A novel uranium-containing coordination polymer: poly­[[aqua­(benzene-1,3,5-tri­carboxyl­ato)­dioxouranium(VI)] monohydrate]

The title compound, {[UO₂(C₉H₄O₆)(H₂O)]·H₂O}_n, is a novel material consisting of a [UO₂]²⁺ ion bonded to five O atoms, four of which are from three separate 1,3,5-tri­carboxylic acid mol­ecules, while the fifth is from a coordinated water mol­ecule. This connectivity gives rise to chains running in the [01] direction.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.012 Å
• R factor = 0.039
• wR factor = 0.071
• Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       HW2    ..  H8B      =       1.89 Ang.

Alert level C
PLAT213_ALERT_2_C Atom O3      has ADP max/min Ratio .............       3.40 prolat
PLAT213_ALERT_2_C Atom O6      has ADP max/min Ratio .............       3.40 prolat
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       3.01
PLAT320_ALERT_2_C Check Hybridisation of  C2     in Main Residue .          ?
PLAT320_ALERT_2_C Check Hybridisation of  C5     in Main Residue .          ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         12
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C5     -   C6       =       1.38 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2#    ..  O3       =       2.64 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          3
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) .       1.24 Ratio

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  10 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
   7 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
   3 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SIR92 (Altomare, 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalMaker (CrystalMaker, 2003); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I)

Crystal data

[UO2(C9H4O6)(H2O)]·H2O	Z = 2
Mr = 514.18	F(000) = 468
Triclinic, P1	Dx = 2.681 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8342 (6) Å	Cell parameters from 1478 reflections
b = 8.3781 (7) Å	θ = 2.6–24.5°
c = 10.6208 (9) Å	µ = 12.79 mm^−1
α = 70.507 (5)°	T = 293 K
β = 75.840 (5)°	Blade, yellow
γ = 87.002 (5)°	0.19 × 0.05 × 0.02 mm
V = 636.85 (9) Å^3

Data collection

Bruker APEX CCD area-detector diffractometer	2589 independent reflections
Radiation source: fine-focus sealed tube	2237 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.039
ω and φ scans	θmax = 26.4°, θmin = 2.1°
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 2002)	h = −8→9
Tmin = 0.469, Tmax = 0.774	k = −10→9
4649 measured reflections	l = −13→11

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.071	H atoms treated by a mixture of independent and constrained refinement
S = 1.18	w = 1/[σ^2(Fo^2) + (0.0071P)^2] where P = (Fo^2 + 2Fc^2)/3
2589 reflections	(Δ/σ)max = 0.001
193 parameters	Δρmax = 1.69 e Å^−3
4 restraints	Δρmin = −2.01 e Å^−3

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
U1	0.24849 (4)	0.25189 (4)	0.08559 (3)	0.02078 (11)
O1	0.4334 (8)	0.0295 (7)	0.1976 (6)	0.0297 (15)
O2	0.1934 (7)	0.0812 (8)	0.3316 (6)	0.0339 (16)
O3	−0.0131 (8)	0.3489 (8)	0.1875 (6)	0.0432 (19)
O4	0.2020 (8)	0.4606 (8)	−0.1103 (6)	0.0351 (16)
O5	0.8047 (8)	−0.5209 (9)	0.6103 (7)	0.0457 (19)
O6	0.8856 (8)	−0.3290 (9)	0.3991 (7)	0.052 (2)
H6	0.9805	−0.3751	0.4002	0.078*
O7	0.1358 (8)	0.1032 (8)	0.0503 (7)	0.0353 (16)
O8	0.4990 (8)	0.2256 (8)	−0.0875 (6)	0.0288 (15)
H8A	0.513 (12)	0.138 (8)	−0.130 (8)	0.043*
H8B	0.620 (5)	0.241 (11)	−0.087 (9)	0.043*
O9	0.3644 (8)	0.3989 (8)	0.1189 (6)	0.0317 (15)
C1	0.3807 (10)	−0.1340 (10)	0.4361 (9)	0.0235 (19)
C2	0.2544 (10)	−0.2004 (10)	0.5598 (8)	0.023 (2)
H2	0.1426	−0.1558	0.5712	0.028*
C3	0.2971 (10)	0.6665 (10)	−0.3342 (8)	0.0227 (19)
C4	0.4657 (10)	0.6026 (10)	−0.3508 (8)	0.0225 (19)
H4	0.4936	0.5124	−0.2802	0.027*
C5	0.5921 (10)	−0.3268 (11)	0.5277 (9)	0.0229 (19)
C6	0.5475 (10)	−0.1977 (10)	0.4211 (8)	0.0216 (19)
H6A	0.6310	−0.1533	0.3383	0.026*
C7	0.3328 (11)	−0.0009 (11)	0.3180 (9)	0.025 (2)
C8	0.1622 (10)	0.5880 (11)	−0.2000 (9)	0.0219 (19)
C9	0.7732 (11)	−0.4005 (12)	0.5148 (9)	0.029 (2)
OW1	0.1760 (11)	0.7387 (10)	0.0735 (11)	0.077 (3)
HW1	0.097 (14)	0.829 (12)	0.044 (14)	0.115*
HW2	0.170 (18)	0.627 (8)	0.143 (10)	0.115*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
U1	0.01561 (16)	0.01974 (17)	0.01964 (18)	0.00691 (12)	−0.00195 (12)	0.00039 (13)
O1	0.031 (3)	0.026 (3)	0.016 (3)	0.014 (3)	0.001 (3)	0.007 (3)
O2	0.024 (3)	0.040 (4)	0.026 (4)	0.016 (3)	0.000 (3)	−0.003 (3)
O3	0.028 (4)	0.051 (4)	0.024 (4)	0.026 (3)	0.011 (3)	0.007 (3)
O4	0.028 (3)	0.037 (4)	0.021 (4)	0.006 (3)	0.002 (3)	0.009 (3)
O5	0.032 (4)	0.053 (5)	0.031 (4)	0.022 (3)	−0.005 (3)	0.008 (4)
O6	0.017 (3)	0.071 (5)	0.044 (5)	0.022 (3)	0.000 (3)	0.002 (4)
O7	0.035 (4)	0.033 (4)	0.040 (4)	−0.001 (3)	−0.016 (3)	−0.009 (3)
O8	0.021 (3)	0.034 (4)	0.030 (4)	0.009 (3)	−0.003 (3)	−0.012 (3)
O9	0.037 (4)	0.033 (4)	0.024 (4)	0.006 (3)	−0.007 (3)	−0.009 (3)
C1	0.018 (4)	0.023 (5)	0.025 (5)	0.004 (4)	−0.002 (4)	−0.004 (4)
C2	0.019 (4)	0.019 (5)	0.026 (5)	0.012 (4)	−0.007 (4)	−0.002 (4)
C3	0.014 (4)	0.029 (5)	0.018 (5)	0.011 (4)	0.000 (3)	−0.003 (4)
C4	0.020 (4)	0.024 (5)	0.019 (5)	0.009 (4)	−0.003 (4)	−0.004 (4)
C5	0.014 (4)	0.027 (5)	0.025 (5)	0.006 (4)	−0.003 (4)	−0.009 (4)
C6	0.017 (4)	0.028 (5)	0.015 (5)	0.010 (4)	−0.004 (3)	−0.003 (4)
C7	0.029 (5)	0.022 (5)	0.023 (5)	0.007 (4)	−0.009 (4)	−0.004 (4)
C8	0.016 (4)	0.027 (5)	0.021 (5)	0.004 (4)	−0.007 (4)	−0.003 (4)
C9	0.017 (5)	0.034 (5)	0.028 (6)	0.007 (4)	−0.004 (4)	−0.002 (5)
OW1	0.050 (5)	0.045 (5)	0.141 (9)	0.012 (4)	−0.050 (6)	−0.020 (6)

Geometric parameters (Å, º)

U1—O9	1.741 (6)	C1—C6	1.378 (10)
U1—O7	1.750 (6)	C1—C2	1.396 (11)
U1—O3	2.315 (5)	C1—C7	1.487 (12)
U1—O4	2.323 (6)	C2—C3^ii	1.389 (11)
U1—O8	2.396 (5)	C2—H2	0.9300
U1—O1	2.463 (6)	C3—C2^iii	1.389 (11)
U1—O2	2.465 (6)	C3—C4	1.393 (10)
U1—C7	2.859 (9)	C3—C8	1.514 (11)
O1—C7	1.277 (9)	C4—C5^iii	1.387 (11)
O2—C7	1.264 (9)	C4—H4	0.9300
O3—C8^i	1.252 (9)	C5—C6	1.382 (11)
O4—C8	1.255 (10)	C5—C4^ii	1.387 (11)
O5—C9	1.233 (10)	C5—C9	1.511 (11)
O6—C9	1.296 (10)	C6—H6A	0.9300
O6—H6	0.8200	C8—O3^i	1.252 (9)
O8—H8A	0.97 (7)	OW1—HW1	0.97 (11)
O8—H8B	0.97 (5)	OW1—HW2	0.97 (9)
O9—U1—O7	178.9 (3)	U1—O8—H8B	125 (5)
O9—U1—O3	89.5 (3)	H8A—O8—H8B	100 (7)
O7—U1—O3	91.6 (3)	C6—C1—C2	120.0 (8)
O9—U1—O4	89.9 (3)	C6—C1—C7	119.9 (7)
O7—U1—O4	90.1 (3)	C2—C1—C7	120.0 (7)
O3—U1—O4	82.2 (2)	C3^ii—C2—C1	119.4 (7)
O9—U1—O8	90.6 (2)	C3^ii—C2—H2	120.3
O7—U1—O8	88.3 (3)	C1—C2—H2	120.3
O3—U1—O8	160.3 (2)	C2^iii—C3—C4	120.1 (7)
O4—U1—O8	78.0 (2)	C2^iii—C3—C8	121.0 (7)
O9—U1—O1	88.6 (3)	C4—C3—C8	118.9 (7)
O7—U1—O1	90.9 (2)	C5^iii—C4—C3	120.0 (8)
O3—U1—O1	127.8 (2)	C5^iii—C4—H4	120.0
O4—U1—O1	149.88 (19)	C3—C4—H4	120.0
O8—U1—O1	71.89 (19)	C6—C5—C4^ii	119.6 (7)
O9—U1—O2	88.3 (2)	C6—C5—C9	122.3 (7)
O7—U1—O2	92.1 (3)	C4^ii—C5—C9	118.1 (8)
O3—U1—O2	75.2 (2)	C1—C6—C5	120.8 (8)
O4—U1—O2	157.42 (19)	C1—C6—H6A	119.6
O8—U1—O2	124.5 (2)	C5—C6—H6A	119.6
O1—U1—O2	52.59 (18)	O2—C7—O1	118.4 (8)
O9—U1—C7	88.0 (3)	O2—C7—C1	122.4 (8)
O7—U1—C7	92.0 (3)	O1—C7—C1	119.2 (7)
O3—U1—C7	101.4 (2)	O2—C7—U1	59.3 (4)
O4—U1—C7	175.8 (2)	O1—C7—U1	59.2 (4)
O8—U1—C7	98.3 (2)	C1—C7—U1	178.3 (6)
O1—U1—C7	26.4 (2)	O3^i—C8—O4	123.6 (8)
O2—U1—C7	26.1 (2)	O3^i—C8—C3	117.2 (7)
C7—O1—U1	94.4 (5)	O4—C8—C3	119.1 (7)
C7—O2—U1	94.6 (5)	O5—C9—O6	124.8 (8)
C8^i—O3—U1	159.3 (6)	O5—C9—C5	120.0 (8)
C8—O4—U1	168.7 (6)	O6—C9—C5	115.2 (8)
C9—O6—H6	109.5	HW1—OW1—HW2	139 (10)
U1—O8—H8A	126 (5)

Symmetry codes: (i) −x, −y+1, −z; (ii) x, y−1, z+1; (iii) x, y+1, z−1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O1^iv	0.97 (7)	1.77 (7)	2.732 (8)	172 (9)
O8—H8B···OW1^v	0.97 (5)	1.66 (5)	2.624 (10)	176 (9)
O6—H6···O5^vi	0.82	1.85	2.669 (8)	176
OW1—HW1···O7^i	0.97 (11)	2.25 (8)	3.086 (10)	144 (11)
OW1—HW1···O7^vii	0.97 (11)	2.36 (11)	2.987 (10)	122 (10)
OW1—HW2···O9	0.97 (9)	2.42 (11)	3.083 (10)	125 (10)
OW1—HW2···O5^viii	0.97 (9)	2.53 (10)	3.280 (12)	134 (10)
OW1—HW2···O3	0.97 (9)	2.64 (10)	3.363 (11)	131 (10)

Symmetry codes: (i) −x, −y+1, −z; (iv) −x+1, −y, −z; (v) −x+1, −y+1, −z; (vi) −x+2, −y−1, −z+1; (vii) x, y+1, z; (viii) −x+1, −y, −z+1.