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In the title compound, [UO2(C18H18N2O4)(C2H6O)], the U atom has a distorted penta­gonal–bipyramidal geometry with a tetra­dentate Schiff base and ethanol ligands in the equatorial plane and oxo atoms in the axial positions. Complex mol­ecules are connected by O—H...O and C—H...O inter­actions, forming dimers in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044771/ob3026sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044771/ob3026Isup2.hkl
Contains datablock I

CCDC reference: 630205

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.016 Å
  • R factor = 0.042
  • wR factor = 0.099
  • Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found




Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.104 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.10 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.35 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C17 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O5 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 16
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

{6,6'-Dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}- (ethanol)dioxouranium(VI) top
Crystal data top
[U(C18H18N2O4)O2(C2H6O)]F(000) = 2448
Mr = 642.44Dx = 1.984 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 65152 reflections
a = 9.2132 (4) Åθ = 1.7–27.2°
b = 23.6595 (10) ŵ = 7.60 mm1
c = 19.7075 (10) ÅT = 296 K
V = 4295.8 (3) Å3Plate, red
Z = 80.43 × 0.23 × 0.05 mm
Data collection top
Stoe IPDS-2
diffractometer
4219 independent reflections
Radiation source: fine-focus sealed tube2789 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.104
Detector resolution: 6.67 pixels mm-1θmax = 26.0°, θmin = 1.7°
ω scansh = 1111
Absorption correction: integration
(X-RED32; Stoe & Cie, 2002)
k = 2929
Tmin = 0.104, Tmax = 0.597l = 2424
57109 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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099H atoms treated by a mixture of independent and constrained refinement
S = 1.10 w = 1/[σ2(Fo2) + (0.0393P)2 + 9.9627P]
where P = (Fo2 + 2Fc2)/3
4219 reflections(Δ/σ)max < 0.001
274 parametersΔρmax = 1.26 e Å3
22 restraintsΔρmin = 0.68 e Å3
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
U10.42021 (3)0.421967 (14)0.126908 (15)0.04687 (11)
O10.3663 (7)0.5146 (3)0.1123 (3)0.0593 (17)
O20.2410 (9)0.5867 (3)0.0290 (3)0.077 (2)
O30.5862 (8)0.2777 (3)0.0106 (4)0.077 (2)
O40.4683 (7)0.3336 (3)0.0907 (3)0.0580 (16)
O50.4521 (8)0.4366 (3)0.0037 (3)0.0661 (19)
O60.6066 (7)0.4376 (3)0.1345 (3)0.0617 (17)
O70.2355 (7)0.4048 (3)0.1230 (3)0.0651 (17)
N10.3791 (7)0.4687 (3)0.2413 (4)0.0477 (17)
N20.4615 (8)0.3569 (3)0.2278 (4)0.0549 (19)
C10.2677 (10)0.5490 (4)0.1379 (4)0.054 (2)
C20.2326 (10)0.5493 (4)0.2080 (4)0.049 (2)
C30.1317 (12)0.5883 (4)0.2318 (5)0.066 (3)
H30.10990.58820.27790.079*
C40.0641 (12)0.6260 (5)0.1919 (5)0.073 (3)
H40.00200.65170.20990.087*
C50.0965 (11)0.6256 (4)0.1214 (6)0.070 (3)
H50.04930.65050.09220.084*
C60.1987 (10)0.5881 (4)0.0963 (4)0.051 (2)
C70.3028 (9)0.5117 (4)0.2551 (5)0.056 (2)
H70.29070.52000.30090.068*
C80.4471 (10)0.4394 (4)0.2984 (4)0.055 (2)
H8A0.41260.45530.34090.066*
H8B0.55160.44410.29650.066*
C90.4092 (11)0.3779 (4)0.2947 (4)0.060 (2)
H9A0.45580.35740.33130.072*
H9B0.30500.37290.29850.072*
C100.5405 (10)0.3126 (5)0.2280 (5)0.063 (3)
H100.55700.29720.27070.075*
C110.6060 (10)0.2837 (4)0.1746 (6)0.060 (3)
C120.7094 (13)0.2427 (5)0.1877 (7)0.072 (3)
H120.73480.23420.23220.086*
C130.7750 (12)0.2142 (4)0.1347 (7)0.078 (3)
H130.84550.18720.14420.094*
C140.7390 (13)0.2247 (5)0.0690 (7)0.075 (3)
H140.78540.20520.03420.090*
C150.6345 (12)0.2638 (5)0.0541 (7)0.068 (3)
C160.5661 (10)0.2955 (4)0.1048 (5)0.054 (2)
C170.358 (2)0.4244 (7)0.0511 (9)0.135 (7)
H17A0.35090.38380.05660.162*
H17B0.39810.44000.09250.162*
C180.2101 (19)0.4480 (9)0.0401 (9)0.164 (9)
H18A0.14930.43860.07800.197*
H18B0.21620.48840.03580.197*
H18C0.16940.43240.00060.197*
C190.1615 (12)0.6191 (6)0.0171 (5)0.077 (3)
H19A0.20130.61450.06180.115*
H19B0.16650.65820.00430.115*
H19C0.06210.60700.01690.115*
C200.6477 (16)0.2479 (6)0.0691 (7)0.105 (5)
H20A0.60390.26190.11000.157*
H20B0.62890.20820.06490.157*
H20C0.75050.25430.07070.157*
H5A0.539 (5)0.442 (7)0.004 (9)0.157*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.04451 (16)0.05380 (19)0.04231 (16)0.00486 (17)0.00274 (16)0.00073 (17)
O10.077 (4)0.057 (4)0.044 (4)0.017 (3)0.011 (3)0.000 (3)
O20.089 (5)0.082 (5)0.058 (4)0.028 (5)0.013 (4)0.014 (4)
O30.085 (5)0.079 (5)0.066 (4)0.014 (5)0.005 (4)0.024 (4)
O40.064 (4)0.055 (4)0.055 (4)0.010 (3)0.000 (3)0.006 (3)
O50.080 (5)0.082 (5)0.036 (3)0.003 (4)0.004 (3)0.005 (3)
O60.066 (4)0.073 (4)0.046 (3)0.005 (3)0.002 (3)0.001 (3)
O70.059 (3)0.086 (5)0.050 (3)0.003 (3)0.005 (3)0.013 (4)
N10.048 (4)0.050 (4)0.045 (4)0.004 (3)0.000 (3)0.001 (3)
N20.056 (4)0.053 (5)0.056 (5)0.001 (4)0.004 (4)0.003 (4)
C10.055 (5)0.053 (5)0.054 (5)0.010 (5)0.002 (4)0.006 (4)
C20.060 (5)0.053 (5)0.035 (4)0.005 (5)0.002 (4)0.005 (4)
C30.078 (7)0.065 (7)0.054 (6)0.014 (5)0.004 (5)0.013 (5)
C40.078 (7)0.081 (8)0.059 (6)0.027 (6)0.009 (5)0.001 (5)
C50.067 (6)0.075 (7)0.067 (6)0.011 (5)0.006 (6)0.007 (6)
C60.057 (5)0.058 (6)0.040 (4)0.005 (4)0.007 (4)0.004 (4)
C70.056 (6)0.062 (6)0.052 (5)0.005 (5)0.004 (4)0.005 (5)
C80.057 (6)0.067 (6)0.040 (4)0.005 (4)0.002 (4)0.000 (4)
C90.070 (6)0.072 (7)0.038 (4)0.000 (6)0.011 (5)0.008 (4)
C100.059 (6)0.067 (7)0.063 (6)0.001 (5)0.007 (5)0.018 (5)
C110.050 (5)0.046 (6)0.084 (7)0.009 (4)0.000 (5)0.002 (5)
C120.070 (8)0.053 (7)0.093 (9)0.001 (5)0.004 (7)0.011 (6)
C130.067 (6)0.054 (6)0.113 (10)0.014 (5)0.004 (7)0.014 (7)
C140.068 (7)0.054 (7)0.104 (9)0.007 (6)0.003 (7)0.006 (6)
C150.059 (6)0.046 (6)0.098 (7)0.005 (6)0.010 (6)0.011 (6)
C160.053 (5)0.043 (5)0.066 (6)0.006 (5)0.012 (5)0.002 (4)
C170.176 (17)0.128 (15)0.100 (11)0.077 (13)0.020 (12)0.013 (11)
C180.124 (14)0.25 (2)0.118 (13)0.066 (16)0.065 (12)0.001 (14)
C190.081 (7)0.100 (10)0.050 (6)0.003 (7)0.001 (5)0.020 (6)
C200.112 (11)0.120 (14)0.083 (9)0.023 (9)0.010 (8)0.038 (8)
Geometric parameters (Å, º) top
U1—O71.752 (7)C7—H70.9300
U1—O61.763 (7)C8—C91.498 (14)
U1—O42.253 (6)C8—H8A0.9700
U1—O12.265 (6)C8—H8B0.9700
U1—O52.471 (6)C9—H9A0.9700
U1—N12.540 (7)C9—H9B0.9700
U1—N22.542 (8)C10—C111.394 (14)
O1—C11.320 (11)C10—H100.9300
O2—C61.383 (10)C11—C121.384 (14)
O2—C191.396 (12)C11—C161.450 (14)
O3—C151.390 (14)C12—C131.382 (16)
O3—C201.464 (13)C12—H120.9300
O4—C161.305 (11)C13—C141.359 (16)
O5—C171.415 (17)C13—H130.9300
O5—H5A0.83 (6)C14—C151.367 (15)
N1—C71.267 (11)C14—H140.9300
N1—C81.461 (11)C15—C161.401 (14)
N2—C101.276 (12)C17—C181.487 (16)
N2—C91.490 (11)C17—H17A0.9700
C1—C61.390 (13)C17—H17B0.9700
C1—C21.418 (11)C18—H18A0.9600
C2—C31.392 (13)C18—H18B0.9600
C2—C71.438 (13)C18—H18C0.9600
C3—C41.343 (14)C19—H19A0.9600
C3—H30.9300C19—H19B0.9600
C4—C51.421 (14)C19—H19C0.9600
C4—H40.9300C20—H20A0.9600
C5—C61.386 (13)C20—H20B0.9600
C5—H50.9300C20—H20C0.9600
O7—U1—O6177.3 (3)N1—C8—H8A109.9
O7—U1—O487.8 (3)C9—C8—H8A109.9
O6—U1—O491.7 (3)N1—C8—H8B109.9
O7—U1—O190.3 (3)C9—C8—H8B109.9
O6—U1—O191.3 (3)H8A—C8—H8B108.3
O4—U1—O1154.2 (2)N2—C9—C8107.0 (7)
O7—U1—O596.1 (3)N2—C9—H9A110.3
O6—U1—O586.5 (3)C8—C9—H9A110.3
O4—U1—O578.2 (2)N2—C9—H9B110.3
O1—U1—O576.4 (2)C8—C9—H9B110.3
O7—U1—N189.7 (3)H9A—C9—H9B108.6
O6—U1—N188.8 (3)N2—C10—C11130.4 (10)
O4—U1—N1135.6 (2)N2—C10—H10114.8
O1—U1—N170.1 (2)C11—C10—H10114.8
O5—U1—N1146.0 (2)C12—C11—C10120.1 (11)
O7—U1—N292.2 (3)C12—C11—C16119.2 (10)
O6—U1—N285.1 (3)C10—C11—C16120.7 (8)
O4—U1—N269.9 (2)C11—C12—C13120.1 (12)
O1—U1—N2135.9 (2)C11—C12—H12120.0
O5—U1—N2146.7 (3)C13—C12—H12120.0
N1—U1—N265.9 (2)C14—C13—C12121.6 (11)
C1—O1—U1134.3 (6)C14—C13—H13119.2
C6—O2—C19117.6 (8)C12—C13—H13119.2
C15—O3—C20118.9 (9)C13—C14—C15120.0 (11)
C16—O4—U1135.2 (6)C13—C14—H14120.0
C17—O5—U1130.4 (8)C15—C14—H14120.0
C17—O5—H5A119 (10)C14—C15—O3125.7 (11)
U1—O5—H5A109 (10)C14—C15—C16121.7 (12)
C7—N1—C8117.0 (8)O3—C15—C16112.6 (10)
C7—N1—U1128.5 (6)O4—C16—C15121.9 (10)
C8—N1—U1114.4 (5)O4—C16—C11120.8 (8)
C10—N2—C9117.1 (8)C15—C16—C11117.3 (9)
C10—N2—U1125.8 (7)O5—C17—C18112.0 (13)
C9—N2—U1116.2 (6)O5—C17—H17A109.2
O1—C1—C6120.0 (8)C18—C17—H17A109.2
O1—C1—C2122.2 (9)O5—C17—H17B109.2
C6—C1—C2117.8 (8)C18—C17—H17B109.2
C3—C2—C1119.0 (9)H17A—C17—H17B107.9
C3—C2—C7119.4 (8)C17—C18—H18A109.5
C1—C2—C7121.5 (8)C17—C18—H18B109.5
C4—C3—C2123.5 (9)H18A—C18—H18B109.5
C4—C3—H3118.2C17—C18—H18C109.5
C2—C3—H3118.2H18A—C18—H18C109.5
C3—C4—C5118.1 (10)H18B—C18—H18C109.5
C3—C4—H4120.9O2—C19—H19A109.5
C5—C4—H4120.9O2—C19—H19B109.5
C6—C5—C4119.7 (9)H19A—C19—H19B109.5
C6—C5—H5120.2O2—C19—H19C109.5
C4—C5—H5120.2H19A—C19—H19C109.5
O2—C6—C5123.3 (9)H19B—C19—H19C109.5
O2—C6—C1114.9 (8)O3—C20—H20A109.5
C5—C6—C1121.8 (8)O3—C20—H20B109.5
N1—C7—C2127.4 (9)H20A—C20—H20B109.5
N1—C7—H7116.3O3—C20—H20C109.5
C2—C7—H7116.3H20A—C20—H20C109.5
N1—C8—C9108.8 (7)H20B—C20—H20C109.5
O7—U1—O1—C144.2 (8)O1—C1—C2—C70.1 (14)
O6—U1—O1—C1133.6 (8)C6—C1—C2—C7177.6 (9)
O4—U1—O1—C1129.9 (8)C1—C2—C3—C40.3 (17)
O5—U1—O1—C1140.4 (8)C7—C2—C3—C4178.0 (11)
N1—U1—O1—C145.3 (8)C2—C3—C4—C50.6 (18)
N2—U1—O1—C149.3 (9)C3—C4—C5—C61.9 (17)
O7—U1—O4—C16140.9 (8)C19—O2—C6—C59.5 (15)
O6—U1—O4—C1636.4 (8)C19—O2—C6—C1171.0 (10)
O1—U1—O4—C16132.8 (8)C4—C5—C6—O2177.1 (10)
O5—U1—O4—C16122.5 (8)C4—C5—C6—C12.3 (16)
N1—U1—O4—C1653.6 (9)O1—C1—C6—O20.6 (13)
N2—U1—O4—C1647.7 (8)C2—C1—C6—O2178.1 (9)
O7—U1—O5—C1710.2 (12)O1—C1—C6—C5178.8 (9)
O6—U1—O5—C17168.7 (12)C2—C1—C6—C51.3 (14)
O4—U1—O5—C1776.2 (12)C8—N1—C7—C2176.0 (9)
O1—U1—O5—C1799.1 (12)U1—N1—C7—C27.8 (14)
N1—U1—O5—C17108.8 (12)C3—C2—C7—N1168.4 (10)
N2—U1—O5—C1793.2 (12)C1—C2—C7—N114.1 (15)
O7—U1—N1—C764.3 (8)C7—N1—C8—C9127.7 (9)
O6—U1—N1—C7118.0 (8)U1—N1—C8—C949.1 (8)
O4—U1—N1—C7150.8 (7)C10—N2—C9—C8128.6 (9)
O1—U1—N1—C726.2 (8)U1—N2—C9—C841.4 (9)
O5—U1—N1—C736.2 (10)N1—C8—C9—N258.1 (10)
N2—U1—N1—C7156.8 (8)C9—N2—C10—C11179.2 (10)
O7—U1—N1—C8112.1 (6)U1—N2—C10—C1110.2 (16)
O6—U1—N1—C865.7 (6)N2—C10—C11—C12167.8 (11)
O4—U1—N1—C825.5 (7)N2—C10—C11—C1612.8 (17)
O1—U1—N1—C8157.5 (6)C10—C11—C12—C13179.6 (10)
O5—U1—N1—C8147.5 (6)C16—C11—C12—C131.0 (16)
N2—U1—N1—C819.5 (6)C11—C12—C13—C141.1 (18)
O7—U1—N2—C10114.9 (8)C12—C13—C14—C150.7 (18)
O6—U1—N2—C1065.6 (8)C13—C14—C15—O3178.8 (11)
O4—U1—N2—C1028.0 (8)C13—C14—C15—C162.5 (18)
O1—U1—N2—C10152.3 (8)C20—O3—C15—C141.3 (17)
O5—U1—N2—C1010.4 (11)C20—O3—C15—C16179.9 (10)
N1—U1—N2—C10156.4 (9)U1—O4—C16—C15137.0 (8)
O7—U1—N2—C976.1 (7)U1—O4—C16—C1144.3 (13)
O6—U1—N2—C9103.4 (7)C14—C15—C16—O4178.7 (10)
O4—U1—N2—C9163.0 (7)O3—C15—C16—O40.1 (14)
O1—U1—N2—C916.7 (8)C14—C15—C16—C112.5 (16)
O5—U1—N2—C9179.4 (6)O3—C15—C16—C11178.7 (8)
N1—U1—N2—C912.6 (6)C12—C11—C16—O4179.5 (9)
U1—O1—C1—C6139.4 (7)C10—C11—C16—O40.2 (14)
U1—O1—C1—C243.2 (13)C12—C11—C16—C150.7 (14)
O1—C1—C2—C3177.4 (9)C10—C11—C16—C15178.6 (9)
C6—C1—C2—C30.0 (14)U1—O5—C17—C1851.3 (19)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O1i0.83 (6)2.53 (15)3.059 (9)124 (15)
O5—H5A···O2i0.83 (6)2.19 (8)2.952 (11)154 (16)
C8—H8B···O7ii0.972.503.183 (11)127
C17—H17B···O1i0.972.453.163 (19)130
C18—H18C···O70.962.573.382 (19)142
C19—H19A···O6i0.962.593.423 (13)145
Symmetry codes: (i) x+1, y+1, z; (ii) x+1/2, y, z+1/2.
 

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