Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807011877/br2033sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807011877/br2033Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (u-O) = 0.002 Å
- R factor = 0.021
- wR factor = 0.044
- Data-to-parameter ratio = 59.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.94 PLAT731_ALERT_1_C Bond Calc 0.81(4), Rep 0.809(19) ...... 2.11 su-Ra O3 -H3 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.853(19) ...... 2.11 su-Ra O4 -H4B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.81(4), Rep 0.809(19) ...... 2.11 su-Ra O3 -H3 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.853(19) ...... 2.11 su-Ra O4 -H4B 1.555 1.555
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.938 Tmax scaled 0.548 Tmin scaled 0.352 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 6 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
Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL97 (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL97.
Cs3[PuO4(OH)2]·3H2O | F(000) = 1356 |
Mr = 789.84 | Dx = 4.539 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 9469 reflections |
a = 12.5381 (3) Å | θ = 2.4–45.0° |
b = 11.4983 (3) Å | µ = 15.03 mm−1 |
c = 8.0195 (2) Å | T = 293 K |
β = 91.3913 (12)° | Fragment, black |
V = 1155.81 (5) Å3 | 0.16 × 0.06 × 0.04 mm |
Z = 4 |
Bruker KAPPA APEX II area-detector diffractometer | 4717 independent reflections |
Radiation source: fine-focus sealed tube | 4033 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ω and φ scans | θmax = 45.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→24 |
Tmin = 0.375, Tmax = 0.585 | k = −22→22 |
23677 measured reflections | l = −15→15 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | All H-atom parameters refined |
wR(F2) = 0.044 | w = 1/[σ2(Fo2) + (0.0176P)2 + 0.383P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.005 |
4717 reflections | Δρmax = 2.11 e Å−3 |
79 parameters | Δρmin = −2.64 e Å−3 |
4 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.01490 (16) |
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 | ||
Pu | 0.2500 | 0.2500 | 0.5000 | 0.01243 (2) | |
Cs1 | 0.301977 (9) | 0.089341 (10) | 0.048753 (16) | 0.02221 (3) | |
Cs2 | 0.0000 | 0.066558 (18) | 0.7500 | 0.02884 (4) | |
O1 | 0.18708 (13) | 0.12102 (12) | 0.3899 (2) | 0.0240 (3) | |
O2 | 0.22676 (14) | 0.18090 (15) | 0.7068 (2) | 0.0269 (3) | |
O3 | 0.42108 (12) | 0.16183 (14) | 0.4997 (2) | 0.0258 (3) | |
H3 | 0.428 (4) | 0.118 (4) | 0.422 (5) | 0.060 (14)* | |
O4 | 0.57271 (14) | 0.31917 (16) | 0.5833 (2) | 0.0286 (3) | |
H4A | 0.590 (3) | 0.315 (3) | 0.685 (3) | 0.041 (10)* | |
H4B | 0.523 (3) | 0.269 (3) | 0.572 (7) | 0.048 (12)* | |
O5 | 0.5000 | 0.0278 (2) | 0.7500 | 0.0329 (5) | |
H5 | 0.474 (3) | 0.074 (3) | 0.679 (4) | 0.036 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pu | 0.01262 (4) | 0.01308 (3) | 0.01151 (3) | −0.00042 (2) | −0.00173 (2) | 0.00081 (2) |
Cs1 | 0.02266 (5) | 0.02072 (5) | 0.02318 (5) | 0.00302 (3) | −0.00102 (4) | −0.00047 (4) |
Cs2 | 0.03000 (9) | 0.03006 (8) | 0.02623 (8) | 0.000 | −0.00439 (7) | 0.000 |
O1 | 0.0254 (7) | 0.0191 (5) | 0.0271 (7) | −0.0027 (4) | −0.0056 (5) | −0.0043 (5) |
O2 | 0.0302 (8) | 0.0316 (7) | 0.0188 (6) | −0.0026 (5) | 0.0006 (5) | 0.0087 (5) |
O3 | 0.0183 (6) | 0.0270 (6) | 0.0319 (8) | 0.0048 (5) | −0.0028 (5) | −0.0047 (6) |
O4 | 0.0229 (7) | 0.0373 (8) | 0.0253 (7) | −0.0058 (6) | −0.0024 (6) | 0.0037 (6) |
O5 | 0.0420 (14) | 0.0241 (10) | 0.0319 (12) | 0.000 | −0.0126 (11) | 0.000 |
Pu—O1i | 1.8889 (14) | Cs2—O2xi | 3.1590 (16) |
Pu—O1 | 1.8889 (14) | Cs2—O4xii | 3.282 (2) |
Pu—O2 | 1.8685 (15) | Cs2—O4xiii | 3.282 (2) |
Pu—O2i | 1.8685 (16) | Cs2—O1xiv | 3.3592 (14) |
Pu—O3 | 2.3726 (15) | Cs2—O1ii | 3.3592 (14) |
Pu—O3i | 2.3726 (15) | Cs2—Cs2xv | 4.2920 (2) |
Pu—Cs1ii | 3.9736 (2) | Cs2—Cs2xiv | 4.2920 (2) |
Pu—Cs1iii | 3.9736 (2) | Cs2—Puxi | 4.3127 (1) |
Pu—Cs1i | 4.1288 (2) | O1—Cs1ii | 3.0757 (16) |
Pu—Cs1 | 4.1288 (2) | O1—Cs2xiv | 3.3592 (14) |
Pu—Cs2 | 4.3127 (1) | O2—Cs1xvi | 3.0644 (16) |
Pu—Cs2i | 4.3127 (1) | O2—Cs1i | 3.3143 (18) |
Cs1—O2iv | 3.0644 (16) | O2—Cs1ii | 3.4944 (18) |
Cs1—O1v | 3.0757 (16) | O3—Cs1ii | 3.2794 (17) |
Cs1—O4vi | 3.0798 (17) | O3—Cs1viii | 3.6011 (15) |
Cs1—O1 | 3.1437 (18) | O3—H3 | 0.809 (19) |
Cs1—O5vii | 3.2232 (10) | O4—Cs1xvii | 3.0798 (17) |
Cs1—O4viii | 3.264 (2) | O4—Cs2i | 3.0958 (19) |
Cs1—O3v | 3.2794 (17) | O4—Cs1viii | 3.264 (2) |
Cs1—O2i | 3.3143 (18) | O4—Cs2xviii | 3.282 (2) |
Cs1—O2v | 3.4944 (18) | O4—H4A | 0.839 (19) |
Cs1—O5iv | 3.5629 (5) | O4—H4B | 0.853 (19) |
Cs1—O3viii | 3.6011 (15) | O5—Cs1ii | 3.2232 (10) |
Cs1—Puix | 3.9736 (2) | O5—Cs1vii | 3.2232 (10) |
Cs1—H3 | 3.37 (4) | O5—Cs1xvi | 3.5629 (5) |
Cs2—O4x | 3.0958 (19) | O5—Cs1viii | 3.5629 (5) |
Cs2—O4i | 3.0958 (19) | O5—H5 | 0.844 (18) |
Cs2—O2 | 3.1590 (17) | ||
O2—Pu—O2i | 180.0 | O2i—Cs1—O2v | 117.392 (8) |
O1—Pu—O2i | 89.49 (8) | O2iv—Cs1—O5iv | 70.79 (4) |
O2i—Pu—O1i | 90.51 (8) | O1v—Cs1—O5iv | 83.82 (4) |
O1—Pu—O2 | 90.51 (8) | O4vi—Cs1—O5iv | 142.70 (4) |
O1—Pu—O3 | 91.79 (6) | O1—Cs1—O5iv | 161.75 (3) |
O2i—Pu—O1 | 89.49 (8) | O5vii—Cs1—O5iv | 73.311 (12) |
O1i—Pu—O1 | 180.00 (5) | O4viii—Cs1—O5iv | 66.03 (5) |
O2—Pu—O3 | 88.84 (7) | O3v—Cs1—O5iv | 54.38 (5) |
O2i—Pu—O3 | 91.16 (7) | O2i—Cs1—O5iv | 130.05 (4) |
O1i—Pu—O3 | 88.21 (6) | O2v—Cs1—O5iv | 105.43 (5) |
O2—Pu—O3i | 91.16 (7) | O2iv—Cs1—O3viii | 95.78 (4) |
O2i—Pu—O3i | 88.84 (7) | O1v—Cs1—O3viii | 125.49 (4) |
O1i—Pu—O3i | 91.79 (6) | O4vi—Cs1—O3viii | 146.63 (4) |
O1—Pu—O3i | 88.21 (6) | O1—Cs1—O3viii | 122.03 (4) |
O3—Pu—O3i | 180.0 | O5vii—Cs1—O3viii | 54.38 (4) |
O2iv—Cs1—O1v | 76.62 (4) | O4viii—Cs1—O3viii | 45.94 (4) |
O2iv—Cs1—O4vi | 72.27 (5) | O3v—Cs1—O3viii | 75.39 (4) |
O1v—Cs1—O4vi | 82.94 (5) | O2i—Cs1—O3viii | 89.90 (4) |
O2iv—Cs1—O1 | 126.96 (4) | O2v—Cs1—O3viii | 120.96 (4) |
O1v—Cs1—O1 | 103.40 (5) | O5iv—Cs1—O3viii | 44.27 (4) |
O4vi—Cs1—O1 | 55.51 (5) | O4x—Cs2—O4i | 129.77 (7) |
O2iv—Cs1—O5vii | 143.92 (3) | O4x—Cs2—O2 | 70.79 (5) |
O1v—Cs1—O5vii | 103.07 (5) | O4i—Cs2—O2 | 88.61 (4) |
O4vi—Cs1—O5vii | 143.80 (4) | O4x—Cs2—O2xi | 88.61 (4) |
O1—Cs1—O5vii | 88.65 (3) | O4i—Cs2—O2xi | 70.79 (5) |
O2iv—Cs1—O4viii | 64.64 (4) | O2—Cs2—O2xi | 130.81 (6) |
O1v—Cs1—O4viii | 136.60 (5) | O4x—Cs2—O4xii | 95.46 (5) |
O4vi—Cs1—O4viii | 102.14 (4) | O4i—Cs2—O4xii | 129.85 (5) |
O1—Cs1—O4viii | 115.02 (4) | O2—Cs2—O4xii | 131.69 (4) |
O5vii—Cs1—O4viii | 97.46 (5) | O2xi—Cs2—O4xii | 93.24 (4) |
O2iv—Cs1—O3v | 109.04 (5) | O4x—Cs2—O4xiii | 129.85 (5) |
O1v—Cs1—O3v | 57.84 (4) | O4i—Cs2—O4xiii | 95.46 (5) |
O4vi—Cs1—O3v | 137.76 (4) | O2—Cs2—O4xiii | 93.24 (4) |
O1—Cs1—O3v | 115.22 (4) | O2xi—Cs2—O4xiii | 131.69 (4) |
O5vii—Cs1—O3v | 49.05 (5) | O4xii—Cs2—O4xiii | 59.82 (6) |
O4viii—Cs1—O3v | 116.73 (4) | O4x—Cs2—O1xiv | 138.54 (5) |
O2iv—Cs1—O2i | 102.70 (4) | O4i—Cs2—O1xiv | 78.21 (4) |
O1v—Cs1—O2i | 144.61 (4) | O2—Cs2—O1xiv | 148.61 (4) |
O4vi—Cs1—O2i | 63.86 (4) | O2xi—Cs2—O1xiv | 71.38 (4) |
O1—Cs1—O2i | 48.27 (4) | O4xii—Cs2—O1xiv | 51.75 (4) |
O5vii—Cs1—O2i | 97.50 (4) | O4xiii—Cs2—O1xiv | 60.40 (4) |
O4viii—Cs1—O2i | 66.84 (4) | O4x—Cs2—O1ii | 78.21 (4) |
O3v—Cs1—O2i | 146.03 (4) | O4i—Cs2—O1ii | 138.54 (5) |
O2iv—Cs1—O2v | 123.38 (5) | O2—Cs2—O1ii | 71.38 (4) |
O1v—Cs1—O2v | 47.40 (4) | O2xi—Cs2—O1ii | 148.61 (4) |
O4vi—Cs1—O2v | 90.60 (4) | O4xii—Cs2—O1ii | 60.40 (4) |
O1—Cs1—O2v | 69.75 (4) | O4xiii—Cs2—O1ii | 51.75 (4) |
O5vii—Cs1—O2v | 70.01 (4) | O1xiv—Cs2—O1ii | 100.11 (5) |
O4viii—Cs1—O2v | 166.89 (4) | Pu—O3—H3 | 112 (4) |
O3v—Cs1—O2v | 52.28 (4) | H4A—O4—H4B | 103 (5) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) x, −y, z+1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, y, z−1; (v) x, −y, z−1/2; (vi) x−1/2, −y+1/2, z−1/2; (vii) −x+1, −y, −z+1; (viii) −x+1, y, −z+1/2; (ix) −x+1/2, y−1/2, −z+1/2; (x) x−1/2, −y+1/2, z+1/2; (xi) −x, y, −z+3/2; (xii) −x+1/2, y−1/2, −z+3/2; (xiii) x−1/2, y−1/2, z; (xiv) −x, −y, −z+1; (xv) −x, −y, −z+2; (xvi) x, y, z+1; (xvii) x+1/2, −y+1/2, z+1/2; (xviii) x+1/2, y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O5vii | 0.81 (2) | 2.36 (2) | 3.137 (2) | 161 (5) |
O4—H4A···O1xvii | 0.84 (2) | 2.16 (3) | 2.899 (3) | 148 (4) |
O4—H4B···O3 | 0.85 (2) | 1.86 (2) | 2.697 (2) | 168 (6) |
O5—H5···O3 | 0.84 (2) | 1.86 (2) | 2.700 (2) | 172 (4) |
Symmetry codes: (vii) −x+1, −y, −z+1; (xvii) x+1/2, −y+1/2, z+1/2. |