, Droege & Barnes, 1996; Kannan, Venugopal, Pillai, Droege, Barnes & Schlmber, 1996; Kannan et al., 1997, 2000, 2001b). The U—O(P) phosphine oxide distance [2.375 (4) Å] is comparable with those reported earlier for uranyl bis(β-diketone)–phosphine adducts (Taylor & McLaren, 1979; Lu et al., 1977; Kannan et al. 2001a). The overall bond lengths and angles show that the U atom has a distorted pentogonal bi-pyramidal geometry. In both the DBM ligands, the benzene rings are not coplanar and they form dihedral angles of 11.9 (4) and 32.9 (5)°, respectively. Fig. 2 shows the crystal packing of the title compound viewed down the b axis. The structure is stabilized by van der Waals interactions. It is noteworthy that the O atoms belonging to the DBM and phosphine oxide moieties participating in the uranium(VI) coordination, are not at all involved in any hydrogen bonding.

Experimental top

[UO2(DBM)2(Ph3PO)] was prepared by refuxing [UO2(DBM)2(H2O)2] (300 mg) with Ph3PO (112 mg) in chloroform for 15 min. The solution was filtered and layered with dodecane. The solution on slow evaporation yielded the title compound in 90% yield. Crystals suitable for the X-ray diffraction analyses were obtained from chloroform/toluene mixture.

Refinement top

All the H atoms were generated geometrically and were allowed to ride on their respective parent atoms with SHELXL97 (Sheldrick, 1997) defaults for bond lengths and isotropic displacement parameters.

Computing details top

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.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing 50% probability displacement ellipsoids and the atom-numbering scheme. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The packing of the molecules of (I), viewed down the b axis.
Bis(1,3-diphenylpropane-1,3-dionato-κ2O,O')dioxo(triphenylphosphine oxide-κO)uranium(VI) top
Crystal data top
[UO2(C15H11O2)2(C18H15OP)]F(000) = 1952
Mr = 994.78Dx = 1.604 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 18.345 (2) Åθ = 10–15°
b = 11.022 (4) ŵ = 4.03 mm1
c = 20.924 (4) ÅT = 293 K
β = 103.170 (13)°Rectangular block, orange
V = 4119.5 (18) Å30.3 × 0.25 × 0.13 mm
Z = 4
Data collection top
Enraf-Nonius CAD-4
diffractometer
5259 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.023
Graphite monochromatorθmax = 25.0°, θmin = 2.0°
ω–2θ scansh = 021
Absorption correction: ψ scan
(North et al., 1968)
k = 013
Tmin = 0.325, Tmax = 0.597l = 2424
7464 measured reflections2 standard reflections every 60min min
7221 independent reflections intensity decay: <1%
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)] = 0.036H-atom parameters constrained
wR(F2) = 0.084 w = 1/[σ2(Fo2) + (0.0316P)2 + 1.9225P]
where P = (Fo2 + 2Fc2)/3
S = 1.29(Δ/σ)max < 0.001
7221 reflectionsΔρmax = 0.96 e Å3
515 parametersΔρmin = 0.92 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00049 (6)
Crystal data top
[UO2(C15H11O2)2(C18H15OP)]V = 4119.5 (18) Å3
Mr = 994.78Z = 4
Monoclinic, P21/cMo Kα radiation
a = 18.345 (2) ŵ = 4.03 mm1
b = 11.022 (4) ÅT = 293 K
c = 20.924 (4) Å0.3 × 0.25 × 0.13 mm
β = 103.170 (13)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
5259 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.023
Tmin = 0.325, Tmax = 0.5972 standard reflections every 60min min
7464 measured reflections intensity decay: <1%
7221 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0360 restraints
wR(F2) = 0.084H-atom parameters constrained
S = 1.29Δρmax = 0.96 e Å3
7221 reflectionsΔρmin = 0.92 e Å3
515 parameters
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
xyzUiso*/Ueq
C10.2374 (6)0.6889 (7)0.5628 (4)0.081 (3)
H10.25210.66960.52430.097*
C20.2526 (5)0.6062 (9)0.6142 (4)0.088 (3)
H20.27630.53300.61010.106*
C30.2317 (5)0.6352 (8)0.6704 (5)0.084 (3)
H30.24210.58170.70570.101*
C40.1960 (5)0.7407 (8)0.6759 (4)0.077 (3)
H40.18070.75800.71440.093*
C50.1819 (5)0.8239 (8)0.6242 (4)0.070 (2)
H50.15900.89740.62910.083*
C60.2016 (4)0.7983 (6)0.5657 (3)0.0516 (18)
C70.1875 (4)0.8807 (6)0.5087 (3)0.0441 (16)
C80.1378 (4)0.9775 (6)0.5034 (3)0.0564 (18)
H80.11500.99090.53810.068*
C90.1199 (4)1.0552 (5)0.4503 (3)0.0412 (15)
C100.0643 (4)1.1555 (6)0.4482 (3)0.0486 (17)
C110.0401 (4)1.1930 (7)0.5031 (4)0.065 (2)
H110.05481.15100.54240.078*
C120.0065 (5)1.2947 (9)0.4989 (5)0.086 (3)
H120.02191.32030.53610.103*
C130.0294 (5)1.3560 (8)0.4427 (6)0.087 (3)
H130.05941.42450.44090.104*
C140.0076 (5)1.3153 (8)0.3875 (5)0.087 (3)
H140.02461.35480.34760.105*
C150.0385 (4)1.2179 (7)0.3910 (4)0.065 (2)
H150.05301.19290.35330.079*
C160.4287 (5)0.6525 (9)0.5145 (6)0.126 (5)
H160.37980.63530.49250.152*
C170.4636 (6)0.5802 (12)0.5657 (7)0.172 (7)
H170.43700.51670.57890.207*
C180.5372 (5)0.5990 (11)0.5982 (6)0.135 (5)
H180.56050.54820.63230.162*
C190.5741 (5)0.6932 (9)0.5791 (4)0.091 (3)
H190.62380.70780.60000.109*
C200.5387 (4)0.7679 (7)0.5287 (4)0.065 (2)
H200.56510.83250.51640.078*
C210.4650 (4)0.7497 (7)0.4956 (4)0.061 (2)
C220.4263 (4)0.8299 (6)0.4415 (3)0.0473 (16)
C230.4660 (4)0.9074 (7)0.4101 (4)0.0571 (18)
H230.51730.91370.42720.068*
C240.4351 (4)0.9769 (6)0.3548 (3)0.0491 (16)
C250.4847 (4)1.0425 (6)0.3192 (3)0.0520 (17)
C260.5529 (4)1.0865 (9)0.3508 (5)0.083 (3)
H260.56941.07510.39590.100*
C270.5981 (6)1.1482 (9)0.3164 (6)0.105 (4)
H270.64441.17790.33850.126*
C280.5747 (6)1.1651 (10)0.2508 (6)0.099 (3)
H280.60501.20670.22820.119*
C290.5077 (6)1.1221 (10)0.2182 (5)0.095 (3)
H290.49191.13440.17330.114*
C300.4618 (5)1.0584 (8)0.2524 (4)0.083 (3)
H300.41611.02710.22980.099*
C310.3202 (5)1.2707 (8)0.2035 (4)0.082 (3)
H310.34791.27800.24640.099*
C320.3545 (7)1.2872 (11)0.1518 (6)0.123 (4)
H320.40531.30500.15950.148*
C330.3128 (7)1.2768 (10)0.0898 (6)0.107 (4)
H330.33561.29030.05500.128*
C340.2402 (7)1.2480 (10)0.0766 (5)0.105 (4)
H340.21391.23850.03340.126*
C350.2036 (5)1.2319 (8)0.1280 (3)0.074 (2)
H350.15281.21400.11940.089*
C360.2448 (4)1.2434 (5)0.1914 (3)0.0450 (16)
C370.0639 (4)1.3319 (6)0.2074 (3)0.0542 (18)
H370.08971.40520.21090.065*
C380.0132 (5)1.3291 (7)0.1818 (4)0.070 (2)
H380.03881.40100.16890.084*
C390.0516 (4)1.2221 (8)0.1755 (4)0.071 (2)
H390.10281.22090.15760.085*
C400.0142 (4)1.1168 (9)0.1955 (4)0.079 (3)
H400.04051.04410.19190.095*
C410.0615 (4)1.1167 (7)0.2209 (4)0.0608 (19)
H410.08601.04390.23370.073*
C420.1022 (3)1.2244 (6)0.2276 (3)0.0436 (15)
C430.2099 (4)1.3547 (6)0.3730 (3)0.058 (2)
H430.19541.28250.38950.070*
C440.2208 (5)1.4595 (7)0.4106 (4)0.079 (3)
H440.21181.45760.45250.095*
C450.2441 (5)1.5650 (6)0.3881 (4)0.071 (2)
H450.25071.63380.41450.086*
C460.2575 (5)1.5696 (7)0.3279 (4)0.070 (2)
H460.27511.64100.31310.084*
C470.2453 (5)1.4685 (6)0.2873 (4)0.065 (2)
H470.25331.47290.24500.077*
C480.2213 (3)1.3614 (5)0.3099 (3)0.0384 (14)
O10.2153 (2)0.8585 (4)0.32443 (18)0.0399 (10)
O20.3073 (2)1.0711 (4)0.44177 (19)0.0479 (11)
O30.2207 (3)0.8538 (4)0.4639 (2)0.0549 (12)
O40.1475 (2)1.0457 (4)0.3997 (2)0.0457 (10)
O50.3551 (2)0.8214 (4)0.4257 (2)0.0559 (12)
O60.3645 (2)0.9845 (4)0.3312 (2)0.0520 (12)
O70.2251 (2)1.1133 (4)0.29911 (18)0.0403 (10)
P10.20126 (9)1.22671 (14)0.25987 (7)0.0358 (4)
U10.262398 (12)0.965493 (19)0.382762 (10)0.03185 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.149 (9)0.056 (5)0.050 (5)0.003 (5)0.050 (5)0.013 (4)
C20.132 (9)0.081 (6)0.058 (5)0.019 (6)0.034 (5)0.016 (5)
C30.105 (7)0.070 (6)0.079 (6)0.003 (6)0.021 (5)0.031 (5)
C40.106 (7)0.086 (6)0.044 (4)0.005 (6)0.027 (5)0.023 (4)
C50.090 (6)0.071 (5)0.046 (4)0.005 (5)0.014 (4)0.002 (4)
C60.069 (5)0.050 (4)0.036 (4)0.002 (4)0.012 (3)0.003 (3)
C70.067 (4)0.044 (4)0.029 (3)0.016 (3)0.027 (3)0.004 (3)
C80.076 (5)0.060 (4)0.041 (4)0.005 (4)0.032 (4)0.007 (4)
C90.047 (4)0.042 (4)0.037 (3)0.006 (3)0.016 (3)0.001 (3)
C100.040 (4)0.049 (4)0.060 (4)0.005 (3)0.017 (3)0.007 (3)
C110.064 (5)0.072 (5)0.061 (5)0.006 (4)0.020 (4)0.010 (4)
C120.074 (6)0.086 (7)0.095 (7)0.011 (5)0.015 (5)0.033 (5)
C130.064 (6)0.065 (6)0.136 (9)0.020 (5)0.030 (6)0.011 (6)
C140.070 (6)0.082 (6)0.122 (8)0.024 (5)0.047 (6)0.029 (6)
C150.063 (5)0.073 (5)0.070 (5)0.017 (4)0.036 (4)0.021 (4)
C160.068 (6)0.117 (9)0.169 (11)0.031 (6)0.025 (7)0.084 (8)
C170.087 (8)0.170 (13)0.233 (15)0.029 (8)0.017 (9)0.146 (12)
C180.053 (6)0.141 (10)0.184 (12)0.000 (6)0.029 (7)0.105 (10)
C190.063 (6)0.108 (8)0.088 (7)0.006 (5)0.012 (5)0.034 (6)
C200.048 (5)0.072 (5)0.070 (5)0.002 (4)0.002 (4)0.004 (4)
C210.041 (4)0.051 (4)0.086 (6)0.007 (4)0.004 (4)0.015 (4)
C220.037 (4)0.041 (4)0.060 (4)0.005 (3)0.002 (3)0.002 (3)
C230.042 (4)0.054 (4)0.075 (5)0.004 (4)0.012 (4)0.008 (4)
C240.048 (4)0.046 (4)0.055 (4)0.007 (4)0.016 (3)0.005 (3)
C250.049 (4)0.056 (4)0.055 (4)0.008 (4)0.020 (3)0.011 (4)
C260.055 (5)0.110 (7)0.089 (6)0.019 (5)0.024 (5)0.019 (6)
C270.072 (7)0.107 (9)0.142 (10)0.019 (6)0.034 (7)0.011 (8)
C280.086 (8)0.116 (9)0.112 (9)0.004 (7)0.059 (7)0.023 (7)
C290.095 (8)0.127 (9)0.070 (6)0.003 (7)0.036 (6)0.014 (6)
C300.074 (6)0.108 (8)0.070 (6)0.015 (5)0.027 (5)0.002 (5)
C310.078 (6)0.113 (8)0.062 (5)0.002 (6)0.027 (5)0.016 (5)
C320.109 (9)0.164 (12)0.116 (9)0.000 (8)0.067 (8)0.062 (9)
C330.119 (9)0.121 (9)0.103 (9)0.033 (8)0.075 (8)0.055 (7)
C340.127 (10)0.131 (10)0.058 (6)0.052 (9)0.025 (6)0.028 (6)
C350.091 (6)0.099 (7)0.038 (4)0.026 (5)0.027 (4)0.020 (4)
C360.049 (4)0.031 (3)0.057 (4)0.002 (3)0.017 (3)0.009 (3)
C370.045 (4)0.050 (4)0.062 (5)0.014 (3)0.002 (3)0.001 (3)
C380.068 (6)0.060 (5)0.077 (6)0.029 (4)0.008 (4)0.007 (4)
C390.036 (4)0.100 (7)0.063 (5)0.011 (5)0.015 (4)0.018 (5)
C400.043 (5)0.080 (6)0.112 (7)0.019 (4)0.014 (5)0.011 (5)
C410.048 (4)0.047 (4)0.089 (6)0.001 (4)0.020 (4)0.002 (4)
C420.043 (4)0.048 (4)0.042 (4)0.010 (3)0.014 (3)0.008 (3)
C430.083 (6)0.046 (4)0.055 (4)0.015 (4)0.036 (4)0.005 (3)
C440.119 (8)0.060 (5)0.059 (5)0.007 (5)0.024 (5)0.000 (4)
C450.103 (7)0.039 (4)0.071 (6)0.003 (4)0.018 (5)0.013 (4)
C460.089 (6)0.046 (5)0.073 (6)0.014 (4)0.018 (5)0.001 (4)
C470.105 (6)0.041 (4)0.054 (4)0.006 (5)0.032 (4)0.002 (4)
C480.035 (3)0.028 (3)0.047 (4)0.001 (3)0.002 (3)0.000 (3)
O10.047 (2)0.038 (2)0.035 (2)0.0058 (19)0.0089 (19)0.0073 (18)
O20.051 (3)0.051 (3)0.036 (2)0.011 (2)0.000 (2)0.0072 (19)
O30.079 (3)0.044 (3)0.050 (3)0.001 (2)0.032 (3)0.011 (2)
O40.045 (2)0.053 (3)0.042 (2)0.003 (2)0.018 (2)0.007 (2)
O50.040 (3)0.048 (3)0.074 (3)0.000 (2)0.003 (2)0.012 (2)
O60.042 (3)0.063 (3)0.050 (3)0.010 (2)0.010 (2)0.007 (2)
O70.048 (3)0.035 (2)0.039 (2)0.008 (2)0.0134 (19)0.0169 (19)
P10.0391 (9)0.0320 (8)0.0361 (8)0.0019 (7)0.0086 (7)0.0056 (7)
U10.03523 (13)0.03071 (12)0.02900 (12)0.00034 (12)0.00623 (8)0.00140 (12)
Geometric parameters (Å, º) top
C1—C61.381 (10)C27—C281.354 (13)
C1—C21.389 (11)C27—H270.93
C1—H10.93C28—C291.349 (13)
C2—C31.356 (11)C28—H280.93
C2—H20.93C29—C301.410 (11)
C3—C41.353 (11)C29—H290.93
C3—H30.93C30—H300.93
C4—C51.398 (10)C31—C361.381 (10)
C4—H40.93C31—C321.381 (11)
C5—C61.381 (9)C31—H310.93
C5—H50.93C32—C331.351 (15)
C6—C71.473 (9)C32—H320.93
C7—O31.265 (7)C33—C341.336 (14)
C7—C81.392 (9)C33—H330.93
C8—C91.381 (9)C34—C351.402 (12)
C8—H80.93C34—H340.93
C9—O41.279 (7)C35—C361.376 (10)
C9—C101.497 (9)C35—H350.93
C10—C151.368 (9)C36—P11.801 (7)
C10—C111.385 (9)C37—C421.394 (8)
C11—C121.401 (11)C37—C381.394 (10)
C11—H110.93C37—H370.93
C12—C131.338 (12)C38—C391.364 (11)
C12—H120.93C38—H380.93
C13—C141.380 (12)C39—C401.364 (11)
C13—H130.93C39—H390.93
C14—C151.358 (10)C40—C411.369 (9)
C14—H140.93C40—H400.93
C15—H150.93C41—C421.392 (9)
C16—C211.367 (11)C41—H410.93
C16—C171.371 (12)C42—P11.789 (6)
C16—H160.93C43—C481.383 (9)
C17—C181.382 (13)C43—C441.387 (10)
C17—H170.93C43—H430.93
C18—C191.350 (13)C44—C451.359 (10)
C18—H180.93C44—H440.93
C19—C201.379 (10)C45—C461.339 (11)
C19—H190.93C45—H450.93
C20—C211.385 (9)C46—C471.388 (10)
C20—H200.93C46—H460.93
C21—C221.484 (9)C47—C481.382 (9)
C22—O51.276 (7)C47—H470.93
C22—C231.382 (9)C48—P11.806 (6)
C23—C241.397 (9)O1—U11.774 (4)
C23—H230.93O2—U11.759 (4)
C24—O61.278 (8)O3—U12.361 (4)
C24—C251.488 (9)O4—U12.385 (4)
C25—C261.364 (10)O5—U12.350 (4)
C25—C301.377 (10)O6—U12.375 (4)
C26—C271.394 (12)O7—P11.505 (4)
C26—H260.93O7—U12.375 (4)
C6—C1—C2123.5 (8)C25—C30—H30120.1
C6—C1—H1118.3C29—C30—H30120.1
C2—C1—H1118.3C36—C31—C32120.1 (9)
C3—C2—C1118.1 (9)C36—C31—H31120.0
C3—C2—H2120.9C32—C31—H31120.0
C1—C2—H2120.9C33—C32—C31118.8 (11)
C4—C3—C2121.0 (8)C33—C32—H32120.6
C4—C3—H3119.5C31—C32—H32120.6
C2—C3—H3119.5C34—C33—C32122.5 (10)
C3—C4—C5120.4 (8)C34—C33—H33118.7
C3—C4—H4119.8C32—C33—H33118.7
C5—C4—H4119.8C33—C34—C35120.1 (10)
C6—C5—C4120.9 (8)C33—C34—H34120.0
C6—C5—H5119.6C35—C34—H34120.0
C4—C5—H5119.6C36—C35—C34118.3 (9)
C5—C6—C1116.2 (7)C36—C35—H35120.9
C5—C6—C7123.9 (7)C34—C35—H35120.9
C1—C6—C7119.9 (6)C35—C36—C31120.2 (7)
O3—C7—C8122.5 (6)C35—C36—P1120.8 (6)
O3—C7—C6115.5 (6)C31—C36—P1119.0 (6)
C8—C7—C6121.9 (6)C42—C37—C38119.6 (7)
C9—C8—C7124.9 (6)C42—C37—H37120.2
C9—C8—H8117.5C38—C37—H37120.2
C7—C8—H8117.5C39—C38—C37120.8 (7)
O4—C9—C8123.3 (6)C39—C38—H38119.6
O4—C9—C10115.6 (5)C37—C38—H38119.6
C8—C9—C10121.2 (6)C38—C39—C40119.6 (7)
C15—C10—C11117.5 (7)C38—C39—H39120.2
C15—C10—C9119.7 (6)C40—C39—H39120.2
C11—C10—C9122.7 (7)C39—C40—C41120.9 (8)
C10—C11—C12119.6 (8)C39—C40—H40119.5
C10—C11—H11120.2C41—C40—H40119.5
C12—C11—H11120.2C40—C41—C42120.8 (7)
C13—C12—C11121.6 (9)C40—C41—H41119.6
C13—C12—H12119.2C42—C41—H41119.6
C11—C12—H12119.2C41—C42—C37118.2 (6)
C12—C13—C14118.6 (8)C41—C42—P1121.7 (5)
C12—C13—H13120.7C37—C42—P1120.0 (5)
C14—C13—H13120.7C48—C43—C44117.6 (7)
C15—C14—C13120.5 (9)C48—C43—H43121.2
C15—C14—H14119.8C44—C43—H43121.2
C13—C14—H14119.8C45—C44—C43122.2 (8)
C14—C15—C10122.2 (8)C45—C44—H44118.9
C14—C15—H15118.9C43—C44—H44118.9
C10—C15—H15118.9C46—C45—C44119.9 (7)
C21—C16—C17120.6 (9)C46—C45—H45120.1
C21—C16—H16119.7C44—C45—H45120.1
C17—C16—H16119.7C45—C46—C47120.5 (7)
C16—C17—C18121.9 (10)C45—C46—H46119.8
C16—C17—H17119.1C47—C46—H46119.8
C18—C17—H17119.1C48—C47—C46119.7 (7)
C19—C18—C17118.0 (9)C48—C47—H47120.1
C19—C18—H18121.0C46—C47—H47120.1
C17—C18—H18121.0C47—C48—C43120.1 (6)
C18—C19—C20120.3 (9)C47—C48—P1122.8 (5)
C18—C19—H19119.8C43—C48—P1117.0 (5)
C20—C19—H19119.8C7—O3—U1134.5 (4)
C19—C20—C21122.1 (8)C9—O4—U1133.1 (4)
C19—C20—H20118.9C22—O5—U1131.1 (4)
C21—C20—H20118.9C24—O6—U1130.8 (4)
C16—C21—C20117.0 (7)P1—O7—U1166.2 (3)
C16—C21—C22120.5 (7)O7—P1—C42109.8 (3)
C20—C21—C22122.5 (7)O7—P1—C36113.0 (3)
O5—C22—C23122.8 (6)C42—P1—C36107.3 (3)
O5—C22—C21116.0 (6)O7—P1—C48111.8 (3)
C23—C22—C21121.2 (6)C42—P1—C48106.6 (3)
C22—C23—C24125.0 (7)C36—P1—C48108.0 (3)
C22—C23—H23117.5O2—U1—O1178.51 (19)
C24—C23—H23117.5O2—U1—O589.82 (18)
O6—C24—C23122.7 (6)O1—U1—O590.56 (18)
O6—C24—C25117.2 (6)O2—U1—O390.97 (18)
C23—C24—C25120.1 (6)O1—U1—O387.77 (17)
C26—C25—C30118.8 (7)O5—U1—O372.39 (16)
C26—C25—C24121.9 (7)O2—U1—O794.22 (17)
C30—C25—C24119.3 (7)O1—U1—O786.32 (16)
C25—C26—C27120.7 (9)O5—U1—O7143.79 (15)
C25—C26—H26119.6O3—U1—O7143.29 (15)
C27—C26—H26119.6O2—U1—O688.20 (18)
C28—C27—C26120.2 (10)O1—U1—O693.28 (17)
C28—C27—H27119.9O5—U1—O669.91 (15)
C26—C27—H27119.9O3—U1—O6142.29 (16)
C29—C28—C27120.4 (10)O7—U1—O674.26 (14)
C29—C28—H28119.8O2—U1—O486.51 (18)
C27—C28—H28119.8O1—U1—O492.30 (17)
C28—C29—C30120.0 (9)O5—U1—O4141.31 (15)
C28—C29—H29120.0O3—U1—O469.19 (15)
C30—C29—H29120.0O7—U1—O474.90 (13)
C25—C30—C29119.9 (9)O6—U1—O4148.20 (14)
C6—C1—C2—C30.7 (15)C38—C37—C42—C410.5 (10)
C1—C2—C3—C41.1 (15)C38—C37—C42—P1179.5 (6)
C2—C3—C4—C52.0 (15)C48—C43—C44—C452.0 (14)
C3—C4—C5—C62.4 (14)C43—C44—C45—C460.2 (15)
C4—C5—C6—C11.9 (12)C44—C45—C46—C472.2 (14)
C4—C5—C6—C7179.1 (7)C45—C46—C47—C481.9 (13)
C2—C1—C6—C51.1 (13)C46—C47—C48—C430.4 (11)
C2—C1—C6—C7179.8 (8)C46—C47—C48—P1178.0 (6)
C5—C6—C7—O3167.7 (7)C44—C43—C48—C472.3 (11)
C1—C6—C7—O311.3 (10)C44—C43—C48—P1176.2 (6)
C5—C6—C7—C815.6 (11)C8—C7—O3—U130.0 (10)
C1—C6—C7—C8165.4 (8)C6—C7—O3—U1153.3 (5)
O3—C7—C8—C91.0 (11)C8—C9—O4—U127.4 (9)
C6—C7—C8—C9177.4 (6)C10—C9—O4—U1154.2 (4)
C7—C8—C9—O40.2 (11)C23—C22—O5—U131.2 (10)
C7—C8—C9—C10178.6 (6)C21—C22—O5—U1149.8 (5)
O4—C9—C10—C159.3 (9)C23—C24—O6—U127.7 (10)
C8—C9—C10—C15169.2 (7)C25—C24—O6—U1154.5 (4)
O4—C9—C10—C11167.3 (6)U1—O7—P1—C4299.4 (10)
C8—C9—C10—C1114.2 (10)U1—O7—P1—C36140.8 (10)
C15—C10—C11—C122.6 (11)U1—O7—P1—C4818.7 (11)
C9—C10—C11—C12174.0 (7)C41—C42—P1—O720.8 (6)
C10—C11—C12—C131.0 (14)C37—C42—P1—O7160.3 (5)
C11—C12—C13—C141.6 (15)C41—C42—P1—C36102.4 (6)
C12—C13—C14—C152.6 (14)C37—C42—P1—C3676.5 (6)
C13—C14—C15—C100.9 (14)C41—C42—P1—C48142.1 (6)
C11—C10—C15—C141.7 (12)C37—C42—P1—C4839.0 (6)
C9—C10—C15—C14175.1 (7)C35—C36—P1—O7110.6 (6)
C21—C16—C17—C183 (2)C31—C36—P1—O770.9 (7)
C16—C17—C18—C191 (3)C35—C36—P1—C4210.6 (7)
C17—C18—C19—C200 (2)C31—C36—P1—C42167.9 (6)
C18—C19—C20—C210.4 (16)C35—C36—P1—C48125.3 (6)
C17—C16—C21—C202.4 (18)C31—C36—P1—C4853.3 (7)
C17—C16—C21—C22178.1 (12)C47—C48—P1—O7142.6 (6)
C19—C20—C21—C160.9 (14)C43—C48—P1—O738.9 (6)
C19—C20—C21—C22179.6 (8)C47—C48—P1—C4297.4 (6)
C16—C21—C22—O516.3 (12)C43—C48—P1—C4281.1 (6)
C20—C21—C22—O5164.3 (7)C47—C48—P1—C3617.7 (7)
C16—C21—C22—C23162.7 (9)C43—C48—P1—C36163.8 (5)
C20—C21—C22—C2316.7 (12)C22—O5—U1—O246.6 (6)
O5—C22—C23—C245.7 (12)C22—O5—U1—O1134.9 (6)
C21—C22—C23—C24173.3 (7)C22—O5—U1—O3137.7 (6)
C22—C23—C24—O67.1 (12)C22—O5—U1—O750.3 (7)
C22—C23—C24—C25170.7 (7)C22—O5—U1—O641.6 (6)
O6—C24—C25—C26150.7 (7)C22—O5—U1—O4130.8 (6)
C23—C24—C25—C2631.4 (11)C7—O3—U1—O249.8 (6)
O6—C24—C25—C3030.0 (10)C7—O3—U1—O1129.4 (6)
C23—C24—C25—C30147.9 (8)C7—O3—U1—O5139.3 (6)
C30—C25—C26—C271.1 (13)C7—O3—U1—O748.6 (7)
C24—C25—C26—C27179.6 (8)C7—O3—U1—O6138.2 (6)
C25—C26—C27—C280.1 (16)C7—O3—U1—O436.1 (6)
C26—C27—C28—C290.3 (18)P1—O7—U1—O229.9 (11)
C27—C28—C29—C300.4 (17)P1—O7—U1—O1148.7 (11)
C26—C25—C30—C291.7 (13)P1—O7—U1—O5125.4 (10)
C24—C25—C30—C29179.0 (8)P1—O7—U1—O367.4 (11)
C28—C29—C30—C251.4 (15)P1—O7—U1—O6116.8 (11)
C36—C31—C32—C330.4 (17)P1—O7—U1—O455.3 (10)
C31—C32—C33—C342 (2)C24—O6—U1—O250.8 (6)
C32—C33—C34—C352.6 (19)C24—O6—U1—O1129.0 (6)
C33—C34—C35—C361.8 (15)C24—O6—U1—O539.6 (6)
C34—C35—C36—C310.4 (12)C24—O6—U1—O338.4 (7)
C34—C35—C36—P1178.9 (6)C24—O6—U1—O7145.7 (6)
C32—C31—C36—C350.3 (13)C24—O6—U1—O4131.3 (5)
C32—C31—C36—P1178.2 (8)C9—O4—U1—O258.2 (5)
C42—C37—C38—C390.9 (12)C9—O4—U1—O1120.9 (5)
C37—C38—C39—C401.1 (13)C9—O4—U1—O527.1 (6)
C38—C39—C40—C411.1 (13)C9—O4—U1—O334.2 (5)
C39—C40—C41—C420.8 (13)C9—O4—U1—O7153.5 (5)
C40—C41—C42—C370.5 (11)C9—O4—U1—O6139.1 (5)
C40—C41—C42—P1179.4 (6)

Experimental details

Crystal data
Chemical formula[UO2(C15H11O2)2(C18H15OP)]
Mr994.78
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)18.345 (2), 11.022 (4), 20.924 (4)
β (°) 103.170 (13)
V3)4119.5 (18)
Z4
Radiation typeMo Kα
µ (mm1)4.03
Crystal size (mm)0.3 × 0.25 × 0.13
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.325, 0.597
No. of measured, independent and
observed [I > 2σ(I)] reflections
7464, 7221, 5259
Rint0.023
(sin θ/λ)max1)0.594
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.084, 1.29
No. of reflections7221
No. of parameters515
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.96, 0.92

Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CAD-4 Software, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1999), SHELXL97.

Selected geometric parameters (Å, º) top
C7—O31.265 (7)O2—U11.759 (4)
C9—O41.279 (7)O3—U12.361 (4)
C22—O51.276 (7)O4—U12.385 (4)
C24—O61.278 (8)O5—U12.350 (4)
C36—P11.801 (7)O6—U12.375 (4)
C42—P11.789 (6)O7—P11.505 (4)
C48—P11.806 (6)O7—U12.375 (4)
O1—U11.774 (4)
C9—C8—C7124.9 (6)O2—U1—O688.20 (18)
C22—C23—C24125.0 (7)O1—U1—O693.28 (17)
O2—U1—O1178.51 (19)O5—U1—O669.91 (15)
O2—U1—O589.82 (18)O3—U1—O6142.29 (16)
O1—U1—O590.56 (18)O7—U1—O674.26 (14)
O2—U1—O390.97 (18)O2—U1—O486.51 (18)
O1—U1—O387.77 (17)O1—U1—O492.30 (17)
O5—U1—O372.39 (16)O5—U1—O4141.31 (15)
O2—U1—O794.22 (17)O3—U1—O469.19 (15)
O1—U1—O786.32 (16)O7—U1—O474.90 (13)
O5—U1—O7143.79 (15)O6—U1—O4148.20 (14)
O3—U1—O7143.29 (15)
 

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