Redetermination of dipotassium diuranyl tris­(oxalate) tetrahydrate

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.

Key indicators

• Single-crystal X-ray study
• T = 297 K
• Mean [sigma](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

---

Computing details

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).

(I)

Crystal data

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) Å^3	0.20 × 0.13 × 0.08 mm
Z = 4

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.017	H-atom parameters not defined
wR(F^2) = 0.042	w = 1/[σ^2(Fo^2) + (0.008P)^2 + 1.2824P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

U—O1^i	1.759 (3)	K1B—U^ix	4.016 (3)
U—O2^ii	1.771 (3)	K1B—K1A^x	4.287 (2)
U—O5^iii	2.456 (2)	O1—U^xi	1.759 (3)
U—O6^iv	2.479 (3)	O2—U^ix	1.771 (3)
U—O8	2.490 (3)	O3—C1	1.245 (4)
U—O4^iii	2.503 (3)	O3—U^xii	2.574 (2)
U—O7^iv	2.510 (3)	O3—K1B^v	2.769 (4)
U—O3^iv	2.574 (2)	O3—K1A^v	2.963 (4)
U—K1B^ii	4.016 (3)	O4—C1	1.252 (4)
U—K1A^ii	4.234 (3)	O4—U^v	2.503 (3)
K1A—K1B	0.676 (3)	O5—C2	1.244 (4)
K1A—O10^v	2.543 (6)	O5—U^v	2.456 (2)
K1A—O9^vi	2.722 (5)	O6—C2	1.248 (4)
K1A—O5	2.765 (4)	O6—U^xii	2.479 (3)
K1A—O2	2.849 (4)	O6—K1B^xi	2.952 (4)
K1A—O3^iii	2.963 (4)	O7—C3	1.242 (4)
K1A—O9^vii	3.076 (5)	O7—U^xii	2.510 (3)
K1A—C2	3.177 (5)	O8—C3^x	1.252 (4)
K1A—O6	3.180 (4)	O9—K1A^xiii	2.722 (5)
K1A—O10^viii	3.335 (6)	O9—K1B^xiii	2.791 (4)
K1A—U^ix	4.234 (3)	O9—K1B^viii	3.042 (5)
K1A—K1B^x	4.287 (2)	O9—K1A^viii	3.076 (5)
K1B—O10^viii	2.696 (6)	O10—K1A^iii	2.543 (6)
K1B—O3^iii	2.769 (4)	O10—K1B^vii	2.696 (6)
K1B—O9^vi	2.792 (4)	O10—K1B^iii	3.145 (5)
K1B—O2	2.862 (4)	O10—K1A^vii	3.335 (6)
K1B—O6^i	2.952 (4)	C1—C2	1.521 (5)
K1B—O9^vii	3.042 (5)	C1—K1B^v	3.511 (4)
K1B—O5	3.102 (4)	C3—O8^x	1.252 (4)
K1B—O10^v	3.145 (5)	C3—C3^xiv	1.514 (7)
K1B—C1^iii	3.511 (4)
O1^i—U—O2^ii	176.78 (12)	K1A—K1B—O9^vi	77.2 (4)
O1^i—U—O5^iii	101.41 (11)	O10^viii—K1B—O9^vi	95.28 (16)
O2^ii—U—O5^iii	80.79 (11)	O3^iii—K1B—O9^vi	167.71 (15)
O1^i—U—O6^iv	102.22 (12)	K1A—K1B—O2	82.1 (5)
O2^ii—U—O6^iv	78.94 (12)	O10^viii—K1B—O2	118.65 (16)
O5^iii—U—O6^iv	112.48 (8)	O3^iii—K1B—O2	98.25 (11)
O1^i—U—O8	91.92 (11)	O9^vi—K1B—O2	93.25 (13)
O2^ii—U—O8	84.92 (11)	K1A—K1B—O6^i	135.8 (5)
O5^iii—U—O8	120.77 (9)	O10^viii—K1B—O6^i	65.56 (14)
O6^iv—U—O8	120.48 (8)	O3^iii—K1B—O6^i	73.73 (10)
O1^i—U—O4^iii	80.76 (12)	O9^vi—K1B—O6^i	116.70 (14)
O2^ii—U—O4^iii	98.24 (12)	O2—K1B—O6^i	56.59 (10)
O5^iii—U—O4^iii	63.89 (8)	K1A—K1B—O9^vii	86.5 (5)
O6^iv—U—O4^iii	175.88 (8)	O10^viii—K1B—O9^vii	72.60 (14)
O8—U—O4^iii	61.91 (8)	O3^iii—K1B—O9^vii	84.50 (11)
O1^i—U—O7^iv	84.39 (11)	O9^vi—K1B—O9^vii	83.38 (13)
O2^ii—U—O7^iv	93.62 (12)	O2—K1B—O9^vii	168.60 (14)
O5^iii—U—O7^iv	172.37 (9)	O6^i—K1B—O9^vii	134.50 (13)
O6^iv—U—O7^iv	61.02 (9)	K1A—K1B—O5	54.5 (4)
O8—U—O7^iv	63.43 (9)	O10^viii—K1B—O5	134.62 (15)
O4^iii—U—O7^iv	122.44 (8)	O3^iii—K1B—O5	51.94 (9)
O1^i—U—O3^iv	78.03 (10)	O9^vi—K1B—O5	129.83 (13)
O2^ii—U—O3^iv	105.13 (11)	O2—K1B—O5	69.72 (10)
O5^iii—U—O3^iv	61.88 (9)	O6^i—K1B—O5	93.20 (11)
O6^iv—U—O3^iv	62.97 (8)	O9^vii—K1B—O5	104.15 (12)
O8—U—O3^iv	169.95 (9)	K1A—K1B—O10^v	24.1 (4)
O4^iii—U—O3^iv	115.32 (8)	O10^viii—K1B—O10^v	134.8 (2)
O7^iv—U—O3^iv	115.23 (9)	O3^iii—K1B—O10^v	97.06 (13)
O1^i—U—K1B^ii	140.51 (10)	O9^vi—K1B—O10^v	75.46 (13)
O2^ii—U—K1B^ii	38.88 (10)	O2—K1B—O10^v	106.15 (14)
O5^iii—U—K1B^ii	112.74 (7)	O6^i—K1B—O10^v	157.56 (16)
O6^iv—U—K1B^ii	47.07 (8)	O9^vii—K1B—O10^v	62.46 (13)
O8—U—K1B^ii	87.36 (8)	O5—K1B—O10^v	65.73 (13)
O4^iii—U—K1B^ii	131.59 (8)	K1A—K1B—C1^iii	109.5 (5)
O7^iv—U—K1B^ii	60.15 (9)	O10^viii—K1B—C1^iii	68.34 (12)
O3^iv—U—K1B^ii	100.58 (7)	O3^iii—K1B—C1^iii	18.44 (8)
O1^i—U—K1A^ii	148.83 (10)	O9^vi—K1B—C1^iii	151.73 (14)
O2^ii—U—K1A^ii	30.30 (10)	O2—K1B—C1^iii	114.69 (11)
O5^iii—U—K1A^ii	106.96 (7)	O6^i—K1B—C1^iii	78.48 (10)
O6^iv—U—K1A^ii	54.98 (8)	O9^vii—K1B—C1^iii	69.99 (10)
O8—U—K1A^ii	84.59 (8)	O5—K1B—C1^iii	68.31 (9)
O4^iii—U—K1A^ii	123.36 (8)	O10^v—K1B—C1^iii	99.33 (12)
O7^iv—U—K1A^ii	66.33 (8)	K1A—K1B—U^ix	104.3 (5)
O3^iv—U—K1A^ii	104.16 (7)	O10^viii—K1B—U^ix	95.96 (13)
K1B^ii—U—K1A^ii	8.90 (5)	O3^iii—K1B—U^ix	99.21 (9)
K1B—K1A—O10^v	149.7 (6)	O9^vi—K1B—U^ix	93.07 (11)
K1B—K1A—O9^vi	88.8 (4)	O2—K1B—U^ix	22.87 (6)
O10^v—K1A—O9^vi	87.51 (17)	O6^i—K1B—U^ix	37.95 (6)
K1B—K1A—O5	114.0 (5)	O9^vii—K1B—U^ix	167.57 (12)
O10^v—K1A—O5	79.28 (16)	O5—K1B—U^ix	87.29 (8)
O9^vi—K1A—O5	153.36 (18)	O10^v—K1B—U^ix	128.21 (13)
K1B—K1A—O2	84.3 (5)	C1^iii—K1B—U^ix	110.89 (9)
O10^v—K1A—O2	125.96 (19)	K1A—K1B—K1A^x	88.3 (4)
O9^vi—K1A—O2	95.05 (14)	O10^viii—K1B—K1A^x	72.59 (15)
O5—K1A—O2	74.92 (11)	O3^iii—K1B—K1A^x	122.73 (9)
K1B—K1A—O3^iii	66.9 (4)	O9^vi—K1B—K1A^x	45.73 (10)
O10^v—K1A—O3^iii	107.18 (15)	O2—K1B—K1A^x	138.97 (9)
O9^vi—K1A—O3^iii	153.01 (16)	O6^i—K1B—K1A^x	132.62 (13)
O5—K1A—O3^iii	53.59 (10)	O9^vii—K1B—K1A^x	39.17 (8)
O2—K1A—O3^iii	94.21 (11)	O5—K1B—K1A^x	133.02 (11)
K1B—K1A—O9^vii	80.8 (5)	O10^v—K1B—K1A^x	69.66 (13)
O10^v—K1A—O9^vii	68.91 (15)	C1^iii—K1B—K1A^x	106.14 (9)
O9^vi—K1A—O9^vii	83.88 (13)	U^ix—K1B—K1A^x	133.54 (6)
O5—K1A—O9^vii	112.04 (13)	U^ix—O2—K1A	131.41 (15)
O2—K1A—O9^vii	165.09 (16)	U^ix—O2—K1B	118.25 (15)
O3^iii—K1A—O9^vii	80.73 (12)	K1A—O2—K1B	13.59 (6)
K1B—K1A—C2	126.1 (5)	C1—O3—U^xii	119.9 (2)
O10^v—K1A—C2	76.90 (16)	C1—O3—K1B^v	116.9 (2)
O9^vi—K1A—C2	131.31 (16)	U^xii—O3—K1B^v	122.94 (11)
O5—K1A—C2	22.85 (8)	C1—O3—K1A^v	123.2 (2)
O2—K1A—C2	61.39 (10)	U^xii—O3—K1A^v	114.22 (10)
O3^iii—K1A—C2	75.03 (10)	K1B^v—O3—K1A^v	12.98 (6)
O9^vii—K1A—C2	129.44 (13)	C1—O4—U^v	121.1 (2)
K1B—K1A—O6	144.6 (5)	C2—O5—U^v	122.2 (2)
O10^v—K1A—O6	63.63 (15)	C2—O5—K1A	97.5 (2)
O9^vi—K1A—O6	110.11 (15)	U^v—O5—K1A	126.03 (13)
O5—K1A—O6	43.25 (8)	C2—O5—K1B	104.3 (2)
O2—K1A—O6	64.99 (10)	U^v—O5—K1B	114.79 (11)
O3^iii—K1A—O6	96.78 (10)	K1A—O5—K1B	11.48 (8)
O9^vii—K1A—O6	129.32 (13)	C2—O6—U^xii	122.9 (2)
C2—K1A—O6	22.65 (8)	C2—O6—K1B^xi	131.6 (2)
K1B—K1A—O10^viii	17.2 (4)	U^xii—O6—K1B^xi	94.98 (11)
O10^v—K1A—O10^viii	132.8 (2)	C2—O6—K1A	78.5 (2)
O9^vi—K1A—O10^viii	83.41 (13)	U^xii—O6—K1A	129.96 (12)
O5—K1A—O10^viii	122.40 (16)	K1B^xi—O6—K1A	100.63 (9)
O2—K1A—O10^viii	101.01 (14)	C3—O7—U^xii	121.4 (2)
O3^iii—K1A—O10^viii	69.94 (12)	C3^x—O8—U	122.0 (2)
O9^vii—K1A—O10^viii	64.09 (13)	K1A^xiii—O9—K1B^xiii	14.01 (7)
C2—K1A—O10^viii	139.38 (16)	K1A^xiii—O9—K1B^viii	95.93 (14)
O6—K1A—O10^viii	160.64 (15)	K1B^xiii—O9—K1B^viii	96.62 (13)
K1B—K1A—U^ix	66.8 (5)	K1A^xiii—O9—K1A^viii	96.12 (13)
O10^v—K1A—U^ix	143.21 (17)	K1B^xiii—O9—K1A^viii	93.74 (13)
O9^vi—K1A—U^ix	89.46 (12)	K1B^viii—O9—K1A^viii	12.67 (6)
O5—K1A—U^ix	87.55 (9)	K1A^iii—O10—K1B^vii	128.6 (2)
O2—K1A—U^ix	18.29 (6)	K1A^iii—O10—K1B^iii	6.23 (11)
O3^iii—K1A—U^ix	91.48 (9)	K1B^vii—O10—K1B^iii	134.8 (2)
O9^vii—K1A—U^ix	147.01 (12)	K1A^iii—O10—K1A^vii	132.8 (2)
C2—K1A—U^ix	77.84 (9)	K1B^vii—O10—K1A^vii	4.24 (10)
O6—K1A—U^ix	83.26 (9)	K1B^iii—O10—K1A^vii	138.98 (19)
O10^viii—K1A—U^ix	83.08 (11)	O3—C1—O4	128.0 (3)
K1B—K1A—K1B^x	91.7 (4)	O3—C1—C2	116.6 (3)
O10^v—K1A—K1B^x	65.04 (15)	O4—C1—C2	115.5 (3)
O9^vi—K1A—K1B^x	44.90 (11)	O3—C1—K1B^v	44.71 (18)
O5—K1A—K1B^x	140.60 (12)	O4—C1—K1B^v	84.0 (2)
O2—K1A—K1B^x	139.91 (10)	C2—C1—K1B^v	159.0 (2)
O3^iii—K1A—K1B^x	120.80 (10)	O5—C2—O6	126.4 (3)
O9^vii—K1A—K1B^x	40.53 (8)	O5—C2—C1	116.9 (3)
C2—K1A—K1B^x	141.48 (13)	O6—C2—C1	116.7 (3)
O6—K1A—K1B^x	123.00 (13)	O5—C2—K1A	59.63 (19)
O10^viii—K1A—K1B^x	76.36 (12)	O6—C2—K1A	78.8 (2)
U^ix—K1A—K1B^x	131.16 (7)	C1—C2—K1A	139.9 (2)
K1A—K1B—O10^viii	158.6 (5)	O7—C3—O8^x	126.9 (3)
K1A—K1B—O3^iii	100.1 (5)	O7—C3—C3^xiv	116.8 (4)
O10^viii—K1B—O3^iii	83.02 (14)	O8^x—C3—C3^xiv	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.