Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804003241/wm6010sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804003241/wm6010Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 299 K
- Mean (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
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).
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) Å3 | 0.12 × 0.10 × 0.01 mm |
Z = 8 |
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 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)] = 0.023 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.048 | w = 1/[σ2(Fo2) + 17.16P] where P = (Fo2 + 2Fc2)/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 |
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. |
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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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 |
U—F1 | 2.157 (4) | Na—O2 | 2.498 (7) |
U—F3 | 2.312 (4) | Na—F4vi | 2.528 (5) |
U—F5 | 2.317 (4) | Na—Naviii | 3.481 (6) |
U—F4i | 2.333 (4) | Na—Uvii | 3.770 (3) |
U—F2ii | 2.337 (4) | Na—Uvi | 3.888 (3) |
U—F5iii | 2.337 (4) | F2—Nav | 2.317 (5) |
U—F4 | 2.369 (4) | F2—Uiv | 2.337 (4) |
U—F2 | 2.389 (4) | F3—Nav | 2.300 (5) |
U—F3iv | 2.420 (4) | F3—Uii | 2.420 (4) |
U—Nav | 3.770 (3) | F4—Ui | 2.333 (4) |
U—Navi | 3.888 (3) | F4—Navi | 2.528 (5) |
U—Ui | 3.9282 (4) | F5—Uix | 2.337 (4) |
Na—F1 | 2.245 (5) | O1—Naviii | 2.347 (6) |
Na—F3vii | 2.300 (5) | O2—Naviii | 2.498 (7) |
Na—F2vii | 2.317 (5) | O2—H2 | 0.8703 |
Na—O1 | 2.347 (6) | ||
F1—U—F3 | 143.38 (15) | F2ii—U—Ui | 136.24 (9) |
F1—U—F5 | 80.89 (16) | F5iii—U—Ui | 65.83 (10) |
F3—U—F5 | 83.53 (14) | F4—U—Ui | 33.06 (9) |
F1—U—F4i | 136.89 (15) | F2—U—Ui | 80.96 (9) |
F3—U—F4i | 70.59 (13) | F3iv—U—Ui | 83.51 (9) |
F5—U—F4i | 140.28 (15) | Nav—U—Ui | 96.19 (5) |
F1—U—F2ii | 79.52 (15) | Navi—U—Ui | 68.80 (5) |
F3—U—F2ii | 64.27 (13) | F1—Na—F3vii | 109.8 (2) |
F5—U—F2ii | 73.26 (13) | F1—Na—F2vii | 155.3 (2) |
F4i—U—F2ii | 117.90 (13) | F3vii—Na—F2vii | 72.45 (16) |
F1—U—F5iii | 79.94 (16) | F1—Na—O1 | 87.70 (15) |
F3—U—F5iii | 93.75 (14) | F3vii—Na—O1 | 162.13 (19) |
F5—U—F5iii | 143.40 (12) | F2vii—Na—O1 | 93.37 (15) |
F4i—U—F5iii | 70.00 (14) | F1—Na—O2 | 80.18 (16) |
F2ii—U—F5iii | 72.78 (13) | F3vii—Na—O2 | 98.5 (2) |
F1—U—F4 | 74.47 (15) | F2vii—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—F4vi | 111.27 (19) |
F4i—U—F4 | 66.68 (15) | F3vii—Na—F4vi | 63.88 (15) |
F2ii—U—F4 | 137.46 (13) | F2vii—Na—F4vi | 92.00 (17) |
F5iii—U—F4 | 69.99 (13) | O1—Na—F4vi | 107.0 (2) |
F1—U—F2 | 134.36 (15) | O2—Na—F4vi | 161.1 (2) |
F3—U—F2 | 70.95 (13) | F1—Na—Naviii | 81.76 (16) |
F5—U—F2 | 74.37 (14) | F3vii—Na—Naviii | 141.46 (14) |
F4i—U—F2 | 69.01 (13) | F2vii—Na—Naviii | 82.59 (15) |
F2ii—U—F2 | 126.65 (10) | O1—Na—Naviii | 42.13 (15) |
F5iii—U—F2 | 138.97 (14) | O2—Na—Naviii | 45.83 (15) |
F4—U—F2 | 95.29 (13) | F4vi—Na—Naviii | 147.63 (13) |
F1—U—F3iv | 73.91 (14) | F1—Na—Uvii | 141.75 (17) |
F3—U—F3iv | 130.38 (7) | F3vii—Na—Uvii | 35.28 (10) |
F5—U—F3iv | 70.24 (13) | F2vii—Na—Uvii | 37.42 (10) |
F4i—U—F3iv | 104.12 (13) | O1—Na—Uvii | 128.96 (11) |
F2ii—U—F3iv | 137.47 (13) | O2—Na—Uvii | 89.56 (12) |
F5iii—U—F3iv | 132.06 (13) | F4vi—Na—Uvii | 72.10 (11) |
F4—U—F3iv | 64.67 (13) | Naviii—Na—Uvii | 116.49 (12) |
F2—U—F3iv | 61.89 (13) | F1—Na—Uvi | 97.28 (14) |
F1—U—Nav | 154.29 (14) | F3vii—Na—Uvi | 35.57 (10) |
F3—U—Nav | 35.08 (10) | F2vii—Na—Uvi | 97.10 (13) |
F5—U—Nav | 73.42 (12) | O1—Na—Uvi | 141.57 (18) |
F4i—U—Nav | 68.04 (11) | O2—Na—Uvi | 130.46 (18) |
F2ii—U—Nav | 93.86 (10) | F4vi—Na—Uvi | 36.04 (10) |
F5iii—U—Nav | 122.10 (12) | Naviii—Na—Uvi | 176.25 (6) |
F4—U—Nav | 123.18 (11) | Uvii—Na—Uvi | 62.23 (5) |
F2—U—Nav | 36.11 (10) | U—F1—Na | 151.3 (2) |
F3iv—U—Nav | 95.96 (10) | Nav—F2—Uiv | 139.73 (19) |
F1—U—Navi | 53.94 (12) | Nav—F2—U | 106.47 (16) |
F3—U—Navi | 160.85 (10) | Uiv—F2—U | 113.78 (15) |
F5—U—Navi | 94.41 (11) | Nav—F3—U | 109.64 (17) |
F4i—U—Navi | 100.44 (10) | Nav—F3—Uii | 110.87 (17) |
F2ii—U—Navi | 133.36 (11) | U—F3—Uii | 113.53 (15) |
F5iii—U—Navi | 99.01 (11) | Ui—F4—U | 113.32 (15) |
F4—U—Navi | 38.90 (10) | Ui—F4—Navi | 130.51 (17) |
F2—U—Navi | 90.12 (10) | U—F4—Navi | 105.06 (16) |
F3iv—U—Navi | 33.56 (10) | U—F5—Uix | 155.0 (2) |
Nav—U—Navi | 126.20 (8) | Naviii—O1—Na | 95.7 (3) |
F1—U—Ui | 105.79 (12) | Naviii—O2—Na | 88.3 (3) |
F3—U—Ui | 104.19 (9) | Naviii—O2—H2 | 114.3 |
F5—U—Ui | 150.15 (10) | Na—O2—H2 | 112.2 |
F4i—U—Ui | 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. |
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