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The title compound, Cs3[PuO4(OH)2]·3H2O, contains centrosymmetric [PuO4(OH)2]3- anions. The Pu atom in this anion has an almost ideal tetra­gonal bipyramidal oxygen environment. The Pu-O distances are 1.8889 (14) and 1.8685 (15) Å in the PuO4 group and 2.3726 (15) Å to the OH groups. In the isostructural NpVII compound, Cs3[NpO4(OH)2]·3H2O, the Np-O distances in the NpO4 group are nearly the same as the Pu-O distances here, but the distances to the OH groups are about 0.04 Å longer.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807011877/br2033sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807011877/br2033Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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.

Tricaesium dihydroxotetraoxoplutonate(VII) trihydrate top
Crystal data top
Cs3[PuO4(OH)2]·3H2OF(000) = 1356
Mr = 789.84Dx = 4.539 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 9469 reflections
a = 12.5381 (3) Åθ = 2.4–45.0°
b = 11.4983 (3) ŵ = 15.03 mm1
c = 8.0195 (2) ÅT = 293 K
β = 91.3913 (12)°Fragment, black
V = 1155.81 (5) Å30.16 × 0.06 × 0.04 mm
Z = 4
Data collection top
Bruker KAPPA APEX II area-detector
diffractometer
4717 independent reflections
Radiation source: fine-focus sealed tube4033 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ω and φ scansθmax = 45.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1624
Tmin = 0.375, Tmax = 0.585k = 2222
23677 measured reflectionsl = 1515
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021All 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 reflectionsΔρmax = 2.11 e Å3
79 parametersΔρmin = 2.64 e Å3
4 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.01490 (16)
Special details top

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 (Å2) top
xyzUiso*/Ueq
Pu0.25000.25000.50000.01243 (2)
Cs10.301977 (9)0.089341 (10)0.048753 (16)0.02221 (3)
Cs20.00000.066558 (18)0.75000.02884 (4)
O10.18708 (13)0.12102 (12)0.3899 (2)0.0240 (3)
O20.22676 (14)0.18090 (15)0.7068 (2)0.0269 (3)
O30.42108 (12)0.16183 (14)0.4997 (2)0.0258 (3)
H30.428 (4)0.118 (4)0.422 (5)0.060 (14)*
O40.57271 (14)0.31917 (16)0.5833 (2)0.0286 (3)
H4A0.590 (3)0.315 (3)0.685 (3)0.041 (10)*
H4B0.523 (3)0.269 (3)0.572 (7)0.048 (12)*
O50.50000.0278 (2)0.75000.0329 (5)
H50.474 (3)0.074 (3)0.679 (4)0.036 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pu0.01262 (4)0.01308 (3)0.01151 (3)0.00042 (2)0.00173 (2)0.00081 (2)
Cs10.02266 (5)0.02072 (5)0.02318 (5)0.00302 (3)0.00102 (4)0.00047 (4)
Cs20.03000 (9)0.03006 (8)0.02623 (8)0.0000.00439 (7)0.000
O10.0254 (7)0.0191 (5)0.0271 (7)0.0027 (4)0.0056 (5)0.0043 (5)
O20.0302 (8)0.0316 (7)0.0188 (6)0.0026 (5)0.0006 (5)0.0087 (5)
O30.0183 (6)0.0270 (6)0.0319 (8)0.0048 (5)0.0028 (5)0.0047 (6)
O40.0229 (7)0.0373 (8)0.0253 (7)0.0058 (6)0.0024 (6)0.0037 (6)
O50.0420 (14)0.0241 (10)0.0319 (12)0.0000.0126 (11)0.000
Geometric parameters (Å, º) top
Pu—O1i1.8889 (14)Cs2—O2xi3.1590 (16)
Pu—O11.8889 (14)Cs2—O4xii3.282 (2)
Pu—O21.8685 (15)Cs2—O4xiii3.282 (2)
Pu—O2i1.8685 (16)Cs2—O1xiv3.3592 (14)
Pu—O32.3726 (15)Cs2—O1ii3.3592 (14)
Pu—O3i2.3726 (15)Cs2—Cs2xv4.2920 (2)
Pu—Cs1ii3.9736 (2)Cs2—Cs2xiv4.2920 (2)
Pu—Cs1iii3.9736 (2)Cs2—Puxi4.3127 (1)
Pu—Cs1i4.1288 (2)O1—Cs1ii3.0757 (16)
Pu—Cs14.1288 (2)O1—Cs2xiv3.3592 (14)
Pu—Cs24.3127 (1)O2—Cs1xvi3.0644 (16)
Pu—Cs2i4.3127 (1)O2—Cs1i3.3143 (18)
Cs1—O2iv3.0644 (16)O2—Cs1ii3.4944 (18)
Cs1—O1v3.0757 (16)O3—Cs1ii3.2794 (17)
Cs1—O4vi3.0798 (17)O3—Cs1viii3.6011 (15)
Cs1—O13.1437 (18)O3—H30.809 (19)
Cs1—O5vii3.2232 (10)O4—Cs1xvii3.0798 (17)
Cs1—O4viii3.264 (2)O4—Cs2i3.0958 (19)
Cs1—O3v3.2794 (17)O4—Cs1viii3.264 (2)
Cs1—O2i3.3143 (18)O4—Cs2xviii3.282 (2)
Cs1—O2v3.4944 (18)O4—H4A0.839 (19)
Cs1—O5iv3.5629 (5)O4—H4B0.853 (19)
Cs1—O3viii3.6011 (15)O5—Cs1ii3.2232 (10)
Cs1—Puix3.9736 (2)O5—Cs1vii3.2232 (10)
Cs1—H33.37 (4)O5—Cs1xvi3.5629 (5)
Cs2—O4x3.0958 (19)O5—Cs1viii3.5629 (5)
Cs2—O4i3.0958 (19)O5—H50.844 (18)
Cs2—O23.1590 (17)
O2—Pu—O2i180.0O2i—Cs1—O2v117.392 (8)
O1—Pu—O2i89.49 (8)O2iv—Cs1—O5iv70.79 (4)
O2i—Pu—O1i90.51 (8)O1v—Cs1—O5iv83.82 (4)
O1—Pu—O290.51 (8)O4vi—Cs1—O5iv142.70 (4)
O1—Pu—O391.79 (6)O1—Cs1—O5iv161.75 (3)
O2i—Pu—O189.49 (8)O5vii—Cs1—O5iv73.311 (12)
O1i—Pu—O1180.00 (5)O4viii—Cs1—O5iv66.03 (5)
O2—Pu—O388.84 (7)O3v—Cs1—O5iv54.38 (5)
O2i—Pu—O391.16 (7)O2i—Cs1—O5iv130.05 (4)
O1i—Pu—O388.21 (6)O2v—Cs1—O5iv105.43 (5)
O2—Pu—O3i91.16 (7)O2iv—Cs1—O3viii95.78 (4)
O2i—Pu—O3i88.84 (7)O1v—Cs1—O3viii125.49 (4)
O1i—Pu—O3i91.79 (6)O4vi—Cs1—O3viii146.63 (4)
O1—Pu—O3i88.21 (6)O1—Cs1—O3viii122.03 (4)
O3—Pu—O3i180.0O5vii—Cs1—O3viii54.38 (4)
O2iv—Cs1—O1v76.62 (4)O4viii—Cs1—O3viii45.94 (4)
O2iv—Cs1—O4vi72.27 (5)O3v—Cs1—O3viii75.39 (4)
O1v—Cs1—O4vi82.94 (5)O2i—Cs1—O3viii89.90 (4)
O2iv—Cs1—O1126.96 (4)O2v—Cs1—O3viii120.96 (4)
O1v—Cs1—O1103.40 (5)O5iv—Cs1—O3viii44.27 (4)
O4vi—Cs1—O155.51 (5)O4x—Cs2—O4i129.77 (7)
O2iv—Cs1—O5vii143.92 (3)O4x—Cs2—O270.79 (5)
O1v—Cs1—O5vii103.07 (5)O4i—Cs2—O288.61 (4)
O4vi—Cs1—O5vii143.80 (4)O4x—Cs2—O2xi88.61 (4)
O1—Cs1—O5vii88.65 (3)O4i—Cs2—O2xi70.79 (5)
O2iv—Cs1—O4viii64.64 (4)O2—Cs2—O2xi130.81 (6)
O1v—Cs1—O4viii136.60 (5)O4x—Cs2—O4xii95.46 (5)
O4vi—Cs1—O4viii102.14 (4)O4i—Cs2—O4xii129.85 (5)
O1—Cs1—O4viii115.02 (4)O2—Cs2—O4xii131.69 (4)
O5vii—Cs1—O4viii97.46 (5)O2xi—Cs2—O4xii93.24 (4)
O2iv—Cs1—O3v109.04 (5)O4x—Cs2—O4xiii129.85 (5)
O1v—Cs1—O3v57.84 (4)O4i—Cs2—O4xiii95.46 (5)
O4vi—Cs1—O3v137.76 (4)O2—Cs2—O4xiii93.24 (4)
O1—Cs1—O3v115.22 (4)O2xi—Cs2—O4xiii131.69 (4)
O5vii—Cs1—O3v49.05 (5)O4xii—Cs2—O4xiii59.82 (6)
O4viii—Cs1—O3v116.73 (4)O4x—Cs2—O1xiv138.54 (5)
O2iv—Cs1—O2i102.70 (4)O4i—Cs2—O1xiv78.21 (4)
O1v—Cs1—O2i144.61 (4)O2—Cs2—O1xiv148.61 (4)
O4vi—Cs1—O2i63.86 (4)O2xi—Cs2—O1xiv71.38 (4)
O1—Cs1—O2i48.27 (4)O4xii—Cs2—O1xiv51.75 (4)
O5vii—Cs1—O2i97.50 (4)O4xiii—Cs2—O1xiv60.40 (4)
O4viii—Cs1—O2i66.84 (4)O4x—Cs2—O1ii78.21 (4)
O3v—Cs1—O2i146.03 (4)O4i—Cs2—O1ii138.54 (5)
O2iv—Cs1—O2v123.38 (5)O2—Cs2—O1ii71.38 (4)
O1v—Cs1—O2v47.40 (4)O2xi—Cs2—O1ii148.61 (4)
O4vi—Cs1—O2v90.60 (4)O4xii—Cs2—O1ii60.40 (4)
O1—Cs1—O2v69.75 (4)O4xiii—Cs2—O1ii51.75 (4)
O5vii—Cs1—O2v70.01 (4)O1xiv—Cs2—O1ii100.11 (5)
O4viii—Cs1—O2v166.89 (4)Pu—O3—H3112 (4)
O3v—Cs1—O2v52.28 (4)H4A—O4—H4B103 (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, z1; (v) x, y, z1/2; (vi) x1/2, y+1/2, z1/2; (vii) x+1, y, z+1; (viii) x+1, y, z+1/2; (ix) x+1/2, y1/2, z+1/2; (x) x1/2, y+1/2, z+1/2; (xi) x, y, z+3/2; (xii) x+1/2, y1/2, z+3/2; (xiii) x1/2, y1/2, 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.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O5vii0.81 (2)2.36 (2)3.137 (2)161 (5)
O4—H4A···O1xvii0.84 (2)2.16 (3)2.899 (3)148 (4)
O4—H4B···O30.85 (2)1.86 (2)2.697 (2)168 (6)
O5—H5···O30.84 (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.
 

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