(Dimethyl­formamide)dioxobis(pentane-2,4-dionato)uranium(VI)

The title complex, [UO₂(C₅H₇O₂)₂(C₃H₇NO)], was obtained as an unexpected product from our attempts to prepare U^IV complexes with imine-type ligands. The title complex was also prepared directly from [UO₂(OAc)₂]·2H₂O, pentane-2,4-dione and DMF. The U^VI atom has a penta­gonal-bipyramidal geometry and is surrounded by seven O atoms. The bond distances and angles are similar to those found previously in similar structures.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.028
• wR factor = 0.060
• Data-to-parameter ratio = 20.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           28.14
           From the CIF: _reflns_number_total               4167
           Count of symmetry unique reflns         2380
           Completeness (_total/calc)            175.08%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1787
           Fraction of Friedel pairs measured     0.751
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   1 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: COLLECT (Bruker, 2003); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: PLATON; software used to prepare material for publication: CRYSTALS, CIFTAB (Sheldrick, 1993) and PLATON (Spek, 2003).

Dioxobis(pentane-2,4-dionato)(dimethylformamide)uranium(VI)

Crystal data

[UO2(C5H7O2)2(C3H7NO)]	F(000) = 1016
Mr = 541.34	Dx = 2.110 Mg m^−3
Orthorhombic, P212121	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: P 2ac 2ab	Cell parameters from 9607 reflections
a = 8.5600 (1) Å	θ = 0–0°
b = 12.8018 (3) Å	µ = 9.56 mm^−1
c = 15.5510 (4) Å	T = 173 K
V = 1704.13 (6) Å^3	Prism, orange
Z = 4	0.15 × 0.10 × 0.08 mm

Data collection

Bruker SMART APEXII diffractometer	3943 reflections with I > 2.0σ(I)
Graphite monochromator	Rint = 0.056
φ & ω scans	θmax = 28.1°, θmin = 2.1°
Absorption correction: multi-scan (DENZO/SCALEPACK; Otwinowski & Minor, 1997)	h = −11→9
Tmin = 0.33, Tmax = 0.47	k = −16→14
12643 measured reflections	l = −20→20
4167 independent reflections

Refinement

Refinement on F^2	H-atom parameters constrained
Least-squares matrix: full	Method = Modified Sheldrick w = 1/[σ^2(F^2) + ( 0.0P)^2 + 5.8P] , where P = (max(Fo^2,0) + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.028	(Δ/σ)max = 0.001
wR(F^2) = 0.060	Δρmax = 0.85 e Å^−3
S = 0.98	Δρmin = −1.08 e Å^−3
4154 reflections	Extinction correction: Larson (1970), Equation 22
201 parameters	Extinction coefficient: 53 (2)
0 restraints	Absolute structure: Flack (1983), 1788 Friedel-pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.02 (1)
Hydrogen site location: inferred from neighbouring sites

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
U1	0.47724 (2)	0.509073 (14)	0.069391 (12)	0.0216
O4	0.5931 (4)	0.4958 (3)	−0.0681 (2)	0.0300
O1	0.2996 (5)	0.5418 (4)	0.0167 (3)	0.0334
O7	0.5844 (6)	0.6763 (3)	0.0311 (3)	0.0314
O6	0.4143 (6)	0.6312 (3)	0.1798 (3)	0.0362
O5	0.3399 (6)	0.4237 (3)	0.1796 (3)	0.0348
N12	0.5105 (7)	0.8216 (3)	−0.0406 (3)	0.0252
O3	0.4545 (6)	0.3366 (3)	0.0213 (3)	0.0355
O2	0.6572 (5)	0.4764 (4)	0.1192 (3)	0.0334
C9	0.3471 (8)	0.6313 (5)	0.2526 (4)	0.0306
C1	0.5013 (11)	0.1632 (5)	−0.0227 (5)	0.0436
C2	0.5272 (9)	0.2788 (4)	−0.0311 (4)	0.0282
C5	0.7465 (8)	0.4543 (6)	−0.1880 (4)	0.0418
C14	0.4951 (8)	0.8780 (5)	−0.1219 (4)	0.0332
C7	0.2846 (8)	0.4444 (5)	0.2545 (4)	0.0301
C10	0.3385 (10)	0.7358 (5)	0.2968 (5)	0.0468
C13	0.4574 (8)	0.8755 (5)	0.0370 (4)	0.0346
C3	0.6258 (8)	0.3167 (5)	−0.0958 (4)	0.0317
C6	0.2151 (10)	0.3537 (6)	0.3015 (5)	0.0446
C11	0.5672 (8)	0.7271 (5)	−0.0362 (4)	0.0281
C4	0.6485 (8)	0.4222 (5)	−0.1125 (4)	0.0285
C8	0.2893 (8)	0.5427 (6)	0.2917 (4)	0.0345
H11	0.5760	0.1253	−0.0575	0.0722*
H12	0.5141	0.1430	0.0362	0.0723*
H13	0.3957	0.1457	−0.0408	0.0722*
H51	0.7870	0.3936	−0.2169	0.0631*
H52	0.8323	0.4972	−0.1693	0.0630*
H53	0.6836	0.4927	−0.2282	0.0632*
H141	0.5252	0.8326	−0.1686	0.0489*
H142	0.5632	0.9384	−0.1217	0.0490*
H143	0.3880	0.9005	−0.1301	0.0489*
H101	0.2891	0.7275	0.3521	0.0710*
H102	0.4412	0.7646	0.3050	0.0711*
H103	0.2777	0.7834	0.2625	0.0711*
H131	0.4339	0.8253	0.0811	0.0519*
H132	0.5376	0.9225	0.0574	0.0521*
H133	0.3629	0.9147	0.0241	0.0520*
H31	0.6799	0.2689	−0.1300	0.0361*
H61	0.1856	0.3744	0.3589	0.0690*
H62	0.2904	0.2982	0.3044	0.0691*
H63	0.1241	0.3299	0.2707	0.0690*
H111	0.5975	0.6950	−0.0880	0.0352*
H81	0.2506	0.5500	0.3479	0.0403*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
U1	0.02390 (11)	0.02064 (9)	0.02030 (10)	0.00037 (7)	0.00136 (7)	−0.00082 (8)
O4	0.036 (2)	0.0261 (18)	0.0283 (18)	−0.0015 (17)	0.0082 (16)	−0.004 (2)
O1	0.030 (2)	0.037 (3)	0.033 (2)	0.009 (2)	−0.0031 (19)	−0.001 (2)
O7	0.041 (3)	0.026 (2)	0.027 (2)	−0.0032 (18)	0.0038 (19)	0.0026 (17)
O6	0.052 (3)	0.025 (2)	0.031 (2)	−0.007 (2)	0.008 (2)	−0.0069 (18)
O5	0.050 (3)	0.029 (2)	0.026 (2)	−0.009 (2)	0.016 (2)	−0.0052 (18)
N12	0.022 (3)	0.025 (2)	0.029 (2)	−0.002 (2)	−0.001 (2)	−0.0011 (17)
O3	0.050 (3)	0.025 (2)	0.031 (2)	−0.003 (2)	0.008 (2)	−0.0078 (17)
O2	0.030 (2)	0.034 (2)	0.036 (2)	−0.004 (2)	−0.0074 (17)	0.007 (2)
C9	0.035 (4)	0.030 (3)	0.027 (3)	−0.002 (3)	−0.001 (3)	−0.007 (3)
C1	0.053 (6)	0.027 (3)	0.051 (4)	−0.002 (3)	−0.004 (4)	−0.008 (3)
C2	0.031 (4)	0.020 (2)	0.034 (3)	0.002 (3)	−0.009 (3)	−0.008 (2)
C5	0.045 (4)	0.048 (4)	0.032 (4)	−0.012 (3)	0.018 (3)	−0.008 (3)
C14	0.027 (4)	0.037 (3)	0.036 (3)	−0.004 (3)	−0.006 (3)	0.005 (2)
C7	0.024 (3)	0.042 (4)	0.025 (3)	−0.005 (3)	0.002 (3)	0.003 (3)
C10	0.066 (5)	0.033 (4)	0.042 (4)	−0.004 (3)	0.006 (4)	−0.012 (3)
C13	0.031 (4)	0.033 (3)	0.040 (3)	0.001 (3)	0.008 (3)	−0.014 (3)
C3	0.035 (4)	0.032 (3)	0.028 (3)	0.006 (3)	0.007 (3)	−0.007 (2)
C6	0.063 (5)	0.041 (4)	0.030 (4)	−0.016 (4)	0.014 (3)	−0.009 (3)
C11	0.028 (4)	0.028 (3)	0.029 (3)	−0.004 (2)	0.002 (2)	−0.002 (2)
C4	0.024 (3)	0.036 (3)	0.025 (3)	−0.003 (3)	−0.002 (2)	−0.006 (3)
C8	0.040 (4)	0.042 (4)	0.022 (3)	−0.004 (3)	0.004 (3)	−0.006 (3)

Geometric parameters (Å, º)

U1—O4	2.364 (4)	C5—C4	1.501 (8)
U1—O1	1.778 (4)	C5—H51	0.962
U1—O7	2.404 (4)	C5—H52	0.962
U1—O6	2.384 (4)	C5—H53	0.960
U1—O5	2.348 (4)	C14—H141	0.965
U1—O3	2.340 (4)	C14—H142	0.968
U1—O2	1.775 (4)	C14—H143	0.970
O4—C4	1.260 (7)	C7—C6	1.495 (9)
O7—C11	1.242 (7)	C7—C8	1.386 (9)
O6—C9	1.270 (8)	C10—H101	0.964
O5—C7	1.286 (7)	C10—H102	0.962
N12—C14	1.462 (7)	C10—H103	0.964
N12—C13	1.462 (7)	C13—H131	0.962
N12—C11	1.306 (8)	C13—H132	0.967
O3—C2	1.265 (7)	C13—H133	0.972
C9—C10	1.506 (9)	C3—C4	1.390 (9)
C9—C8	1.380 (9)	C3—H31	0.934
C1—C2	1.503 (8)	C6—H61	0.965
C1—H11	0.969	C6—H62	0.960
C1—H12	0.958	C6—H63	0.964
C1—H13	0.973	C11—H111	0.940
C2—C3	1.400 (9)	C8—H81	0.939
O4—U1—O1	87.63 (17)	H51—C5—H52	109.1
O4—U1—O7	71.33 (14)	C4—C5—H53	109.6
O1—U1—O7	90.14 (19)	H51—C5—H53	108.2
O4—U1—O6	142.52 (14)	H52—C5—H53	109.5
O1—U1—O6	89.09 (19)	N12—C14—H141	109.2
O7—U1—O6	71.35 (15)	N12—C14—H142	109.8
O4—U1—O5	146.83 (14)	H141—C14—H142	108.8
O1—U1—O5	91.01 (19)	N12—C14—H143	110.2
O7—U1—O5	141.83 (14)	H141—C14—H143	109.4
O6—U1—O5	70.52 (15)	H142—C14—H143	109.4
O4—U1—O3	71.23 (14)	O5—C7—C6	115.5 (6)
O1—U1—O3	90.2 (2)	O5—C7—C8	123.7 (6)
O7—U1—O3	142.51 (15)	C6—C7—C8	120.8 (6)
O6—U1—O3	146.14 (15)	C9—C10—H101	109.3
O5—U1—O3	75.64 (15)	C9—C10—H102	110.9
O4—U1—O2	90.78 (17)	H101—C10—H102	109.0
O1—U1—O2	178.40 (19)	C9—C10—H103	109.5
O7—U1—O2	89.24 (18)	H101—C10—H103	109.1
O6—U1—O2	92.1 (2)	H102—C10—H103	109.0
O5—U1—O2	90.38 (19)	N12—C13—H131	109.7
O3—U1—O2	89.4 (2)	N12—C13—H132	110.1
U1—O4—C4	135.0 (4)	H131—C13—H132	109.3
U1—O7—C11	129.1 (4)	N12—C13—H133	109.4
U1—O6—C9	138.2 (4)	H131—C13—H133	108.6
U1—O5—C7	138.6 (4)	H132—C13—H133	109.7
C14—N12—C13	116.9 (5)	C2—C3—C4	123.7 (6)
C14—N12—C11	122.4 (5)	C2—C3—H31	118.8
C13—N12—C11	120.7 (5)	C4—C3—H31	117.5
U1—O3—C2	135.8 (4)	C7—C6—H61	110.1
O6—C9—C10	115.5 (6)	C7—C6—H62	109.3
O6—C9—C8	123.7 (6)	H61—C6—H62	109.6
C10—C9—C8	120.7 (6)	C7—C6—H63	108.9
C2—C1—H11	110.3	H61—C6—H63	109.6
C2—C1—H12	109.4	H62—C6—H63	109.4
H11—C1—H12	108.9	N12—C11—O7	125.0 (6)
C2—C1—H13	109.8	N12—C11—H111	117.7
H11—C1—H13	109.6	O7—C11—H111	117.4
H12—C1—H13	108.7	C5—C4—C3	119.3 (6)
C1—C2—O3	116.5 (6)	C5—C4—O4	115.8 (6)
C1—C2—C3	119.5 (6)	C3—C4—O4	124.9 (6)
O3—C2—C3	123.9 (5)	C7—C8—C9	125.0 (6)
C4—C5—H51	110.2	C7—C8—H81	117.9
C4—C5—H52	110.2	C9—C8—H81	117.1
O1—U1—O3—C2	111.8 (6)	O2—U1—O7—C11	141.0 (6)
O2—U1—O3—C2	−66.6 (6)	O3—U1—O7—C11	53.0 (7)
O4—U1—O3—C2	24.4 (6)	O4—U1—O7—C11	49.9 (5)
O5—U1—O3—C2	−157.2 (6)	O5—U1—O7—C11	−129.4 (5)
O6—U1—O3—C2	−159.5 (6)	O6—U1—O7—C11	−126.6 (6)
O7—U1—O3—C2	21.3 (8)	U1—O3—C2—C1	162.2 (5)
O1—U1—O4—C4	−112.9 (6)	U1—O3—C2—C3	−19.0 (11)
O2—U1—O4—C4	67.3 (6)	U1—O4—C4—C3	14.3 (10)
O3—U1—O4—C4	−21.8 (5)	U1—O4—C4—C5	−165.3 (4)
O5—U1—O4—C4	−24.6 (6)	U1—O5—C7—C6	−175.2 (5)
O6—U1—O4—C4	161.7 (5)	U1—O5—C7—C8	3.8 (11)
O7—U1—O4—C4	156.2 (6)	U1—O6—C9—C8	2.5 (11)
O1—U1—O5—C7	−93.5 (7)	U1—O6—C9—C10	−179.6 (5)
O2—U1—O5—C7	87.2 (7)	U1—O7—C11—N12	121.8 (6)
O3—U1—O5—C7	176.5 (7)	C14—N12—C11—O7	179.1 (6)
O4—U1—O5—C7	179.2 (6)	C13—N12—C11—O7	−1.6 (11)
O6—U1—O5—C7	−4.9 (6)	O3—C2—C3—C4	−3.5 (11)
O7—U1—O5—C7	−2.0 (8)	C1—C2—C3—C4	175.3 (7)
O1—U1—O6—C9	93.0 (7)	C2—C3—C4—O4	5.5 (11)
O2—U1—O6—C9	−88.0 (7)	C2—C3—C4—C5	−175.0 (6)
O3—U1—O6—C9	4.0 (8)	O5—C7—C8—C9	2.9 (11)
O4—U1—O6—C9	178.0 (6)	C6—C7—C8—C9	−178.2 (7)
O5—U1—O6—C9	1.6 (6)	C7—C8—C9—O6	−5.7 (11)
O7—U1—O6—C9	−176.5 (7)	C7—C8—C9—C10	176.5 (7)
O1—U1—O7—C11	−37.6 (6)