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
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (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
Alert Level B:
PLAT_601 Alert B Structure Contains Solvent Accessible VOIDS of . 104.00 A 3
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
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).
Crystal data top
Na8.5H1.5[GeW9O4]·20H2O | V = 2557.3 (3) Å3 |
Mr = 2828.45 | Z = 2 |
Triclinic, P1 | Dx = 3.673 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.7107 Å |
a = 12.6563 (9) Å | Cell parameters from 11591 reflections |
b = 13.260 (1) Å | θ = 2.3–30.0° |
c = 18.491 (2) Å | µ = 20.95 mm−1 |
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-1 | Rint = 0.075 |
ω scans | θmax = 30.0° |
Absorption correction: numerical (Higashi, 1995) | h = −17→17 |
Tmin = 0.041, Tmax = 0.173 | k = −18→16 |
18682 measured reflections | l = −25→25 |
14391 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.076 | H-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 reflections | Δρmax = 4.29 e Å−3 |
586 parameters | Δρmin = −3.55 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
W1 | 0.87225 (7) | 0.60592 (7) | 0.17323 (5) | 0.0345 (2) | 0.90 |
W2 | 0.62005 (9) | 0.71135 (8) | 0.10329 (5) | 0.0340 (2) | 0.90 |
W3 | 0.64582 (7) | 0.86501 (7) | 0.21001 (4) | 0.0272 (2) | 0.90 |
W4 | 0.84816 (6) | 0.48673 (6) | 0.39393 (4) | 0.0282 (2) | |
W5 | 0.82619 (6) | 0.33553 (6) | 0.28916 (4) | 0.0285 (2) | |
W6 | 0.54287 (7) | 0.44894 (6) | 0.21402 (4) | 0.0269 (2) | |
W7 | 0.31876 (7) | 0.70217 (6) | 0.24552 (4) | 0.0289 (2) | |
W8 | 0.34845 (6) | 0.88039 (6) | 0.35719 (4) | 0.0247 (2) | |
W9 | 0.59412 (6) | 0.77585 (6) | 0.42908 (4) | 0.0237 (2) | |
W10 | 0.814 (1) | 0.739 (1) | 0.2264 (7) | 0.070 (4) | 0.10 |
W11 | 0.798 (1) | 0.579 (1) | 0.1229 (5) | 0.063 (3) | 0.10 |
W12 | 0.574 (1) | 0.8391 (10) | 0.1519 (6) | 0.065 (3) | 0.10 |
Ge1 | 0.5908 (1) | 0.6129 (1) | 0.31006 (9) | 0.0207 (4) | |
Na1 | 0.3505 (7) | 0.4692 (7) | 0.4118 (4) | 0.043 (2) | |
Na2 | 0.6117 (8) | 0.1982 (7) | 0.3607 (5) | 0.045 (2) | |
Na3 | 0.3252 (7) | 0.2950 (7) | 0.3024 (5) | 0.044 (2) | |
Na4 | 0.372 (1) | 0.644 (1) | 0.5185 (8) | 0.036 (4) | 0.50 |
Na5 | 0.7054 (9) | 0.7433 (9) | −0.1298 (5) | 0.059 (3) | |
Na6 | 0.1200 (9) | 0.7638 (9) | 0.4318 (6) | 0.064 (3) | |
Na7 | 0.879 (1) | 0.069 (1) | 0.4442 (8) | 0.091 (4) | |
Na8 | 0.643 (2) | 0.476 (2) | 0.0123 (8) | 0.157 (9) | |
Na9 | 0.189 (2) | 0.947 (2) | 0.0841 (9) | 0.154 (8) | |
O1 | 1.025 (1) | 0.575 (1) | 0.119 (1) | 0.051 (5) | 0.90 |
O2 | 0.602 (1) | 0.752 (1) | 0.0076 (8) | 0.037 (4) | 0.90 |
O3 | 0.652 (1) | 1.002 (1) | 0.1768 (8) | 0.043 (4) | 0.90 |
O4 | 0.977 (1) | 0.484 (1) | 0.410 (1) | 0.058 (5) | |
O5 | 0.941 (1) | 0.230 (1) | 0.2349 (9) | 0.048 (4) | |
O6 | 0.575 (1) | 0.375 (1) | 0.1398 (7) | 0.041 (4) | |
O7 | 0.211 (1) | 0.788 (1) | 0.1915 (8) | 0.044 (4) | |
O8 | 0.246 (1) | 1.025 (1) | 0.3369 (7) | 0.037 (4) | |
O9 | 0.655 (1) | 0.850 (1) | 0.4558 (8) | 0.038 (4) | |
O10 | 0.799 (1) | 0.647 (1) | 0.0839 (8) | 0.036 (4) | 0.90 |
O11 | 0.622 (1) | 0.854 (1) | 0.1127 (7) | 0.028 (3) | 0.90 |
O12 | 0.815 (1) | 0.774 (1) | 0.1657 (7) | 0.031 (3) | 0.90 |
O13 | 0.860 (1) | 0.468 (1) | 0.1966 (7) | 0.034 (3) | |
O14 | 0.629 (1) | 0.559 (1) | 0.1330 (7) | 0.043 (4) | |
O15 | 0.452 (1) | 0.759 (1) | 0.1641 (8) | 0.040 (4) | |
O16 | 0.480 (1) | 0.900 (1) | 0.2525 (7) | 0.037 (4) | |
O17 | 0.676 (1) | 0.823 (1) | 0.3076 (7) | 0.033 (3) | |
O18 | 0.884 (1) | 0.588 (1) | 0.2775 (8) | 0.038 (4) | |
O19 | 0.927 (1) | 0.363 (1) | 0.3341 (7) | 0.033 (3) | |
O20 | 0.691 (1) | 0.379 (1) | 0.2434 (7) | 0.034 (3) | |
O21 | 0.400 (1) | 0.575 (1) | 0.1872 (7) | 0.040 (4) | |
O22 | 0.3092 (10) | 0.809 (1) | 0.2993 (7) | 0.033 (3) | |
O23 | 0.450 (1) | 0.907 (1) | 0.4045 (7) | 0.029 (3) | |
O24 | 0.732 (1) | 0.635 (1) | 0.4154 (7) | 0.032 (3) | |
O25 | 0.665 (1) | 0.681 (1) | 0.2226 (6) | 0.028 (3) | |
O26 | 0.7041 (9) | 0.490 (1) | 0.3474 (7) | 0.030 (3) | |
O27 | 0.4854 (10) | 0.5779 (9) | 0.2912 (6) | 0.023 (3) | |
O28 | 0.5089 (10) | 0.7117 (9) | 0.3758 (6) | 0.023 (3) | |
O29 | 0.773 (1) | 0.254 (1) | 0.3734 (8) | 0.044 (4) | |
O30 | 0.465 (1) | 0.3772 (9) | 0.2941 (7) | 0.029 (3) | |
O31 | 0.235 (1) | 0.635 (1) | 0.3274 (7) | 0.035 (3) | |
O32 | 0.263 (1) | 0.833 (1) | 0.4471 (7) | 0.034 (3) | |
O33 | 0.519 (1) | 0.7219 (10) | 0.5213 (7) | 0.028 (3) | |
O34 | 0.791 (1) | 0.412 (1) | 0.4842 (8) | 0.045 (4) | |
O35 | 0.728 (2) | 0.549 (2) | −0.115 (1) | 0.101 (7)* | |
O36 | 0.886 (2) | 0.683 (2) | −0.088 (1) | 0.085 (6)* | |
O37 | 0.653 (2) | 0.941 (2) | −0.145 (1) | 0.082 (6)* | |
O38 | 0.015 (2) | 0.939 (2) | 0.349 (1) | 0.080 (5)* | |
O39 | −0.015 (2) | 0.873 (2) | 0.549 (1) | 0.117 (8)* | |
O40 | 0.573 (2) | 0.369 (2) | −0.027 (1) | 0.080 (5)* | |
O41 | 0.840 (2) | 0.402 (2) | 0.046 (1) | 0.118 (8)* | |
O42 | 0.386 (2) | 0.967 (2) | 0.011 (1) | 0.083 (6)* | |
O43 | 0.122 (2) | 1.032 (2) | 0.201 (1) | 0.104 (7)* | |
O44 | 0.124 (2) | 1.140 (2) | 0.009 (2) | 0.120 (8)* | |
O45 | −0.036 (2) | 0.705 (2) | 0.437 (1) | 0.099 (7)* | |
O46 | 0.257 (3) | 0.867 (3) | −0.034 (2) | 0.140 (10)* | |
O47 | −0.071 (4) | 0.807 (4) | 0.288 (2) | 0.22 (1)* | |
O48 | 0.178 (2) | 0.500 (2) | 0.259 (1) | 0.069 (5)* | |
O49 | 0.460 (1) | 0.222 (1) | 0.1803 (9) | 0.056 (4)* | |
O50 | 0.187 (1) | 0.250 (1) | 0.2690 (7) | 0.040 (3)* | |
O51 | 0.444 (1) | 0.129 (1) | 0.3826 (8) | 0.045 (3)* | |
O52 | 0.216 (1) | 0.368 (1) | 0.4254 (8) | 0.049 (3)* | |
O53 | 0.739 (2) | 0.094 (2) | 0.259 (1) | 0.098 (7)* | |
O54 | 0.715 (1) | 0.035 (1) | 0.4488 (9) | 0.052 (4)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W1 | 0.0248 (4) | 0.0289 (4) | 0.0428 (5) | −0.0120 (4) | 0.0057 (3) | −0.0104 (3) |
W2 | 0.0483 (5) | 0.0324 (5) | 0.0244 (4) | −0.0207 (4) | −0.0081 (4) | −0.0021 (3) |
W3 | 0.0309 (4) | 0.0221 (4) | 0.0279 (4) | −0.0138 (3) | −0.0021 (3) | −0.0034 (3) |
W4 | 0.0217 (3) | 0.0240 (3) | 0.0388 (4) | −0.0051 (3) | −0.0082 (3) | −0.0108 (3) |
W5 | 0.0246 (3) | 0.0234 (3) | 0.0353 (4) | −0.0077 (3) | −0.0015 (3) | −0.0114 (3) |
W6 | 0.0347 (4) | 0.0253 (3) | 0.0252 (3) | −0.0144 (3) | −0.0057 (3) | −0.0077 (3) |
W7 | 0.0339 (4) | 0.0259 (4) | 0.0303 (3) | −0.0101 (3) | −0.0135 (3) | −0.0054 (3) |
W8 | 0.0251 (3) | 0.0199 (3) | 0.0286 (3) | −0.0068 (3) | −0.0075 (3) | −0.0057 (2) |
W9 | 0.0246 (3) | 0.0198 (3) | 0.0282 (3) | −0.0077 (3) | −0.0076 (3) | −0.0064 (2) |
W10 | 0.057 (6) | 0.092 (9) | 0.064 (7) | −0.058 (7) | 0.017 (5) | −0.008 (6) |
W11 | 0.074 (7) | 0.069 (7) | 0.029 (4) | −0.035 (6) | 0.017 (4) | −0.009 (4) |
W12 | 0.073 (7) | 0.054 (7) | 0.040 (5) | −0.026 (6) | −0.006 (5) | 0.020 (5) |
Ge1 | 0.0227 (8) | 0.0197 (8) | 0.0215 (8) | −0.0097 (7) | −0.0034 (6) | −0.0056 (6) |
Na1 | 0.040 (4) | 0.041 (5) | 0.041 (4) | −0.007 (4) | −0.011 (4) | −0.013 (3) |
Na2 | 0.051 (5) | 0.038 (5) | 0.048 (4) | −0.024 (4) | −0.005 (4) | −0.005 (4) |
Na3 | 0.039 (4) | 0.043 (5) | 0.054 (5) | −0.009 (4) | −0.013 (4) | −0.025 (4) |
Na4 | 0.052 (9) | 0.022 (7) | 0.040 (8) | −0.023 (7) | −0.023 (7) | 0.012 (6) |
Na5 | 0.071 (6) | 0.059 (6) | 0.041 (4) | −0.026 (5) | −0.007 (4) | −0.006 (4) |
Na6 | 0.051 (6) | 0.051 (6) | 0.072 (6) | −0.004 (5) | −0.021 (5) | −0.006 (5) |
Na7 | 0.071 (8) | 0.082 (9) | 0.103 (9) | −0.019 (7) | −0.004 (7) | −0.029 (7) |
Na8 | 0.17 (2) | 0.26 (3) | 0.069 (9) | −0.14 (2) | −0.010 (10) | 0.01 (1) |
Na9 | 0.15 (2) | 0.19 (2) | 0.10 (1) | −0.08 (2) | −0.03 (1) | 0.02 (1) |
O1 | 0.027 (8) | 0.04 (1) | 0.07 (1) | −0.012 (7) | 0.012 (7) | −0.028 (8) |
O2 | 0.042 (8) | 0.046 (9) | 0.031 (7) | −0.023 (8) | −0.006 (6) | −0.012 (6) |
O3 | 0.047 (9) | 0.044 (9) | 0.034 (7) | −0.028 (8) | −0.009 (7) | 0.013 (7) |
O4 | 0.033 (8) | 0.05 (1) | 0.10 (1) | −0.014 (7) | −0.015 (8) | −0.032 (9) |
O5 | 0.020 (6) | 0.043 (9) | 0.062 (9) | −0.002 (6) | 0.016 (6) | −0.032 (7) |
O6 | 0.056 (9) | 0.046 (9) | 0.037 (7) | −0.031 (8) | −0.001 (6) | −0.023 (6) |
O7 | 0.052 (9) | 0.026 (7) | 0.058 (9) | −0.006 (6) | −0.033 (7) | −0.005 (6) |
O8 | 0.037 (7) | 0.029 (7) | 0.044 (7) | −0.010 (6) | −0.016 (6) | −0.003 (6) |
O9 | 0.045 (8) | 0.024 (7) | 0.050 (8) | −0.009 (6) | −0.016 (6) | −0.018 (6) |
O10 | 0.056 (10) | 0.039 (9) | 0.020 (6) | −0.031 (8) | 0.000 (6) | −0.004 (6) |
O11 | 0.036 (7) | 0.022 (7) | 0.014 (6) | −0.016 (6) | 0.007 (5) | 0.004 (5) |
O12 | 0.034 (7) | 0.017 (6) | 0.024 (6) | −0.008 (6) | 0.002 (6) | 0.005 (5) |
O13 | 0.032 (6) | 0.023 (6) | 0.037 (7) | −0.012 (6) | 0.008 (5) | −0.006 (5) |
O14 | 0.067 (10) | 0.032 (7) | 0.040 (7) | −0.028 (7) | −0.003 (7) | −0.016 (6) |
O15 | 0.051 (8) | 0.027 (7) | 0.043 (7) | −0.013 (6) | −0.019 (7) | −0.001 (6) |
O16 | 0.043 (8) | 0.038 (8) | 0.030 (6) | −0.023 (7) | −0.004 (6) | 0.002 (5) |
O17 | 0.025 (6) | 0.041 (8) | 0.030 (6) | −0.016 (6) | 0.003 (5) | −0.008 (5) |
O18 | 0.035 (7) | 0.031 (7) | 0.055 (8) | −0.016 (6) | −0.018 (6) | −0.002 (6) |
O19 | 0.048 (8) | 0.025 (6) | 0.030 (6) | −0.012 (6) | −0.008 (6) | −0.015 (5) |
O20 | 0.020 (6) | 0.031 (7) | 0.048 (7) | 0.007 (5) | −0.008 (5) | −0.028 (6) |
O21 | 0.064 (9) | 0.038 (8) | 0.030 (6) | −0.026 (7) | −0.028 (7) | 0.006 (5) |
O22 | 0.016 (5) | 0.049 (8) | 0.028 (6) | −0.009 (6) | 0.003 (5) | −0.015 (6) |
O23 | 0.029 (6) | 0.026 (6) | 0.033 (6) | −0.010 (5) | −0.008 (5) | −0.006 (5) |
O24 | 0.017 (5) | 0.036 (7) | 0.036 (6) | −0.001 (5) | −0.001 (5) | −0.018 (5) |
O25 | 0.030 (6) | 0.026 (6) | 0.022 (5) | −0.013 (5) | 0.007 (5) | −0.008 (4) |
O26 | 0.006 (4) | 0.026 (6) | 0.046 (7) | 0.002 (5) | 0.001 (5) | −0.012 (5) |
O27 | 0.024 (5) | 0.026 (6) | 0.033 (6) | −0.016 (5) | −0.011 (5) | −0.009 (5) |
O28 | 0.023 (5) | 0.007 (5) | 0.038 (6) | 0.004 (4) | −0.012 (5) | −0.012 (4) |
O29 | 0.038 (8) | 0.019 (6) | 0.059 (9) | −0.010 (6) | 0.000 (7) | −0.002 (6) |
O30 | 0.027 (6) | 0.014 (5) | 0.045 (7) | −0.007 (5) | −0.015 (5) | 0.003 (5) |
O31 | 0.024 (6) | 0.026 (7) | 0.044 (7) | 0.001 (5) | −0.014 (6) | −0.004 (5) |
O32 | 0.037 (7) | 0.028 (7) | 0.037 (7) | −0.007 (6) | −0.019 (6) | −0.004 (5) |
O33 | 0.026 (6) | 0.022 (6) | 0.037 (6) | −0.005 (5) | −0.009 (5) | −0.011 (5) |
O34 | 0.059 (9) | 0.023 (7) | 0.049 (8) | −0.006 (7) | −0.022 (7) | −0.007 (6) |
Geometric parameters (Å, º) top
W1—O1 | 1.77 (1) | W12—O25 | 2.14 (1) |
W1—O13 | 1.82 (1) | W12—O15 | 2.17 (2) |
W1—O18 | 1.92 (1) | Ge1—O26 | 1.75 (1) |
W1—O12 | 1.98 (1) | Ge1—O27 | 1.759 (9) |
W1—O10 | 1.98 (1) | Ge1—O28 | 1.77 (1) |
W1—O25 | 2.29 (1) | Ge1—O25 | 1.78 (1) |
W2—O2 | 1.75 (1) | Na1—O31 | 2.44 (1) |
W2—O14 | 1.89 (1) | Na1—O30 | 2.48 (2) |
W2—O15 | 1.94 (1) | Na1—O34i | 2.51 (2) |
W2—O11 | 1.96 (1) | Na1—O52 | 2.51 (2) |
W2—O10 | 1.96 (2) | Na1—O33i | 2.53 (1) |
W2—O25 | 2.34 (1) | Na1—O27 | 2.77 (1) |
W3—O3 | 1.77 (1) | Na2—O53 | 2.35 (2) |
W3—O17 | 1.84 (1) | Na2—O54 | 2.41 (2) |
W3—O16 | 1.86 (1) | Na2—O33i | 2.44 (1) |
W3—O12 | 1.94 (1) | Na2—O30 | 2.53 (1) |
W3—O11 | 1.98 (1) | Na2—O51 | 2.55 (2) |
W3—O25 | 2.28 (1) | Na2—O29 | 2.56 (2) |
W4—O4 | 1.73 (1) | Na2—O20 | 3.02 (2) |
W4—O34 | 1.77 (1) | Na3—O50 | 2.39 (1) |
W4—O24 | 1.90 (1) | Na3—O30 | 2.41 (1) |
W4—O19 | 1.94 (1) | Na3—O51 | 2.42 (2) |
W4—O18 | 2.19 (1) | Na3—O52 | 2.45 (2) |
W4—O26 | 2.24 (1) | Na3—O49 | 2.47 (2) |
W5—O29 | 1.73 (1) | Na3—O48 | 2.56 (2) |
W5—O5 | 1.75 (1) | Na4—O32 | 2.45 (2) |
W5—O20 | 1.94 (1) | Na4—O29i | 2.45 (2) |
W5—O19 | 1.94 (1) | Na4—O34i | 2.51 (2) |
W5—O13 | 2.14 (1) | Na4—O33 | 2.52 (2) |
W5—O26 | 2.25 (1) | Na4—O26i | 2.75 (2) |
W6—O6 | 1.75 (1) | Na4—O28 | 2.77 (2) |
W6—O30 | 1.76 (1) | Na5—O37 | 2.34 (2) |
W6—O20 | 1.87 (1) | Na5—O36 | 2.37 (2) |
W6—O21 | 1.92 (1) | Na5—O49ii | 2.38 (2) |
W6—O14 | 2.15 (1) | Na5—O35 | 2.39 (3) |
W6—O27 | 2.26 (1) | Na5—O2 | 2.44 (2) |
W7—O7 | 1.73 (1) | Na5—O50ii | 2.46 (2) |
W7—O31 | 1.78 (1) | Na6—O34i | 2.39 (2) |
W7—O22 | 1.90 (1) | Na6—O45 | 2.40 (2) |
W7—O21 | 1.95 (1) | Na6—O38 | 2.43 (2) |
W7—O15 | 2.10 (1) | Na6—O32 | 2.49 (2) |
W7—O27 | 2.25 (1) | Na6—O31 | 2.56 (2) |
W8—O32 | 1.76 (1) | Na6—O39 | 2.61 (3) |
W8—O8 | 1.77 (1) | Na6—O22 | 2.92 (2) |
W8—O22 | 1.92 (1) | Na7—O39i | 2.23 (3) |
W8—O23 | 1.98 (1) | Na7—O54 | 2.28 (2) |
W8—O16 | 2.12 (1) | Na7—O29 | 2.41 (2) |
W8—O28 | 2.26 (1) | Na7—O32i | 2.44 (2) |
W9—O9 | 1.75 (1) | Na7—O38iii | 2.46 (2) |
W9—O33 | 1.76 (1) | Na7—O39iii | 2.81 (3) |
W9—O24 | 1.90 (1) | Na8—O35 | 2.35 (3) |
W9—O23 | 1.94 (1) | Na8—O40 | 2.35 (3) |
W9—O17 | 2.16 (1) | Na8—O6 | 2.42 (2) |
W9—O28 | 2.218 (10) | Na8—O41 | 2.46 (3) |
W10—O18 | 1.87 (2) | Na8—O40ii | 2.54 (3) |
W10—O17 | 2.00 (2) | Na8—O14 | 2.69 (2) |
W10—O25 | 2.37 (1) | Na9—O7 | 2.41 (2) |
W11—O13 | 1.77 (2) | Na9—O44 | 2.43 (3) |
W11—O14 | 2.21 (2) | Na9—O46 | 2.43 (4) |
W11—O25 | 2.32 (1) | Na9—O43 | 2.45 (3) |
W12—O16 | 2.01 (2) | Na9—O42 | 2.50 (3) |
| | | |
O1—W1—O13 | 103.3 (6) | O6—W6—O20 | 101.7 (6) |
O1—W1—O18 | 102.7 (7) | O6—W6—O21 | 96.0 (6) |
O1—W1—O12 | 99.3 (7) | O6—W6—O14 | 90.4 (5) |
O1—W1—O10 | 97.1 (7) | O6—W6—O27 | 167.9 (6) |
O1—W1—O25 | 167.2 (6) | O30—W6—O20 | 96.5 (5) |
O13—W1—O18 | 90.3 (5) | O30—W6—O21 | 96.4 (5) |
O13—W1—O12 | 157.2 (5) | O30—W6—O14 | 168.1 (5) |
O13—W1—O10 | 88.3 (6) | O30—W6—O27 | 86.3 (5) |
O13—W1—O25 | 86.1 (5) | O20—W6—O21 | 155.5 (5) |
O18—W1—O12 | 88.1 (5) | O20—W6—O14 | 81.6 (6) |
O18—W1—O10 | 160.0 (6) | O20—W6—O27 | 86.3 (4) |
O18—W1—O25 | 85.9 (5) | O21—W6—O14 | 81.5 (6) |
O12—W1—O10 | 85.6 (6) | O21—W6—O27 | 73.8 (4) |
O12—W1—O25 | 71.2 (5) | O14—W6—O27 | 81.8 (4) |
O10—W1—O25 | 74.1 (5) | O7—W7—O31 | 102.0 (6) |
O2—W2—O14 | 103.9 (6) | O7—W7—O22 | 101.6 (6) |
O2—W2—O15 | 102.0 (6) | O7—W7—O21 | 96.3 (6) |
O2—W2—O11 | 98.3 (6) | O7—W7—O15 | 92.2 (6) |
O2—W2—O10 | 100.8 (6) | O7—W7—O27 | 167.5 (6) |
O2—W2—O25 | 168.8 (5) | O31—W7—O22 | 95.2 (5) |
O14—W2—O15 | 87.4 (6) | O31—W7—O21 | 96.3 (6) |
O14—W2—O11 | 157.7 (5) | O31—W7—O15 | 165.8 (5) |
O14—W2—O10 | 87.5 (6) | O31—W7—O27 | 86.3 (4) |
O14—W2—O25 | 85.7 (5) | O22—W7—O21 | 156.1 (5) |
O15—W2—O11 | 89.1 (5) | O22—W7—O15 | 81.0 (5) |
O15—W2—O10 | 157.2 (5) | O22—W7—O27 | 86.6 (4) |
O15—W2—O25 | 84.0 (5) | O21—W7—O15 | 82.7 (5) |
O11—W2—O10 | 87.2 (6) | O21—W7—O27 | 73.3 (4) |
O11—W2—O25 | 72.1 (5) | O15—W7—O27 | 79.8 (4) |
O10—W2—O25 | 73.5 (5) | O32—W8—O8 | 100.6 (6) |
O3—W3—O17 | 103.1 (6) | O32—W8—O22 | 93.2 (5) |
O3—W3—O16 | 103.0 (6) | O32—W8—O23 | 94.8 (5) |
O3—W3—O12 | 98.0 (6) | O32—W8—O16 | 167.3 (5) |
O3—W3—O11 | 96.4 (6) | O32—W8—O28 | 87.8 (5) |
O3—W3—O25 | 166.0 (6) | O8—W8—O22 | 100.4 (5) |
O17—W3—O16 | 91.6 (5) | O8—W8—O23 | 98.1 (5) |
O17—W3—O12 | 90.9 (5) | O8—W8—O16 | 92.1 (6) |
O17—W3—O11 | 160.2 (5) | O8—W8—O28 | 168.0 (5) |
O17—W3—O25 | 87.3 (5) | O22—W8—O23 | 158.2 (5) |
O16—W3—O12 | 157.7 (6) | O22—W8—O16 | 84.1 (5) |
O16—W3—O11 | 87.4 (5) | O22—W8—O28 | 87.5 (4) |
O16—W3—O25 | 85.8 (5) | O23—W8—O16 | 83.7 (5) |
O12—W3—O11 | 82.9 (6) | O23—W8—O28 | 72.5 (4) |
O12—W3—O25 | 72.2 (5) | O16—W8—O28 | 79.7 (5) |
O11—W3—O25 | 72.9 (5) | O9—W9—O33 | 101.1 (6) |
O4—W4—O34 | 101.7 (7) | O9—W9—O24 | 100.5 (6) |
O4—W4—O24 | 101.1 (6) | O9—W9—O23 | 97.4 (5) |
O4—W4—O19 | 98.8 (6) | O9—W9—O17 | 90.0 (5) |
O4—W4—O18 | 89.5 (7) | O9—W9—O28 | 168.6 (5) |
O4—W4—O26 | 168.0 (6) | O33—W9—O24 | 95.5 (5) |
O34—W4—O24 | 94.8 (6) | O33—W9—O23 | 96.2 (5) |
O34—W4—O19 | 98.3 (6) | O33—W9—O17 | 168.9 (5) |
O34—W4—O18 | 168.6 (5) | O33—W9—O28 | 87.8 (4) |
O34—W4—O26 | 88.6 (5) | O24—W9—O23 | 156.3 (5) |
O24—W4—O19 | 153.4 (5) | O24—W9—O17 | 81.6 (5) |
O24—W4—O18 | 81.0 (5) | O24—W9—O28 | 85.6 (4) |
O24—W4—O26 | 84.0 (4) | O23—W9—O17 | 83.0 (5) |
O19—W4—O18 | 81.6 (5) | O23—W9—O28 | 74.3 (4) |
O19—W4—O26 | 73.4 (5) | O17—W9—O28 | 81.4 (4) |
O18—W4—O26 | 80.4 (4) | O18—W10—O17 | 105.8 (8) |
O29—W5—O5 | 102.5 (7) | O18—W10—O25 | 84.6 (6) |
O29—W5—O20 | 95.2 (6) | O18—W10—O47iv | 90 (1) |
O29—W5—O19 | 95.3 (6) | O17—W10—O25 | 81.2 (5) |
O29—W5—O13 | 167.2 (6) | O13—W11—O14 | 102.1 (7) |
O29—W5—O26 | 87.4 (5) | O13—W11—O25 | 86.4 (6) |
O5—W5—O20 | 100.8 (6) | O14—W11—O25 | 79.3 (5) |
O5—W5—O19 | 99.0 (6) | O16—W12—O25 | 86.1 (6) |
O5—W5—O13 | 90.3 (6) | O16—W12—O15 | 92.4 (7) |
O5—W5—O26 | 168.1 (5) | O25—W12—O15 | 83.6 (6) |
O20—W5—O19 | 155.1 (5) | O26—Ge1—O27 | 111.5 (5) |
O20—W5—O13 | 81.4 (5) | O26—Ge1—O28 | 111.3 (5) |
O20—W5—O26 | 84.7 (4) | O26—Ge1—O25 | 107.7 (5) |
O19—W5—O13 | 83.4 (5) | O27—Ge1—O28 | 108.0 (5) |
O19—W5—O26 | 73.2 (5) | O27—Ge1—O25 | 110.5 (5) |
O13—W5—O26 | 80.0 (4) | O28—Ge1—O25 | 107.8 (5) |
O6—W6—O30 | 101.6 (6) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z; (iii) x+1, y−1, z; (iv) x+1, y, z. |