Sodium penta­fluoro­uranate(IV) monohydrate, Na[UF₅]·H₂O

Na[UF₅]·H₂O crystallizes in the orthorhombic space group Pbcn. It contains a uranium(IV) ion, which is coordinated by nine F^- ions yielding a tricapped trigonal prism. Some of the F^- ions function as bridging ligands coordinating to the Na⁺ ion. The latter is coordinated by four F^- ions. Together with two mol­ecules of water of crystallization, a distorted octahedral coordination around Na⁺ is obtained.

Key indicators

• Single-crystal X-ray study
• T = 299 K
• Mean [sigma](U-F) = 0.004 Å
• H-atom completeness 51%
• R factor = 0.023
• wR factor = 0.047
• Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......         O1

Alert level B
CHEMS01_ALERT_1_B  The sum formula contains elements in the wrong order.
            H  precedes F
            Sequence must be C, H, then alphabetical.

Alert level C
CRYSC01_ALERT_1_C The word below has not been recognised as a standard
            identifier.
            Emerald
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.31
PLAT431_ALERT_2_C Short Inter HL..A Contact  F1     ..  O1       =       2.97 Ang.

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:H2 F5 Na1 O1 U1
            Atom count from the _atom_site data:  H1 F5 Na1 O1 U1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    8
           From the CIF: _chemical_formula_sum  H2 F5 Na O U
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           H         16.00      8.00    8.00
           F         40.00     40.00    0.00
           Na         8.00      8.00    0.00
           O          8.00      8.00    0.00
           U          8.00      8.00    0.00

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

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: KappaCCD; cell refinement: DIRAX (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: maXus (Mackay et al., 1999).

Sodium pentafluorouranate(IV) monohydrate

Crystal data

Na[UF5]·H2O	Dx = 5.391 Mg m^−3
Mr = 374.03	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbcn	Cell parameters from 100 reflections
Hall symbol: -P 2n 2ab	θ = 4.0–21.0°
a = 6.9928 (6) Å	µ = 35.33 mm^−1
b = 8.7617 (4) Å	T = 299 K
c = 15.0426 (10) Å	Plate, emerald green
V = 921.64 (11) Å^3	0.12 × 0.10 × 0.01 mm
Z = 8

Data collection

Bruker–Nonius KappaCCD diffractometer	1175 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.036
φ and ω scans	θmax = 30.0°, θmin = 4.5°
Absorption correction: numerical (HABITUS; Herrendorf & Bärnighausen, 1997)	h = −9→9
Tmin = 0.023, Tmax = 0.820	k = −12→12
13694 measured reflections	l = −20→21
1341 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)] = 0.023	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.048	w = 1/[σ^2(Fo^2) + 17.16P] where P = (Fo^2 + 2Fc^2)/3
S = 1.25	(Δ/σ)max < 0.001
1341 reflections	Δρmax = 4.05 e Å^−3
74 parameters	Δρmin = −1.75 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
U	0.16400 (3)	0.33118 (2)	0.460431 (14)	0.00697 (7)
Na	0.2954 (5)	0.3599 (4)	0.1842 (2)	0.0276 (7)
F1	0.1533 (6)	0.3346 (5)	0.3172 (3)	0.0201 (8)
F2	−0.0123 (5)	0.2010 (4)	0.5733 (3)	0.0123 (7)
F3	0.3629 (5)	0.2856 (4)	0.5803 (2)	0.0114 (7)
F4	−0.0845 (5)	0.5037 (4)	0.4236 (2)	0.0132 (7)
F5	0.2092 (5)	0.0735 (4)	0.4332 (3)	0.0171 (9)
O1	0.5000	0.5396 (8)	0.2500	0.0254 (17)
O2	0.5000	0.1554 (9)	0.2500	0.0302 (18)
H2	0.5566	0.1008	0.2095	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
U	0.00621 (10)	0.00549 (9)	0.00921 (11)	0.00049 (8)	−0.00006 (8)	0.00000 (8)
Na	0.0260 (17)	0.0412 (19)	0.0157 (15)	−0.0057 (15)	−0.0002 (12)	−0.0090 (13)
F1	0.020 (2)	0.028 (2)	0.0128 (19)	0.001 (2)	−0.0004 (16)	−0.0008 (17)
F2	0.0103 (17)	0.0117 (16)	0.0150 (18)	−0.0012 (15)	−0.0014 (15)	0.0020 (14)
F3	0.0105 (17)	0.0136 (16)	0.0102 (18)	0.0019 (15)	0.0001 (14)	0.0008 (14)
F4	0.0156 (18)	0.0112 (16)	0.0126 (18)	0.0014 (16)	−0.0038 (15)	−0.0038 (16)
F5	0.016 (2)	0.0043 (15)	0.031 (2)	0.0018 (15)	−0.0033 (16)	0.0002 (16)
O1	0.029 (4)	0.017 (3)	0.030 (4)	0.000	0.000 (4)	0.000
O2	0.042 (5)	0.029 (4)	0.019 (4)	0.000	0.009 (4)	0.000

Geometric parameters (Å, º)

U—F1	2.157 (4)	Na—O2	2.498 (7)
U—F3	2.312 (4)	Na—F4^vi	2.528 (5)
U—F5	2.317 (4)	Na—Na^viii	3.481 (6)
U—F4^i	2.333 (4)	Na—U^vii	3.770 (3)
U—F2^ii	2.337 (4)	Na—U^vi	3.888 (3)
U—F5^iii	2.337 (4)	F2—Na^v	2.317 (5)
U—F4	2.369 (4)	F2—U^iv	2.337 (4)
U—F2	2.389 (4)	F3—Na^v	2.300 (5)
U—F3^iv	2.420 (4)	F3—U^ii	2.420 (4)
U—Na^v	3.770 (3)	F4—U^i	2.333 (4)
U—Na^vi	3.888 (3)	F4—Na^vi	2.528 (5)
U—U^i	3.9282 (4)	F5—U^ix	2.337 (4)
Na—F1	2.245 (5)	O1—Na^viii	2.347 (6)
Na—F3^vii	2.300 (5)	O2—Na^viii	2.498 (7)
Na—F2^vii	2.317 (5)	O2—H2	0.8703
Na—O1	2.347 (6)
F1—U—F3	143.38 (15)	F2^ii—U—U^i	136.24 (9)
F1—U—F5	80.89 (16)	F5^iii—U—U^i	65.83 (10)
F3—U—F5	83.53 (14)	F4—U—U^i	33.06 (9)
F1—U—F4^i	136.89 (15)	F2—U—U^i	80.96 (9)
F3—U—F4^i	70.59 (13)	F3^iv—U—U^i	83.51 (9)
F5—U—F4^i	140.28 (15)	Na^v—U—U^i	96.19 (5)
F1—U—F2^ii	79.52 (15)	Na^vi—U—U^i	68.80 (5)
F3—U—F2^ii	64.27 (13)	F1—Na—F3^vii	109.8 (2)
F5—U—F2^ii	73.26 (13)	F1—Na—F2^vii	155.3 (2)
F4^i—U—F2^ii	117.90 (13)	F3^vii—Na—F2^vii	72.45 (16)
F1—U—F5^iii	79.94 (16)	F1—Na—O1	87.70 (15)
F3—U—F5^iii	93.75 (14)	F3^vii—Na—O1	162.13 (19)
F5—U—F5^iii	143.40 (12)	F2^vii—Na—O1	93.37 (15)
F4^i—U—F5^iii	70.00 (14)	F1—Na—O2	80.18 (16)
F2^ii—U—F5^iii	72.78 (13)	F3^vii—Na—O2	98.5 (2)
F1—U—F4	74.47 (15)	F2^vii—Na—O2	75.23 (14)
F3—U—F4	137.21 (13)	O1—Na—O2	88.0 (2)
F5—U—F4	132.90 (13)	F1—Na—F4^vi	111.27 (19)
F4^i—U—F4	66.68 (15)	F3^vii—Na—F4^vi	63.88 (15)
F2^ii—U—F4	137.46 (13)	F2^vii—Na—F4^vi	92.00 (17)
F5^iii—U—F4	69.99 (13)	O1—Na—F4^vi	107.0 (2)
F1—U—F2	134.36 (15)	O2—Na—F4^vi	161.1 (2)
F3—U—F2	70.95 (13)	F1—Na—Na^viii	81.76 (16)
F5—U—F2	74.37 (14)	F3^vii—Na—Na^viii	141.46 (14)
F4^i—U—F2	69.01 (13)	F2^vii—Na—Na^viii	82.59 (15)
F2^ii—U—F2	126.65 (10)	O1—Na—Na^viii	42.13 (15)
F5^iii—U—F2	138.97 (14)	O2—Na—Na^viii	45.83 (15)
F4—U—F2	95.29 (13)	F4^vi—Na—Na^viii	147.63 (13)
F1—U—F3^iv	73.91 (14)	F1—Na—U^vii	141.75 (17)
F3—U—F3^iv	130.38 (7)	F3^vii—Na—U^vii	35.28 (10)
F5—U—F3^iv	70.24 (13)	F2^vii—Na—U^vii	37.42 (10)
F4^i—U—F3^iv	104.12 (13)	O1—Na—U^vii	128.96 (11)
F2^ii—U—F3^iv	137.47 (13)	O2—Na—U^vii	89.56 (12)
F5^iii—U—F3^iv	132.06 (13)	F4^vi—Na—U^vii	72.10 (11)
F4—U—F3^iv	64.67 (13)	Na^viii—Na—U^vii	116.49 (12)
F2—U—F3^iv	61.89 (13)	F1—Na—U^vi	97.28 (14)
F1—U—Na^v	154.29 (14)	F3^vii—Na—U^vi	35.57 (10)
F3—U—Na^v	35.08 (10)	F2^vii—Na—U^vi	97.10 (13)
F5—U—Na^v	73.42 (12)	O1—Na—U^vi	141.57 (18)
F4^i—U—Na^v	68.04 (11)	O2—Na—U^vi	130.46 (18)
F2^ii—U—Na^v	93.86 (10)	F4^vi—Na—U^vi	36.04 (10)
F5^iii—U—Na^v	122.10 (12)	Na^viii—Na—U^vi	176.25 (6)
F4—U—Na^v	123.18 (11)	U^vii—Na—U^vi	62.23 (5)
F2—U—Na^v	36.11 (10)	U—F1—Na	151.3 (2)
F3^iv—U—Na^v	95.96 (10)	Na^v—F2—U^iv	139.73 (19)
F1—U—Na^vi	53.94 (12)	Na^v—F2—U	106.47 (16)
F3—U—Na^vi	160.85 (10)	U^iv—F2—U	113.78 (15)
F5—U—Na^vi	94.41 (11)	Na^v—F3—U	109.64 (17)
F4^i—U—Na^vi	100.44 (10)	Na^v—F3—U^ii	110.87 (17)
F2^ii—U—Na^vi	133.36 (11)	U—F3—U^ii	113.53 (15)
F5^iii—U—Na^vi	99.01 (11)	U^i—F4—U	113.32 (15)
F4—U—Na^vi	38.90 (10)	U^i—F4—Na^vi	130.51 (17)
F2—U—Na^vi	90.12 (10)	U—F4—Na^vi	105.06 (16)
F3^iv—U—Na^vi	33.56 (10)	U—F5—U^ix	155.0 (2)
Na^v—U—Na^vi	126.20 (8)	Na^viii—O1—Na	95.7 (3)
F1—U—U^i	105.79 (12)	Na^viii—O2—Na	88.3 (3)
F3—U—U^i	104.19 (9)	Na^viii—O2—H2	114.3
F5—U—U^i	150.15 (10)	Na—O2—H2	112.2
F4^i—U—U^i	33.63 (9)

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