The redetermined structure of K2(UO2)2(C2O4)3·4H2O shows significantly improved precision of the positional and displacement parameters. Linear uranyl cations are connected by tetradentate bridging oxalate groups yielding a two-dimensional network. These nets are stacked to form the crystal structure.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 297 K
- Mean (C-C) = 0.005 Å
- Disorder in solvent or counterion
- R factor = 0.017
- wR factor = 0.042
- Data-to-parameter ratio = 14.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 9.00 Perc.
General Notes
ABSTM_02 The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.191 0.498
Tmin and Tmax expected: 0.080 0.259
RR = 1.241
Please check that your absorption correction is appropriate.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: KappaCCD Software (Nonius, 1997); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Crystal data top
K2(UO2)2(C2O4)3·4H2O | Dx = 3.398 Mg m−3 |
Mr = 473.16 | Mo Kα radiation, λ = 0.71073 Å |
Monoclinic, P21/n | Cell parameters from 2170 reflections |
a = 8.9277 (1) Å | θ = 2.9–35.0° |
b = 19.4774 (3) Å | µ = 18.03 mm−1 |
c = 5.3946 (1) Å | T = 297 K |
β = 99.6283 (7)° | Needle, yellow |
V = 924.84 (2) Å3 | 0.20 × 0.13 × 0.08 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 1980 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.068 |
CCD scans | θmax = 27.6°, θmin = 4.2° |
Absorption correction: numerical (HABITUS; Herrendorf & Bärnighausen, 1997) | h = −11→11 |
Tmin = 0.191, Tmax = 0.498 | k = −25→25 |
16994 measured reflections | l = −7→7 |
2125 independent reflections | |
Refinement top
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)] = 0.017 | H-atom parameters not defined |
wR(F2) = 0.042 | w = 1/[σ2(Fo2) + (0.008P)2 + 1.2824P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max = 0.001 |
2125 reflections | Δρmax = 1.47 e Å−3 |
145 parameters | Δρmin = −1.65 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
U | 0.990470 (12) | 0.165880 (6) | 0.04563 (2) | 0.01403 (6) | |
K1A | 0.3935 (4) | 0.09923 (15) | 0.5119 (6) | 0.0462 (7) | 0.50 |
K1B | 0.3988 (3) | 0.09949 (14) | 0.3884 (5) | 0.0381 (6) | 0.50 |
O1 | 0.8754 (3) | 0.16699 (12) | 0.7473 (5) | 0.0246 (6) | |
O2 | 0.1035 (3) | 0.15987 (13) | 0.3477 (5) | 0.0261 (6) | |
O3 | 0.0645 (3) | 0.28113 (13) | 0.8663 (5) | 0.0237 (5) | |
O4 | 0.2348 (3) | 0.33664 (11) | 0.6775 (6) | 0.0232 (6) | |
O5 | 0.4106 (3) | 0.22788 (13) | 0.7313 (5) | 0.0242 (6) | |
O6 | 0.2494 (3) | 0.17457 (13) | 0.9391 (6) | 0.0244 (6) | |
O7 | 0.1074 (3) | 0.06155 (13) | 0.8824 (6) | 0.0343 (7) | |
O8 | 0.8870 (3) | 0.05261 (13) | 0.1487 (6) | 0.0313 (7) | |
O9 | 0.2083 (4) | 0.46744 (19) | 0.0418 (7) | 0.0530 (9) | |
O10 | 1.0064 (5) | 0.4308 (3) | 0.4632 (8) | 0.0851 (16) | |
C1 | 0.1870 (4) | 0.28643 (17) | 0.7866 (6) | 0.0182 (7) | |
C2 | 0.2919 (4) | 0.22440 (17) | 0.8229 (6) | 0.0176 (6) | |
C3 | 0.0634 (4) | 0.00277 (16) | 0.9232 (7) | 0.0232 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
U | 0.01377 (8) | 0.01028 (8) | 0.01960 (9) | 0.00031 (4) | 0.00729 (6) | −0.00001 (4) |
K1A | 0.0447 (14) | 0.0250 (11) | 0.0634 (19) | 0.0057 (9) | −0.0064 (16) | −0.0069 (14) |
K1B | 0.0292 (10) | 0.0291 (11) | 0.0549 (16) | −0.0019 (8) | 0.0037 (13) | 0.0038 (13) |
O1 | 0.0250 (14) | 0.0274 (16) | 0.0213 (14) | −0.0013 (10) | 0.0039 (12) | −0.0028 (9) |
O2 | 0.0232 (14) | 0.0345 (16) | 0.0207 (14) | 0.0045 (10) | 0.0038 (11) | 0.0037 (10) |
O3 | 0.0194 (12) | 0.0188 (13) | 0.0367 (15) | 0.0016 (10) | 0.0154 (11) | 0.0041 (10) |
O4 | 0.0203 (13) | 0.0149 (13) | 0.0370 (16) | 0.0010 (9) | 0.0123 (12) | 0.0063 (9) |
O5 | 0.0230 (12) | 0.0146 (12) | 0.0393 (15) | 0.0016 (10) | 0.0182 (11) | 0.0046 (10) |
O6 | 0.0204 (13) | 0.0152 (12) | 0.0403 (17) | −0.0014 (9) | 0.0125 (12) | 0.0073 (10) |
O7 | 0.0362 (15) | 0.0124 (13) | 0.063 (2) | 0.0010 (11) | 0.0325 (15) | 0.0002 (12) |
O8 | 0.0348 (15) | 0.0123 (12) | 0.0538 (18) | 0.0002 (10) | 0.0276 (14) | −0.0014 (11) |
O9 | 0.068 (2) | 0.047 (2) | 0.049 (2) | 0.0192 (18) | 0.0258 (18) | 0.0063 (15) |
O10 | 0.107 (4) | 0.066 (3) | 0.079 (3) | 0.044 (2) | 0.006 (3) | 0.012 (2) |
C1 | 0.0186 (15) | 0.0172 (17) | 0.0196 (16) | −0.0006 (13) | 0.0059 (13) | −0.0009 (13) |
C2 | 0.0166 (15) | 0.0157 (16) | 0.0217 (17) | −0.0023 (12) | 0.0064 (13) | 0.0021 (12) |
C3 | 0.0227 (17) | 0.0124 (18) | 0.0368 (19) | 0.0004 (12) | 0.0121 (15) | −0.0009 (14) |
Geometric parameters (Å, º) top
U—O1i | 1.759 (3) | K1B—Uix | 4.016 (3) |
U—O2ii | 1.771 (3) | K1B—K1Ax | 4.287 (2) |
U—O5iii | 2.456 (2) | O1—Uxi | 1.759 (3) |
U—O6iv | 2.479 (3) | O2—Uix | 1.771 (3) |
U—O8 | 2.490 (3) | O3—C1 | 1.245 (4) |
U—O4iii | 2.503 (3) | O3—Uxii | 2.574 (2) |
U—O7iv | 2.510 (3) | O3—K1Bv | 2.769 (4) |
U—O3iv | 2.574 (2) | O3—K1Av | 2.963 (4) |
U—K1Bii | 4.016 (3) | O4—C1 | 1.252 (4) |
U—K1Aii | 4.234 (3) | O4—Uv | 2.503 (3) |
K1A—K1B | 0.676 (3) | O5—C2 | 1.244 (4) |
K1A—O10v | 2.543 (6) | O5—Uv | 2.456 (2) |
K1A—O9vi | 2.722 (5) | O6—C2 | 1.248 (4) |
K1A—O5 | 2.765 (4) | O6—Uxii | 2.479 (3) |
K1A—O2 | 2.849 (4) | O6—K1Bxi | 2.952 (4) |
K1A—O3iii | 2.963 (4) | O7—C3 | 1.242 (4) |
K1A—O9vii | 3.076 (5) | O7—Uxii | 2.510 (3) |
K1A—C2 | 3.177 (5) | O8—C3x | 1.252 (4) |
K1A—O6 | 3.180 (4) | O9—K1Axiii | 2.722 (5) |
K1A—O10viii | 3.335 (6) | O9—K1Bxiii | 2.791 (4) |
K1A—Uix | 4.234 (3) | O9—K1Bviii | 3.042 (5) |
K1A—K1Bx | 4.287 (2) | O9—K1Aviii | 3.076 (5) |
K1B—O10viii | 2.696 (6) | O10—K1Aiii | 2.543 (6) |
K1B—O3iii | 2.769 (4) | O10—K1Bvii | 2.696 (6) |
K1B—O9vi | 2.792 (4) | O10—K1Biii | 3.145 (5) |
K1B—O2 | 2.862 (4) | O10—K1Avii | 3.335 (6) |
K1B—O6i | 2.952 (4) | C1—C2 | 1.521 (5) |
K1B—O9vii | 3.042 (5) | C1—K1Bv | 3.511 (4) |
K1B—O5 | 3.102 (4) | C3—O8x | 1.252 (4) |
K1B—O10v | 3.145 (5) | C3—C3xiv | 1.514 (7) |
K1B—C1iii | 3.511 (4) | | |
| | | |
O1i—U—O2ii | 176.78 (12) | K1A—K1B—O9vi | 77.2 (4) |
O1i—U—O5iii | 101.41 (11) | O10viii—K1B—O9vi | 95.28 (16) |
O2ii—U—O5iii | 80.79 (11) | O3iii—K1B—O9vi | 167.71 (15) |
O1i—U—O6iv | 102.22 (12) | K1A—K1B—O2 | 82.1 (5) |
O2ii—U—O6iv | 78.94 (12) | O10viii—K1B—O2 | 118.65 (16) |
O5iii—U—O6iv | 112.48 (8) | O3iii—K1B—O2 | 98.25 (11) |
O1i—U—O8 | 91.92 (11) | O9vi—K1B—O2 | 93.25 (13) |
O2ii—U—O8 | 84.92 (11) | K1A—K1B—O6i | 135.8 (5) |
O5iii—U—O8 | 120.77 (9) | O10viii—K1B—O6i | 65.56 (14) |
O6iv—U—O8 | 120.48 (8) | O3iii—K1B—O6i | 73.73 (10) |
O1i—U—O4iii | 80.76 (12) | O9vi—K1B—O6i | 116.70 (14) |
O2ii—U—O4iii | 98.24 (12) | O2—K1B—O6i | 56.59 (10) |
O5iii—U—O4iii | 63.89 (8) | K1A—K1B—O9vii | 86.5 (5) |
O6iv—U—O4iii | 175.88 (8) | O10viii—K1B—O9vii | 72.60 (14) |
O8—U—O4iii | 61.91 (8) | O3iii—K1B—O9vii | 84.50 (11) |
O1i—U—O7iv | 84.39 (11) | O9vi—K1B—O9vii | 83.38 (13) |
O2ii—U—O7iv | 93.62 (12) | O2—K1B—O9vii | 168.60 (14) |
O5iii—U—O7iv | 172.37 (9) | O6i—K1B—O9vii | 134.50 (13) |
O6iv—U—O7iv | 61.02 (9) | K1A—K1B—O5 | 54.5 (4) |
O8—U—O7iv | 63.43 (9) | O10viii—K1B—O5 | 134.62 (15) |
O4iii—U—O7iv | 122.44 (8) | O3iii—K1B—O5 | 51.94 (9) |
O1i—U—O3iv | 78.03 (10) | O9vi—K1B—O5 | 129.83 (13) |
O2ii—U—O3iv | 105.13 (11) | O2—K1B—O5 | 69.72 (10) |
O5iii—U—O3iv | 61.88 (9) | O6i—K1B—O5 | 93.20 (11) |
O6iv—U—O3iv | 62.97 (8) | O9vii—K1B—O5 | 104.15 (12) |
O8—U—O3iv | 169.95 (9) | K1A—K1B—O10v | 24.1 (4) |
O4iii—U—O3iv | 115.32 (8) | O10viii—K1B—O10v | 134.8 (2) |
O7iv—U—O3iv | 115.23 (9) | O3iii—K1B—O10v | 97.06 (13) |
O1i—U—K1Bii | 140.51 (10) | O9vi—K1B—O10v | 75.46 (13) |
O2ii—U—K1Bii | 38.88 (10) | O2—K1B—O10v | 106.15 (14) |
O5iii—U—K1Bii | 112.74 (7) | O6i—K1B—O10v | 157.56 (16) |
O6iv—U—K1Bii | 47.07 (8) | O9vii—K1B—O10v | 62.46 (13) |
O8—U—K1Bii | 87.36 (8) | O5—K1B—O10v | 65.73 (13) |
O4iii—U—K1Bii | 131.59 (8) | K1A—K1B—C1iii | 109.5 (5) |
O7iv—U—K1Bii | 60.15 (9) | O10viii—K1B—C1iii | 68.34 (12) |
O3iv—U—K1Bii | 100.58 (7) | O3iii—K1B—C1iii | 18.44 (8) |
O1i—U—K1Aii | 148.83 (10) | O9vi—K1B—C1iii | 151.73 (14) |
O2ii—U—K1Aii | 30.30 (10) | O2—K1B—C1iii | 114.69 (11) |
O5iii—U—K1Aii | 106.96 (7) | O6i—K1B—C1iii | 78.48 (10) |
O6iv—U—K1Aii | 54.98 (8) | O9vii—K1B—C1iii | 69.99 (10) |
O8—U—K1Aii | 84.59 (8) | O5—K1B—C1iii | 68.31 (9) |
O4iii—U—K1Aii | 123.36 (8) | O10v—K1B—C1iii | 99.33 (12) |
O7iv—U—K1Aii | 66.33 (8) | K1A—K1B—Uix | 104.3 (5) |
O3iv—U—K1Aii | 104.16 (7) | O10viii—K1B—Uix | 95.96 (13) |
K1Bii—U—K1Aii | 8.90 (5) | O3iii—K1B—Uix | 99.21 (9) |
K1B—K1A—O10v | 149.7 (6) | O9vi—K1B—Uix | 93.07 (11) |
K1B—K1A—O9vi | 88.8 (4) | O2—K1B—Uix | 22.87 (6) |
O10v—K1A—O9vi | 87.51 (17) | O6i—K1B—Uix | 37.95 (6) |
K1B—K1A—O5 | 114.0 (5) | O9vii—K1B—Uix | 167.57 (12) |
O10v—K1A—O5 | 79.28 (16) | O5—K1B—Uix | 87.29 (8) |
O9vi—K1A—O5 | 153.36 (18) | O10v—K1B—Uix | 128.21 (13) |
K1B—K1A—O2 | 84.3 (5) | C1iii—K1B—Uix | 110.89 (9) |
O10v—K1A—O2 | 125.96 (19) | K1A—K1B—K1Ax | 88.3 (4) |
O9vi—K1A—O2 | 95.05 (14) | O10viii—K1B—K1Ax | 72.59 (15) |
O5—K1A—O2 | 74.92 (11) | O3iii—K1B—K1Ax | 122.73 (9) |
K1B—K1A—O3iii | 66.9 (4) | O9vi—K1B—K1Ax | 45.73 (10) |
O10v—K1A—O3iii | 107.18 (15) | O2—K1B—K1Ax | 138.97 (9) |
O9vi—K1A—O3iii | 153.01 (16) | O6i—K1B—K1Ax | 132.62 (13) |
O5—K1A—O3iii | 53.59 (10) | O9vii—K1B—K1Ax | 39.17 (8) |
O2—K1A—O3iii | 94.21 (11) | O5—K1B—K1Ax | 133.02 (11) |
K1B—K1A—O9vii | 80.8 (5) | O10v—K1B—K1Ax | 69.66 (13) |
O10v—K1A—O9vii | 68.91 (15) | C1iii—K1B—K1Ax | 106.14 (9) |
O9vi—K1A—O9vii | 83.88 (13) | Uix—K1B—K1Ax | 133.54 (6) |
O5—K1A—O9vii | 112.04 (13) | Uix—O2—K1A | 131.41 (15) |
O2—K1A—O9vii | 165.09 (16) | Uix—O2—K1B | 118.25 (15) |
O3iii—K1A—O9vii | 80.73 (12) | K1A—O2—K1B | 13.59 (6) |
K1B—K1A—C2 | 126.1 (5) | C1—O3—Uxii | 119.9 (2) |
O10v—K1A—C2 | 76.90 (16) | C1—O3—K1Bv | 116.9 (2) |
O9vi—K1A—C2 | 131.31 (16) | Uxii—O3—K1Bv | 122.94 (11) |
O5—K1A—C2 | 22.85 (8) | C1—O3—K1Av | 123.2 (2) |
O2—K1A—C2 | 61.39 (10) | Uxii—O3—K1Av | 114.22 (10) |
O3iii—K1A—C2 | 75.03 (10) | K1Bv—O3—K1Av | 12.98 (6) |
O9vii—K1A—C2 | 129.44 (13) | C1—O4—Uv | 121.1 (2) |
K1B—K1A—O6 | 144.6 (5) | C2—O5—Uv | 122.2 (2) |
O10v—K1A—O6 | 63.63 (15) | C2—O5—K1A | 97.5 (2) |
O9vi—K1A—O6 | 110.11 (15) | Uv—O5—K1A | 126.03 (13) |
O5—K1A—O6 | 43.25 (8) | C2—O5—K1B | 104.3 (2) |
O2—K1A—O6 | 64.99 (10) | Uv—O5—K1B | 114.79 (11) |
O3iii—K1A—O6 | 96.78 (10) | K1A—O5—K1B | 11.48 (8) |
O9vii—K1A—O6 | 129.32 (13) | C2—O6—Uxii | 122.9 (2) |
C2—K1A—O6 | 22.65 (8) | C2—O6—K1Bxi | 131.6 (2) |
K1B—K1A—O10viii | 17.2 (4) | Uxii—O6—K1Bxi | 94.98 (11) |
O10v—K1A—O10viii | 132.8 (2) | C2—O6—K1A | 78.5 (2) |
O9vi—K1A—O10viii | 83.41 (13) | Uxii—O6—K1A | 129.96 (12) |
O5—K1A—O10viii | 122.40 (16) | K1Bxi—O6—K1A | 100.63 (9) |
O2—K1A—O10viii | 101.01 (14) | C3—O7—Uxii | 121.4 (2) |
O3iii—K1A—O10viii | 69.94 (12) | C3x—O8—U | 122.0 (2) |
O9vii—K1A—O10viii | 64.09 (13) | K1Axiii—O9—K1Bxiii | 14.01 (7) |
C2—K1A—O10viii | 139.38 (16) | K1Axiii—O9—K1Bviii | 95.93 (14) |
O6—K1A—O10viii | 160.64 (15) | K1Bxiii—O9—K1Bviii | 96.62 (13) |
K1B—K1A—Uix | 66.8 (5) | K1Axiii—O9—K1Aviii | 96.12 (13) |
O10v—K1A—Uix | 143.21 (17) | K1Bxiii—O9—K1Aviii | 93.74 (13) |
O9vi—K1A—Uix | 89.46 (12) | K1Bviii—O9—K1Aviii | 12.67 (6) |
O5—K1A—Uix | 87.55 (9) | K1Aiii—O10—K1Bvii | 128.6 (2) |
O2—K1A—Uix | 18.29 (6) | K1Aiii—O10—K1Biii | 6.23 (11) |
O3iii—K1A—Uix | 91.48 (9) | K1Bvii—O10—K1Biii | 134.8 (2) |
O9vii—K1A—Uix | 147.01 (12) | K1Aiii—O10—K1Avii | 132.8 (2) |
C2—K1A—Uix | 77.84 (9) | K1Bvii—O10—K1Avii | 4.24 (10) |
O6—K1A—Uix | 83.26 (9) | K1Biii—O10—K1Avii | 138.98 (19) |
O10viii—K1A—Uix | 83.08 (11) | O3—C1—O4 | 128.0 (3) |
K1B—K1A—K1Bx | 91.7 (4) | O3—C1—C2 | 116.6 (3) |
O10v—K1A—K1Bx | 65.04 (15) | O4—C1—C2 | 115.5 (3) |
O9vi—K1A—K1Bx | 44.90 (11) | O3—C1—K1Bv | 44.71 (18) |
O5—K1A—K1Bx | 140.60 (12) | O4—C1—K1Bv | 84.0 (2) |
O2—K1A—K1Bx | 139.91 (10) | C2—C1—K1Bv | 159.0 (2) |
O3iii—K1A—K1Bx | 120.80 (10) | O5—C2—O6 | 126.4 (3) |
O9vii—K1A—K1Bx | 40.53 (8) | O5—C2—C1 | 116.9 (3) |
C2—K1A—K1Bx | 141.48 (13) | O6—C2—C1 | 116.7 (3) |
O6—K1A—K1Bx | 123.00 (13) | O5—C2—K1A | 59.63 (19) |
O10viii—K1A—K1Bx | 76.36 (12) | O6—C2—K1A | 78.8 (2) |
Uix—K1A—K1Bx | 131.16 (7) | C1—C2—K1A | 139.9 (2) |
K1A—K1B—O10viii | 158.6 (5) | O7—C3—O8x | 126.9 (3) |
K1A—K1B—O3iii | 100.1 (5) | O7—C3—C3xiv | 116.8 (4) |
O10viii—K1B—O3iii | 83.02 (14) | O8x—C3—C3xiv | 116.3 (4) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) x+1/2, −y+1/2, z−1/2; (iv) x+1, y, z−1; (v) x−1/2, −y+1/2, z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) x−1/2, −y+1/2, z−1/2; (ix) x−1, y, z; (x) −x+1, −y, −z+1; (xi) x, y, z+1; (xii) x−1, y, z+1; (xiii) −x+1/2, y+1/2, −z+1/2; (xiv) −x, −y, −z+2. |