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The crystal structure of the title compound, [U(NO3)2O2(C10H17Cl3N3O2P)2], is composed of centrosymmetric [UO2(L)2(NO3)2] mol­ecules {L is N-[bis­(pyrrolidin-1-yl)phosphor­yl]-2,2,2-trichloro­acetamide, C10H17Cl3N3O2P}. The UVI ion, located on an inversion center, is eight-coordinated with axial oxido ligands and six equatorial oxygen atoms of the phosphoryl and nitrate groups in a slightly distorted hexa­gonal-bipyramidal geometry. One of the pyrrolidine fragments in the ligand is disordered over two conformation (occupancy ratio 0.58:0.42). Intra­molecular N—H...O hydrogen bonds between the amine and nitrate groups are found.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810006422/dn2539sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536810006422/dn2539Isup2.hkl
Contains datablock I

CCDC reference: 769900

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in main residue
  • R factor = 0.034
  • wR factor = 0.085
  • Data-to-parameter ratio = 21.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C9
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for U PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C10 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 10 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 7 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 43 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 14
Alert level G PLAT301_ALERT_3_G Note: Main Residue Disorder ................... 14.00 Perc. PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 56 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 16 PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 1.00 Deg. C6B -N2 -C6A 1.555 1.555 1.555 PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 6.40 Deg. C3B -N2 -C3A 1.555 1.555 1.555 PLAT793_ALERT_4_G The Model has Chirality at P1 (Verify) .... S PLAT811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms .... !
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 9 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

As a part of our study of coordination compounds based on carbacylamidophosphates with C(O)NHP(O) structural fragment we obtained the title compound UO2(L)2(NO3)2 (L = 2,2,2-trichloro- N-[di(1-pyrrolidinyl)phosphoryl]acetamide) (1), and solved its crystal structure. It was shown previously that L is able to form complexes with lanthanides (Znovjyak et al., 2009).

The crystal structure of 1 is made of centrosymmetric molecules UO2(L)2(NO3)2 and uranium is located on an inversion center. The analysis of the bond lengths and angles of 1 indicates that the coordination polyhedra of the uranium ions are slightly distorted hexagonal bipyramids. The axial vertices are occupied by two oxido ligands while six oxygen atoms of monodentate coordinated L ligands and bidentate coordinated nitrate groups lie in the equatorial plane. The nitrate groups additionally form intramolecular hydrogen bonding with the hydrogen atoms of the N—H groups of the L ligands (Table 1). In the crystal structure of the complex, the phosphoryl and carbonyl groups are in the trans position to each other which was early observed in the structure of the free L (Gholivand et al., 2006) and similar complex with uranium ion (Amirkhanov et al., 1997). It was shown that 2,2,2-trichloro-N-[di(1-pyrrolidinyl)phosphoryl]acetamide aggregates into non-centrosymmetric dimers (L)2, therefore in the following will be given two values of bond lengths due to comparison of non-coordinated and coordinated L.

The planar four-membered metalocycle UONO is characterised by an average angle U—O—N equal to 98.1 °. Bond length U—O(oxido ligand) is equal to 1.754 (3) Å while U—O(NO3) and U—O(PO) are 2.523 (3)-2.573 (3) Å and 2.334 (3) Å, respectively. The O—N—O angle of the chelate ring (114.3 (3) °) are shorter as compared to other angles O—N—O (122.3 (4)-123.3 (4) °). N—O(non-coordinated) and N—O(coordinated) distances fall in the range of 1.204 (5) Å and 1.265 (4)-1.270 (5) Å, respectively. In the coordinated L ligand the P—O bond length is slightly increased upon coordination (1.492 (3) Å). In the case of the non-coordinated molecule L they are 1.479 Å and 1.469 Å. The P—N bond distances between phosphorus atoms and nitrogen atoms of the pyrrolidine substituents are shortened with respect to observed values in L (1.613 (4)-1.625 (4) Å) and fall in the range 1.605 (3)-1.613 (4) Å, that can be explained by increasing π-donor bonding in the (Npyr)2P(O) fragment due to coordination. In 1, the P—N(NH) bond length (1.695 (3) Å) is shortened as compared to (L)2 (1.697 and 1.707 Å). The C—N distance is increased while C—O distance do not change upon ligand coordination and are equal to 1.359 (4) Å and 1.196 (5) Å, respectively. Angles in the fragment C(O)NHP(O) are slightly changed upon coordination in the range of 2-3°.

Related literature top

For the synthesis and coordination properties of the ligand L, see: Znovjyak et al. (2009). For a structural investigation of L, see: Gholivand et al. (2006). For the synthesis and structural investigation of a uranium(IV)-containing complex with a similar ligand, see: Amirkhanov et al. (1997).

Experimental top

The synthesis of L was carried out according to the procedure described previously (Znovjyak et al., 2009).

Hydrated nitrate UO2(NO3)22H2O (1 mmol) was solved upon heating in a CH3CN (10 ml). The solution was dehydrated by HC(OC2H5)3 (2 mmol), then heated to the boiling point and cooled down. The resulting solution was added to the solution of L (2 mmol) in CH3OH (10 ml) and was left in a vacuum desiccator over CaCl2 at room temperature. After 1 day, the yellow crystals were filtered off and washed with cold isopropanol and dried on the air (yield 80%). IR (KBr, cm-1): 3280 ν(NH), 2990 ν(CH), 2890 ν(CH), 1730 ν(CO), 1530, 1440 ν(CN), 1380, 1275, 1215, 1145 ν(PO), 1085, 1030, 940, 890, 820, 680 ν(CCl).

Refinement top

All H atoms were placed at calculated positions and treated as riding on their parent atoms [C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C), N—H = 0.86 Å and Uiso(H) = 1.2Ueq(N)]. In one pyrrolidine group, atoms C3—C6 were treated as disordered between two orientations A and B, respectively, with the occupancies to 0.58 and 0.42.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Burnett & Johnson, 1996; Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. View of the centrosymmetric molecule of 1 with atom numbering scheme. Displacement ellipsoids are drawn at 30% probability level. Hydrogen atoms not involved in hydrogen bonding omitted for clarity. [Symmetry code: (i) -x+1, -y+1, -z+1]
Bis{N-[bis(pyrrolidin-1-yl)phosphoryl]-2,2,2- trichloroacetamide}dinitratodioxidouranium(VI) top
Crystal data top
[U(NO3)2O2(C10H17Cl3N3O2P)2]Z = 1
Mr = 1091.22F(000) = 530
Triclinic, P1Dx = 1.893 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.8292 (7) ÅCell parameters from 35271 reflections
b = 10.3436 (8) Åθ = 3.0–40.8°
c = 10.4475 (6) ŵ = 4.80 mm1
α = 71.905 (6)°T = 293 K
β = 84.391 (5)°Block, yellow
γ = 71.475 (6)°0.40 × 0.30 × 0.20 mm
V = 957.34 (11) Å3
Data collection top
Oxford Diffraction Xcalibur3
diffractometer
5523 independent reflections
Radiation source: fine-focus sealed tube5486 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.090
Detector resolution: 16.1827 pixels mm-1θmax = 30.0°, θmin = 3.0°
ω–scansh = 1313
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)
k = 1414
Tmin = 0.250, Tmax = 0.447l = 1414
22849 measured reflections
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)] = 0.034H-atom parameters constrained
wR(F2) = 0.085 w = 1/[σ2(Fo2) + (0.0645P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.001
5523 reflectionsΔρmax = 1.93 e Å3
260 parametersΔρmin = 1.68 e Å3
56 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0164 (15)
Crystal data top
[U(NO3)2O2(C10H17Cl3N3O2P)2]γ = 71.475 (6)°
Mr = 1091.22V = 957.34 (11) Å3
Triclinic, P1Z = 1
a = 9.8292 (7) ÅMo Kα radiation
b = 10.3436 (8) ŵ = 4.80 mm1
c = 10.4475 (6) ÅT = 293 K
α = 71.905 (6)°0.40 × 0.30 × 0.20 mm
β = 84.391 (5)°
Data collection top
Oxford Diffraction Xcalibur3
diffractometer
5523 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)
5486 reflections with I > 2σ(I)
Tmin = 0.250, Tmax = 0.447Rint = 0.090
22849 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03456 restraints
wR(F2) = 0.085H-atom parameters constrained
S = 0.98Δρmax = 1.93 e Å3
5523 reflectionsΔρmin = 1.68 e Å3
260 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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*/UeqOcc. (<1)
U0.50000.50000.50000.03209 (7)
Cl11.08718 (12)0.15464 (16)0.42224 (11)0.0674 (3)
Cl21.27581 (13)0.08470 (15)0.60993 (14)0.0711 (3)
Cl31.23459 (15)0.1967 (2)0.6270 (2)0.0834 (4)
P10.74992 (8)0.19775 (8)0.75384 (8)0.03262 (14)
O10.6348 (3)0.2904 (3)0.6531 (3)0.0474 (6)
O21.0554 (3)0.0118 (4)0.8039 (3)0.0613 (9)
O30.5489 (3)0.6026 (4)0.5826 (3)0.0526 (6)
O40.6361 (3)0.5934 (3)0.2862 (3)0.0520 (7)
O50.7579 (3)0.4078 (4)0.4326 (3)0.0588 (8)
O60.8601 (4)0.4932 (4)0.2460 (4)0.0688 (10)
N10.8984 (3)0.1713 (3)0.6561 (3)0.0373 (5)
H10.89050.22450.57380.045*
N30.7074 (3)0.0571 (3)0.8365 (3)0.0420 (6)
N40.7559 (3)0.4981 (4)0.3181 (3)0.0432 (6)
C11.0286 (3)0.0743 (4)0.6952 (3)0.0383 (6)
C21.1511 (4)0.0847 (4)0.5899 (4)0.0445 (7)
N20.7919 (3)0.2608 (4)0.8625 (4)0.0450 (6)
C3A0.6874 (16)0.2992 (18)0.9673 (15)0.056 (4)0.58
H3A10.71450.23001.05490.067*0.58
H3A20.59150.30500.94530.067*0.58
C4A0.6950 (10)0.4427 (12)0.9649 (15)0.072 (3)0.58
H4A10.66280.46281.04940.086*0.58
H4A20.63840.51830.89170.086*0.58
C5A0.8571 (12)0.4237 (17)0.9427 (18)0.084 (4)0.58
H5A10.87710.51440.91550.101*0.58
H5A20.91290.36091.02230.101*0.58
C6A0.884 (2)0.355 (2)0.828 (2)0.066 (6)0.58
H6A10.85640.42700.74150.079*0.58
H6A20.98400.30070.82410.079*0.58
C3B0.692 (3)0.282 (3)0.974 (2)0.075 (7)0.42
H3B10.59350.32710.94190.090*0.42
H3B20.69790.19191.04260.090*0.42
C4B0.743 (2)0.377 (2)1.0253 (19)0.096 (5)0.42
H4B10.81320.32081.09610.115*0.42
H4B20.66340.43931.06110.115*0.42
C5B0.810 (3)0.4639 (19)0.904 (3)0.096 (6)0.42
H5B10.73790.54340.84730.116*0.42
H5B20.87890.49950.93220.116*0.42
C6B0.885 (3)0.352 (3)0.831 (3)0.072 (8)0.42
H6B10.88950.39610.73490.086*0.42
H6B20.98110.29880.86550.086*0.42
C70.6093 (4)0.0065 (5)0.7792 (4)0.0497 (8)
H7A0.63620.00580.68750.060*
H7B0.51090.06660.77970.060*
C80.6270 (8)0.1427 (7)0.8705 (8)0.0852 (18)
H8A0.54260.14570.92650.102*
H8B0.64080.20850.81800.102*
C90.7537 (12)0.1812 (7)0.9542 (8)0.109 (3)
H9A0.83780.23400.91450.131*
H9B0.74020.24111.04350.131*
C100.7735 (5)0.0494 (5)0.9627 (4)0.0582 (10)
H10A0.87440.05880.96690.070*
H10B0.72500.02401.04090.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U0.02715 (9)0.02741 (9)0.03229 (10)0.00624 (5)0.00343 (5)0.00313 (5)
Cl10.0505 (5)0.0857 (9)0.0435 (5)0.0017 (5)0.0060 (4)0.0091 (5)
Cl20.0527 (6)0.0636 (7)0.0744 (7)0.0138 (5)0.0040 (5)0.0225 (6)
Cl30.0579 (6)0.0868 (10)0.1247 (13)0.0366 (7)0.0060 (7)0.0446 (10)
P10.0271 (3)0.0258 (3)0.0332 (3)0.0036 (2)0.0009 (2)0.0033 (3)
O10.0287 (10)0.0412 (13)0.0442 (12)0.0003 (9)0.0008 (9)0.0152 (10)
O20.0430 (14)0.067 (2)0.0440 (14)0.0099 (13)0.0099 (11)0.0004 (14)
O30.0576 (16)0.0518 (17)0.0555 (16)0.0269 (13)0.0045 (12)0.0136 (13)
O40.0400 (12)0.0461 (15)0.0446 (13)0.0036 (11)0.0033 (10)0.0110 (11)
O50.0386 (13)0.0545 (18)0.0472 (14)0.0013 (11)0.0060 (11)0.0173 (12)
O60.0469 (15)0.072 (2)0.0606 (18)0.0101 (15)0.0194 (14)0.0037 (16)
N10.0283 (11)0.0379 (14)0.0335 (12)0.0001 (9)0.0020 (9)0.0032 (10)
N30.0400 (13)0.0332 (14)0.0412 (14)0.0116 (11)0.0122 (11)0.0093 (11)
N40.0355 (13)0.0411 (15)0.0393 (14)0.0073 (11)0.0042 (10)0.0016 (11)
C10.0307 (13)0.0410 (17)0.0385 (14)0.0019 (11)0.0061 (11)0.0124 (13)
C20.0318 (14)0.0473 (19)0.0478 (18)0.0044 (13)0.0006 (12)0.0124 (15)
N20.0428 (14)0.0428 (16)0.0518 (16)0.0165 (12)0.0106 (12)0.0170 (14)
C3A0.052 (6)0.067 (7)0.056 (6)0.023 (5)0.034 (6)0.035 (6)
C4A0.049 (4)0.071 (6)0.106 (8)0.009 (4)0.013 (5)0.054 (6)
C5A0.054 (5)0.094 (9)0.141 (11)0.028 (6)0.021 (6)0.087 (9)
C6A0.055 (10)0.064 (10)0.107 (12)0.043 (8)0.032 (9)0.049 (9)
C3B0.073 (13)0.066 (11)0.082 (14)0.011 (8)0.019 (9)0.024 (9)
C4B0.112 (13)0.102 (13)0.096 (11)0.030 (10)0.004 (9)0.064 (10)
C5B0.109 (16)0.059 (9)0.134 (14)0.019 (9)0.002 (11)0.055 (9)
C6B0.055 (14)0.066 (15)0.100 (15)0.006 (10)0.007 (9)0.042 (12)
C70.0418 (17)0.052 (2)0.054 (2)0.0214 (16)0.0004 (14)0.0055 (17)
C80.089 (4)0.058 (3)0.110 (5)0.046 (3)0.009 (3)0.000 (3)
C90.171 (8)0.042 (3)0.102 (5)0.043 (4)0.060 (5)0.024 (3)
C100.059 (2)0.048 (2)0.0467 (19)0.0157 (18)0.0118 (16)0.0179 (16)
Geometric parameters (Å, º) top
U—O31.754 (3)C4A—C5A1.546 (12)
U—O3i1.754 (3)C4A—H4A10.9700
U—O12.334 (2)C4A—H4A20.9700
U—O1i2.334 (2)C5A—C6A1.538 (13)
U—O52.523 (3)C5A—H5A10.9700
U—O5i2.523 (3)C5A—H5A20.9700
U—O4i2.571 (3)C6A—H6A10.9700
U—O42.571 (3)C6A—H6A20.9700
Cl1—C21.768 (4)C3B—C4B1.482 (16)
Cl2—C21.753 (4)C3B—H3B10.9700
Cl3—C21.764 (4)C3B—H3B20.9700
P1—O11.491 (2)C4B—C5B1.542 (18)
P1—N31.604 (3)C4B—H4B10.9700
P1—N21.615 (3)C4B—H4B20.9700
P1—N11.696 (3)C5B—C6B1.531 (15)
O2—C11.197 (5)C5B—H5B10.9700
O4—N41.267 (4)C5B—H5B20.9700
O5—N41.265 (4)C6B—H6B10.9700
O6—N41.208 (4)C6B—H6B20.9700
N1—C11.357 (4)C7—C81.507 (8)
N1—H10.8600C7—H7A0.9700
N3—C101.478 (5)C7—H7B0.9700
N3—C71.481 (5)C8—C91.468 (10)
C1—C21.556 (5)C8—H8A0.9700
N2—C6B1.460 (14)C8—H8B0.9700
N2—C6A1.475 (8)C9—C101.467 (8)
N2—C3B1.473 (14)C9—H9A0.9700
N2—C3A1.484 (7)C9—H9B0.9700
C3A—C4A1.502 (13)C10—H10A0.9700
C3A—H3A10.9700C10—H10B0.9700
C3A—H3A20.9700
O3—U—O3i180.00 (13)C4A—C3A—H3A2111.1
O3—U—O190.47 (14)H3A1—C3A—H3A2109.0
O3i—U—O189.53 (14)C3A—C4A—C5A101.7 (8)
O3—U—O1i89.53 (14)C3A—C4A—H4A1111.4
O3i—U—O1i90.47 (14)C5A—C4A—H4A1111.4
O1—U—O1i180.0C3A—C4A—H4A2111.4
O3—U—O590.00 (14)C5A—C4A—H4A2111.4
O3i—U—O590.00 (14)H4A1—C4A—H4A2109.3
O1—U—O565.33 (9)C6A—C5A—C4A99.5 (10)
O1i—U—O5114.67 (9)C6A—C5A—H5A1111.9
O3—U—O5i90.00 (14)C4A—C5A—H5A1111.9
O3i—U—O5i90.00 (14)C6A—C5A—H5A2111.9
O1—U—O5i114.67 (9)C4A—C5A—H5A2111.9
O1i—U—O5i65.33 (9)H5A1—C5A—H5A2109.6
O5—U—O5i180.0N2—C6A—C5A103.7 (8)
O3—U—O4i88.35 (13)N2—C6A—H6A1111.0
O3i—U—O4i91.65 (13)C5A—C6A—H6A1111.0
O1—U—O4i65.33 (8)N2—C6A—H6A2111.0
O1i—U—O4i114.67 (8)C5A—C6A—H6A2111.0
O5—U—O4i130.60 (9)H6A1—C6A—H6A2109.0
O5i—U—O4i49.40 (9)C4B—C3B—N2102.4 (11)
O3—U—O491.65 (13)C4B—C3B—H3B1111.3
O3i—U—O488.35 (13)N2—C3B—H3B1111.3
O1—U—O4114.67 (8)C4B—C3B—H3B2111.3
O1i—U—O465.33 (8)N2—C3B—H3B2111.3
O5—U—O449.40 (9)H3B1—C3B—H3B2109.2
O5i—U—O4130.60 (9)C3B—C4B—C5B105.9 (13)
O4i—U—O4180.0C3B—C4B—H4B1110.6
O1—P1—N3108.41 (16)C5B—C4B—H4B1110.6
O1—P1—N2119.57 (19)C3B—C4B—H4B2110.6
N3—P1—N2107.23 (17)C5B—C4B—H4B2110.6
O1—P1—N1102.49 (14)H4B1—C4B—H4B2108.7
N3—P1—N1115.72 (16)C6B—C5B—C4B101.6 (13)
N2—P1—N1103.76 (15)C6B—C5B—H5B1111.5
P1—O1—U157.1 (2)C4B—C5B—H5B1111.5
N4—O4—U96.89 (19)C6B—C5B—H5B2111.5
N4—O5—U99.3 (2)C4B—C5B—H5B2111.5
C1—N1—P1126.3 (2)H5B1—C5B—H5B2109.3
C1—N1—H1116.9N2—C6B—C5B102.6 (11)
P1—N1—H1116.9N2—C6B—H6B1111.2
C10—N3—C7110.9 (3)C5B—C6B—H6B1111.2
C10—N3—P1127.0 (3)N2—C6B—H6B2111.2
C7—N3—P1121.4 (2)C5B—C6B—H6B2111.2
O6—N4—O5122.5 (3)H6B1—C6B—H6B2109.2
O6—N4—O4123.1 (3)N3—C7—C8104.1 (4)
O5—N4—O4114.4 (3)N3—C7—H7A110.9
O2—C1—N1125.1 (3)C8—C7—H7A110.9
O2—C1—C2119.3 (3)N3—C7—H7B110.9
N1—C1—C2115.5 (3)C8—C7—H7B110.9
C1—C2—Cl2109.9 (3)H7A—C7—H7B108.9
C1—C2—Cl3105.5 (2)C9—C8—C7106.4 (4)
Cl2—C2—Cl3109.3 (2)C9—C8—H8A110.4
C1—C2—Cl1112.6 (2)C7—C8—H8A110.4
Cl2—C2—Cl1108.7 (2)C9—C8—H8B110.4
Cl3—C2—Cl1110.8 (2)C7—C8—H8B110.4
C6B—N2—C6A1 (2)H8A—C8—H8B108.6
C6B—N2—C3B113.4 (9)C8—C9—C10108.4 (5)
C6A—N2—C3B113.9 (9)C8—C9—H9A110.0
C6B—N2—C3A109.0 (9)C10—C9—H9A110.0
C6A—N2—C3A109.3 (6)C8—C9—H9B110.0
C3B—N2—C3A6.4 (17)C10—C9—H9B110.0
C6B—N2—P1123.2 (10)H9A—C9—H9B108.4
C6A—N2—P1122.1 (7)C9—C10—N3103.0 (4)
C3B—N2—P1118.4 (8)C9—C10—H10A111.2
C3A—N2—P1120.3 (6)N3—C10—H10A111.2
N2—C3A—C4A103.5 (7)C9—C10—H10B111.2
N2—C3A—H3A1111.1N3—C10—H10B111.2
C4A—C3A—H3A1111.1H10A—C10—H10B109.1
N2—C3A—H3A2111.1
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O50.862.132.877 (4)145

Experimental details

Crystal data
Chemical formula[U(NO3)2O2(C10H17Cl3N3O2P)2]
Mr1091.22
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.8292 (7), 10.3436 (8), 10.4475 (6)
α, β, γ (°)71.905 (6), 84.391 (5), 71.475 (6)
V3)957.34 (11)
Z1
Radiation typeMo Kα
µ (mm1)4.80
Crystal size (mm)0.40 × 0.30 × 0.20
Data collection
DiffractometerOxford Diffraction Xcalibur3
diffractometer
Absorption correctionMulti-scan
(CrysAlis RED; Oxford Diffraction, 2006)
Tmin, Tmax0.250, 0.447
No. of measured, independent and
observed [I > 2σ(I)] reflections
22849, 5523, 5486
Rint0.090
(sin θ/λ)max1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.085, 0.98
No. of reflections5523
No. of parameters260
No. of restraints56
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.93, 1.68

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Burnett & Johnson, 1996; Farrugia, 1997), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O50.862.132.877 (4)145.0
 

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