Potassium bis(μ-sulfato-1κO:2κO′)bis­[cis-dioxido-cis-bis(sulfato-κO)tungstate(VI)]

The title compound, K₈[{W^VIO₂(SO₄)₂}₂(μ-SO₄)₂], precipitated from a melt of tungsten trioxide and potassium sulfate in potassium pyro­sulfate. The W^VI coordination sphere in the independent K₄[W^VIO₂(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.

Key indicators

• Single-crystal X-ray study
• T = 120 K
• Mean [sigma](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

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Computing details

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)]

Crystal data

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) Å^3	0.18 × 0.10 × 0.05 mm
Z = 2

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.013	Secondary atom site location: difference Fourier map
wR(F^2) = 0.031	w = 1/[σ^2(Fo^2) + (0.0121P)^2 + 2.1788P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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—K3^viii	3.033 (2)
W1—O4^i	2.0302 (18)	O10—K2^iii	2.799 (3)
W1—O7	1.9681 (19)	O10—K1^viii	2.823 (3)
W1—O11	2.0930 (18)	O10—K2	3.102 (3)
W1—K2	3.8311 (6)	O11—K1^v	2.931 (2)
W1—K4	3.9646 (6)	O11—K4	3.116 (2)
W1—K1	4.1090 (6)	O12—K2^ix	2.802 (2)
S1—O5	1.441 (2)	O12—K1	2.827 (2)
S1—O6	1.447 (2)	O12—K3^ix	2.828 (2)
S1—O3	1.4861 (19)	O13—K2^v	2.752 (2)
S1—O4	1.5349 (19)	O13—K3^v	3.070 (2)
S2—O9	1.441 (2)	O13—K4	3.152 (2)
S2—O10	1.443 (2)	O14—K4^x	2.738 (2)
S2—O8	1.445 (2)	O14—K3^v	2.762 (2)
S2—O7	1.5700 (19)	O14—K2^ix	2.925 (2)
S2—K4	3.4505 (9)	K1—O1^ix	2.695 (2)
S2—K2	3.6281 (9)	K1—O10^x	2.823 (3)
S3—O13	1.452 (2)	K1—O3^iv	2.873 (2)
S3—O12	1.462 (2)	K1—O11^iv	2.931 (2)
S3—O14	1.464 (2)	K1—O5^iv	3.063 (2)
S3—O11	1.5296 (19)	K1—K3	4.3605 (9)
S3—K4	3.6369 (9)	K2—O6^iii	2.610 (2)
O1—K1^ii	2.695 (2)	K2—O13^iv	2.752 (2)
O1—K2	2.784 (2)	K2—O10^iii	2.799 (3)
O2—K1	2.682 (2)	K2—O12^ii	2.802 (2)
O8—K1	2.681 (2)	K2—O14^ii	2.925 (2)
O6—K2^iii	2.610 (2)	K2—K3	4.0732 (9)
O5—K3^i	2.632 (2)	K3—O5^i	2.632 (2)
O8—K4^iv	2.692 (2)	K3—O14^iv	2.762 (2)
O8—K2	3.401 (2)	K3—O12^ii	2.828 (2)
O2—K3	3.020 (2)	K3—O6^xi	2.896 (2)
O3—K1^v	2.873 (2)	K3—O5^xi	3.029 (2)
O3—K4	3.246 (2)	K3—O9^x	3.033 (2)
O4—W1^i	2.0302 (18)	K3—O13^iv	3.070 (2)
O4—K4^vi	3.208 (2)	K4—O8^v	2.692 (2)
O5—K3^vii	3.029 (2)	K4—O6^xii	2.733 (2)
O5—K1^v	3.063 (2)	K4—O14^viii	2.738 (2)
O6—K4^vi	2.733 (2)	K4—O4^xii	3.208 (2)
O6—K3^vii	2.896 (2)
O2—W1—O1	101.20 (9)	O1^ix—K1—K3	136.63 (5)
O2—W1—O7	97.61 (9)	O10^x—K1—K3	75.97 (5)
O1—W1—O7	97.03 (9)	O12—K1—K3	110.60 (4)
O2—W1—O4^i	96.59 (8)	O3^iv—K1—K3	124.70 (4)
O1—W1—O4^i	94.34 (9)	O11^iv—K1—K3	73.22 (4)
O7—W1—O4^i	159.71 (8)	O5^iv—K1—K3	158.11 (4)
O2—W1—O11	98.49 (9)	W1—K1—K3	59.215 (12)
O1—W1—O11	159.97 (8)	O6^iii—K2—O13^iv	73.89 (6)
O7—W1—O11	83.92 (8)	O6^iii—K2—O1	163.86 (6)
O4^i—W1—O11	79.70 (8)	O13^iv—K2—O1	107.36 (7)
O2—W1—O3	170.94 (8)	O6^iii—K2—O10^iii	120.78 (7)
O1—W1—O3	87.85 (8)	O13^iv—K2—O10^iii	160.39 (8)
O7—W1—O3	81.56 (8)	O1—K2—O10^iii	62.55 (6)
O4^i—W1—O3	82.13 (7)	O6^iii—K2—O12^ii	117.39 (6)
O11—W1—O3	72.45 (7)	O13^iv—K2—O12^ii	78.19 (6)
O2—W1—K2	72.55 (7)	O1—K2—O12^ii	78.18 (6)
O1—W1—K2	41.49 (7)	O10^iii—K2—O12^ii	83.09 (7)
O7—W1—K2	72.03 (6)	O6^iii—K2—O14^ii	71.41 (6)
O4^i—W1—K2	126.40 (5)	O13^iv—K2—O14^ii	82.12 (6)
O11—W1—K2	152.55 (5)	O1—K2—O14^ii	124.68 (6)
O3—W1—K2	115.43 (5)	O10^iii—K2—O14^ii	90.30 (7)
O2—W1—K4	119.39 (6)	O12^ii—K2—O14^ii	49.84 (6)
O1—W1—K4	119.67 (7)	O6^iii—K2—O10	80.50 (6)
O7—W1—K4	39.36 (6)	O13^iv—K2—O10	102.26 (6)
O4^i—W1—K4	120.43 (5)	O1—K2—O10	83.55 (6)
O11—W1—K4	51.24 (6)	O10^iii—K2—O10	93.51 (8)
O3—W1—K4	54.96 (5)	O12^ii—K2—O10	160.89 (6)
K2—W1—K4	109.780 (13)	O14^ii—K2—O10	149.23 (6)
O2—W1—K1	26.17 (7)	O6^iii—K2—O8	85.37 (6)
O1—W1—K1	118.37 (7)	O13^iv—K2—O8	62.89 (6)
O7—W1—K1	76.23 (6)	O1—K2—O8	81.21 (6)
O4^i—W1—K1	112.69 (5)	O10^iii—K2—O8	127.21 (7)
O11—W1—K1	81.38 (5)	O12^ii—K2—O8	127.45 (6)
O3—W1—K1	147.20 (5)	O14^ii—K2—O8	142.44 (6)
K2—W1—K1	80.229 (13)	O10—K2—O8	42.64 (6)
K4—W1—K1	93.217 (13)	O6^iii—K2—S2	91.91 (5)
O5—S1—O6	113.55 (12)	O13^iv—K2—S2	86.33 (5)
O5—S1—O3	108.53 (11)	O1—K2—S2	72.27 (4)
O6—S1—O3	111.37 (11)	O10^iii—K2—S2	104.89 (6)
O5—S1—O4	110.08 (11)	O12^ii—K2—S2	140.64 (5)
O6—S1—O4	105.74 (11)	O14^ii—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)	O6^iii—K2—W1	142.56 (5)
O10—S2—O8	111.01 (14)	O13^iv—K2—W1	90.50 (5)
O9—S2—O7	104.42 (13)	O1—K2—W1	24.25 (4)
O10—S2—O7	104.51 (14)	O10^iii—K2—W1	84.07 (5)
O8—S2—O7	107.70 (11)	O12^ii—K2—W1	91.26 (4)
O9—S2—K4	54.98 (9)	O14^ii—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)	O6^iii—K2—K3	120.06 (5)
O10—S2—K2	57.54 (12)	O13^iv—K2—K3	48.89 (5)
O8—S2—K2	69.44 (9)	O1—K2—K3	67.35 (4)
O7—S2—K2	81.26 (8)	O10^iii—K2—K3	112.43 (6)
K4—S2—K2	128.56 (2)	O12^ii—K2—K3	43.91 (4)
O13—S3—O12	112.38 (13)	O14^ii—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)	O5^i—K3—O14^iv	163.90 (7)
O13—S3—K4	59.27 (9)	O5^i—K3—O12^ii	80.84 (6)
O12—S3—K4	94.73 (9)	O14^iv—K3—O12^ii	110.10 (6)
O14—S3—K4	153.59 (9)	O5^i—K3—O6^xi	122.16 (6)
O11—S3—K4	58.24 (8)	O14^iv—K3—O6^xi	69.84 (6)
W1—O1—K1^ii	144.97 (10)	O12^ii—K3—O6^xi	95.33 (6)
W1—O1—K2	114.26 (9)	O5^i—K3—O2	71.21 (6)
K1^ii—O1—K2	92.09 (6)	O14^iv—K3—O2	95.02 (6)
W1—O2—K1	137.50 (10)	O12^ii—K3—O2	98.09 (6)
W1—O2—K3	122.23 (9)	O6^xi—K3—O2	162.58 (6)
K1—O2—K3	99.58 (6)	O5^i—K3—O5^xi	86.61 (6)
S1—O3—W1	138.03 (12)	O14^iv—K3—O5^xi	96.34 (6)
S1—O3—K1^v	102.32 (9)	O12^ii—K3—O5^xi	123.45 (6)
W1—O3—K1^v	107.61 (7)	O6^xi—K3—O5^xi	48.07 (5)
S1—O3—K4	118.47 (10)	O2—K3—O5^xi	129.14 (6)
W1—O3—K4	90.93 (6)	O5^i—K3—O9^x	71.47 (6)
K1^v—O3—K4	89.32 (5)	O14^iv—K3—O9^x	94.63 (7)
S1—O4—W1^i	129.39 (11)	O12^ii—K3—O9^x	148.78 (6)
S1—O4—K4^vi	89.44 (8)	O6^xi—K3—O9^x	111.34 (6)
W1^i—O4—K4^vi	123.03 (8)	O2—K3—O9^x	59.85 (6)
S1—O5—K3^i	148.88 (12)	O5^xi—K3—O9^x	69.90 (6)
S1—O5—K3^vii	95.03 (9)	O5^i—K3—O13^iv	129.35 (6)
K3^i—O5—K3^vii	93.39 (6)	O14^iv—K3—O13^iv	48.49 (6)
S1—O5—K1^v	95.34 (9)	O12^ii—K3—O13^iv	72.74 (6)
K3^i—O5—K1^v	101.38 (6)	O6^xi—K3—O13^iv	102.98 (6)
K3^vii—O5—K1^v	131.27 (7)	O2—K3—O13^iv	70.79 (5)
S1—O6—K2^iii	139.68 (12)	O5^xi—K3—O13^iv	143.91 (6)
S1—O6—K4^vi	112.18 (10)	O9^x—K3—O13^iv	114.42 (7)
K2^iii—O6—K4^vi	94.49 (6)	O5^i—K3—K2	89.42 (5)
S1—O6—K3^vii	100.59 (10)	O14^iv—K3—K2	90.94 (4)
K2^iii—O6—K3^vii	101.05 (6)	O12^ii—K3—K2	43.40 (4)
K4^vi—O6—K3^vii	104.78 (6)	O6^xi—K3—K2	125.87 (4)
S2—O7—W1	138.10 (12)	O2—K3—K2	60.70 (4)
S2—O7—K4	102.85 (9)	O5^xi—K3—K2	166.82 (4)
W1—O7—K4	113.58 (8)	O9^x—K3—K2	120.55 (5)
S2—O8—K1	135.99 (12)	O13^iv—K3—K2	42.49 (4)
S2—O8—K4^iv	115.26 (11)	O5^i—K3—K1	105.59 (5)
K1—O8—K4^iv	106.65 (7)	O14^iv—K3—K1	59.14 (5)
S2—O8—K2	87.11 (9)	O12^ii—K3—K1	118.00 (5)
K1—O8—K2	114.14 (7)	O6^xi—K3—K1	125.59 (4)
K4^iv—O8—K2	79.26 (5)	O2—K3—K1	37.34 (4)
S2—O9—K4	100.81 (11)	O5^xi—K3—K1	118.50 (4)
S2—O9—K3^viii	124.91 (13)	O9^x—K3—K1	58.88 (5)
K4—O9—K3^viii	134.25 (8)	O13^iv—K3—K1	55.63 (4)
S2—O10—K2^iii	120.94 (13)	K2—K3—K1	74.678 (16)
S2—O10—K1^viii	124.31 (16)	O8^v—K4—O6^xii	98.73 (6)
K2^iii—O10—K1^viii	89.11 (7)	O8^v—K4—O14^viii	100.49 (7)
S2—O10—K2	99.35 (13)	O6^xii—K4—O14^viii	123.73 (6)
K2^iii—O10—K2	86.49 (8)	O8^v—K4—O7	122.14 (6)
K1^viii—O10—K2	130.64 (9)	O6^xii—K4—O7	122.65 (6)
S3—O11—W1	139.75 (12)	O14^viii—K4—O7	88.87 (6)
S3—O11—K1^v	107.75 (9)	O8^v—K4—O9	166.53 (7)
W1—O11—K1^v	109.46 (7)	O6^xii—K4—O9	80.82 (6)
S3—O11—K4	97.09 (9)	O14^viii—K4—O9	90.75 (7)
W1—O11—K4	97.17 (7)	O7—K4—O9	50.05 (6)
K1^v—O11—K4	90.84 (5)	O8^v—K4—O11	77.17 (6)
S3—O12—K2^ix	98.86 (10)	O6^xii—K4—O11	106.54 (6)
S3—O12—K1	140.80 (11)	O14^viii—K4—O11	129.15 (6)
K2^ix—O12—K1	88.97 (6)	O7—K4—O11	54.81 (6)
S3—O12—K3^ix	115.18 (11)	O9—K4—O11	90.00 (6)
K2^ix—O12—K3^ix	92.68 (6)	O8^v—K4—O13	67.22 (6)
K1—O12—K3^ix	102.63 (7)	O6^xii—K4—O13	66.00 (6)
S3—O13—K2^v	174.14 (13)	O14^viii—K4—O13	166.38 (6)
S3—O13—K3^v	93.38 (10)	O7—K4—O13	92.92 (6)
K2^v—O13—K3^v	88.62 (6)	O9—K4—O13	100.75 (7)
S3—O13—K4	97.41 (10)	O11—K4—O13	44.56 (5)
K2^v—O13—K4	83.01 (6)	O8^v—K4—O4^xii	116.99 (6)
K3^v—O13—K4	154.06 (8)	O6^xii—K4—O4^xii	46.34 (5)
S3—O14—K4^x	136.11 (12)	O14^viii—K4—O4^xii	77.95 (6)
S3—O14—K3^v	106.39 (11)	O7—K4—O4^xii	120.80 (6)
K4^x—O14—K3^v	110.00 (7)	O9—K4—O4^xii	72.42 (6)
S3—O14—K2^ix	93.68 (10)	O11—K4—O4^xii	148.74 (5)
K4^x—O14—K2^ix	105.37 (7)	O13—K4—O4^xii	112.34 (5)
K3^v—O14—K2^ix	96.78 (6)	O8^v—K4—O3	70.66 (6)
O8—K1—O2	65.63 (6)	O6^xii—K4—O3	152.66 (6)
O8—K1—O1^ix	136.19 (7)	O14^viii—K4—O3	83.46 (6)
O2—K1—O1^ix	143.43 (6)	O7—K4—O3	53.75 (5)
O8—K1—O10^x	155.28 (7)	O9—K4—O3	103.65 (6)
O2—K1—O10^x	89.85 (7)	O11—K4—O3	47.26 (5)
O1^ix—K1—O10^x	63.32 (7)	O13—K4—O3	86.73 (5)
O8—K1—O12	87.15 (6)	O4^xii—K4—O3	160.88 (5)
O2—K1—O12	72.53 (6)	O8^v—K4—S2	148.30 (5)
O1^ix—K1—O12	79.22 (6)	O6^xii—K4—S2	103.12 (5)
O10^x—K1—O12	82.20 (7)	O14^viii—K4—S2	86.20 (5)
O8—K1—O3^iv	77.08 (6)	O7—K4—S2	26.33 (4)
O2—K1—O3^iv	140.05 (6)	O9—K4—S2	24.21 (4)
O1^ix—K1—O3^iv	74.96 (6)	O11—K4—S2	74.77 (4)
O10^x—K1—O3^iv	127.43 (7)	O13—K4—S2	101.30 (4)
O12—K1—O3^iv	120.87 (6)	O4^xii—K4—S2	94.70 (4)
O8—K1—O11^iv	80.65 (6)	O3—K4—S2	79.51 (4)
O2—K1—O11^iv	105.80 (6)	O8^v—K4—S3	79.53 (5)
O1^ix—K1—O11^iv	106.79 (6)	O6^xii—K4—S3	81.90 (4)
O10^x—K1—O11^iv	110.70 (7)	O14^viii—K4—S3	153.59 (5)
O12—K1—O11^iv	167.08 (6)	O7—K4—S3	69.70 (5)
O3^iv—K1—O11^iv	52.18 (5)	O9—K4—S3	87.09 (6)
O8—K1—O5^iv	71.46 (6)	O11—K4—S3	24.67 (4)
O2—K1—O5^iv	125.78 (6)	O13—K4—S3	23.32 (4)
O1^ix—K1—O5^iv	64.78 (6)	O4^xii—K4—S3	125.93 (4)
O10^x—K1—O5^iv	125.77 (7)	O3—K4—S3	71.54 (4)
O12—K1—O5^iv	73.83 (6)	S2—K4—S3	81.11 (2)
O3^iv—K1—O5^iv	47.07 (5)	O8^v—K4—W1	95.92 (5)
O11^iv—K1—O5^iv	98.06 (5)	O6^xii—K4—W1	128.70 (4)
O8—K1—W1	57.40 (4)	O14^viii—K4—W1	101.09 (5)
O2—K1—W1	16.33 (4)	O7—K4—W1	27.06 (4)
O1^ix—K1—W1	137.85 (5)	O9—K4—W1	74.46 (5)
O10^x—K1—W1	98.09 (6)	O11—K4—W1	31.59 (3)
O12—K1—W1	60.18 (4)	O13—K4—W1	75.37 (4)
O3^iv—K1—W1	134.46 (4)	O4^xii—K4—W1	146.84 (4)
O11^iv—K1—W1	115.29 (4)	O3—K4—W1	34.11 (3)
O5^iv—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.