Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805029922/bh6027sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805029922/bh6027Isup2.hkl |
CCDC reference: 287446
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.022
- wR factor = 0.051
- Data-to-parameter ratio = 20.9
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.168 0.289 Tmin and Tmax expected: 0.121 0.289 RR = 1.391 Please check that your absorption correction is appropriate. PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.36 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.26 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C2 H4 O2
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 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Crystals of (I) were obtained as an admixture in an attempt to recrystallize anhydrous uranyl acetate in glacial acetic acid at 413 K.
All H atoms were initially located in a difference Fourier map. The methyl H atoms were then constrained to an ideal geometry, with C—H distances of 0.96 Å and Uiso(H) = 1.5Ueq(C), but each group was allowed to rotate freely about its C—C bond. The positions of H atoms bonded to O atoms were refined freely along with isotropic displacement parameters.
Data collection: P3/PC (Siemens, 1989); cell refinement: P3/PC; data reduction: P3/PC; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL.
[UO2(C2H3O2)2(H2O)2]·2C2H4O2 | Z = 1 |
Mr = 544.25 | F(000) = 254 |
Triclinic, P1 | Dx = 2.291 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.914 (2) Å | Cell parameters from 24 reflections |
b = 7.822 (2) Å | θ = 13.1–14.0° |
c = 8.211 (2) Å | µ = 10.34 mm−1 |
α = 95.00 (2)° | T = 293 K |
β = 113.74 (2)° | Irregular, yellow |
γ = 99.79 (2)° | 0.24 × 0.18 × 0.12 mm |
V = 394.6 (2) Å3 |
Siemens P3/PC diffractometer | 2316 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.021 |
Graphite monochromator | θmax = 30.1°, θmin = 2.7° |
ω/2θ scans | h = 0→9 |
Absorption correction: ψ scan (North et al., 1968) | k = −11→10 |
Tmin = 0.168, Tmax = 0.289 | l = −11→10 |
2494 measured reflections | 2 standard reflections every 98 reflections |
2316 independent reflections | intensity decay: 0.0% |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.022 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.051 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0313P)2] where P = (Fo2 + 2Fc2)/3 |
2316 reflections | (Δ/σ)max < 0.001 |
111 parameters | Δρmax = 1.36 e Å−3 |
0 restraints | Δρmin = −1.55 e Å−3 |
[UO2(C2H3O2)2(H2O)2]·2C2H4O2 | γ = 99.79 (2)° |
Mr = 544.25 | V = 394.6 (2) Å3 |
Triclinic, P1 | Z = 1 |
a = 6.914 (2) Å | Mo Kα radiation |
b = 7.822 (2) Å | µ = 10.34 mm−1 |
c = 8.211 (2) Å | T = 293 K |
α = 95.00 (2)° | 0.24 × 0.18 × 0.12 mm |
β = 113.74 (2)° |
Siemens P3/PC diffractometer | 2316 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.021 |
Tmin = 0.168, Tmax = 0.289 | 2 standard reflections every 98 reflections |
2494 measured reflections | intensity decay: 0.0% |
2316 independent reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.051 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 1.36 e Å−3 |
2316 reflections | Δρmin = −1.55 e Å−3 |
111 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
U | 0.5000 | 0.5000 | 0.5000 | 0.02319 (6) | |
O1 | 0.8816 (4) | 0.6529 (4) | 0.6462 (4) | 0.0421 (7) | |
H1A | 0.936 (10) | 0.717 (8) | 0.754 (9) | 0.052 (15)* | |
H1B | 0.964 (14) | 0.638 (11) | 0.613 (12) | 0.09 (3)* | |
O2 | 0.5474 (5) | 0.4010 (4) | 0.6929 (4) | 0.0388 (6) | |
O3 | 0.4226 (4) | 0.2003 (3) | 0.3289 (4) | 0.0388 (6) | |
O4 | 0.7500 (4) | 0.3501 (3) | 0.4119 (4) | 0.0347 (5) | |
C1 | 0.6119 (6) | 0.2055 (4) | 0.3420 (5) | 0.0284 (6) | |
C2 | 0.6669 (7) | 0.0461 (5) | 0.2752 (7) | 0.0422 (9) | |
H2A | 0.5488 | −0.0538 | 0.2437 | 0.063* | |
H2B | 0.7952 | 0.0252 | 0.3681 | 0.063* | |
H2C | 0.6923 | 0.0639 | 0.1706 | 0.063* | |
O5 | 0.0829 (6) | −0.1835 (5) | −0.0019 (4) | 0.0480 (7) | |
O6 | 0.1202 (5) | −0.0887 (4) | 0.2740 (4) | 0.0405 (6) | |
H6 | 0.217 (10) | −0.006 (8) | 0.272 (8) | 0.049 (15)* | |
C3 | 0.0257 (6) | −0.1988 (5) | 0.1181 (5) | 0.0332 (7) | |
C4 | −0.1547 (9) | −0.3402 (6) | 0.1096 (7) | 0.0507 (11) | |
H4A | −0.1605 | −0.4471 | 0.0391 | 0.076* | |
H4B | −0.2897 | −0.3048 | 0.0545 | 0.076* | |
H4C | −0.1300 | −0.3594 | 0.2295 | 0.076* |
U11 | U22 | U33 | U12 | U13 | U23 | |
U | 0.01944 (8) | 0.02120 (8) | 0.02777 (9) | 0.00096 (5) | 0.01174 (6) | −0.00310 (5) |
O1 | 0.0222 (12) | 0.0482 (16) | 0.0470 (16) | −0.0042 (11) | 0.0164 (11) | −0.0211 (13) |
O2 | 0.0422 (15) | 0.0369 (13) | 0.0379 (14) | 0.0070 (11) | 0.0185 (12) | 0.0062 (11) |
O3 | 0.0248 (12) | 0.0300 (12) | 0.0569 (17) | 0.0010 (9) | 0.0184 (12) | −0.0119 (11) |
O4 | 0.0266 (11) | 0.0294 (11) | 0.0466 (15) | 0.0003 (9) | 0.0195 (11) | −0.0085 (10) |
C1 | 0.0284 (15) | 0.0292 (14) | 0.0294 (15) | 0.0051 (12) | 0.0159 (13) | −0.0014 (12) |
C2 | 0.044 (2) | 0.0322 (17) | 0.057 (2) | 0.0092 (15) | 0.0303 (19) | −0.0053 (16) |
O5 | 0.0474 (17) | 0.0554 (18) | 0.0382 (15) | 0.0018 (14) | 0.0213 (13) | −0.0047 (13) |
O6 | 0.0463 (16) | 0.0355 (13) | 0.0344 (14) | −0.0029 (12) | 0.0186 (12) | −0.0038 (11) |
C3 | 0.0358 (17) | 0.0293 (15) | 0.0328 (17) | 0.0087 (13) | 0.0130 (14) | 0.0015 (13) |
C4 | 0.054 (3) | 0.040 (2) | 0.050 (2) | −0.0085 (19) | 0.023 (2) | −0.0008 (18) |
U—O2i | 1.760 (3) | C1—C2 | 1.487 (5) |
U—O2 | 1.760 (3) | C2—H2A | 0.9600 |
U—O1 | 2.441 (3) | C2—H2B | 0.9600 |
U—O1i | 2.441 (3) | C2—H2C | 0.9600 |
U—O3i | 2.480 (3) | O5—C3 | 1.208 (5) |
U—O3 | 2.480 (3) | O6—C3 | 1.323 (4) |
U—O4 | 2.536 (3) | O6—H6 | 0.86 (6) |
U—O4i | 2.536 (3) | C3—C4 | 1.493 (6) |
O1—H1A | 0.88 (7) | C4—H4A | 0.9600 |
O1—H1B | 0.75 (9) | C4—H4B | 0.9600 |
O3—C1 | 1.262 (4) | C4—H4C | 0.9600 |
O4—C1 | 1.265 (4) | ||
O2i—U—O2 | 180.000 (1) | O3—U—O4i | 128.94 (8) |
O2i—U—O1 | 92.61 (14) | O4—U—O4i | 180.000 (1) |
O2—U—O1 | 87.39 (14) | U—O1—H1A | 121 (4) |
O2i—U—O1i | 87.39 (13) | U—O1—H1B | 124 (7) |
O2—U—O1i | 92.61 (14) | H1A—O1—H1B | 114 (7) |
O1—U—O1i | 180.0 | C1—O3—U | 96.8 (2) |
O2i—U—O3i | 86.98 (13) | C1—O4—U | 94.0 (2) |
O2—U—O3i | 93.02 (13) | O3—C1—O4 | 117.7 (3) |
O1—U—O3i | 64.58 (10) | O3—C1—C2 | 120.4 (3) |
O1i—U—O3i | 115.42 (10) | O4—C1—C2 | 121.9 (3) |
O2i—U—O3 | 93.02 (13) | C1—C2—H2A | 109.5 |
O2—U—O3 | 86.98 (13) | C1—C2—H2B | 109.5 |
O1—U—O3 | 115.42 (10) | H2A—C2—H2B | 109.5 |
O1i—U—O3 | 64.58 (10) | C1—C2—H2C | 109.5 |
O3i—U—O3 | 180.0 | H2A—C2—H2C | 109.5 |
O2i—U—O4 | 86.50 (12) | H2B—C2—H2C | 109.5 |
O2—U—O4 | 93.50 (12) | C3—O6—H6 | 110 (4) |
O1—U—O4 | 65.22 (9) | O5—C3—O6 | 122.3 (4) |
O1i—U—O4 | 114.78 (9) | O5—C3—C4 | 125.0 (4) |
O3i—U—O4 | 128.94 (8) | O6—C3—C4 | 112.7 (4) |
O3—U—O4 | 51.06 (8) | C3—C4—H4A | 109.5 |
O2i—U—O4i | 93.50 (12) | C3—C4—H4B | 109.5 |
O2—U—O4i | 86.50 (12) | H4A—C4—H4B | 109.5 |
O1—U—O4i | 114.78 (9) | C3—C4—H4C | 109.5 |
O1i—U—O4i | 65.22 (9) | H4A—C4—H4C | 109.5 |
O3i—U—O4i | 51.06 (8) | H4B—C4—H4C | 109.5 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6···O3 | 0.86 (6) | 1.84 (6) | 2.672 (4) | 163 (6) |
O1—H1A···O5ii | 0.88 (7) | 1.86 (7) | 2.727 (4) | 168 (6) |
O1—H1B···O4iii | 0.75 (9) | 2.05 (9) | 2.778 (4) | 163 (9) |
Symmetry codes: (ii) x+1, y+1, z+1; (iii) −x+2, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [UO2(C2H3O2)2(H2O)2]·2C2H4O2 |
Mr | 544.25 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 6.914 (2), 7.822 (2), 8.211 (2) |
α, β, γ (°) | 95.00 (2), 113.74 (2), 99.79 (2) |
V (Å3) | 394.6 (2) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 10.34 |
Crystal size (mm) | 0.24 × 0.18 × 0.12 |
Data collection | |
Diffractometer | Siemens P3/PC diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.168, 0.289 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2494, 2316, 2316 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.705 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.051, 1.05 |
No. of reflections | 2316 |
No. of parameters | 111 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.36, −1.55 |
Computer programs: P3/PC (Siemens, 1989), P3/PC, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 1998), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6···O3 | 0.86 (6) | 1.84 (6) | 2.672 (4) | 163 (6) |
O1—H1A···O5i | 0.88 (7) | 1.86 (7) | 2.727 (4) | 168 (6) |
O1—H1B···O4ii | 0.75 (9) | 2.05 (9) | 2.778 (4) | 163 (9) |
Symmetry codes: (i) x+1, y+1, z+1; (ii) −x+2, −y+1, −z+1. |
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Carboxylate compounds of the actinides play a significant role in laboratory practice and radiochemical industry. Several uranyl compounds are known, in which both acetate anions and acetic acid molecules are present (Ramos Silva et al., 1999; Grigor'ev et al., 2004). Here, we present a further example of a uranyl acetate compound, (I), containing acetic acid as solvate.
The U atom in compound (I) lies on an inversion centre. Itscoordination polyhedron is a distorted hexagonal bipyramid, with the equatorial positions occupied by four O atoms of two bidentate-chelating acetate anions and two O atoms of coordination water molecules (Fig. 1). Crystallographically independent bond lengths in the U-atom environment are given in Table 1.
The coordination water and solvate acetic acid molecules act as H donors in several types of hydrogen bonds (Table 2). The acceptors in these bonds are O atoms of acetate anions and acetic acid. The hydrogen bonding results in the formation of infinite chains in the [100] direction (Fig. 2) and these chains are combined into layers parallel to the (011) plane (Fig. 3).