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The title complex, bis­(tetra­phenyl­phospho­nium) dioxobis(py­ridine-2,6-dicarbo­thio­ato-O,N,O')­uranium(VI), (C24H20P)2[UO2(C7H3NO2S2)2], was prepared by reacting two equivalents of ­pyridine-2,6-bis­(mono­thio­carboxyl­ate) (pdtc) with uranyl nitrate. The geometry of the eight-coordinate U atom is hexagonal bipyramidal, with the uranyl O atoms in apical positions. This is the first reported complex in which this ligand binds a metal through the O and not the S atoms. Principal bond lengths include uranyl lengths of 1.774 (2) Å, U-O distances of 2.434 (2) and 2.447 (3) Å, and two U-N distances of 2.647 (3) Å. The anion lies on an inversion centre.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100017285/bk1565sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100017285/bk1565Isup2.hkl
Contains datablock I

CCDC reference: 162542

Comment top

First identified as a bacterial metabolite (Ockels et al., 1978), pyridine-2,6-bis(monothiocarboxylate) (pdtc) has been isolated from several strains of Psuedomonas and is produced as an extracellular reducing agent (Lee et al., 1999). This reductant has been proven to be a necessary component in carbon tetrachloride decomposition and its production varies with environmental conditions. In the course of our studies of the interactions of extracellular microbial chelators with actinides, we isolated the complex of pdtc bound to the dioxouranium(VI) (uranyl) ion. When pdtc is combined with hard metal ions such as FeIII or UVI, one of two structures forms, either a polymeric or a monomeric species. The monomeric species is generally isolated if there is an excess of metal, otherwise the very insoluble polymeric species is favoured. The complexes are sparingly soluble in aqueous solution and small crystallites precipitate rapidly. To slow down crystallization and improve the solubility of the complex in organic solvents, the bis(tetraphenylphosphonium) salt of pdtc was used, to give the title complex, (I). By using acetonitrile/water (80/20) as the solvent, large yellow blocks were isolated from the reaction. The crystals were harvested after 50% of the solvent had evaporated. When the complex was prepared in pure acetonitrile, a platelike crystal morphology was observed, but the structure was the same as that of the block crystals. X-ray quality crystals of the polymeric species have not yet been obtained, but efforts to isolate them and complexes of this ligand with other actinides are on-going. \sch

The unit cell of (I) contains two tetraphenylphosphonium cations, with the [UO2(pdtc)2]2- anion sitting on an inversion centre. Fig. 2 shows a view down the a axis of the unit cell, illustrating the stacking of the tetraphenylphosphonium cations and the relative orientation of the cations and the anion. The coordination environment of the U atom is hexagonal bipyramidal, with two axial O atoms, and with two tridentate pdtc ligands bound through four carbonyl O atoms and two pyridine N atoms in the equatorial plane. This is the first example of a metal being bound through the O and not the S atoms of this ligand. Previous structures of metal complexes of pdtc include structures with PdII (Espinet et al., 1994), NiII, NiIII and CoIII (Kruger & Holm, 1990), and the hard ion FeIII (Hildebrand et al., 1984). In all these cases, the ligand is tridentate as in (I) but binds to the metal in an NS2 fashion.

For the non-sulfur-containing ligand, pyridine-2,6-dicarboxylate (PDC), the uranyl structures for two monomers (Marangoni et al., 1974; Cousson et al., 1991) and a polymer (Immirzi et al., 1975) are known. The repeat unit of the polymer consists of a linear uranyl group equatorially surrounded by five ligand atoms: two carboxylate O atoms and the N atom of one PDC ion, an O atom of an adjacent PDC ligand and one water molecule. The bridging carboxylate leads to a polymeric structure in the form of a single helix. The uranyl group binds two axial O atoms at 1.76 (2) Å, a pyridine N atom at 2.51 (2) Å, two carboxylate O atoms at 2.36 (1) and 2.42 (2) Å, another carboxylate O atom from an adjacent PDC unit at 2.33 Å and a bound water at 2.42 (2) Å. One of the monomer structures (Marangoni et al., 1974?) contains two axial O atoms and two tridentate ligands, at bond lengths of U—N 2.73 (2) Å, and U—O 2.37 (2) and 2.42 (3) Å (correct ref?). The longer bond lengths to the tridentate ligand in the monomer studied by Marangoni et al. (1974) (correct?) and the current structure are consistent with the coordination number of 6 in the equatorial plane, versus 5 for the polymer.

Related literature top

For related literature, see: Cousson et al. (1991); Espinet et al. (1994); Hildebrand et al. (1983, 1984); Immirzi et al. (1975); Lee et al. (1999); Marangoni et al. (1974); Ockels et al. (1978).

Experimental top

The pdtc used in the preparation of (I) was synthesized using the method of Hildebrand et al. (1983). A solution of [pdtc][PPh4]2 (8.47 mg, 0.010 mmol) dissolved in acetontrile (5 ml) was slowly added to an aqueous solution (1 ml) of uranyl nitrate (12 mg, 0.0304 mmol). The resulting solution was not stirred and was allowed to stand, loosely capped, in a fume hood for 96 h. Yellow block crystals were harvested by decanting the mother liquor and coating the crystals with mineral oil. Synthesis of the monomeric species is quantitative based on the ligand.

Refinement top

H atoms were placed in ideal positions and refined as riding, with their displacement parameters fixed at 1.2Ueq of their parent atoms. C—H = ? The final difference Fourier map contained a peak of 1.21 e Å-3 located 0.8 Å from U.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with the atom-numbering scheme. Displacement ellipsoids are shown at the 40% probability level and H atoms are drawn as small spheres of arbitrary radii.
[Figure 2] Fig. 2. The view down the a axis of the unit cell of (I).
bis(tetraphenylphosphonium) dioxobis(pyridine-2,6-dicarbothioate-O,N,O')uranium(VI) top
Crystal data top
2C24H20P·[UO2(C7H3NO2S2)2]Z = 1
Mr = 1343.22F(000) = 666
Triclinic, P1Dx = 1.655 Mg m3
a = 9.2351 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.607 (1) ÅCell parameters from 4192 reflections
c = 13.807 (1) Åθ = 1.5–23.3°
α = 77.891 (1)°µ = 3.28 mm1
β = 81.46 (1)°T = 293 K
γ = 69.14 (1)°Block, yellow
V = 1347.7 (2) Å30.32 × 0.25 × 0.20 mm
Data collection top
Siemens P4/PC CCD area-detector
diffractometer
5605 independent reflections
Radiation source: fine-focus sealed tube5485 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
Detector resolution: 8.192 pixels/mm pixels mm-1θmax = 28.5°, θmin = 1.5°
ω scansh = 1111
Absorption correction: empirical (using intensity measurements)
(SADABS in SHELXL97; Sheldrick, 1997)
k = 1415
Tmin = 0.31, Tmax = 0.52l = 1818
9541 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0345P)2]
where P = (Fo2 + 2Fc2)/3
5605 reflections(Δ/σ)max = 0.001
349 parametersΔρmax = 1.21 e Å3
0 restraintsΔρmin = 1.95 e Å3
Crystal data top
2C24H20P·[UO2(C7H3NO2S2)2]γ = 69.14 (1)°
Mr = 1343.22V = 1347.7 (2) Å3
Triclinic, P1Z = 1
a = 9.2351 (7) ÅMo Kα radiation
b = 11.607 (1) ŵ = 3.28 mm1
c = 13.807 (1) ÅT = 293 K
α = 77.891 (1)°0.32 × 0.25 × 0.20 mm
β = 81.46 (1)°
Data collection top
Siemens P4/PC CCD area-detector
diffractometer
5605 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS in SHELXL97; Sheldrick, 1997)
5485 reflections with I > 2σ(I)
Tmin = 0.31, Tmax = 0.52Rint = 0.031
9541 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.073H-atom parameters constrained
S = 1.04Δρmax = 1.21 e Å3
5605 reflectionsΔρmin = 1.95 e Å3
349 parameters
Special details top

Experimental. Intensities were measured with a Siemens CCD area detector

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
U111/210.01711 (6)
P11.91206 (10)0.82300 (8)1.31795 (6)0.01793 (18)
S11.22784 (13)0.65734 (11)0.66912 (7)0.0359 (2)
S21.46942 (13)0.19370 (10)1.16174 (8)0.0384 (2)
O11.0710 (3)0.5803 (3)0.82793 (18)0.0287 (6)
O21.2009 (3)0.3387 (2)1.0960 (2)0.0291 (6)
O1U1.0284 (3)0.6208 (2)1.04690 (19)0.0260 (5)
N11.2961 (3)0.4462 (3)0.9324 (2)0.0188 (6)
C11.2009 (4)0.5838 (3)0.7849 (3)0.0218 (7)
C21.3353 (4)0.5112 (3)0.8464 (2)0.0206 (7)
C31.4876 (4)0.5073 (3)0.8184 (3)0.0242 (7)
H3A1.51150.55500.75930.029*
C41.6031 (4)0.4314 (3)0.8795 (3)0.0252 (8)
H4A1.70550.42860.86290.030*
C51.5636 (4)0.3593 (3)0.9663 (3)0.0232 (7)
H5A1.63990.30501.00720.028*
C61.4086 (4)0.3695 (3)0.9911 (2)0.0192 (7)
C71.3475 (4)0.3031 (3)1.0837 (3)0.0224 (7)
C201.8303 (4)0.8952 (3)1.4256 (3)0.0219 (7)
C211.7228 (5)1.0161 (4)1.4126 (3)0.0343 (9)
H21A1.70161.06021.34890.041*
C221.6479 (6)1.0703 (4)1.4940 (4)0.0470 (12)
H22A1.57831.15181.48520.056*
C231.6759 (6)1.0039 (4)1.5890 (3)0.0432 (11)
H23A1.62391.04061.64380.052*
C241.7796 (6)0.8847 (4)1.6026 (3)0.0379 (10)
H24A1.79670.84041.66660.045*
C251.8599 (5)0.8288 (4)1.5215 (3)0.0275 (8)
H25A1.93220.74841.53110.033*
C301.7515 (4)0.8058 (3)1.2705 (3)0.0200 (7)
C311.6867 (4)0.8810 (3)1.1847 (3)0.0248 (8)
H31A1.73290.93641.14600.030*
C321.5528 (5)0.8732 (4)1.1570 (3)0.0347 (9)
H32A1.50940.92321.09940.042*
C331.4837 (5)0.7917 (4)1.2144 (3)0.0341 (10)
H33A1.39290.78771.19600.041*
C341.5484 (5)0.7160 (4)1.2990 (3)0.0332 (9)
H34A1.50200.66011.33670.040*
C351.6815 (5)0.7224 (3)1.3281 (3)0.0279 (8)
H35A1.72440.67161.38560.033*
C402.0520 (4)0.6700 (3)1.3483 (2)0.0211 (7)
C412.1702 (5)0.6498 (4)1.4103 (3)0.0284 (8)
H41A2.17490.71541.43700.034*
C422.2787 (5)0.5319 (4)1.4311 (3)0.0348 (9)
H42A2.35540.51761.47320.042*
C432.2739 (5)0.4345 (4)1.3894 (3)0.0346 (9)
H43A2.34720.35521.40400.042*
C442.1608 (5)0.4545 (4)1.3261 (3)0.0317 (9)
H44A2.15950.38931.29730.038*
C452.0500 (5)0.5717 (3)1.3062 (3)0.0259 (8)
H45A1.97340.58501.26430.031*
C502.0018 (4)0.9167 (3)1.2267 (2)0.0200 (7)
C512.0085 (5)1.0293 (4)1.2428 (3)0.0297 (8)
H51A1.96371.05861.30170.036*
C522.0818 (5)1.0976 (4)1.1711 (3)0.0339 (9)
H52A2.08481.17331.18140.041*
C532.1503 (5)1.0530 (4)1.0844 (3)0.0295 (8)
H53A2.20011.09871.03670.035*
C542.1456 (5)0.9406 (4)1.0677 (3)0.0282 (8)
H54A2.19270.91131.00910.034*
C552.0711 (4)0.8722 (3)1.1380 (3)0.0235 (7)
H55A2.06700.79731.12660.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.01507 (10)0.01840 (10)0.01858 (10)0.00667 (7)0.00183 (7)0.00246 (6)
P10.0184 (5)0.0192 (4)0.0162 (4)0.0070 (4)0.0020 (3)0.0014 (3)
S10.0338 (6)0.0450 (6)0.0216 (5)0.0109 (5)0.0006 (4)0.0045 (4)
S20.0270 (6)0.0330 (5)0.0425 (6)0.0030 (4)0.0093 (5)0.0124 (4)
O10.0213 (14)0.0381 (15)0.0223 (13)0.0080 (12)0.0018 (11)0.0008 (11)
O20.0181 (14)0.0283 (14)0.0341 (14)0.0060 (11)0.0026 (11)0.0065 (11)
O1U0.0267 (14)0.0287 (13)0.0265 (13)0.0132 (11)0.0011 (11)0.0068 (11)
N10.0163 (15)0.0176 (13)0.0220 (14)0.0043 (11)0.0004 (11)0.0058 (11)
C10.0215 (19)0.0210 (17)0.0219 (17)0.0064 (14)0.0005 (14)0.0041 (14)
C20.0223 (19)0.0220 (17)0.0184 (16)0.0071 (14)0.0003 (14)0.0066 (13)
C30.023 (2)0.0287 (19)0.0236 (17)0.0114 (15)0.0037 (14)0.0082 (15)
C40.0182 (19)0.0318 (19)0.0281 (18)0.0089 (15)0.0048 (15)0.0140 (16)
C50.0170 (18)0.0257 (18)0.0276 (18)0.0055 (14)0.0003 (14)0.0104 (15)
C60.0173 (18)0.0166 (15)0.0229 (17)0.0035 (13)0.0015 (14)0.0060 (13)
C70.023 (2)0.0179 (16)0.0237 (17)0.0043 (14)0.0026 (15)0.0027 (13)
C200.0226 (19)0.0244 (17)0.0202 (16)0.0098 (15)0.0009 (14)0.0054 (14)
C210.035 (2)0.033 (2)0.028 (2)0.0043 (18)0.0001 (17)0.0042 (17)
C220.050 (3)0.033 (2)0.049 (3)0.001 (2)0.001 (2)0.017 (2)
C230.055 (3)0.043 (3)0.034 (2)0.018 (2)0.009 (2)0.019 (2)
C240.053 (3)0.042 (2)0.0210 (19)0.020 (2)0.0023 (18)0.0073 (17)
C250.033 (2)0.0280 (19)0.0231 (18)0.0119 (17)0.0024 (16)0.0042 (15)
C300.0170 (18)0.0225 (17)0.0213 (16)0.0059 (14)0.0023 (14)0.0060 (13)
C310.023 (2)0.0265 (18)0.0236 (17)0.0072 (15)0.0032 (15)0.0013 (14)
C320.030 (2)0.041 (2)0.032 (2)0.0065 (18)0.0124 (18)0.0062 (18)
C330.025 (2)0.037 (2)0.045 (2)0.0076 (18)0.0095 (19)0.0198 (19)
C340.029 (2)0.032 (2)0.045 (2)0.0171 (18)0.0011 (18)0.0106 (18)
C350.029 (2)0.0269 (19)0.0275 (19)0.0124 (16)0.0025 (16)0.0007 (15)
C400.0211 (19)0.0208 (16)0.0189 (16)0.0069 (14)0.0015 (14)0.0017 (13)
C410.022 (2)0.034 (2)0.0290 (19)0.0113 (16)0.0026 (16)0.0023 (16)
C420.021 (2)0.045 (2)0.033 (2)0.0089 (18)0.0060 (17)0.0053 (18)
C430.027 (2)0.0251 (19)0.035 (2)0.0012 (17)0.0042 (17)0.0084 (16)
C440.033 (2)0.0220 (18)0.032 (2)0.0028 (17)0.0043 (17)0.0035 (16)
C450.028 (2)0.0256 (18)0.0227 (17)0.0087 (16)0.0003 (15)0.0028 (14)
C500.0227 (19)0.0208 (16)0.0172 (15)0.0103 (14)0.0042 (14)0.0025 (13)
C510.037 (2)0.031 (2)0.0262 (19)0.0173 (18)0.0004 (17)0.0075 (16)
C520.047 (3)0.031 (2)0.031 (2)0.024 (2)0.0063 (19)0.0007 (16)
C530.028 (2)0.035 (2)0.0258 (19)0.0167 (17)0.0037 (16)0.0072 (16)
C540.027 (2)0.0301 (19)0.0213 (17)0.0066 (16)0.0020 (15)0.0005 (15)
C550.023 (2)0.0220 (17)0.0242 (17)0.0067 (15)0.0027 (15)0.0021 (14)
Geometric parameters (Å, º) top
U1—O1Ui1.774 (2)C20—C211.394 (5)
U1—O1U1.774 (2)C20—C251.396 (5)
U1—O2i2.434 (2)C21—C221.376 (6)
U1—O22.434 (2)C22—C231.384 (7)
U1—O12.447 (3)C23—C241.367 (7)
U1—O1i2.447 (3)C24—C251.392 (6)
U1—N12.647 (3)C30—C311.388 (5)
U1—N1i2.647 (3)C30—C351.400 (5)
P1—C301.795 (3)C31—C321.385 (5)
P1—C401.793 (4)C32—C331.377 (6)
P1—C501.792 (4)C33—C341.377 (6)
P1—C201.795 (4)C34—C351.379 (5)
S1—C11.675 (4)C40—C451.392 (5)
S2—C71.676 (4)C40—C411.411 (5)
O1—C11.268 (5)C41—C421.380 (6)
O2—C71.263 (4)C42—C431.389 (6)
N1—C21.342 (4)C43—C441.386 (6)
N1—C61.347 (4)C44—C451.382 (5)
C1—C21.497 (5)C50—C511.396 (5)
C2—C31.390 (5)C50—C551.404 (5)
C3—C41.383 (5)C51—C521.385 (5)
C4—C51.391 (5)C52—C531.379 (6)
C5—C61.389 (5)C53—C541.387 (5)
C6—C71.493 (5)C54—C551.383 (5)
O1Ui—U1—O1U180.00 (7)N1—C2—C1113.5 (3)
O1Ui—U1—O2i92.16 (11)C3—C2—C1124.5 (3)
O1U—U1—O2i87.84 (10)C4—C3—C2119.1 (4)
O1Ui—U1—O287.84 (10)C3—C4—C5118.9 (3)
O1U—U1—O292.16 (11)C6—C5—C4119.1 (3)
O2i—U1—O2180.00 (11)N1—C6—C5121.6 (3)
O1Ui—U1—O186.74 (10)N1—C6—C7113.0 (3)
O1U—U1—O193.26 (10)C5—C6—C7125.3 (3)
O2i—U1—O161.58 (9)O2—C7—C6113.9 (3)
O2—U1—O1118.42 (9)O2—C7—S2125.4 (3)
O1Ui—U1—O1i93.26 (10)C6—C7—S2120.6 (3)
O1U—U1—O1i86.74 (10)C21—C20—C25119.7 (4)
O2i—U1—O1i118.42 (9)C21—C20—P1118.4 (3)
O2—U1—O1i61.58 (9)C25—C20—P1121.5 (3)
O1—U1—O1i180.0C22—C21—C20120.0 (4)
O1Ui—U1—N195.04 (10)C21—C22—C23120.2 (4)
O1U—U1—N184.96 (10)C24—C23—C22120.2 (4)
O2i—U1—N1120.25 (9)C23—C24—C25120.7 (4)
O2—U1—N159.75 (9)C20—C25—C24119.1 (4)
O1—U1—N159.77 (9)C31—C30—C35119.8 (3)
O1i—U1—N1120.23 (9)C31—C30—P1122.0 (3)
O1Ui—U1—N1i84.96 (10)C35—C30—P1117.9 (3)
O1U—U1—N1i95.04 (10)C30—C31—C32119.7 (4)
O2i—U1—N1i59.75 (9)C33—C32—C31120.3 (4)
O2—U1—N1i120.25 (9)C34—C33—C32120.2 (4)
O1—U1—N1i120.23 (9)C33—C34—C35120.5 (4)
O1i—U1—N1i59.77 (9)C34—C35—C30119.5 (3)
N1—U1—N1i180.0C45—C40—C41119.4 (3)
C30—P1—C40107.77 (16)C45—C40—P1120.1 (3)
C30—P1—C50110.97 (16)C41—C40—P1120.4 (3)
C40—P1—C50108.83 (17)C42—C41—C40119.5 (4)
C30—P1—C20105.17 (16)C41—C42—C43120.2 (4)
C40—P1—C20112.27 (16)C44—C43—C42120.6 (4)
C50—P1—C20111.73 (16)C43—C44—C45119.6 (4)
C1—O1—U1130.8 (2)C40—C45—C44120.5 (3)
C7—O2—U1132.0 (2)C51—C50—C55119.7 (3)
C2—N1—C6119.2 (3)C51—C50—P1122.0 (3)
C2—N1—U1119.6 (2)C55—C50—P1118.4 (3)
C6—N1—U1120.3 (2)C52—C51—C50120.1 (4)
O1—C1—C2113.7 (3)C53—C52—C51119.8 (4)
O1—C1—S1125.2 (3)C52—C53—C54120.7 (4)
C2—C1—S1121.1 (3)C55—C54—C53120.1 (4)
N1—C2—C3122.0 (3)C54—C55—C50119.6 (3)
Symmetry code: (i) x+2, y+1, z+2.

Experimental details

Crystal data
Chemical formula2C24H20P·[UO2(C7H3NO2S2)2]
Mr1343.22
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.2351 (7), 11.607 (1), 13.807 (1)
α, β, γ (°)77.891 (1), 81.46 (1), 69.14 (1)
V3)1347.7 (2)
Z1
Radiation typeMo Kα
µ (mm1)3.28
Crystal size (mm)0.32 × 0.25 × 0.20
Data collection
DiffractometerSiemens P4/PC CCD area-detector
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SADABS in SHELXL97; Sheldrick, 1997)
Tmin, Tmax0.31, 0.52
No. of measured, independent and
observed [I > 2σ(I)] reflections
9541, 5605, 5485
Rint0.031
(sin θ/λ)max1)0.670
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.073, 1.04
No. of reflections5605
No. of parameters349
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.21, 1.95

Computer programs: SMART (Siemens, 1996), SAINT (Bruker, 1998), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
U1—O1U1.774 (2)S1—C11.675 (4)
U1—O22.434 (2)S2—C71.676 (4)
U1—O12.447 (3)O1—C11.268 (5)
U1—N12.647 (3)O2—C71.263 (4)
O1Ui—U1—O1U180.00 (7)O1U—U1—N184.96 (10)
O1U—U1—O292.16 (11)O2—U1—N159.75 (9)
O1U—U1—O193.26 (10)O1—U1—N159.77 (9)
O2—U1—O1118.42 (9)
Symmetry code: (i) x+2, y+1, z+2.
 

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