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The title compound, 8.5-sodium 1.5-hydrogen tetratriaconta­oxononatungstomonogermanate(10−) icosahydrate, contains A-α- and A-β-type trivacant Keggin [GeW9O34]10− anions, which are disordered in an approximately 1:9 ratio. Pairs of anions related by a center of symmetry are linked via O—Na—O bonding to form a quasi-sandwich-type [Na10(H2O)14(GeW9O34)2]10− complex.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803015344/br6108sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803015344/br6108Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](Ge-O) = 0.013 Å
  • Some non-H atoms missing
  • Disorder in solvent or counterion
  • R factor = 0.076
  • wR factor = 0.163
  • Data-to-parameter ratio = 24.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
PLAT_601 Alert B Structure Contains Solvent Accessible VOIDS of . 104.00 A   3
Yellow Alert Alert Level C:
PLAT_213 Alert C Atom O5 has ADP max/min Ratio ............. 3.30 oblate PLAT_213 Alert C Atom O11 has ADP max/min Ratio ............. 3.20 prolat PLAT_213 Alert C Atom O26 has ADP max/min Ratio ............. 3.30 oblate PLAT_213 Alert C Atom O28 has ADP max/min Ratio ............. 3.70 oblate PLAT_302 Alert C Anion/Solvent Disorder ......................... 2.00 Perc. General Notes
FORMU_01 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:H41.5 Ge1 Na8.5 O54 W9 Atom count from the _atom_site data: Ge1 Na8.5 O53.4 W9 CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum Ge H41.50 Na8.50 O54 W9 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff Ge 2.00 2.00 0.00 H 83.00 0.00 83.00 Na 17.00 17.00 0.00 O 108.00 106.80 1.20 W 18.00 18.00 0.00 Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests CHEMW_03 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 2828.45 TEST: Calculate formula weight from _atom_site_* atom mass num sum Na 22.99 8.50 195.41 Ge 72.59 1.00 72.59 W 183.85 9.00 1654.65 O 16.00 53.40 854.35 H 1.01 0.00 0.00 Calculated formula weight 2777.00 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
5 Alert Level C = Please check

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: TEXSAN Ver. 1.11 (Molecular Structure Corporation, 2000); program(s) used to solve structure: SYSTEM90 (Yonggeng et al., 1994); program(s) used to refine structure: TEXSAN Ver. 1.11; software used to prepare material for publication: TEXSAN Ver. 1.11, ORTEP II (Johnson, 1976).

(I) top
Crystal data top
Na8.5H1.5[GeW9O4]·20H2OV = 2557.3 (3) Å3
Mr = 2828.45Z = 2
Triclinic, P1Dx = 3.673 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.7107 Å
a = 12.6563 (9) ÅCell parameters from 11591 reflections
b = 13.260 (1) Åθ = 2.3–30.0°
c = 18.491 (2) ŵ = 20.95 mm1
α = 72.576 (3)°T = 296 K
β = 70.078 (3)°Block, colorless
γ = 62.848 (3)°0.15 × 0.15 × 0.08 mm
Data collection top
Rigaku R-AXIS RAPID Imaging Plate
diffractometer
9852 reflections with F2 > 2σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.075
ω scansθmax = 30.0°
Absorption correction: numerical
(Higashi, 1995)
h = 1717
Tmin = 0.041, Tmax = 0.173k = 1816
18682 measured reflectionsl = 2525
14391 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.076H-atom parameters not defined
wR(F2) = 0.163 w = 1/[σ2(Fo2) + (0.05P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.56(Δ/σ)max = 0.0004
14383 reflectionsΔρmax = 4.29 e Å3
586 parametersΔρmin = 3.55 e Å3
Primary atom site location: structure-invariant direct methods
Special details top

Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
W10.87225 (7)0.60592 (7)0.17323 (5)0.0345 (2)0.90
W20.62005 (9)0.71135 (8)0.10329 (5)0.0340 (2)0.90
W30.64582 (7)0.86501 (7)0.21001 (4)0.0272 (2)0.90
W40.84816 (6)0.48673 (6)0.39393 (4)0.0282 (2)
W50.82619 (6)0.33553 (6)0.28916 (4)0.0285 (2)
W60.54287 (7)0.44894 (6)0.21402 (4)0.0269 (2)
W70.31876 (7)0.70217 (6)0.24552 (4)0.0289 (2)
W80.34845 (6)0.88039 (6)0.35719 (4)0.0247 (2)
W90.59412 (6)0.77585 (6)0.42908 (4)0.0237 (2)
W100.814 (1)0.739 (1)0.2264 (7)0.070 (4)0.10
W110.798 (1)0.579 (1)0.1229 (5)0.063 (3)0.10
W120.574 (1)0.8391 (10)0.1519 (6)0.065 (3)0.10
Ge10.5908 (1)0.6129 (1)0.31006 (9)0.0207 (4)
Na10.3505 (7)0.4692 (7)0.4118 (4)0.043 (2)
Na20.6117 (8)0.1982 (7)0.3607 (5)0.045 (2)
Na30.3252 (7)0.2950 (7)0.3024 (5)0.044 (2)
Na40.372 (1)0.644 (1)0.5185 (8)0.036 (4)0.50
Na50.7054 (9)0.7433 (9)0.1298 (5)0.059 (3)
Na60.1200 (9)0.7638 (9)0.4318 (6)0.064 (3)
Na70.879 (1)0.069 (1)0.4442 (8)0.091 (4)
Na80.643 (2)0.476 (2)0.0123 (8)0.157 (9)
Na90.189 (2)0.947 (2)0.0841 (9)0.154 (8)
O11.025 (1)0.575 (1)0.119 (1)0.051 (5)0.90
O20.602 (1)0.752 (1)0.0076 (8)0.037 (4)0.90
O30.652 (1)1.002 (1)0.1768 (8)0.043 (4)0.90
O40.977 (1)0.484 (1)0.410 (1)0.058 (5)
O50.941 (1)0.230 (1)0.2349 (9)0.048 (4)
O60.575 (1)0.375 (1)0.1398 (7)0.041 (4)
O70.211 (1)0.788 (1)0.1915 (8)0.044 (4)
O80.246 (1)1.025 (1)0.3369 (7)0.037 (4)
O90.655 (1)0.850 (1)0.4558 (8)0.038 (4)
O100.799 (1)0.647 (1)0.0839 (8)0.036 (4)0.90
O110.622 (1)0.854 (1)0.1127 (7)0.028 (3)0.90
O120.815 (1)0.774 (1)0.1657 (7)0.031 (3)0.90
O130.860 (1)0.468 (1)0.1966 (7)0.034 (3)
O140.629 (1)0.559 (1)0.1330 (7)0.043 (4)
O150.452 (1)0.759 (1)0.1641 (8)0.040 (4)
O160.480 (1)0.900 (1)0.2525 (7)0.037 (4)
O170.676 (1)0.823 (1)0.3076 (7)0.033 (3)
O180.884 (1)0.588 (1)0.2775 (8)0.038 (4)
O190.927 (1)0.363 (1)0.3341 (7)0.033 (3)
O200.691 (1)0.379 (1)0.2434 (7)0.034 (3)
O210.400 (1)0.575 (1)0.1872 (7)0.040 (4)
O220.3092 (10)0.809 (1)0.2993 (7)0.033 (3)
O230.450 (1)0.907 (1)0.4045 (7)0.029 (3)
O240.732 (1)0.635 (1)0.4154 (7)0.032 (3)
O250.665 (1)0.681 (1)0.2226 (6)0.028 (3)
O260.7041 (9)0.490 (1)0.3474 (7)0.030 (3)
O270.4854 (10)0.5779 (9)0.2912 (6)0.023 (3)
O280.5089 (10)0.7117 (9)0.3758 (6)0.023 (3)
O290.773 (1)0.254 (1)0.3734 (8)0.044 (4)
O300.465 (1)0.3772 (9)0.2941 (7)0.029 (3)
O310.235 (1)0.635 (1)0.3274 (7)0.035 (3)
O320.263 (1)0.833 (1)0.4471 (7)0.034 (3)
O330.519 (1)0.7219 (10)0.5213 (7)0.028 (3)
O340.791 (1)0.412 (1)0.4842 (8)0.045 (4)
O350.728 (2)0.549 (2)0.115 (1)0.101 (7)*
O360.886 (2)0.683 (2)0.088 (1)0.085 (6)*
O370.653 (2)0.941 (2)0.145 (1)0.082 (6)*
O380.015 (2)0.939 (2)0.349 (1)0.080 (5)*
O390.015 (2)0.873 (2)0.549 (1)0.117 (8)*
O400.573 (2)0.369 (2)0.027 (1)0.080 (5)*
O410.840 (2)0.402 (2)0.046 (1)0.118 (8)*
O420.386 (2)0.967 (2)0.011 (1)0.083 (6)*
O430.122 (2)1.032 (2)0.201 (1)0.104 (7)*
O440.124 (2)1.140 (2)0.009 (2)0.120 (8)*
O450.036 (2)0.705 (2)0.437 (1)0.099 (7)*
O460.257 (3)0.867 (3)0.034 (2)0.140 (10)*
O470.071 (4)0.807 (4)0.288 (2)0.22 (1)*
O480.178 (2)0.500 (2)0.259 (1)0.069 (5)*
O490.460 (1)0.222 (1)0.1803 (9)0.056 (4)*
O500.187 (1)0.250 (1)0.2690 (7)0.040 (3)*
O510.444 (1)0.129 (1)0.3826 (8)0.045 (3)*
O520.216 (1)0.368 (1)0.4254 (8)0.049 (3)*
O530.739 (2)0.094 (2)0.259 (1)0.098 (7)*
O540.715 (1)0.035 (1)0.4488 (9)0.052 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.0248 (4)0.0289 (4)0.0428 (5)0.0120 (4)0.0057 (3)0.0104 (3)
W20.0483 (5)0.0324 (5)0.0244 (4)0.0207 (4)0.0081 (4)0.0021 (3)
W30.0309 (4)0.0221 (4)0.0279 (4)0.0138 (3)0.0021 (3)0.0034 (3)
W40.0217 (3)0.0240 (3)0.0388 (4)0.0051 (3)0.0082 (3)0.0108 (3)
W50.0246 (3)0.0234 (3)0.0353 (4)0.0077 (3)0.0015 (3)0.0114 (3)
W60.0347 (4)0.0253 (3)0.0252 (3)0.0144 (3)0.0057 (3)0.0077 (3)
W70.0339 (4)0.0259 (4)0.0303 (3)0.0101 (3)0.0135 (3)0.0054 (3)
W80.0251 (3)0.0199 (3)0.0286 (3)0.0068 (3)0.0075 (3)0.0057 (2)
W90.0246 (3)0.0198 (3)0.0282 (3)0.0077 (3)0.0076 (3)0.0064 (2)
W100.057 (6)0.092 (9)0.064 (7)0.058 (7)0.017 (5)0.008 (6)
W110.074 (7)0.069 (7)0.029 (4)0.035 (6)0.017 (4)0.009 (4)
W120.073 (7)0.054 (7)0.040 (5)0.026 (6)0.006 (5)0.020 (5)
Ge10.0227 (8)0.0197 (8)0.0215 (8)0.0097 (7)0.0034 (6)0.0056 (6)
Na10.040 (4)0.041 (5)0.041 (4)0.007 (4)0.011 (4)0.013 (3)
Na20.051 (5)0.038 (5)0.048 (4)0.024 (4)0.005 (4)0.005 (4)
Na30.039 (4)0.043 (5)0.054 (5)0.009 (4)0.013 (4)0.025 (4)
Na40.052 (9)0.022 (7)0.040 (8)0.023 (7)0.023 (7)0.012 (6)
Na50.071 (6)0.059 (6)0.041 (4)0.026 (5)0.007 (4)0.006 (4)
Na60.051 (6)0.051 (6)0.072 (6)0.004 (5)0.021 (5)0.006 (5)
Na70.071 (8)0.082 (9)0.103 (9)0.019 (7)0.004 (7)0.029 (7)
Na80.17 (2)0.26 (3)0.069 (9)0.14 (2)0.010 (10)0.01 (1)
Na90.15 (2)0.19 (2)0.10 (1)0.08 (2)0.03 (1)0.02 (1)
O10.027 (8)0.04 (1)0.07 (1)0.012 (7)0.012 (7)0.028 (8)
O20.042 (8)0.046 (9)0.031 (7)0.023 (8)0.006 (6)0.012 (6)
O30.047 (9)0.044 (9)0.034 (7)0.028 (8)0.009 (7)0.013 (7)
O40.033 (8)0.05 (1)0.10 (1)0.014 (7)0.015 (8)0.032 (9)
O50.020 (6)0.043 (9)0.062 (9)0.002 (6)0.016 (6)0.032 (7)
O60.056 (9)0.046 (9)0.037 (7)0.031 (8)0.001 (6)0.023 (6)
O70.052 (9)0.026 (7)0.058 (9)0.006 (6)0.033 (7)0.005 (6)
O80.037 (7)0.029 (7)0.044 (7)0.010 (6)0.016 (6)0.003 (6)
O90.045 (8)0.024 (7)0.050 (8)0.009 (6)0.016 (6)0.018 (6)
O100.056 (10)0.039 (9)0.020 (6)0.031 (8)0.000 (6)0.004 (6)
O110.036 (7)0.022 (7)0.014 (6)0.016 (6)0.007 (5)0.004 (5)
O120.034 (7)0.017 (6)0.024 (6)0.008 (6)0.002 (6)0.005 (5)
O130.032 (6)0.023 (6)0.037 (7)0.012 (6)0.008 (5)0.006 (5)
O140.067 (10)0.032 (7)0.040 (7)0.028 (7)0.003 (7)0.016 (6)
O150.051 (8)0.027 (7)0.043 (7)0.013 (6)0.019 (7)0.001 (6)
O160.043 (8)0.038 (8)0.030 (6)0.023 (7)0.004 (6)0.002 (5)
O170.025 (6)0.041 (8)0.030 (6)0.016 (6)0.003 (5)0.008 (5)
O180.035 (7)0.031 (7)0.055 (8)0.016 (6)0.018 (6)0.002 (6)
O190.048 (8)0.025 (6)0.030 (6)0.012 (6)0.008 (6)0.015 (5)
O200.020 (6)0.031 (7)0.048 (7)0.007 (5)0.008 (5)0.028 (6)
O210.064 (9)0.038 (8)0.030 (6)0.026 (7)0.028 (7)0.006 (5)
O220.016 (5)0.049 (8)0.028 (6)0.009 (6)0.003 (5)0.015 (6)
O230.029 (6)0.026 (6)0.033 (6)0.010 (5)0.008 (5)0.006 (5)
O240.017 (5)0.036 (7)0.036 (6)0.001 (5)0.001 (5)0.018 (5)
O250.030 (6)0.026 (6)0.022 (5)0.013 (5)0.007 (5)0.008 (4)
O260.006 (4)0.026 (6)0.046 (7)0.002 (5)0.001 (5)0.012 (5)
O270.024 (5)0.026 (6)0.033 (6)0.016 (5)0.011 (5)0.009 (5)
O280.023 (5)0.007 (5)0.038 (6)0.004 (4)0.012 (5)0.012 (4)
O290.038 (8)0.019 (6)0.059 (9)0.010 (6)0.000 (7)0.002 (6)
O300.027 (6)0.014 (5)0.045 (7)0.007 (5)0.015 (5)0.003 (5)
O310.024 (6)0.026 (7)0.044 (7)0.001 (5)0.014 (6)0.004 (5)
O320.037 (7)0.028 (7)0.037 (7)0.007 (6)0.019 (6)0.004 (5)
O330.026 (6)0.022 (6)0.037 (6)0.005 (5)0.009 (5)0.011 (5)
O340.059 (9)0.023 (7)0.049 (8)0.006 (7)0.022 (7)0.007 (6)
Geometric parameters (Å, º) top
W1—O11.77 (1)W12—O252.14 (1)
W1—O131.82 (1)W12—O152.17 (2)
W1—O181.92 (1)Ge1—O261.75 (1)
W1—O121.98 (1)Ge1—O271.759 (9)
W1—O101.98 (1)Ge1—O281.77 (1)
W1—O252.29 (1)Ge1—O251.78 (1)
W2—O21.75 (1)Na1—O312.44 (1)
W2—O141.89 (1)Na1—O302.48 (2)
W2—O151.94 (1)Na1—O34i2.51 (2)
W2—O111.96 (1)Na1—O522.51 (2)
W2—O101.96 (2)Na1—O33i2.53 (1)
W2—O252.34 (1)Na1—O272.77 (1)
W3—O31.77 (1)Na2—O532.35 (2)
W3—O171.84 (1)Na2—O542.41 (2)
W3—O161.86 (1)Na2—O33i2.44 (1)
W3—O121.94 (1)Na2—O302.53 (1)
W3—O111.98 (1)Na2—O512.55 (2)
W3—O252.28 (1)Na2—O292.56 (2)
W4—O41.73 (1)Na2—O203.02 (2)
W4—O341.77 (1)Na3—O502.39 (1)
W4—O241.90 (1)Na3—O302.41 (1)
W4—O191.94 (1)Na3—O512.42 (2)
W4—O182.19 (1)Na3—O522.45 (2)
W4—O262.24 (1)Na3—O492.47 (2)
W5—O291.73 (1)Na3—O482.56 (2)
W5—O51.75 (1)Na4—O322.45 (2)
W5—O201.94 (1)Na4—O29i2.45 (2)
W5—O191.94 (1)Na4—O34i2.51 (2)
W5—O132.14 (1)Na4—O332.52 (2)
W5—O262.25 (1)Na4—O26i2.75 (2)
W6—O61.75 (1)Na4—O282.77 (2)
W6—O301.76 (1)Na5—O372.34 (2)
W6—O201.87 (1)Na5—O362.37 (2)
W6—O211.92 (1)Na5—O49ii2.38 (2)
W6—O142.15 (1)Na5—O352.39 (3)
W6—O272.26 (1)Na5—O22.44 (2)
W7—O71.73 (1)Na5—O50ii2.46 (2)
W7—O311.78 (1)Na6—O34i2.39 (2)
W7—O221.90 (1)Na6—O452.40 (2)
W7—O211.95 (1)Na6—O382.43 (2)
W7—O152.10 (1)Na6—O322.49 (2)
W7—O272.25 (1)Na6—O312.56 (2)
W8—O321.76 (1)Na6—O392.61 (3)
W8—O81.77 (1)Na6—O222.92 (2)
W8—O221.92 (1)Na7—O39i2.23 (3)
W8—O231.98 (1)Na7—O542.28 (2)
W8—O162.12 (1)Na7—O292.41 (2)
W8—O282.26 (1)Na7—O32i2.44 (2)
W9—O91.75 (1)Na7—O38iii2.46 (2)
W9—O331.76 (1)Na7—O39iii2.81 (3)
W9—O241.90 (1)Na8—O352.35 (3)
W9—O231.94 (1)Na8—O402.35 (3)
W9—O172.16 (1)Na8—O62.42 (2)
W9—O282.218 (10)Na8—O412.46 (3)
W10—O181.87 (2)Na8—O40ii2.54 (3)
W10—O172.00 (2)Na8—O142.69 (2)
W10—O252.37 (1)Na9—O72.41 (2)
W11—O131.77 (2)Na9—O442.43 (3)
W11—O142.21 (2)Na9—O462.43 (4)
W11—O252.32 (1)Na9—O432.45 (3)
W12—O162.01 (2)Na9—O422.50 (3)
O1—W1—O13103.3 (6)O6—W6—O20101.7 (6)
O1—W1—O18102.7 (7)O6—W6—O2196.0 (6)
O1—W1—O1299.3 (7)O6—W6—O1490.4 (5)
O1—W1—O1097.1 (7)O6—W6—O27167.9 (6)
O1—W1—O25167.2 (6)O30—W6—O2096.5 (5)
O13—W1—O1890.3 (5)O30—W6—O2196.4 (5)
O13—W1—O12157.2 (5)O30—W6—O14168.1 (5)
O13—W1—O1088.3 (6)O30—W6—O2786.3 (5)
O13—W1—O2586.1 (5)O20—W6—O21155.5 (5)
O18—W1—O1288.1 (5)O20—W6—O1481.6 (6)
O18—W1—O10160.0 (6)O20—W6—O2786.3 (4)
O18—W1—O2585.9 (5)O21—W6—O1481.5 (6)
O12—W1—O1085.6 (6)O21—W6—O2773.8 (4)
O12—W1—O2571.2 (5)O14—W6—O2781.8 (4)
O10—W1—O2574.1 (5)O7—W7—O31102.0 (6)
O2—W2—O14103.9 (6)O7—W7—O22101.6 (6)
O2—W2—O15102.0 (6)O7—W7—O2196.3 (6)
O2—W2—O1198.3 (6)O7—W7—O1592.2 (6)
O2—W2—O10100.8 (6)O7—W7—O27167.5 (6)
O2—W2—O25168.8 (5)O31—W7—O2295.2 (5)
O14—W2—O1587.4 (6)O31—W7—O2196.3 (6)
O14—W2—O11157.7 (5)O31—W7—O15165.8 (5)
O14—W2—O1087.5 (6)O31—W7—O2786.3 (4)
O14—W2—O2585.7 (5)O22—W7—O21156.1 (5)
O15—W2—O1189.1 (5)O22—W7—O1581.0 (5)
O15—W2—O10157.2 (5)O22—W7—O2786.6 (4)
O15—W2—O2584.0 (5)O21—W7—O1582.7 (5)
O11—W2—O1087.2 (6)O21—W7—O2773.3 (4)
O11—W2—O2572.1 (5)O15—W7—O2779.8 (4)
O10—W2—O2573.5 (5)O32—W8—O8100.6 (6)
O3—W3—O17103.1 (6)O32—W8—O2293.2 (5)
O3—W3—O16103.0 (6)O32—W8—O2394.8 (5)
O3—W3—O1298.0 (6)O32—W8—O16167.3 (5)
O3—W3—O1196.4 (6)O32—W8—O2887.8 (5)
O3—W3—O25166.0 (6)O8—W8—O22100.4 (5)
O17—W3—O1691.6 (5)O8—W8—O2398.1 (5)
O17—W3—O1290.9 (5)O8—W8—O1692.1 (6)
O17—W3—O11160.2 (5)O8—W8—O28168.0 (5)
O17—W3—O2587.3 (5)O22—W8—O23158.2 (5)
O16—W3—O12157.7 (6)O22—W8—O1684.1 (5)
O16—W3—O1187.4 (5)O22—W8—O2887.5 (4)
O16—W3—O2585.8 (5)O23—W8—O1683.7 (5)
O12—W3—O1182.9 (6)O23—W8—O2872.5 (4)
O12—W3—O2572.2 (5)O16—W8—O2879.7 (5)
O11—W3—O2572.9 (5)O9—W9—O33101.1 (6)
O4—W4—O34101.7 (7)O9—W9—O24100.5 (6)
O4—W4—O24101.1 (6)O9—W9—O2397.4 (5)
O4—W4—O1998.8 (6)O9—W9—O1790.0 (5)
O4—W4—O1889.5 (7)O9—W9—O28168.6 (5)
O4—W4—O26168.0 (6)O33—W9—O2495.5 (5)
O34—W4—O2494.8 (6)O33—W9—O2396.2 (5)
O34—W4—O1998.3 (6)O33—W9—O17168.9 (5)
O34—W4—O18168.6 (5)O33—W9—O2887.8 (4)
O34—W4—O2688.6 (5)O24—W9—O23156.3 (5)
O24—W4—O19153.4 (5)O24—W9—O1781.6 (5)
O24—W4—O1881.0 (5)O24—W9—O2885.6 (4)
O24—W4—O2684.0 (4)O23—W9—O1783.0 (5)
O19—W4—O1881.6 (5)O23—W9—O2874.3 (4)
O19—W4—O2673.4 (5)O17—W9—O2881.4 (4)
O18—W4—O2680.4 (4)O18—W10—O17105.8 (8)
O29—W5—O5102.5 (7)O18—W10—O2584.6 (6)
O29—W5—O2095.2 (6)O18—W10—O47iv90 (1)
O29—W5—O1995.3 (6)O17—W10—O2581.2 (5)
O29—W5—O13167.2 (6)O13—W11—O14102.1 (7)
O29—W5—O2687.4 (5)O13—W11—O2586.4 (6)
O5—W5—O20100.8 (6)O14—W11—O2579.3 (5)
O5—W5—O1999.0 (6)O16—W12—O2586.1 (6)
O5—W5—O1390.3 (6)O16—W12—O1592.4 (7)
O5—W5—O26168.1 (5)O25—W12—O1583.6 (6)
O20—W5—O19155.1 (5)O26—Ge1—O27111.5 (5)
O20—W5—O1381.4 (5)O26—Ge1—O28111.3 (5)
O20—W5—O2684.7 (4)O26—Ge1—O25107.7 (5)
O19—W5—O1383.4 (5)O27—Ge1—O28108.0 (5)
O19—W5—O2673.2 (5)O27—Ge1—O25110.5 (5)
O13—W5—O2680.0 (4)O28—Ge1—O25107.8 (5)
O6—W6—O30101.6 (6)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y+1, z; (iii) x+1, y1, z; (iv) x+1, y, z.
 

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