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From an aqueous solution of uranyl nitrate hexa­hydrate and tetra-n-butyl­ammonium nitrate, single crystals of the title compound, (C16H36N)2[U2(NO3)4(OH)2O4], were obtained. The structure features a dimeric hydroxo-bridged tetra­nitratodihydroxobis[dioxouranate(VI)] dianion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805021045/hk6022sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805021045/hk6022Isup2.hkl
Contains datablock I

CCDC reference: 282384

Key indicators

  • Single-crystal X-ray study
  • T = 299 K
  • Mean [sigma](C-C) = 0.015 Å
  • H-atom completeness 98%
  • R factor = 0.052
  • wR factor = 0.101
  • Data-to-parameter ratio = 20.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for U1 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C32 H74 N6 O18 U2 Atom count from the _atom_site data: C32 H72 N6 O18 U2 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C32 H74 N6 O18 U2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 64.00 64.00 0.00 H 148.00 144.00 4.00 N 12.00 12.00 0.00 O 36.00 36.00 0.00 U 4.00 4.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX/LSQ (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: maXus (Mackay et al., 1999).

Tetra-n-butylammonium di-µ-hydroxo-bis[dinitratodioxouranium(VI)] top
Crystal data top
(C16H36N)2[U2(NO3)4(OH)2O4]F(000) = 1268
Mr = 1307.02Dx = 1.811 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 58 reflections
a = 12.8335 (13) Åθ = 4.6–18.4°
b = 13.217 (2) ŵ = 6.82 mm1
c = 14.148 (3) ÅT = 299 K
β = 94.239 (11)°Fragment, yellow
V = 2393.1 (7) Å30.25 × 0.22 × 0.20 mm
Z = 2
Data collection top
Bruker Nonius KappaCCD area-detector
diffractometer
3712 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.061
φ and ω scansθmax = 27.5°, θmin = 4.5°
Absorption correction: numerical
(HABITUS; Herrendorf & Bärnighausen, 1997)
h = 1516
Tmin = 0.390, Tmax = 0.498k = 1717
25561 measured reflectionsl = 1818
5427 independent 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)] = 0.052H-atom parameters constrained
wR(F2) = 0.101 w = 1/[σ2(Fo2) + (0.005P)2 + 11.1326P]
where P = (Fo2 + 2Fc2)/3
S = 1.27(Δ/σ)max < 0.001
5427 reflectionsΔρmax = 1.06 e Å3
262 parametersΔρmin = 0.81 e Å3
0 restraints
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
U10.45557 (3)0.46251 (3)0.12328 (2)0.05669 (11)
O60.6308 (5)0.4683 (6)0.2160 (4)0.0764 (17)
O30.2606 (5)0.4554 (6)0.0835 (5)0.0840 (19)
O90.5926 (4)0.5042 (5)0.0337 (4)0.0681 (17)
O70.5024 (5)0.4365 (5)0.2976 (4)0.0724 (17)
O10.4387 (5)0.5877 (4)0.1544 (4)0.0705 (17)
O20.4711 (6)0.3342 (5)0.0997 (4)0.0793 (19)
N20.5992 (6)0.4538 (6)0.2967 (5)0.068 (2)
O80.6561 (5)0.4602 (6)0.3677 (5)0.093 (2)
O40.3094 (5)0.4173 (5)0.2252 (5)0.0742 (17)
O50.1450 (5)0.4296 (6)0.1831 (5)0.095 (2)
N10.2349 (7)0.4338 (6)0.1648 (7)0.074 (2)
N30.4326 (5)0.2489 (5)0.5313 (5)0.0582 (17)
C50.4075 (7)0.1979 (7)0.6212 (6)0.068 (2)
C60.3791 (7)0.2632 (8)0.7019 (7)0.074 (3)
C130.5138 (6)0.3313 (6)0.5475 (6)0.060 (2)
C90.4715 (7)0.1654 (6)0.4706 (6)0.065 (2)
C10.3385 (7)0.3028 (7)0.4854 (7)0.071 (2)
C140.6173 (7)0.2975 (7)0.5950 (7)0.066 (2)
C150.6889 (8)0.3878 (8)0.6090 (7)0.076 (3)
C100.5059 (8)0.1926 (8)0.3754 (6)0.073 (3)
C110.5577 (9)0.1027 (8)0.3319 (8)0.089 (3)
C70.3575 (10)0.1971 (10)0.7851 (8)0.098 (4)
C20.2442 (9)0.2423 (9)0.4646 (10)0.104 (4)
C30.1561 (9)0.3111 (10)0.4169 (9)0.104 (4)
C160.7896 (8)0.3628 (9)0.6622 (9)0.100 (4)
C120.5864 (9)0.1217 (11)0.2353 (9)0.112 (4)
C80.3364 (10)0.2499 (11)0.8716 (8)0.116 (5)
C40.1107 (11)0.3847 (12)0.4761 (11)0.127 (5)
H5A0.34810.15440.60910.082*
H5B0.46650.15850.64520.082*
H6A0.43690.30730.71900.088*
H6B0.31840.30290.68310.088*
H13A0.52760.35980.48730.072*
H13B0.48750.38300.58700.072*
H9A0.53250.13600.50300.078*
H9B0.41850.11450.46010.078*
H1A0.31880.35740.52520.085*
H1B0.35640.32930.42560.085*
H14A0.60520.26650.65460.079*
H14B0.64750.24880.55480.079*
H15A0.70190.41500.54810.091*
H15B0.65330.43730.64440.091*
H10A0.44500.21140.33580.087*
H10B0.55360.24850.38080.087*
H11A0.61960.08530.37080.107*
H11B0.51050.04620.32880.107*
H7A0.29820.15500.76790.118*
H7B0.41740.15540.80120.118*
H2A0.25970.18730.42360.125*
H2B0.22180.21590.52300.125*
H3A0.18640.35000.36870.125*
H3B0.09950.27120.38870.125*
H16A0.83240.42220.67060.120*
H16B0.82510.31320.62670.120*
H16C0.77650.33550.72300.120*
H12A0.61930.06300.21080.134*
H12B0.63440.17750.23720.134*
H12C0.52530.13840.19520.134*
H8A0.32350.20270.92100.139*
H8B0.27570.29150.85840.139*
H8C0.39500.29180.89170.139*
H4A0.05980.42510.44020.153*
H4B0.16440.42770.50480.153*
H4C0.07740.34890.52470.153*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.06183 (19)0.05555 (18)0.05267 (18)0.00310 (19)0.00418 (12)0.00399 (18)
O60.070 (4)0.103 (5)0.056 (4)0.007 (4)0.002 (3)0.013 (4)
O30.071 (4)0.109 (6)0.072 (4)0.017 (4)0.004 (3)0.002 (4)
O90.062 (3)0.097 (5)0.045 (3)0.013 (3)0.001 (3)0.011 (3)
O70.071 (4)0.086 (5)0.061 (4)0.002 (4)0.011 (3)0.014 (3)
O10.079 (4)0.054 (4)0.076 (4)0.003 (3)0.010 (3)0.003 (3)
O20.108 (5)0.057 (4)0.074 (4)0.002 (4)0.016 (4)0.002 (3)
N20.079 (5)0.068 (5)0.057 (4)0.025 (5)0.004 (4)0.007 (4)
O80.087 (5)0.126 (6)0.063 (4)0.025 (5)0.013 (3)0.000 (4)
O40.072 (4)0.083 (5)0.069 (4)0.015 (4)0.013 (3)0.002 (3)
O50.061 (4)0.109 (6)0.117 (6)0.017 (4)0.023 (4)0.030 (5)
N10.064 (5)0.066 (5)0.091 (6)0.013 (4)0.008 (5)0.022 (5)
N30.059 (4)0.055 (4)0.060 (4)0.002 (3)0.001 (3)0.001 (3)
C50.061 (5)0.069 (6)0.074 (6)0.006 (5)0.002 (5)0.014 (5)
C60.059 (5)0.091 (7)0.071 (6)0.004 (5)0.012 (5)0.001 (6)
C130.065 (5)0.050 (5)0.064 (5)0.001 (4)0.007 (4)0.003 (4)
C90.070 (6)0.051 (5)0.074 (6)0.006 (4)0.001 (5)0.013 (4)
C10.062 (6)0.074 (6)0.075 (6)0.006 (5)0.005 (5)0.009 (5)
C140.065 (5)0.057 (5)0.075 (6)0.004 (4)0.005 (5)0.003 (5)
C150.083 (7)0.070 (6)0.074 (6)0.011 (5)0.004 (5)0.006 (5)
C100.078 (6)0.077 (6)0.065 (6)0.000 (5)0.012 (5)0.004 (5)
C110.101 (8)0.082 (7)0.089 (7)0.017 (6)0.031 (6)0.019 (6)
C70.104 (9)0.113 (10)0.080 (7)0.036 (7)0.025 (6)0.002 (7)
C20.084 (8)0.083 (8)0.139 (11)0.009 (6)0.029 (7)0.005 (7)
C30.076 (7)0.111 (10)0.121 (10)0.001 (7)0.025 (7)0.010 (8)
C160.081 (7)0.101 (9)0.115 (9)0.000 (7)0.019 (7)0.013 (7)
C120.094 (8)0.132 (11)0.111 (10)0.011 (8)0.020 (7)0.020 (9)
C80.113 (10)0.156 (13)0.081 (8)0.043 (9)0.013 (7)0.006 (8)
C40.110 (10)0.123 (12)0.145 (13)0.012 (9)0.017 (9)0.006 (10)
Geometric parameters (Å, º) top
U1—O11.730 (6)C5—H5B0.9601
U1—O21.743 (6)C6—H6A0.9602
U1—O9i2.303 (5)C6—H6B0.9603
U1—O92.309 (5)C13—H13A0.9597
U1—O72.518 (6)C13—H13B0.9597
U1—O62.520 (6)C9—H9A0.9596
U1—O42.521 (6)C9—H9B0.9604
U1—O32.525 (6)C1—H1A0.9606
U1—N12.959 (9)C1—H1B0.9592
U1—N22.960 (7)C14—H14A0.9604
U1—U1i3.8780 (9)C14—H14B0.9595
O6—N21.255 (9)C15—H15A0.9595
O3—N11.254 (10)C15—H15B0.9599
O9—U1i2.303 (5)C10—H10A0.9600
O7—N21.263 (9)C10—H10B0.9589
N2—O81.201 (9)C11—H11A0.9603
O4—N11.252 (9)C11—H11B0.9605
O5—N11.203 (9)C7—H7A0.9595
N3—C51.496 (10)C7—H7B0.9595
N3—C91.505 (10)C2—H2A0.9600
N3—C11.507 (10)C2—H2B0.9603
N3—C131.513 (10)C3—H3A0.9590
C5—C61.497 (12)C3—H3B0.9602
C6—C71.507 (13)C16—H16A0.9605
C13—C141.511 (11)C16—H16B0.9609
C9—C101.492 (12)C16—H16C0.9590
C1—C21.463 (13)C12—H12A0.9602
C14—C151.510 (12)C12—H12B0.9600
C15—C161.485 (13)C12—H12C0.9590
C10—C111.514 (13)C8—H8A0.9603
C11—C121.462 (14)C8—H8B0.9604
C7—C81.452 (15)C8—H8C0.9599
C2—C31.564 (15)C4—H4A0.9595
C3—C41.434 (16)C4—H4B0.9599
C5—H5A0.9600C4—H4C0.9606
O1—U1—O2176.2 (3)C8—C7—C6115.8 (11)
O1—U1—O9i91.9 (3)C1—C2—C3109.2 (9)
O2—U1—O9i91.6 (3)C4—C3—C2117.1 (12)
O1—U1—O991.5 (3)N3—C5—H5A109.6
O2—U1—O991.4 (3)C6—C5—H5A104.2
O9i—U1—O965.5 (2)N3—C5—H5B109.4
O1—U1—O784.7 (2)C6—C5—H5B105.9
O2—U1—O791.8 (3)H5A—C5—H5B109.5
O9i—U1—O7176.3 (2)C5—C6—H6A108.3
O9—U1—O7115.71 (19)C7—C6—H6A109.8
O1—U1—O687.8 (3)C5—C6—H6B110.0
O2—U1—O691.1 (3)C7—C6—H6B109.9
O9i—U1—O6131.42 (19)H6A—C6—H6B109.5
O9—U1—O665.91 (19)C14—C13—H13A107.3
O7—U1—O649.84 (19)N3—C13—H13A108.6
O1—U1—O488.2 (3)C14—C13—H13B106.7
O2—U1—O488.8 (3)N3—C13—H13B109.4
O9i—U1—O4116.0 (2)H13A—C13—H13B109.5
O9—U1—O4178.4 (2)C10—C9—H9A104.1
O7—U1—O462.7 (2)N3—C9—H9A108.5
O6—U1—O4112.5 (2)C10—C9—H9B106.4
O1—U1—O387.2 (3)N3—C9—H9B109.9
O2—U1—O392.7 (3)H9A—C9—H9B109.5
O9i—U1—O366.5 (2)C2—C1—H1A106.2
O9—U1—O3131.9 (2)N3—C1—H1A109.9
O7—U1—O3112.0 (2)C2—C1—H1B105.7
O6—U1—O3161.6 (2)N3—C1—H1B108.4
O4—U1—O349.6 (2)H1A—C1—H1B109.5
O1—U1—N186.1 (3)C15—C14—H14A111.0
O2—U1—N192.2 (3)C13—C14—H14A108.8
O9i—U1—N191.4 (2)C15—C14—H14B109.8
O9—U1—N1156.7 (2)C13—C14—H14B108.4
O7—U1—N187.2 (2)H14A—C14—H14B109.4
O6—U1—N1137.0 (2)C16—C15—H15A109.7
O4—U1—N124.8 (2)C14—C15—H15A108.8
O3—U1—N124.9 (2)C16—C15—H15B108.5
O1—U1—N284.7 (2)C14—C15—H15B107.4
O2—U1—N292.7 (3)H15A—C15—H15B109.5
O9i—U1—N2155.9 (2)C9—C10—H10A107.8
O9—U1—N290.7 (2)C11—C10—H10A109.2
O7—U1—N225.04 (19)C9—C10—H10B110.1
O6—U1—N224.86 (19)C11—C10—H10B109.9
O4—U1—N287.7 (2)H10A—C10—H10B109.5
O3—U1—N2136.8 (2)C12—C11—H11A108.8
N1—U1—N2112.1 (2)C10—C11—H11A108.9
O1—U1—U1i92.0 (2)C12—C11—H11B107.0
O2—U1—U1i91.8 (2)C10—C11—H11B109.5
O9i—U1—U1i32.82 (14)H11A—C11—H11B109.4
O9—U1—U1i32.72 (13)C8—C7—H7A107.4
O7—U1—U1i148.31 (15)C6—C7—H7A109.0
O6—U1—U1i98.62 (14)C8—C7—H7B105.8
O4—U1—U1i148.84 (16)C6—C7—H7B109.2
O3—U1—U1i99.27 (16)H7A—C7—H7B109.5
N1—U1—U1i124.12 (19)C1—C2—H2A109.3
N2—U1—U1i123.31 (17)C3—C2—H2A110.8
N2—O6—U197.6 (5)C1—C2—H2B108.7
N1—O3—U197.3 (5)C3—C2—H2B109.2
U1i—O9—U1114.5 (2)H2A—C2—H2B109.5
N2—O7—U197.5 (5)C4—C3—H3A104.8
O8—N2—O6122.2 (9)C2—C3—H3A107.5
O8—N2—O7122.9 (8)C4—C3—H3B106.7
O6—N2—O7114.9 (7)C2—C3—H3B111.1
O8—N2—U1173.7 (7)H3A—C3—H3B109.4
O6—N2—U157.5 (4)C15—C16—H16A110.4
O7—N2—U157.5 (4)C15—C16—H16B108.4
N1—O4—U197.6 (5)H16A—C16—H16B109.5
O5—N1—O4122.8 (9)C15—C16—H16C109.6
O5—N1—O3122.0 (9)H16A—C16—H16C109.5
O4—N1—O3115.2 (8)H16B—C16—H16C109.5
O5—N1—U1175.2 (6)C11—C12—H12A110.3
O4—N1—U157.6 (4)C11—C12—H12B108.1
O3—N1—U157.8 (4)H12A—C12—H12B109.4
C5—N3—C9104.8 (7)C11—C12—H12C109.9
C5—N3—C1111.3 (7)H12A—C12—H12C109.5
C9—N3—C1112.9 (7)H12B—C12—H12C109.5
C5—N3—C13112.6 (6)C7—C8—H8A110.7
C9—N3—C13111.1 (7)C7—C8—H8B108.1
C1—N3—C13104.3 (6)H8A—C8—H8B109.4
N3—C5—C6118.0 (8)C7—C8—H8C109.6
C5—C6—C7109.3 (9)H8A—C8—H8C109.4
C14—C13—N3115.3 (7)H8B—C8—H8C109.5
C10—C9—N3118.1 (7)C3—C4—H4A111.0
C2—C1—N3117.0 (8)C3—C4—H4B109.8
C15—C14—C13109.3 (7)H4A—C4—H4B109.5
C16—C15—C14112.9 (9)C3—C4—H4C107.8
C9—C10—C11110.3 (8)H4A—C4—H4C109.4
C12—C11—C10113.2 (10)H4B—C4—H4C109.4
Symmetry code: (i) x+1, y+1, z.
 

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