The title compound, K8[{WVIO2(SO4)2}2(μ-SO4)2], precipitated from a melt of tungsten trioxide and potassium sulfate in potassium pyrosulfate. The WVI coordination sphere in the independent K4[WVIO2(SO4)3] moiety is completed by inversion symmetry, resulting in a dimer with two bridging sulfate ligands and a unit cell with two dimeric units.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean
(S-O) = 0.002 Å
- R factor = 0.013
- wR factor = 0.031
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.99 Ratio
PLAT430_ALERT_2_C Short Inter D...A Contact O1 .. O10 .. 2.90 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5
K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: CIFTAB in SHELX97-2 (Sheldrick, 2001).
Octapotassium
di-µ-sulfato-
κ2O:
O'-bis[
cis-dioxo-
cis-disulfatotungstate(VI)]
top
Crystal data top
K8[WO4(SO4)6] | F(000) = 1240 |
Mr = 1320.86 | Dx = 3.266 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5682 reflections |
a = 9.4362 (5) Å | θ = 2.5–28.0° |
b = 13.9625 (7) Å | µ = 10.38 mm−1 |
c = 10.1948 (5) Å | T = 120 K |
β = 90.780 (1)° | Tabular, colorless |
V = 1343.07 (12) Å3 | 0.18 × 0.10 × 0.05 mm |
Z = 2 | |
Data collection top
Bruker Platform/CCD diffractometer | 2458 independent reflections |
Radiation source: normal-focus sealed tube | 2429 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
profile data from ω scans | θmax = 25.3°, θmin = 2.5° |
Absorption correction: integration XPREP (Bruker, 2001) | h = −11→11 |
Tmin = 0.245, Tmax = 0.619 | k = −16→16 |
13095 measured reflections | l = −12→12 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.013 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.031 | w = 1/[σ2(Fo2) + (0.0121P)2 + 2.1788P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max = 0.001 |
2458 reflections | Δρmax = 0.58 e Å−3 |
199 parameters | Δρmin = −0.44 e Å−3 |
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. Five frame series were filtered for statistical outliers then corrected for
absorption by integration using SHELXTL/XPREP (Bruker, 2001)
before using SAINT/SADABS (Bruker, 2002) to sort, merge, and
scale the combined data. A series of identical frames was collected twice
during the experiment to monitor decay. No decay correction was applied.
Systematic conditions suggested the unambiguous space group. The structure was
solved by direct methods (Sheldrick, 2001). The space group choice was
confirmed by successful convergence of the full-matrix least-squares
refinement on F2 (Sheldrick, 2001). The highest peaks in the final
difference Fourier map were 0.98 Å and 0.87 Å from atoms W1 and O1,
respectively; the deepest hole was 0.74 Å from S3. The final map had no
other significant features. A final analysis of variance between observed and
calculated structure factors showed no dependence on amplitude or resolution. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
W1 | 0.167155 (11) | 0.378486 (7) | 0.083299 (10) | 0.00768 (4) | |
S1 | 0.08697 (7) | 0.49756 (5) | −0.20754 (6) | 0.00853 (13) | |
S2 | 0.47796 (7) | 0.28010 (5) | 0.02132 (7) | 0.01076 (14) | |
S3 | 0.02707 (7) | 0.15499 (5) | 0.04722 (6) | 0.00912 (13) | |
O1 | 0.2338 (2) | 0.49339 (14) | 0.09336 (19) | 0.0153 (4) | |
O2 | 0.2094 (2) | 0.33519 (14) | 0.23580 (19) | 0.0137 (4) | |
O3 | 0.0958 (2) | 0.41250 (13) | −0.12018 (18) | 0.0115 (4) | |
O4 | 0.03432 (19) | 0.58184 (13) | −0.12471 (19) | 0.0114 (4) | |
O5 | −0.0130 (2) | 0.47739 (14) | −0.31210 (18) | 0.0135 (4) | |
O6 | 0.2256 (2) | 0.52544 (13) | −0.25320 (19) | 0.0130 (4) | |
O7 | 0.3270 (2) | 0.32171 (15) | −0.01132 (19) | 0.0166 (4) | |
O8 | 0.4858 (2) | 0.26308 (15) | 0.16109 (19) | 0.0178 (4) | |
O9 | 0.4873 (3) | 0.19490 (17) | −0.0578 (2) | 0.0308 (6) | |
O10 | 0.5747 (3) | 0.35493 (19) | −0.0166 (3) | 0.0338 (6) | |
O11 | 0.0556 (2) | 0.25956 (13) | 0.01147 (19) | 0.0133 (4) | |
O12 | 0.1453 (2) | 0.11950 (13) | 0.1276 (2) | 0.0160 (4) | |
O13 | 0.0135 (2) | 0.10445 (14) | −0.0768 (2) | 0.0181 (5) | |
O14 | −0.1057 (2) | 0.15340 (15) | 0.1199 (2) | 0.0167 (4) | |
K1 | 0.32372 (6) | 0.17573 (4) | 0.33893 (6) | 0.01357 (13) | |
K2 | 0.50716 (6) | 0.50475 (5) | 0.19847 (6) | 0.01533 (13) | |
K3 | 0.20905 (6) | 0.46053 (5) | 0.47727 (6) | 0.01602 (13) | |
K4 | 0.24597 (6) | 0.21985 (4) | −0.22989 (6) | 0.01415 (13) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W1 | 0.00668 (6) | 0.00793 (6) | 0.00842 (7) | 0.00067 (4) | −0.00051 (4) | −0.00047 (4) |
S1 | 0.0078 (3) | 0.0089 (3) | 0.0088 (3) | 0.0011 (2) | 0.0006 (2) | 0.0009 (3) |
S2 | 0.0074 (3) | 0.0141 (3) | 0.0109 (3) | 0.0023 (3) | 0.0007 (2) | 0.0002 (3) |
S3 | 0.0094 (3) | 0.0077 (3) | 0.0102 (3) | −0.0008 (3) | 0.0003 (3) | 0.0002 (3) |
O1 | 0.0136 (10) | 0.0149 (10) | 0.0175 (11) | −0.0035 (8) | −0.0003 (8) | −0.0009 (8) |
O2 | 0.0126 (10) | 0.0167 (10) | 0.0120 (10) | 0.0044 (8) | 0.0004 (8) | −0.0001 (8) |
O3 | 0.0151 (10) | 0.0085 (9) | 0.0108 (10) | 0.0007 (8) | −0.0006 (8) | 0.0014 (8) |
O4 | 0.0074 (9) | 0.0109 (10) | 0.0157 (10) | 0.0012 (8) | −0.0006 (7) | −0.0023 (8) |
O5 | 0.0158 (10) | 0.0138 (10) | 0.0108 (10) | 0.0017 (8) | −0.0033 (8) | 0.0005 (8) |
O6 | 0.0108 (10) | 0.0124 (9) | 0.0158 (10) | 0.0009 (8) | 0.0049 (8) | 0.0006 (8) |
O7 | 0.0103 (10) | 0.0284 (12) | 0.0110 (10) | 0.0105 (9) | −0.0004 (8) | −0.0035 (9) |
O8 | 0.0133 (10) | 0.0286 (12) | 0.0114 (10) | 0.0035 (9) | −0.0006 (8) | 0.0036 (9) |
O9 | 0.0398 (15) | 0.0277 (13) | 0.0246 (13) | 0.0219 (11) | −0.0095 (11) | −0.0112 (10) |
O10 | 0.0204 (13) | 0.0469 (15) | 0.0341 (14) | −0.0161 (11) | −0.0016 (10) | 0.0169 (12) |
O11 | 0.0163 (10) | 0.0085 (9) | 0.0149 (10) | −0.0035 (8) | −0.0038 (8) | 0.0009 (8) |
O12 | 0.0138 (11) | 0.0125 (10) | 0.0216 (11) | −0.0002 (8) | −0.0045 (9) | 0.0022 (8) |
O13 | 0.0302 (12) | 0.0125 (10) | 0.0115 (10) | −0.0031 (9) | 0.0014 (9) | −0.0023 (8) |
O14 | 0.0108 (10) | 0.0189 (11) | 0.0205 (11) | −0.0026 (8) | 0.0047 (8) | −0.0001 (9) |
K1 | 0.0117 (3) | 0.0126 (3) | 0.0163 (3) | −0.0004 (2) | −0.0019 (2) | 0.0031 (2) |
K2 | 0.0126 (3) | 0.0200 (3) | 0.0133 (3) | 0.0034 (2) | −0.0029 (2) | −0.0022 (2) |
K3 | 0.0135 (3) | 0.0224 (3) | 0.0121 (3) | 0.0026 (3) | −0.0017 (2) | 0.0028 (3) |
K4 | 0.0141 (3) | 0.0137 (3) | 0.0146 (3) | −0.0010 (2) | −0.0026 (2) | −0.0006 (2) |
Geometric parameters (Å, º) top
W1—O1 | 1.7258 (19) | O7—K4 | 2.743 (2) |
W1—O2 | 1.7102 (19) | O9—K4 | 2.877 (2) |
W1—O3 | 2.2237 (19) | O9—K3viii | 3.033 (2) |
W1—O4i | 2.0302 (18) | O10—K2iii | 2.799 (3) |
W1—O7 | 1.9681 (19) | O10—K1viii | 2.823 (3) |
W1—O11 | 2.0930 (18) | O10—K2 | 3.102 (3) |
W1—K2 | 3.8311 (6) | O11—K1v | 2.931 (2) |
W1—K4 | 3.9646 (6) | O11—K4 | 3.116 (2) |
W1—K1 | 4.1090 (6) | O12—K2ix | 2.802 (2) |
S1—O5 | 1.441 (2) | O12—K1 | 2.827 (2) |
S1—O6 | 1.447 (2) | O12—K3ix | 2.828 (2) |
S1—O3 | 1.4861 (19) | O13—K2v | 2.752 (2) |
S1—O4 | 1.5349 (19) | O13—K3v | 3.070 (2) |
S2—O9 | 1.441 (2) | O13—K4 | 3.152 (2) |
S2—O10 | 1.443 (2) | O14—K4x | 2.738 (2) |
S2—O8 | 1.445 (2) | O14—K3v | 2.762 (2) |
S2—O7 | 1.5700 (19) | O14—K2ix | 2.925 (2) |
S2—K4 | 3.4505 (9) | K1—O1ix | 2.695 (2) |
S2—K2 | 3.6281 (9) | K1—O10x | 2.823 (3) |
S3—O13 | 1.452 (2) | K1—O3iv | 2.873 (2) |
S3—O12 | 1.462 (2) | K1—O11iv | 2.931 (2) |
S3—O14 | 1.464 (2) | K1—O5iv | 3.063 (2) |
S3—O11 | 1.5296 (19) | K1—K3 | 4.3605 (9) |
S3—K4 | 3.6369 (9) | K2—O6iii | 2.610 (2) |
O1—K1ii | 2.695 (2) | K2—O13iv | 2.752 (2) |
O1—K2 | 2.784 (2) | K2—O10iii | 2.799 (3) |
O2—K1 | 2.682 (2) | K2—O12ii | 2.802 (2) |
O8—K1 | 2.681 (2) | K2—O14ii | 2.925 (2) |
O6—K2iii | 2.610 (2) | K2—K3 | 4.0732 (9) |
O5—K3i | 2.632 (2) | K3—O5i | 2.632 (2) |
O8—K4iv | 2.692 (2) | K3—O14iv | 2.762 (2) |
O8—K2 | 3.401 (2) | K3—O12ii | 2.828 (2) |
O2—K3 | 3.020 (2) | K3—O6xi | 2.896 (2) |
O3—K1v | 2.873 (2) | K3—O5xi | 3.029 (2) |
O3—K4 | 3.246 (2) | K3—O9x | 3.033 (2) |
O4—W1i | 2.0302 (18) | K3—O13iv | 3.070 (2) |
O4—K4vi | 3.208 (2) | K4—O8v | 2.692 (2) |
O5—K3vii | 3.029 (2) | K4—O6xii | 2.733 (2) |
O5—K1v | 3.063 (2) | K4—O14viii | 2.738 (2) |
O6—K4vi | 2.733 (2) | K4—O4xii | 3.208 (2) |
O6—K3vii | 2.896 (2) | | |
| | | |
O2—W1—O1 | 101.20 (9) | O1ix—K1—K3 | 136.63 (5) |
O2—W1—O7 | 97.61 (9) | O10x—K1—K3 | 75.97 (5) |
O1—W1—O7 | 97.03 (9) | O12—K1—K3 | 110.60 (4) |
O2—W1—O4i | 96.59 (8) | O3iv—K1—K3 | 124.70 (4) |
O1—W1—O4i | 94.34 (9) | O11iv—K1—K3 | 73.22 (4) |
O7—W1—O4i | 159.71 (8) | O5iv—K1—K3 | 158.11 (4) |
O2—W1—O11 | 98.49 (9) | W1—K1—K3 | 59.215 (12) |
O1—W1—O11 | 159.97 (8) | O6iii—K2—O13iv | 73.89 (6) |
O7—W1—O11 | 83.92 (8) | O6iii—K2—O1 | 163.86 (6) |
O4i—W1—O11 | 79.70 (8) | O13iv—K2—O1 | 107.36 (7) |
O2—W1—O3 | 170.94 (8) | O6iii—K2—O10iii | 120.78 (7) |
O1—W1—O3 | 87.85 (8) | O13iv—K2—O10iii | 160.39 (8) |
O7—W1—O3 | 81.56 (8) | O1—K2—O10iii | 62.55 (6) |
O4i—W1—O3 | 82.13 (7) | O6iii—K2—O12ii | 117.39 (6) |
O11—W1—O3 | 72.45 (7) | O13iv—K2—O12ii | 78.19 (6) |
O2—W1—K2 | 72.55 (7) | O1—K2—O12ii | 78.18 (6) |
O1—W1—K2 | 41.49 (7) | O10iii—K2—O12ii | 83.09 (7) |
O7—W1—K2 | 72.03 (6) | O6iii—K2—O14ii | 71.41 (6) |
O4i—W1—K2 | 126.40 (5) | O13iv—K2—O14ii | 82.12 (6) |
O11—W1—K2 | 152.55 (5) | O1—K2—O14ii | 124.68 (6) |
O3—W1—K2 | 115.43 (5) | O10iii—K2—O14ii | 90.30 (7) |
O2—W1—K4 | 119.39 (6) | O12ii—K2—O14ii | 49.84 (6) |
O1—W1—K4 | 119.67 (7) | O6iii—K2—O10 | 80.50 (6) |
O7—W1—K4 | 39.36 (6) | O13iv—K2—O10 | 102.26 (6) |
O4i—W1—K4 | 120.43 (5) | O1—K2—O10 | 83.55 (6) |
O11—W1—K4 | 51.24 (6) | O10iii—K2—O10 | 93.51 (8) |
O3—W1—K4 | 54.96 (5) | O12ii—K2—O10 | 160.89 (6) |
K2—W1—K4 | 109.780 (13) | O14ii—K2—O10 | 149.23 (6) |
O2—W1—K1 | 26.17 (7) | O6iii—K2—O8 | 85.37 (6) |
O1—W1—K1 | 118.37 (7) | O13iv—K2—O8 | 62.89 (6) |
O7—W1—K1 | 76.23 (6) | O1—K2—O8 | 81.21 (6) |
O4i—W1—K1 | 112.69 (5) | O10iii—K2—O8 | 127.21 (7) |
O11—W1—K1 | 81.38 (5) | O12ii—K2—O8 | 127.45 (6) |
O3—W1—K1 | 147.20 (5) | O14ii—K2—O8 | 142.44 (6) |
K2—W1—K1 | 80.229 (13) | O10—K2—O8 | 42.64 (6) |
K4—W1—K1 | 93.217 (13) | O6iii—K2—S2 | 91.91 (5) |
O5—S1—O6 | 113.55 (12) | O13iv—K2—S2 | 86.33 (5) |
O5—S1—O3 | 108.53 (11) | O1—K2—S2 | 72.27 (4) |
O6—S1—O3 | 111.37 (11) | O10iii—K2—S2 | 104.89 (6) |
O5—S1—O4 | 110.08 (11) | O12ii—K2—S2 | 140.64 (5) |
O6—S1—O4 | 105.74 (11) | O14ii—K2—S2 | 161.80 (5) |
O3—S1—O4 | 107.39 (11) | O10—K2—S2 | 23.11 (4) |
O9—S2—O10 | 113.86 (16) | O8—K2—S2 | 23.45 (3) |
O9—S2—O8 | 114.42 (14) | O6iii—K2—W1 | 142.56 (5) |
O10—S2—O8 | 111.01 (14) | O13iv—K2—W1 | 90.50 (5) |
O9—S2—O7 | 104.42 (13) | O1—K2—W1 | 24.25 (4) |
O10—S2—O7 | 104.51 (14) | O10iii—K2—W1 | 84.07 (5) |
O8—S2—O7 | 107.70 (11) | O12ii—K2—W1 | 91.26 (4) |
O9—S2—K4 | 54.98 (9) | O14ii—K2—W1 | 141.10 (4) |
O10—S2—K4 | 112.02 (11) | O10—K2—W1 | 69.66 (4) |
O8—S2—K4 | 135.65 (9) | O8—K2—W1 | 57.39 (3) |
O7—S2—K4 | 50.82 (8) | S2—K2—W1 | 52.554 (14) |
O9—S2—K2 | 171.05 (11) | O6iii—K2—K3 | 120.06 (5) |
O10—S2—K2 | 57.54 (12) | O13iv—K2—K3 | 48.89 (5) |
O8—S2—K2 | 69.44 (9) | O1—K2—K3 | 67.35 (4) |
O7—S2—K2 | 81.26 (8) | O10iii—K2—K3 | 112.43 (6) |
K4—S2—K2 | 128.56 (2) | O12ii—K2—K3 | 43.91 (4) |
O13—S3—O12 | 112.38 (13) | O14ii—K2—K3 | 83.25 (4) |
O13—S3—O14 | 111.54 (13) | O10—K2—K3 | 122.77 (5) |
O12—S3—O14 | 111.29 (13) | O8—K2—K3 | 83.53 (4) |
O13—S3—O11 | 105.67 (11) | S2—K2—K3 | 99.66 (2) |
O12—S3—O11 | 108.77 (11) | W1—K2—K3 | 63.939 (14) |
O14—S3—O11 | 106.83 (12) | O5i—K3—O14iv | 163.90 (7) |
O13—S3—K4 | 59.27 (9) | O5i—K3—O12ii | 80.84 (6) |
O12—S3—K4 | 94.73 (9) | O14iv—K3—O12ii | 110.10 (6) |
O14—S3—K4 | 153.59 (9) | O5i—K3—O6xi | 122.16 (6) |
O11—S3—K4 | 58.24 (8) | O14iv—K3—O6xi | 69.84 (6) |
W1—O1—K1ii | 144.97 (10) | O12ii—K3—O6xi | 95.33 (6) |
W1—O1—K2 | 114.26 (9) | O5i—K3—O2 | 71.21 (6) |
K1ii—O1—K2 | 92.09 (6) | O14iv—K3—O2 | 95.02 (6) |
W1—O2—K1 | 137.50 (10) | O12ii—K3—O2 | 98.09 (6) |
W1—O2—K3 | 122.23 (9) | O6xi—K3—O2 | 162.58 (6) |
K1—O2—K3 | 99.58 (6) | O5i—K3—O5xi | 86.61 (6) |
S1—O3—W1 | 138.03 (12) | O14iv—K3—O5xi | 96.34 (6) |
S1—O3—K1v | 102.32 (9) | O12ii—K3—O5xi | 123.45 (6) |
W1—O3—K1v | 107.61 (7) | O6xi—K3—O5xi | 48.07 (5) |
S1—O3—K4 | 118.47 (10) | O2—K3—O5xi | 129.14 (6) |
W1—O3—K4 | 90.93 (6) | O5i—K3—O9x | 71.47 (6) |
K1v—O3—K4 | 89.32 (5) | O14iv—K3—O9x | 94.63 (7) |
S1—O4—W1i | 129.39 (11) | O12ii—K3—O9x | 148.78 (6) |
S1—O4—K4vi | 89.44 (8) | O6xi—K3—O9x | 111.34 (6) |
W1i—O4—K4vi | 123.03 (8) | O2—K3—O9x | 59.85 (6) |
S1—O5—K3i | 148.88 (12) | O5xi—K3—O9x | 69.90 (6) |
S1—O5—K3vii | 95.03 (9) | O5i—K3—O13iv | 129.35 (6) |
K3i—O5—K3vii | 93.39 (6) | O14iv—K3—O13iv | 48.49 (6) |
S1—O5—K1v | 95.34 (9) | O12ii—K3—O13iv | 72.74 (6) |
K3i—O5—K1v | 101.38 (6) | O6xi—K3—O13iv | 102.98 (6) |
K3vii—O5—K1v | 131.27 (7) | O2—K3—O13iv | 70.79 (5) |
S1—O6—K2iii | 139.68 (12) | O5xi—K3—O13iv | 143.91 (6) |
S1—O6—K4vi | 112.18 (10) | O9x—K3—O13iv | 114.42 (7) |
K2iii—O6—K4vi | 94.49 (6) | O5i—K3—K2 | 89.42 (5) |
S1—O6—K3vii | 100.59 (10) | O14iv—K3—K2 | 90.94 (4) |
K2iii—O6—K3vii | 101.05 (6) | O12ii—K3—K2 | 43.40 (4) |
K4vi—O6—K3vii | 104.78 (6) | O6xi—K3—K2 | 125.87 (4) |
S2—O7—W1 | 138.10 (12) | O2—K3—K2 | 60.70 (4) |
S2—O7—K4 | 102.85 (9) | O5xi—K3—K2 | 166.82 (4) |
W1—O7—K4 | 113.58 (8) | O9x—K3—K2 | 120.55 (5) |
S2—O8—K1 | 135.99 (12) | O13iv—K3—K2 | 42.49 (4) |
S2—O8—K4iv | 115.26 (11) | O5i—K3—K1 | 105.59 (5) |
K1—O8—K4iv | 106.65 (7) | O14iv—K3—K1 | 59.14 (5) |
S2—O8—K2 | 87.11 (9) | O12ii—K3—K1 | 118.00 (5) |
K1—O8—K2 | 114.14 (7) | O6xi—K3—K1 | 125.59 (4) |
K4iv—O8—K2 | 79.26 (5) | O2—K3—K1 | 37.34 (4) |
S2—O9—K4 | 100.81 (11) | O5xi—K3—K1 | 118.50 (4) |
S2—O9—K3viii | 124.91 (13) | O9x—K3—K1 | 58.88 (5) |
K4—O9—K3viii | 134.25 (8) | O13iv—K3—K1 | 55.63 (4) |
S2—O10—K2iii | 120.94 (13) | K2—K3—K1 | 74.678 (16) |
S2—O10—K1viii | 124.31 (16) | O8v—K4—O6xii | 98.73 (6) |
K2iii—O10—K1viii | 89.11 (7) | O8v—K4—O14viii | 100.49 (7) |
S2—O10—K2 | 99.35 (13) | O6xii—K4—O14viii | 123.73 (6) |
K2iii—O10—K2 | 86.49 (8) | O8v—K4—O7 | 122.14 (6) |
K1viii—O10—K2 | 130.64 (9) | O6xii—K4—O7 | 122.65 (6) |
S3—O11—W1 | 139.75 (12) | O14viii—K4—O7 | 88.87 (6) |
S3—O11—K1v | 107.75 (9) | O8v—K4—O9 | 166.53 (7) |
W1—O11—K1v | 109.46 (7) | O6xii—K4—O9 | 80.82 (6) |
S3—O11—K4 | 97.09 (9) | O14viii—K4—O9 | 90.75 (7) |
W1—O11—K4 | 97.17 (7) | O7—K4—O9 | 50.05 (6) |
K1v—O11—K4 | 90.84 (5) | O8v—K4—O11 | 77.17 (6) |
S3—O12—K2ix | 98.86 (10) | O6xii—K4—O11 | 106.54 (6) |
S3—O12—K1 | 140.80 (11) | O14viii—K4—O11 | 129.15 (6) |
K2ix—O12—K1 | 88.97 (6) | O7—K4—O11 | 54.81 (6) |
S3—O12—K3ix | 115.18 (11) | O9—K4—O11 | 90.00 (6) |
K2ix—O12—K3ix | 92.68 (6) | O8v—K4—O13 | 67.22 (6) |
K1—O12—K3ix | 102.63 (7) | O6xii—K4—O13 | 66.00 (6) |
S3—O13—K2v | 174.14 (13) | O14viii—K4—O13 | 166.38 (6) |
S3—O13—K3v | 93.38 (10) | O7—K4—O13 | 92.92 (6) |
K2v—O13—K3v | 88.62 (6) | O9—K4—O13 | 100.75 (7) |
S3—O13—K4 | 97.41 (10) | O11—K4—O13 | 44.56 (5) |
K2v—O13—K4 | 83.01 (6) | O8v—K4—O4xii | 116.99 (6) |
K3v—O13—K4 | 154.06 (8) | O6xii—K4—O4xii | 46.34 (5) |
S3—O14—K4x | 136.11 (12) | O14viii—K4—O4xii | 77.95 (6) |
S3—O14—K3v | 106.39 (11) | O7—K4—O4xii | 120.80 (6) |
K4x—O14—K3v | 110.00 (7) | O9—K4—O4xii | 72.42 (6) |
S3—O14—K2ix | 93.68 (10) | O11—K4—O4xii | 148.74 (5) |
K4x—O14—K2ix | 105.37 (7) | O13—K4—O4xii | 112.34 (5) |
K3v—O14—K2ix | 96.78 (6) | O8v—K4—O3 | 70.66 (6) |
O8—K1—O2 | 65.63 (6) | O6xii—K4—O3 | 152.66 (6) |
O8—K1—O1ix | 136.19 (7) | O14viii—K4—O3 | 83.46 (6) |
O2—K1—O1ix | 143.43 (6) | O7—K4—O3 | 53.75 (5) |
O8—K1—O10x | 155.28 (7) | O9—K4—O3 | 103.65 (6) |
O2—K1—O10x | 89.85 (7) | O11—K4—O3 | 47.26 (5) |
O1ix—K1—O10x | 63.32 (7) | O13—K4—O3 | 86.73 (5) |
O8—K1—O12 | 87.15 (6) | O4xii—K4—O3 | 160.88 (5) |
O2—K1—O12 | 72.53 (6) | O8v—K4—S2 | 148.30 (5) |
O1ix—K1—O12 | 79.22 (6) | O6xii—K4—S2 | 103.12 (5) |
O10x—K1—O12 | 82.20 (7) | O14viii—K4—S2 | 86.20 (5) |
O8—K1—O3iv | 77.08 (6) | O7—K4—S2 | 26.33 (4) |
O2—K1—O3iv | 140.05 (6) | O9—K4—S2 | 24.21 (4) |
O1ix—K1—O3iv | 74.96 (6) | O11—K4—S2 | 74.77 (4) |
O10x—K1—O3iv | 127.43 (7) | O13—K4—S2 | 101.30 (4) |
O12—K1—O3iv | 120.87 (6) | O4xii—K4—S2 | 94.70 (4) |
O8—K1—O11iv | 80.65 (6) | O3—K4—S2 | 79.51 (4) |
O2—K1—O11iv | 105.80 (6) | O8v—K4—S3 | 79.53 (5) |
O1ix—K1—O11iv | 106.79 (6) | O6xii—K4—S3 | 81.90 (4) |
O10x—K1—O11iv | 110.70 (7) | O14viii—K4—S3 | 153.59 (5) |
O12—K1—O11iv | 167.08 (6) | O7—K4—S3 | 69.70 (5) |
O3iv—K1—O11iv | 52.18 (5) | O9—K4—S3 | 87.09 (6) |
O8—K1—O5iv | 71.46 (6) | O11—K4—S3 | 24.67 (4) |
O2—K1—O5iv | 125.78 (6) | O13—K4—S3 | 23.32 (4) |
O1ix—K1—O5iv | 64.78 (6) | O4xii—K4—S3 | 125.93 (4) |
O10x—K1—O5iv | 125.77 (7) | O3—K4—S3 | 71.54 (4) |
O12—K1—O5iv | 73.83 (6) | S2—K4—S3 | 81.11 (2) |
O3iv—K1—O5iv | 47.07 (5) | O8v—K4—W1 | 95.92 (5) |
O11iv—K1—O5iv | 98.06 (5) | O6xii—K4—W1 | 128.70 (4) |
O8—K1—W1 | 57.40 (4) | O14viii—K4—W1 | 101.09 (5) |
O2—K1—W1 | 16.33 (4) | O7—K4—W1 | 27.06 (4) |
O1ix—K1—W1 | 137.85 (5) | O9—K4—W1 | 74.46 (5) |
O10x—K1—W1 | 98.09 (6) | O11—K4—W1 | 31.59 (3) |
O12—K1—W1 | 60.18 (4) | O13—K4—W1 | 75.37 (4) |
O3iv—K1—W1 | 134.46 (4) | O4xii—K4—W1 | 146.84 (4) |
O11iv—K1—W1 | 115.29 (4) | O3—K4—W1 | 34.11 (3) |
O5iv—K1—W1 | 109.94 (4) | S2—K4—W1 | 52.420 (14) |
O8—K1—K3 | 87.15 (5) | S3—K4—W1 | 53.042 (14) |
O2—K1—K3 | 43.08 (4) | | |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x+1, −y+1, −z; (iv) x+1/2, −y+1/2, z+1/2; (v) x−1/2, −y+1/2, z−1/2; (vi) −x+1/2, y+1/2, −z−1/2; (vii) x, y, z−1; (viii) x+1/2, −y+1/2, 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+1; (xii) −x+1/2, y−1/2, −z−1/2. |