Ba5(IO6)2: crystal structure evolution from room temperature to 80 K

Bi, D.W.; Baral, P.R.; Magrez, A.

doi:10.1107/S2056989021004990

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ISSN: 2056-9890

Volume 77| Part 6| June 2021| Pages 634-637

https://doi.org/10.1107/S2056989021004990

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Ba₅(IO₆)₂: crystal structure evolution from room temperature to 80 K

David Wenhua Bi,^a ^* Priya Ranjan Baral ^a and Arnaud Magrez ^a

^aCrystal Growth Facility, Institute of Physics, École Polytechnique Fédérale de Lausanne (EPFL), Switzerland
^*Correspondence e-mail: wen.bi@epfl.ch

Edited by P. Roussel, ENSCL, France (Received 26 April 2021; accepted 11 May 2021; online 14 May 2021)

The crystal structure of Ba₅(IO₆)₂, pentabarium bis(orthoperiodate), has been re-investigated at room temperature based on single-crystal X-ray diffraction data. In comparison with a previous crystal structure determination by the Rietveld method, an improved precision of the structural parameters was achieved. Additionally, low-temperature measurements allowed the crystal structure evolution to be studied down to 80 K. No evidence of structural transition was found even at the lowest temperature. Upon cooling, the lattice contraction is more pronounced along the b axis. This contraction is found to be inhomogeneous along different crystallographic axes. The interatomic distances between different Ba atoms reduce drastically with lowering temperature, resulting in a closer packing around the IO₆ octahedra, which remain largely unaffected.

Keywords: Single-crystal structure; low-temperature X-ray diffraction; space-group determination.

CCDC references: 2083048; 2083047

1. Database survey

No structural model was found before 2014, even though the compound had been known for a long time. Two different records with structural models from Rietveld refinement against polycrystalline diffraction patterns were found in both the ICSD (426639 & 237982) and PDF4 v2020 (04-021-7777 & 01-083-9132). However, those models have no information about the ADPs. No similar structure can be found in COD before April 2021. Obviously, the high-quality model presented herein will be very useful for research activities related to iodate materials.

2. Chemical context

Orthoperiodates are compounds based on the (IO₆)⁵⁻ anion in which iodine is in the oxidation state +7. Pentasodium orthoperiodate was the first synthesized by oxidation of sodium iodide in air in the presence of Na₂O (Zintl & Morawietz, 1940 ). About 30 years later, ammonium orthoperiodates were studied for their antiferroelectric properties (Gränicher et al., 1968 ). Pentacalcium orthoperiodate was foreseen as a stable nutritional complement of iodine for bovines (Moss &Miller, 1970 ). In the past three years, orthoperiodates have regained interest. They act as a stabilizing agent of Pickering solution, which is used to harvest cellulose nanocrystals (Liu et al., 2018 ; Liu et al., 2020 ) and chitin nanocrystals (Liu et al., 2021 ) in high yield from microcrystalline samples. When used as ligands, orthoperiodates were found to enhance the stability of water oxidation catalysts (Chakraborty et al., 2018 ).

Among alkaline earth orthoperiodates, M₅(IO₆)₂ with M = Ca, Sr and Ba are the only ones to be reported in the literature since the 1960s. They are produced by a controlled oxidation of alkaline earth iodide at temperature above 723 K or by precipitation from alkaline earth hydroxide and periodic acid. Alkaline earth orthoperiodates are also observed during the course of decomposition of iodates, dimesoperiodates (Sanyal & Nag, 1977 ) and periodates (Balek & Julák, 1972 ). Ca₅(IO₆)₂ and Ba₅(IO₆)₂ are solids formed during the thermochemical production of hydrogen from water using a combination of iodine with Ca or Ba metals, respectively (Mizuta et al., 1978 ).

The first crystallographic data on Ba₅(IO₆) were published in 2014 (Kubel et al., 2014 ). Ba₅(IO₆)₂ differs structurally from Ca₅(IO₆)₂ and Sr₅(IO₆)₂ (Hummel et al., 2015 ). At room temperature, Ba₅(IO₆)₂ exhibits orthorhombic symmetry while Sr and Ca orthoperiodates are isomorphic and crystallize with rhombohedral symmetry. The structure of Ba₅(IO₆)₂ was refined from powder XRD data as single crystals were not available. The low-temperature dependence of the Ba₅(IO₆)₂ structure, and in particular the evolution of the periodate (IO₆)⁵⁻ anion, has not previously been reported.

3. Structural commentary

According to the comprehensive description given by Hummel et al., 2015, Ba₅(IO₆)₂ contains two crystallographically independent iodine atoms, which are placed in the centre of distorted octahedra formed by oxygen atoms, also confirmed by our room-temperature single-crystal XRD (SCXRD) data. Perpendicular to the a axis, the crystal structure of Ba₅(IO₆)₂ is made up of alternating layers formed by I(6)O₆ and I(7)O₆ octahedra, respectively, as shown in Fig. 1. These IO₆ octahedra from two consecutive layers do not share any direct connection to each other. The octahedra are symmetrically distributed in three dimensions over the crystal structure between the five different barium atoms of the Ba₅(IO₆)₂ structure.

Figure 1
The crystal structure of Ba₅(IO₆)₂ visualized along different crystallographic axes. Green, violet and red balls represents barium, iodine and oxygen atoms, respectively.

In order to detect any possible structural transitions in Ba₅(IO₆)₂, SCXRD measurements were also performed at 100 K and 80 K. By comparing the results obtained at 80 K with those of 298 K, average thermal dilation coefficients of 4.8 × 10 ⁻⁶ K⁻¹, 17.56 × 10 ⁻⁶ K⁻¹, 5.23 × 10 ⁻⁶ K⁻¹ were found along a, b and c axes, respectively.

The temperature evolution of the IO₆ octahedra are quite different from the barium atom `matrix' within which they are distributed. As can be seen in Fig. 2, the IO₆ octahedra at 80 K are almost identical with respect to interatomic distances and angles to the ones refined at 298 K. However, the interatomic distances between Ba atoms are very sensitive to the temperature in another way. They dramatically expand when Ba₅(IO₆)₂ is heated from 80 K to 298 K (Fig. 3). Except for the Ba2—Ba4 distance, all the interatomic distances show a dilation coefficient that is up to one order of magnitude higher than those of the lattice constant.

Figure 2
Bond lengths (in Å) and equatorial plane angles (in °) for the two IO₆ octahedra of the Ba₅(IO₆)₂ structure. The values obtained at 80 K and 298 K are indicated in blue and red, respectively.

Figure 3
Dilation coefficient of the Ba—Ba interatomic distances from 80 K to 298 K.

In conclusion, single crystals of Ba₅(IO₆)₂ have been grown using a flux method. The crystal structures at two different temperatures, from 298 K down to 80 K, have been refined using high-quality SCXRD data. We confirm the assignment of the structure to the centrosymmetric space group Pnma (No. 62), which cannot be distinguished via extinction rules from the Pna2₁ (No. 33) space group by powder XRD. From the low-temperature XRD data, evolution of the lattice constants was found to be inhomogeneous. While IO₆ octahedra size and distortion do not change drastically between 80 K and 298 K, the packing of the barium atoms around the octahedra grows upon cooling. This leads to an increase of the density from 6.097 (8) g cm⁻³ at 298 K to 6.134 (7) g cm⁻³ at 80 K.

4. Synthesis and crystallization

Iron oxalate dihydrate (FeC₂O₄·2H₂O), barium carbonate (BaCO₃) and barium iodide dihydrate (BaI₂·2H₂O) were mixed in a molar ratio 2:2:10 and placed in an alumina crucible. The mixture was heated to 1273 K at a rate of 100 K per hour. The furnace was maintained at this temperature for 24 h, followed by a slow cooling to 1173 K at a rate of 1 K per hour, and was finally quenched to room temperature. The whole synthesis process took place under atmospheric conditions. Crystals were collected from the wall of the crucible.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1.

Table 1
Experimental details

	298 K	80 K
Crystal data
Chemical formula	Ba₅(IO₆)₂	Ba₅I₂O₁₂
M_r	1132.50	1132.50
Crystal system, space group	Orthorhombic, Pnma	Orthorhombic, Pnma
Temperature (K)	298	80
a, b, c (Å)	19.7568 (2), 5.9003 (1), 10.5869 (1)	19.7361 (3), 5.8779 (1), 10.5749 (1)
V (Å³)	1234.13 (3)	1226.76 (3)
Z	4	4
Radiation type	Mo Kα	Mo Kα
μ (mm⁻¹)	20.78	20.90
Crystal size (mm)	0.22 × 0.12 × 0.08	0.22 × 0.12 × 0.08

Data collection
Diffractometer	XtaLAB Synergy-I with HyPix3000	XtaLAB Synergy-I with HyPix3000
Absorption correction	Gaussian (CrysAlis PRO; Rigaku OD, 2020 $[Rigaku OD (2020). CrysAlis PRO. Rigaku Oxford Diffraction, Yarnton, England.]$ )	Gaussian (CrysAlis PRO; Rigaku OD, 2020 $[Rigaku OD (2020). CrysAlis PRO. Rigaku Oxford Diffraction, Yarnton, England.]$ )
T_min, T_max	0.029, 0.494	0.150, 0.750
No. of measured, independent and observed [I > 2σ(I)] reflections	57653, 2543, 2407	16187, 2529, 2462
R_int	0.058	0.033
(sin θ/λ)_max (Å⁻¹)	0.769	0.769

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.046, 1.16	0.022, 0.043, 1.25
No. of reflections	2543	2529
No. of parameters	104	104
Δρ_max, Δρ_min (e Å⁻³)	1.39, −1.54	1.90, −1.60
Computer programs: CrysAlis PRO (Rigaku OD, 2020 $[Rigaku OD (2020). CrysAlis PRO. Rigaku Oxford Diffraction, Yarnton, England.]$ ), SHELXT2018/3 (Sheldrick, 2015a ), SHELXL2018/3 (Sheldrick, 2015b ) and OLEX2 (Dolomanov et al., 2009 ).

On considering the large value of beam attenuation coefficient of the title compound, a nice crystal with small size and Mo Kα radiation was selected for structure determination.

Data sets were collected up to the resolution of 0.6 Å at two different temperatures. No restraints were applied for the refinement at 298 K, but one O atom in the structure at 80 K had abnormal ADPs, and an EADP constraint was applied on it to eliminate the level B checkCIF alert. Then both models were modified to follow the same bonding and labelling style as the one in the database, and the EADP constraint was removed.

Supporting information

CCDC references: 2083048; 2083047

Crystal structure: contains datablocks 80K, 298K. DOI: https://doi.org/10.1107/S2056989021004990/ru2075sup1.cif

Structure factors: contains datablock 298K. DOI: https://doi.org/10.1107/S2056989021004990/ru2075298Ksup2.hkl

Structure factors: contains datablock 80K. DOI: https://doi.org/10.1107/S2056989021004990/ru207580Ksup4.hkl

checkCIF report

Computing details top

For both structures, data collection: CrysAlis PRO (Rigaku OD, 2020); cell refinement: CrysAlis PRO (Rigaku OD, 2020); data reduction: CrysAlis PRO (Rigaku OD, 2020); program(s) used to solve structure: SHELXT2018/3 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Pentabarium bis(orthoperiodate) (298K) top

Crystal data top

Ba₅(IO₆)₂	D_x = 6.095 Mg m⁻³
M_r = 1132.50	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 29837 reflections
a = 19.7568 (2) Å	θ = 2.2–36.3°
b = 5.9003 (1) Å	µ = 20.78 mm⁻¹
c = 10.5869 (1) Å	T = 298 K
V = 1234.13 (3) Å³	Prism, brown
Z = 4	0.22 × 0.12 × 0.08 mm
F(000) = 1928

Data collection top

XtaLAB Synergy-I with HyPix3000 diffractometer	2407 reflections with I > 2σ(I)
ω Scan scans	R_int = 0.058
Absorption correction: gaussian (CrysAlisPro; Rigaku OD, 2020)	θ_max = 33.1°, θ_min = 2.1°
T_min = 0.029, T_max = 0.494	h = −30→30
57653 measured reflections	k = −9→9
2543 independent reflections	l = −16→16

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0162P)² + 4.6175P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.021	(Δ/σ)_max = 0.001
wR(F²) = 0.046	Δρ_max = 1.39 e Å⁻³
S = 1.16	Δρ_min = −1.54 e Å⁻³
2543 reflections	Extinction correction: SHELXL2018/3 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
104 parameters	Extinction coefficient: 0.00080 (3)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.04831 (2)	0.250000	0.08907 (3)	0.01014 (6)
Ba2	0.14123 (2)	0.250000	0.38321 (3)	0.00819 (6)
Ba3	0.19933 (2)	0.250000	0.74019 (3)	0.01149 (6)
Ba4	0.34287 (2)	0.250000	0.47502 (3)	0.00930 (6)
Ba5	0.42814 (2)	0.250000	0.08851 (3)	0.01175 (6)
I6	0.01315 (2)	0.250000	0.74877 (3)	0.00578 (6)
I7	0.23901 (2)	0.250000	0.10140 (3)	0.00659 (6)
O8	0.03751 (13)	0.5222 (4)	0.3320 (2)	0.0132 (5)
O9	0.18857 (14)	0.0239 (4)	0.1828 (2)	0.0141 (5)
O10	0.28823 (15)	0.0235 (5)	0.0184 (3)	0.0184 (6)
O11	0.43557 (13)	0.5199 (4)	0.3281 (3)	0.0134 (5)
O12	0.07500 (19)	0.250000	0.6116 (4)	0.0135 (7)
O13	0.3027 (2)	0.250000	0.2338 (4)	0.0182 (8)
O14	0.45600 (19)	0.250000	0.6074 (3)	0.0123 (7)
O15	0.6730 (2)	0.250000	0.5248 (4)	0.0178 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba1	0.01190 (13)	0.00841 (12)	0.01012 (12)	0.000	−0.00023 (9)	0.000
Ba2	0.00924 (12)	0.00836 (11)	0.00698 (11)	0.000	−0.00090 (9)	0.000
Ba3	0.01612 (14)	0.00807 (12)	0.01028 (12)	0.000	0.00336 (10)	0.000
Ba4	0.01039 (12)	0.00840 (12)	0.00911 (12)	0.000	−0.00143 (9)	0.000
Ba5	0.01280 (13)	0.00815 (12)	0.01431 (13)	0.000	−0.00272 (10)	0.000
I6	0.00691 (12)	0.00474 (11)	0.00569 (11)	0.000	0.00027 (9)	0.000
I7	0.00812 (13)	0.00585 (12)	0.00581 (12)	0.000	0.00011 (9)	0.000
O8	0.0130 (12)	0.0104 (11)	0.0162 (12)	0.0040 (9)	−0.0013 (9)	0.0057 (10)
O9	0.0186 (13)	0.0092 (11)	0.0146 (12)	−0.0044 (9)	0.0066 (10)	0.0003 (9)
O10	0.0228 (14)	0.0133 (12)	0.0190 (13)	0.0074 (10)	0.0078 (11)	−0.0009 (10)
O11	0.0132 (12)	0.0086 (11)	0.0183 (12)	−0.0032 (9)	0.0038 (10)	0.0040 (10)
O12	0.0135 (17)	0.0151 (17)	0.0120 (16)	0.000	0.0082 (13)	0.000
O13	0.0192 (19)	0.0201 (19)	0.0154 (18)	0.000	−0.0103 (15)	0.000
O14	0.0114 (16)	0.0143 (16)	0.0113 (16)	0.000	−0.0035 (13)	0.000
O15	0.0130 (17)	0.029 (2)	0.0113 (17)	0.000	0.0048 (14)	0.000

Geometric parameters (Å, º) top

Ba1—O8ⁱ	3.040 (3)	Ba4—I7^viii	3.6209 (2)
Ba1—O8	3.040 (3)	Ba4—O9^ix	2.799 (3)
Ba1—O9	3.232 (3)	Ba4—O9^viii	2.799 (3)
Ba1—O9ⁱ	3.232 (3)	Ba4—O10^ix	3.086 (3)
Ba1—O11ⁱⁱ	3.095 (3)	Ba4—O10^viii	3.086 (3)
Ba1—O11ⁱⁱⁱ	3.095 (3)	Ba4—O11ⁱ	2.883 (2)
Ba1—O11^iv	2.875 (3)	Ba4—O11	2.883 (2)
Ba1—O11^v	2.875 (3)	Ba4—O13	2.675 (4)
Ba1—O14ⁱⁱ	2.9578 (3)	Ba4—O14	2.638 (4)
Ba1—O14^vi	2.9578 (3)	Ba4—O15^xii	2.9668 (4)
Ba1—O14^iv	2.766 (4)	Ba4—O15^xiii	2.9668 (4)
Ba1—O15^iv	2.743 (4)	Ba5—I6ⁱⁱ	3.5954 (2)
Ba2—Ba3	3.9498 (4)	Ba5—O8ⁱⁱ	3.105 (3)
Ba2—Ba5^vii	3.9123 (3)	Ba5—O8^xiv	2.821 (3)
Ba2—Ba5^viii	3.9123 (3)	Ba5—O8^xv	2.821 (3)
Ba2—I7	3.5543 (4)	Ba5—O8ⁱⁱⁱ	3.105 (3)
Ba2—O8	2.659 (2)	Ba5—O10ⁱ	3.159 (3)
Ba2—O8ⁱ	2.659 (2)	Ba5—O10	3.159 (3)
Ba2—O9ⁱ	2.675 (3)	Ba5—O11	2.999 (3)
Ba2—O9	2.675 (3)	Ba5—O11ⁱ	2.999 (3)
Ba2—O10^viii	2.568 (3)	Ba5—O12^vi	2.9609 (3)
Ba2—O10^ix	2.568 (3)	Ba5—O12ⁱⁱ	2.9609 (3)
Ba2—O12	2.749 (4)	Ba5—O13	2.917 (4)
Ba3—I7^viii	3.5138 (2)	I6—O8^xvi	1.881 (2)
Ba3—I7^vii	3.5138 (2)	I6—O8^xvii	1.881 (2)
Ba3—O9^ix	2.808 (3)	I6—O11^vii	1.891 (2)
Ba3—O9^viii	2.808 (3)	I6—O11^x	1.891 (2)
Ba3—O10^ix	2.860 (3)	I6—O12	1.898 (3)
Ba3—O10^viii	2.860 (3)	I6—O14^xi	1.896 (4)
Ba3—O11^vii	3.132 (3)	I7—O9ⁱ	1.875 (2)
Ba3—O11^x	3.132 (3)	I7—O9	1.875 (2)
Ba3—O12	2.809 (4)	I7—O10ⁱ	1.872 (3)
Ba3—O13^vii	2.9512 (1)	I7—O10	1.872 (3)
Ba3—O13^viii	2.9512 (1)	I7—O13	1.883 (4)
Ba3—O15^xi	2.542 (4)	I7—O15^iv	1.866 (4)
Ba4—I7^vii	3.6209 (2)

O8—Ba1—O8ⁱ	63.79 (9)	O8ⁱⁱⁱ—Ba5—O10	78.61 (7)
O8—Ba1—O9ⁱ	65.31 (7)	O8^xv—Ba5—O10	119.97 (7)
O8ⁱ—Ba1—O9ⁱ	91.06 (7)	O8ⁱⁱ—Ba5—O10	99.72 (7)
O8—Ba1—O9	91.06 (7)	O8^xiv—Ba5—O10	168.92 (7)
O8ⁱ—Ba1—O9	65.31 (7)	O8ⁱⁱⁱ—Ba5—O10ⁱ	99.72 (7)
O8—Ba1—O11ⁱⁱⁱ	173.91 (7)	O8ⁱⁱ—Ba5—O10ⁱ	78.61 (7)
O8ⁱ—Ba1—O11ⁱⁱⁱ	122.06 (6)	O8^xv—Ba5—O10ⁱ	168.92 (7)
O8—Ba1—O11ⁱⁱ	122.06 (6)	O8^xiv—Ba5—O10ⁱ	119.97 (7)
O8ⁱ—Ba1—O11ⁱⁱ	173.91 (7)	O8^xiv—Ba5—O11	53.68 (7)
O9ⁱ—Ba1—O9	48.76 (9)	O8^xv—Ba5—O11ⁱ	53.68 (7)
O11^v—Ba1—O8	88.87 (7)	O8^xv—Ba5—O11	90.72 (7)
O11^iv—Ba1—O8	52.77 (7)	O8^xiv—Ba5—O11ⁱ	90.72 (7)
O11^v—Ba1—O8ⁱ	52.77 (7)	O8^xiv—Ba5—O12ⁱⁱ	54.84 (9)
O11^iv—Ba1—O8ⁱ	88.87 (7)	O8^xv—Ba5—O12^vi	54.84 (9)
O11^v—Ba1—O9ⁱ	143.07 (7)	O8^xv—Ba5—O12ⁱⁱ	123.97 (9)
O11^v—Ba1—O9	110.00 (6)	O8^xiv—Ba5—O12^vi	123.97 (9)
O11ⁱⁱⁱ—Ba1—O9	90.27 (6)	O8^xv—Ba5—O13	119.58 (8)
O11^iv—Ba1—O9ⁱ	110.00 (6)	O8^xiv—Ba5—O13	119.58 (8)
O11^iv—Ba1—O9	143.07 (7)	O10ⁱ—Ba5—I6ⁱⁱ	92.63 (5)
O11ⁱⁱⁱ—Ba1—O9ⁱ	111.53 (7)	O10—Ba5—I6ⁱⁱ	137.76 (5)
O11ⁱⁱ—Ba1—O9	111.53 (7)	O10ⁱ—Ba5—O10	50.07 (10)
O11ⁱⁱ—Ba1—O9ⁱ	90.27 (6)	O11ⁱ—Ba5—I6ⁱⁱ	91.20 (5)
O11ⁱⁱⁱ—Ba1—O11ⁱⁱ	52.03 (9)	O11—Ba5—I6ⁱⁱ	31.71 (5)
O11^v—Ba1—O11^iv	67.28 (10)	O11—Ba5—O8ⁱⁱ	119.95 (6)
O11^v—Ba1—O11ⁱⁱ	126.51 (4)	O11ⁱ—Ba5—O8ⁱⁱ	163.54 (7)
O11^v—Ba1—O11ⁱⁱⁱ	96.26 (7)	O11ⁱ—Ba5—O8ⁱⁱⁱ	119.94 (6)
O11^iv—Ba1—O11ⁱⁱⁱ	126.51 (4)	O11—Ba5—O8ⁱⁱⁱ	163.54 (7)
O11^iv—Ba1—O11ⁱⁱ	96.26 (7)	O11ⁱ—Ba5—O10	90.96 (7)
O11^iv—Ba1—O14ⁱⁱ	53.50 (8)	O11—Ba5—O10	117.80 (7)
O11^v—Ba1—O14ⁱⁱ	120.68 (9)	O11ⁱ—Ba5—O10ⁱ	117.80 (7)
O11^v—Ba1—O14^vi	53.50 (8)	O11—Ba5—O10ⁱ	90.96 (7)
O11^iv—Ba1—O14^vi	120.68 (9)	O11ⁱ—Ba5—O11	64.16 (9)
O14^iv—Ba1—O8ⁱ	126.15 (7)	O12ⁱⁱ—Ba5—I6ⁱⁱ	31.82 (7)
O14^vi—Ba1—O8ⁱ	54.23 (8)	O12^vi—Ba5—I6ⁱⁱ	141.76 (7)
O14ⁱⁱ—Ba1—O8ⁱ	118.00 (8)	O12ⁱⁱ—Ba5—O8ⁱⁱ	69.23 (9)
O14ⁱⁱ—Ba1—O8	54.23 (8)	O12^vi—Ba5—O8ⁱⁱ	120.53 (9)
O14^vi—Ba1—O8	118.00 (8)	O12^vi—Ba5—O8ⁱⁱⁱ	69.23 (9)
O14^iv—Ba1—O8	126.15 (7)	O12ⁱⁱ—Ba5—O8ⁱⁱⁱ	120.53 (9)
O14^iv—Ba1—O9	142.77 (7)	O12^vi—Ba5—O10	65.13 (9)
O14ⁱⁱ—Ba1—O9ⁱ	65.97 (8)	O12ⁱⁱ—Ba5—O10	115.00 (9)
O14^iv—Ba1—O9ⁱ	142.77 (7)	O12ⁱⁱ—Ba5—O10ⁱ	65.13 (8)
O14ⁱⁱ—Ba1—O9	114.60 (9)	O12^vi—Ba5—O10ⁱ	115.00 (9)
O14^vi—Ba1—O9	65.97 (8)	O12^vi—Ba5—O11	117.42 (9)
O14^vi—Ba1—O9ⁱ	114.60 (9)	O12ⁱⁱ—Ba5—O11ⁱ	117.42 (9)
O14^iv—Ba1—O11^iv	73.66 (8)	O12^vi—Ba5—O11ⁱ	53.28 (9)
O14^iv—Ba1—O11^v	73.66 (8)	O12ⁱⁱ—Ba5—O11	53.28 (9)
O14^vi—Ba1—O11ⁱⁱ	119.94 (8)	O12ⁱⁱ—Ba5—O12^vi	170.25 (15)
O14^iv—Ba1—O11ⁱⁱⁱ	52.89 (8)	O13—Ba5—I6ⁱⁱ	91.45 (4)
O14ⁱⁱ—Ba1—O11ⁱⁱ	67.92 (8)	O13—Ba5—O8ⁱⁱⁱ	130.30 (8)
O14ⁱⁱ—Ba1—O11ⁱⁱⁱ	119.94 (8)	O13—Ba5—O8ⁱⁱ	130.30 (8)
O14^iv—Ba1—O11ⁱⁱ	52.89 (8)	O13—Ba5—O10ⁱ	51.70 (8)
O14^vi—Ba1—O11ⁱⁱⁱ	67.92 (8)	O13—Ba5—O10	51.70 (8)
O14^iv—Ba1—O14ⁱⁱ	91.74 (7)	O13—Ba5—O11	66.15 (8)
O14^iv—Ba1—O14^vi	91.74 (7)	O13—Ba5—O11ⁱ	66.15 (8)
O14ⁱⁱ—Ba1—O14^vi	171.78 (14)	O13—Ba5—O12ⁱⁱ	86.49 (8)
O15^iv—Ba1—O8	115.77 (8)	O13—Ba5—O12^vi	86.49 (8)
O15^iv—Ba1—O8ⁱ	115.77 (8)	Ba1^xvi—I6—Ba1^xviii	109.041 (11)
O15^iv—Ba1—O9ⁱ	50.55 (8)	Ba1^xvi—I6—Ba1^xix	66.305 (7)
O15^iv—Ba1—O9	50.55 (8)	Ba1^xviii—I6—Ba1^xix	66.305 (7)
O15^iv—Ba1—O11ⁱⁱ	61.00 (8)	Ba1^xvi—I6—Ba3	110.289 (7)
O15^iv—Ba1—O11^v	146.09 (5)	Ba1^xix—I6—Ba3	80.504 (9)
O15^iv—Ba1—O11^iv	146.09 (5)	Ba1^xviii—I6—Ba3	110.289 (7)
O15^iv—Ba1—O11ⁱⁱⁱ	61.00 (8)	Ba5^viii—I6—Ba1^xvi	179.188 (10)
O15^iv—Ba1—O14^iv	105.18 (11)	Ba5^vii—I6—Ba1^xviii	179.188 (10)
O15^iv—Ba1—O14ⁱⁱ	93.13 (7)	Ba5^viii—I6—Ba1^xviii	70.339 (6)
O15^iv—Ba1—O14^vi	93.13 (7)	Ba5^viii—I6—Ba1^xix	113.722 (7)
Ba1—Ba2—Ba3	166.371 (11)	Ba5^vii—I6—Ba1^xix	113.722 (7)
Ba1—Ba2—Ba5^vii	107.497 (7)	Ba5^vii—I6—Ba1^xvi	70.339 (6)
Ba1—Ba2—Ba5^viii	107.497 (8)	Ba5^viii—I6—Ba3	70.481 (7)
Ba5^viii—Ba2—Ba3	64.547 (6)	Ba5^vii—I6—Ba3	70.481 (7)
Ba5^vii—Ba2—Ba3	64.547 (6)	Ba5^viii—I6—Ba5^vii	110.276 (11)
Ba5^vii—Ba2—Ba5^viii	97.888 (9)	O8^xvi—I6—Ba1^xviii	128.23 (8)
I7—Ba2—Ba1	63.445 (8)	O8^xvi—I6—Ba1^xix	123.16 (8)
I7—Ba2—Ba3	130.184 (10)	O8^xvii—I6—Ba1^xviii	57.00 (8)
I7—Ba2—Ba5^vii	131.052 (5)	O8^xvii—I6—Ba1^xix	123.16 (8)
I7—Ba2—Ba5^viii	131.052 (5)	O8^xvii—I6—Ba1^xvi	128.23 (8)
O8—Ba2—Ba1	55.46 (6)	O8^xvi—I6—Ba1^xvi	57.00 (8)
O8ⁱ—Ba2—Ba1	55.46 (6)	O8^xvi—I6—Ba3	121.37 (8)
O8ⁱ—Ba2—Ba3	114.77 (6)	O8^xvii—I6—Ba3	121.37 (8)
O8—Ba2—Ba3	114.77 (6)	O8^xvi—I6—Ba5^vii	51.02 (8)
O8—Ba2—Ba5^vii	52.26 (6)	O8^xvii—I6—Ba5^vii	122.91 (8)
O8—Ba2—Ba5^viii	107.38 (6)	O8^xvii—I6—Ba5^viii	51.02 (8)
O8ⁱ—Ba2—Ba5^viii	52.26 (6)	O8^xvi—I6—Ba5^viii	122.91 (8)
O8ⁱ—Ba2—Ba5^vii	107.38 (6)	O8^xvii—I6—O8^xvi	91.20 (16)
O8—Ba2—I7	104.34 (6)	O8^xvi—I6—O11^vii	88.51 (11)
O8ⁱ—Ba2—I7	104.34 (6)	O8^xvii—I6—O11^vii	179.34 (12)
O8—Ba2—O8ⁱ	74.30 (11)	O8^xvii—I6—O11^x	88.51 (11)
O8—Ba2—O9ⁱ	78.85 (8)	O8^xvi—I6—O11^x	179.34 (12)
O8ⁱ—Ba2—O9ⁱ	114.13 (8)	O8^xvii—I6—O12	89.69 (12)
O8—Ba2—O9	114.14 (8)	O8^xvi—I6—O12	89.69 (12)
O8ⁱ—Ba2—O9	78.85 (8)	O8^xvii—I6—O14^xi	92.76 (11)
O8—Ba2—O12	79.19 (9)	O8^xvi—I6—O14^xi	92.76 (11)
O8ⁱ—Ba2—O12	79.19 (9)	O11^vii—I6—Ba1^xviii	123.62 (8)
O9ⁱ—Ba2—Ba1	59.62 (6)	O11^x—I6—Ba1^xviii	52.00 (8)
O9—Ba2—Ba1	59.63 (6)	O11^x—I6—Ba1^xvi	123.62 (8)
O9ⁱ—Ba2—Ba3	131.09 (6)	O11^vii—I6—Ba1^xix	57.47 (8)
O9—Ba2—Ba3	131.09 (6)	O11^vii—I6—Ba1^xvi	52.00 (8)
O9ⁱ—Ba2—Ba5^viii	159.91 (5)	O11^x—I6—Ba1^xix	57.47 (8)
O9—Ba2—Ba5^vii	159.91 (5)	O11^x—I6—Ba3	58.35 (8)
O9ⁱ—Ba2—Ba5^vii	100.78 (5)	O11^vii—I6—Ba3	58.35 (8)
O9—Ba2—Ba5^viii	100.78 (5)	O11^vii—I6—Ba5^vii	56.48 (8)
O9ⁱ—Ba2—I7	31.15 (5)	O11^x—I6—Ba5^vii	128.75 (8)
O9—Ba2—I7	31.15 (5)	O11^x—I6—Ba5^viii	56.48 (8)
O9ⁱ—Ba2—O9	59.83 (11)	O11^vii—I6—Ba5^viii	128.75 (8)
O9ⁱ—Ba2—O12	149.76 (5)	O11^vii—I6—O11^x	91.77 (16)
O9—Ba2—O12	149.76 (5)	O11^vii—I6—O12	89.72 (12)
O10^viii—Ba2—Ba1	139.09 (6)	O11^x—I6—O12	89.72 (12)
O10^ix—Ba2—Ba1	139.09 (6)	O11^vii—I6—O14^xi	87.84 (11)
O10^viii—Ba2—Ba3	46.29 (6)	O11^x—I6—O14^xi	87.84 (11)
O10^ix—Ba2—Ba3	46.29 (6)	O12—I6—Ba1^xix	129.02 (12)
O10^ix—Ba2—Ba5^viii	110.75 (6)	O12—I6—Ba1^xvi	125.337 (9)
O10^viii—Ba2—Ba5^vii	110.75 (6)	O12—I6—Ba1^xviii	125.337 (9)
O10^ix—Ba2—Ba5^vii	53.61 (7)	O12—I6—Ba3	48.52 (12)
O10^viii—Ba2—Ba5^viii	53.61 (7)	O12—I6—Ba5^vii	55.336 (10)
O10^ix—Ba2—I7	99.96 (7)	O12—I6—Ba5^viii	55.336 (10)
O10^viii—Ba2—I7	99.96 (7)	O14^xi—I6—Ba1^xviii	54.531 (6)
O10^viii—Ba2—O8ⁱ	98.76 (9)	O14^xi—I6—Ba1^xvi	54.531 (6)
O10^ix—Ba2—O8ⁱ	155.68 (8)	O14^xi—I6—Ba1^xix	47.47 (11)
O10^ix—Ba2—O8	98.76 (9)	O14^xi—I6—Ba3	127.97 (11)
O10^viii—Ba2—O8	155.68 (8)	O14^xi—I6—Ba5^viii	124.833 (6)
O10^ix—Ba2—O9ⁱ	86.50 (9)	O14^xi—I6—Ba5^vii	124.833 (6)
O10^viii—Ba2—O9	86.50 (9)	O14^xi—I6—O12	176.49 (17)
O10^viii—Ba2—O9ⁱ	124.45 (9)	Ba2—I7—Ba4^vi	93.860 (7)
O10^ix—Ba2—O9	124.45 (9)	Ba2—I7—Ba4ⁱⁱ	93.860 (7)
O10^ix—Ba2—O10^viii	77.86 (13)	Ba2—I7—Ba5	125.013 (10)
O10^viii—Ba2—O12	76.60 (9)	Ba3^vi—I7—Ba2	80.642 (7)
O10^ix—Ba2—O12	76.60 (9)	Ba3ⁱⁱ—I7—Ba2	80.642 (7)
O12—Ba2—Ba1	121.05 (8)	Ba3ⁱⁱ—I7—Ba3^vi	114.195 (11)
O12—Ba2—Ba3	45.32 (8)	Ba3^vi—I7—Ba4ⁱⁱ	173.462 (11)
O12—Ba2—Ba5^vii	49.054 (7)	Ba3ⁱⁱ—I7—Ba4^vi	173.462 (11)
O12—Ba2—Ba5^viii	49.054 (7)	Ba3ⁱⁱ—I7—Ba4ⁱⁱ	67.997 (6)
O12—Ba2—I7	175.50 (8)	Ba3^vi—I7—Ba4^vi	67.997 (6)
I7^viii—Ba3—I7^vii	114.196 (11)	Ba3^vi—I7—Ba5	70.658 (7)
O9^ix—Ba3—I7^vii	32.11 (5)	Ba3ⁱⁱ—I7—Ba5	70.658 (7)
O9^viii—Ba3—I7^viii	32.11 (5)	Ba4^vi—I7—Ba4ⁱⁱ	109.129 (11)
O9^viii—Ba3—I7^vii	96.85 (5)	Ba4ⁱⁱ—I7—Ba5	115.660 (7)
O9^ix—Ba3—I7^viii	96.85 (5)	Ba4^vi—I7—Ba5	115.660 (7)
O9^ix—Ba3—O9^viii	70.27 (10)	O9ⁱ—I7—Ba2	47.57 (8)
O9^ix—Ba3—O10^ix	55.24 (7)	O9—I7—Ba2	47.57 (8)
O9^viii—Ba3—O10^viii	55.24 (7)	O9ⁱ—I7—Ba3ⁱⁱ	52.75 (8)
O9^ix—Ba3—O10^viii	94.55 (8)	O9—I7—Ba3^vi	52.75 (8)
O9^viii—Ba3—O10^ix	94.55 (8)	O9ⁱ—I7—Ba3^vi	126.11 (8)
O9^ix—Ba3—O11^x	169.96 (7)	O9—I7—Ba3ⁱⁱ	126.11 (8)
O9^viii—Ba3—O11^vii	169.96 (7)	O9ⁱ—I7—Ba4ⁱⁱ	49.66 (8)
O9^ix—Ba3—O11^vii	119.07 (7)	O9ⁱ—I7—Ba4^vi	120.80 (9)
O9^viii—Ba3—O11^x	119.07 (7)	O9—I7—Ba4ⁱⁱ	120.80 (9)
O9^ix—Ba3—O12	125.79 (7)	O9—I7—Ba4^vi	49.66 (8)
O9^viii—Ba3—O12	125.79 (7)	O9—I7—Ba5	123.22 (9)
O9^viii—Ba3—O13^viii	55.27 (9)	O9ⁱ—I7—Ba5	123.22 (9)
O9^ix—Ba3—O13^viii	125.51 (9)	O9ⁱ—I7—O9	90.71 (16)
O9^ix—Ba3—O13^vii	55.27 (9)	O9ⁱ—I7—O13	90.74 (13)
O9^viii—Ba3—O13^vii	125.51 (9)	O9—I7—O13	90.74 (13)
O10^viii—Ba3—I7^viii	32.12 (5)	O10—I7—Ba2	132.56 (9)
O10^viii—Ba3—I7^vii	95.77 (6)	O10ⁱ—I7—Ba2	132.56 (9)
O10^ix—Ba3—I7^vii	32.12 (5)	O10—I7—Ba3^vi	54.32 (9)
O10^ix—Ba3—I7^viii	95.77 (6)	O10ⁱ—I7—Ba3ⁱⁱ	54.32 (9)
O10^viii—Ba3—O10^ix	68.70 (11)	O10—I7—Ba3ⁱⁱ	128.00 (9)
O10^viii—Ba3—O11^vii	124.17 (7)	O10ⁱ—I7—Ba3^vi	128.00 (9)
O10^ix—Ba3—O11^x	124.17 (7)	O10—I7—Ba4ⁱⁱ	129.82 (9)
O10^viii—Ba3—O11^x	94.17 (8)	O10ⁱ—I7—Ba4^vi	129.82 (9)
O10^ix—Ba3—O11^vii	94.17 (8)	O10ⁱ—I7—Ba4ⁱⁱ	58.46 (9)
O10^viii—Ba3—O13^vii	123.11 (10)	O10—I7—Ba4^vi	58.46 (9)
O10^ix—Ba3—O13^vii	54.42 (9)	O10ⁱ—I7—Ba5	57.57 (9)
O10^viii—Ba3—O13^viii	54.42 (9)	O10—I7—Ba5	57.57 (9)
O10^ix—Ba3—O13^viii	123.11 (10)	O10—I7—O9	89.07 (12)
O11^x—Ba3—I7^viii	93.18 (5)	O10ⁱ—I7—O9	179.10 (13)
O11^x—Ba3—I7^vii	141.54 (4)	O10ⁱ—I7—O9ⁱ	89.08 (12)
O11^vii—Ba3—I7^viii	141.54 (4)	O10—I7—O9ⁱ	179.10 (13)
O11^vii—Ba3—I7^vii	93.18 (5)	O10—I7—O10ⁱ	91.12 (17)
O11^x—Ba3—O11^vii	51.36 (9)	O10—I7—O13	90.13 (13)
O12—Ba3—I7^viii	95.76 (4)	O10ⁱ—I7—O13	90.13 (13)
O12—Ba3—I7^vii	95.76 (4)	O13—I7—Ba2	74.83 (13)
O12—Ba3—O10^viii	71.16 (8)	O13—I7—Ba3ⁱⁱ	57.126 (7)
O12—Ba3—O10^ix	71.16 (8)	O13—I7—Ba3^vi	57.126 (7)
O12—Ba3—O11^x	53.13 (8)	O13—I7—Ba4ⁱⁱ	124.989 (15)
O12—Ba3—O11^vii	53.13 (8)	O13—I7—Ba4^vi	124.989 (15)
O12—Ba3—O13^vii	88.69 (9)	O13—I7—Ba5	50.18 (13)
O12—Ba3—O13^viii	88.69 (9)	O15^iv—I7—Ba2	102.78 (12)
O13^viii—Ba3—I7^viii	32.40 (7)	O15^iv—I7—Ba3^vi	122.781 (9)
O13^vii—Ba3—I7^vii	32.40 (7)	O15^iv—I7—Ba3ⁱⁱ	122.781 (9)
O13^vii—Ba3—I7^viii	146.54 (7)	O15^iv—I7—Ba4ⁱⁱ	54.796 (11)
O13^viii—Ba3—I7^vii	146.54 (7)	O15^iv—I7—Ba4^vi	54.796 (11)
O13^viii—Ba3—O11^vii	115.38 (9)	O15^iv—I7—Ba5	132.21 (12)
O13^vii—Ba3—O11^x	115.38 (9)	O15^iv—I7—O9	87.58 (12)
O13^viii—Ba3—O11^x	64.04 (9)	O15^iv—I7—O9ⁱ	87.58 (12)
O13^vii—Ba3—O11^vii	64.04 (9)	O15^iv—I7—O10ⁱ	91.54 (13)
O13^viii—Ba3—O13^vii	176.94 (17)	O15^iv—I7—O10	91.54 (13)
O15^xi—Ba3—I7^vii	118.70 (3)	O15^iv—I7—O13	177.61 (18)
O15^xi—Ba3—I7^viii	118.70 (3)	Ba1—O8—Ba5^vii	162.43 (9)
O15^xi—Ba3—O9^ix	111.90 (9)	Ba2—O8—Ba1	78.42 (7)
O15^xi—Ba3—O9^viii	111.90 (9)	Ba2—O8—Ba5^iv	100.70 (8)
O15^xi—Ba3—O10^viii	145.22 (6)	Ba2—O8—Ba5^vii	85.11 (7)
O15^xi—Ba3—O10^ix	145.22 (6)	Ba5^iv—O8—Ba1	90.31 (7)
O15^xi—Ba3—O11^x	62.30 (9)	Ba5^iv—O8—Ba5^vii	98.80 (8)
O15^xi—Ba3—O11^vii	62.30 (9)	I6^xvi—O8—Ba1	91.73 (10)
O15^xi—Ba3—O12	107.21 (11)	I6^xvi—O8—Ba2	159.07 (13)
O15^xi—Ba3—O13^viii	91.14 (8)	I6^xvi—O8—Ba5^iv	97.75 (10)
O15^xi—Ba3—O13^vii	91.14 (8)	I6^xvi—O8—Ba5^vii	101.80 (10)
I7^viii—Ba4—I7^vii	109.128 (11)	Ba2—O9—Ba1	74.80 (6)
O9^viii—Ba4—I7^viii	30.70 (5)	Ba2—O9—Ba3^vi	113.03 (10)
O9^ix—Ba4—I7^vii	30.70 (5)	Ba2—O9—Ba4^vi	146.46 (11)
O9^ix—Ba4—I7^viii	94.64 (6)	Ba3^vi—O9—Ba1	168.60 (10)
O9^viii—Ba4—I7^vii	94.64 (6)	Ba4^vi—O9—Ba1	78.85 (7)
O9^ix—Ba4—O9^viii	70.52 (11)	Ba4^vi—O9—Ba3^vi	90.73 (7)
O9^viii—Ba4—O10^viii	52.77 (7)	I7—O9—Ba1	91.20 (10)
O9^ix—Ba4—O10^viii	89.92 (8)	I7—O9—Ba2	101.28 (10)
O9^ix—Ba4—O10^ix	52.77 (7)	I7—O9—Ba3^vi	95.15 (10)
O9^viii—Ba4—O10^ix	89.92 (8)	I7—O9—Ba4^vi	99.64 (10)
O9^viii—Ba4—O11ⁱ	104.24 (8)	Ba2^vi—O10—Ba3^vi	93.24 (8)
O9^ix—Ba4—O11ⁱ	152.12 (8)	Ba2^vi—O10—Ba4^vi	92.53 (8)
O9^viii—Ba4—O11	152.12 (8)	Ba2^vi—O10—Ba5	85.52 (8)
O9^ix—Ba4—O11	104.24 (8)	Ba3^vi—O10—Ba4^vi	84.22 (7)
O9^ix—Ba4—O15^xiii	123.37 (9)	Ba3^vi—O10—Ba5	88.32 (8)
O9^viii—Ba4—O15^xii	123.37 (9)	Ba4^vi—O10—Ba5	172.17 (10)
O9^viii—Ba4—O15^xiii	53.26 (9)	I7—O10—Ba2^vi	172.83 (15)
O9^ix—Ba4—O15^xii	53.26 (9)	I7—O10—Ba3^vi	93.56 (10)
O10^ix—Ba4—I7^viii	89.77 (5)	I7—O10—Ba4^vi	90.41 (10)
O10^ix—Ba4—I7^vii	31.13 (5)	I7—O10—Ba5	92.41 (11)
O10^viii—Ba4—I7^vii	89.77 (5)	Ba1^xiv—O11—Ba1^vii	83.74 (7)
O10^viii—Ba4—I7^viii	31.13 (5)	Ba1^vii—O11—Ba3ⁱⁱ	99.37 (7)
O10^viii—Ba4—O10^ix	63.04 (10)	Ba1^xiv—O11—Ba3ⁱⁱ	171.81 (9)
O11ⁱ—Ba4—I7^vii	158.97 (5)	Ba1^xiv—O11—Ba4	91.24 (7)
O11ⁱ—Ba4—I7^viii	91.89 (5)	Ba1^xiv—O11—Ba5	90.09 (7)
O11—Ba4—I7^vii	91.89 (5)	Ba4—O11—Ba1^vii	79.99 (7)
O11—Ba4—I7^viii	158.97 (5)	Ba4—O11—Ba3ⁱⁱ	81.91 (6)
O11ⁱ—Ba4—O10^ix	154.47 (7)	Ba4—O11—Ba5	97.58 (7)
O11—Ba4—O10^viii	154.47 (7)	Ba5—O11—Ba1^vii	173.30 (10)
O11ⁱ—Ba4—O10^viii	108.94 (7)	Ba5—O11—Ba3ⁱⁱ	86.40 (7)
O11—Ba4—O10^ix	108.94 (7)	I6ⁱⁱ—O11—Ba1^xiv	96.78 (10)
O11—Ba4—O11ⁱ	67.08 (10)	I6ⁱⁱ—O11—Ba1^vii	91.52 (9)
O11—Ba4—O15^xiii	128.10 (9)	I6ⁱⁱ—O11—Ba3ⁱⁱ	90.73 (9)
O11ⁱ—Ba4—O15^xiii	61.20 (9)	I6ⁱⁱ—O11—Ba4	167.64 (13)
O11ⁱ—Ba4—O15^xii	128.10 (9)	I6ⁱⁱ—O11—Ba5	91.82 (10)
O11—Ba4—O15^xii	61.20 (9)	Ba2—O12—Ba3	90.58 (11)
O13—Ba4—I7^vii	102.72 (5)	Ba2—O12—Ba5^viii	86.42 (7)
O13—Ba4—I7^viii	102.72 (5)	Ba2—O12—Ba5^vii	86.42 (7)
O13—Ba4—O9^ix	133.19 (8)	Ba3—O12—Ba5^viii	93.34 (8)
O13—Ba4—O9^viii	133.19 (8)	Ba3—O12—Ba5^vii	93.34 (8)
O13—Ba4—O10^ix	83.85 (9)	Ba5^viii—O12—Ba5^vii	170.24 (15)
O13—Ba4—O10^viii	83.85 (9)	I6—O12—Ba2	168.4 (2)
O13—Ba4—O11ⁱ	70.94 (9)	I6—O12—Ba3	101.07 (15)
O13—Ba4—O11	70.94 (9)	I6—O12—Ba5^viii	92.84 (7)
O13—Ba4—O15^xii	88.24 (8)	I6—O12—Ba5^vii	92.84 (7)
O13—Ba4—O15^xiii	88.24 (8)	Ba3^vi—O13—Ba3ⁱⁱ	176.94 (17)
O14—Ba4—I7^viii	100.50 (5)	Ba4—O13—Ba3ⁱⁱ	88.97 (8)
O14—Ba4—I7^vii	100.50 (5)	Ba4—O13—Ba3^vi	88.97 (8)
O14—Ba4—O9^viii	76.73 (8)	Ba4—O13—Ba5	104.54 (13)
O14—Ba4—O9^ix	76.73 (8)	Ba5—O13—Ba3ⁱⁱ	91.35 (9)
O14—Ba4—O10^ix	129.20 (8)	Ba5—O13—Ba3^vi	91.35 (9)
O14—Ba4—O10^viii	129.20 (8)	I7—O13—Ba3ⁱⁱ	90.47 (7)
O14—Ba4—O11	75.43 (9)	I7—O13—Ba3^vi	90.47 (7)
O14—Ba4—O11ⁱ	75.43 (9)	I7—O13—Ba4	155.4 (2)
O14—Ba4—O13	139.37 (12)	I7—O13—Ba5	100.10 (16)
O14—Ba4—O15^xii	95.13 (8)	Ba1^xiv—O14—Ba1^vii	88.26 (7)
O14—Ba4—O15^xiii	95.13 (8)	Ba1^xiv—O14—Ba1^viii	88.26 (7)
O15^xiii—Ba4—I7^viii	30.93 (7)	Ba1^viii—O14—Ba1^vii	171.78 (14)
O15^xii—Ba4—I7^vii	30.93 (7)	Ba4—O14—Ba1^vii	86.60 (7)
O15^xii—Ba4—I7^viii	139.69 (7)	Ba4—O14—Ba1^xiv	99.15 (12)
O15^xiii—Ba4—I7^vii	139.69 (7)	Ba4—O14—Ba1^viii	86.60 (7)
O15^xiii—Ba4—O10^viii	52.49 (9)	I6^xx—O14—Ba1^viii	94.00 (7)
O15^xii—Ba4—O10^viii	115.52 (9)	I6^xx—O14—Ba1^vii	94.00 (7)
O15^xiii—Ba4—O10^ix	115.52 (9)	I6^xx—O14—Ba1^xiv	102.20 (15)
O15^xii—Ba4—O10^ix	52.49 (9)	I6^xx—O14—Ba4	158.65 (19)
O15^xiii—Ba4—O15^xii	167.84 (15)	Ba1^xiv—O15—Ba4^xiii	84.56 (8)
O8ⁱⁱ—Ba5—I6ⁱⁱ	89.25 (5)	Ba1^xiv—O15—Ba4^xii	84.56 (8)
O8^xiv—Ba5—I6ⁱⁱ	31.23 (5)	Ba3^xx—O15—Ba1^xiv	127.86 (15)
O8^xv—Ba5—I6ⁱⁱ	94.55 (5)	Ba3^xx—O15—Ba4^xii	91.20 (8)
O8ⁱⁱⁱ—Ba5—I6ⁱⁱ	134.22 (5)	Ba3^xx—O15—Ba4^xiii	91.20 (8)
O8^xiv—Ba5—O8ⁱⁱ	81.20 (8)	Ba4^xiii—O15—Ba4^xii	167.84 (15)
O8^xiv—Ba5—O8ⁱⁱⁱ	109.88 (5)	I7^xiv—O15—Ba1^xiv	108.24 (17)
O8^xv—Ba5—O8ⁱⁱⁱ	81.20 (8)	I7^xiv—O15—Ba3^xx	123.91 (19)
O8^xv—Ba5—O8ⁱⁱ	109.88 (5)	I7^xiv—O15—Ba4^xii	94.27 (7)
O8ⁱⁱⁱ—Ba5—O8ⁱⁱ	51.30 (9)	I7^xiv—O15—Ba4^xiii	94.27 (7)
O8^xiv—Ba5—O8^xv	69.41 (10)

Ba1^xviii—I6—O12—Ba2	93.41 (9)	Ba5—I7—O9—Ba1	−175.958 (13)
Ba1^xix—I6—O12—Ba2	180.000 (1)	Ba5—I7—O9—Ba2	109.30 (8)
Ba1^xvi—I6—O12—Ba2	−93.41 (9)	Ba5—I7—O9—Ba3^vi	−5.44 (11)
Ba1^xvi—I6—O12—Ba3	86.59 (9)	Ba5—I7—O9—Ba4^vi	−97.06 (9)
Ba1^xviii—I6—O12—Ba3	−86.59 (9)	Ba5—I7—O10—Ba3^vi	88.46 (9)
Ba1^xix—I6—O12—Ba3	0.000 (1)	Ba5—I7—O10—Ba4^vi	172.70 (11)
Ba1^xix—I6—O12—Ba5^vii	−93.97 (8)	Ba5—I7—O13—Ba3ⁱⁱ	91.45 (9)
Ba1^xviii—I6—O12—Ba5^vii	179.445 (14)	Ba5—I7—O13—Ba3^vi	−91.45 (9)
Ba1^xvi—I6—O12—Ba5^vii	−7.38 (17)	Ba5—I7—O13—Ba4	180.000 (1)
Ba1^xvi—I6—O12—Ba5^viii	−179.445 (14)	O8^xvi—I6—O12—Ba2	−45.60 (8)
Ba1^xix—I6—O12—Ba5^viii	93.97 (8)	O8^xvii—I6—O12—Ba2	45.60 (8)
Ba1^xviii—I6—O12—Ba5^viii	7.38 (17)	O8^xvi—I6—O12—Ba3	134.40 (8)
Ba2—I7—O9—Ba1	74.74 (8)	O8^xvii—I6—O12—Ba3	−134.40 (8)
Ba2—I7—O9—Ba3^vi	−114.74 (12)	O8^xvi—I6—O12—Ba5^viii	−131.63 (12)
Ba2—I7—O9—Ba4^vi	153.64 (15)	O8^xvii—I6—O12—Ba5^viii	−40.43 (12)
Ba2—I7—O10—Ba3^vi	−21.39 (15)	O8^xvi—I6—O12—Ba5^vii	40.43 (12)
Ba2—I7—O10—Ba4^vi	62.85 (12)	O8^xvii—I6—O12—Ba5^vii	131.63 (12)
Ba2—I7—O10—Ba5	−109.85 (8)	O9ⁱ—I7—O9—Ba1	52.50 (12)
Ba2—I7—O13—Ba3ⁱⁱ	−88.55 (9)	O9ⁱ—I7—O9—Ba2	−22.24 (16)
Ba2—I7—O13—Ba3^vi	88.55 (9)	O9ⁱ—I7—O9—Ba3^vi	−136.98 (6)
Ba2—I7—O13—Ba4	0.0	O9ⁱ—I7—O9—Ba4^vi	131.40 (6)
Ba2—I7—O13—Ba5	180.000 (1)	O9—I7—O10—Ba3^vi	−42.80 (11)
Ba3—I6—O12—Ba2	180.000 (2)	O9—I7—O10—Ba4^vi	41.44 (10)
Ba3—I6—O12—Ba5^vii	−93.97 (8)	O9—I7—O10—Ba5	−131.26 (10)
Ba3—I6—O12—Ba5^viii	93.97 (8)	O9ⁱ—I7—O13—Ba3^vi	133.91 (12)
Ba3^vi—I7—O9—Ba1	−170.52 (11)	O9—I7—O13—Ba3ⁱⁱ	−133.91 (12)
Ba3ⁱⁱ—I7—O9—Ba1	94.75 (8)	O9—I7—O13—Ba3^vi	43.19 (12)
Ba3ⁱⁱ—I7—O9—Ba2	20.00 (14)	O9ⁱ—I7—O13—Ba3ⁱⁱ	−43.19 (12)
Ba3^vi—I7—O9—Ba2	114.74 (12)	O9—I7—O13—Ba4	−45.36 (8)
Ba3ⁱⁱ—I7—O9—Ba3^vi	−94.73 (8)	O9ⁱ—I7—O13—Ba4	45.36 (8)
Ba3ⁱⁱ—I7—O9—Ba4^vi	173.643 (17)	O9ⁱ—I7—O13—Ba5	−134.64 (8)
Ba3^vi—I7—O9—Ba4^vi	−91.62 (9)	O9—I7—O13—Ba5	134.64 (8)
Ba3ⁱⁱ—I7—O10—Ba3^vi	94.55 (9)	O10—I7—O9—Ba1	−126.63 (10)
Ba3ⁱⁱ—I7—O10—Ba4^vi	178.780 (19)	O10—I7—O9—Ba2	158.63 (12)
Ba3^vi—I7—O10—Ba4^vi	84.23 (8)	O10—I7—O9—Ba3^vi	43.89 (11)
Ba3ⁱⁱ—I7—O10—Ba5	6.08 (12)	O10—I7—O9—Ba4^vi	−47.73 (12)
Ba3^vi—I7—O10—Ba5	−88.46 (9)	O10ⁱ—I7—O10—Ba3^vi	138.08 (6)
Ba3^vi—I7—O13—Ba3ⁱⁱ	−177.09 (17)	O10ⁱ—I7—O10—Ba4^vi	−137.69 (7)
Ba3ⁱⁱ—I7—O13—Ba3^vi	177.09 (17)	O10ⁱ—I7—O10—Ba5	49.61 (14)
Ba3ⁱⁱ—I7—O13—Ba4	88.55 (9)	O10—I7—O13—Ba3^vi	−45.89 (12)
Ba3^vi—I7—O13—Ba4	−88.55 (9)	O10—I7—O13—Ba3ⁱⁱ	137.02 (12)
Ba3^vi—I7—O13—Ba5	91.45 (9)	O10ⁱ—I7—O13—Ba3ⁱⁱ	45.89 (12)
Ba3ⁱⁱ—I7—O13—Ba5	−91.45 (9)	O10ⁱ—I7—O13—Ba3^vi	−137.02 (12)
Ba4ⁱⁱ—I7—O9—Ba1	10.77 (10)	O10ⁱ—I7—O13—Ba4	134.44 (9)
Ba4^vi—I7—O9—Ba1	−78.90 (8)	O10—I7—O13—Ba4	−134.44 (9)
Ba4^vi—I7—O9—Ba2	−153.64 (15)	O10—I7—O13—Ba5	45.56 (9)
Ba4ⁱⁱ—I7—O9—Ba2	−63.97 (11)	O10ⁱ—I7—O13—Ba5	−45.56 (9)
Ba4ⁱⁱ—I7—O9—Ba3^vi	−178.708 (17)	O11^vii—I6—O12—Ba2	−134.11 (8)
Ba4^vi—I7—O9—Ba3^vi	91.62 (9)	O11^x—I6—O12—Ba2	134.11 (8)
Ba4ⁱⁱ—I7—O9—Ba4^vi	89.67 (8)	O11^vii—I6—O12—Ba3	45.89 (8)
Ba4ⁱⁱ—I7—O10—Ba3^vi	−173.595 (18)	O11^x—I6—O12—Ba3	−45.89 (8)
Ba4^vi—I7—O10—Ba3^vi	−84.23 (8)	O11^vii—I6—O12—Ba5^viii	139.85 (11)
Ba4ⁱⁱ—I7—O10—Ba4^vi	−89.36 (9)	O11^vii—I6—O12—Ba5^vii	−48.08 (11)
Ba4^vi—I7—O10—Ba5	−172.70 (11)	O11^x—I6—O12—Ba5^viii	48.08 (11)
Ba4ⁱⁱ—I7—O10—Ba5	97.94 (9)	O11^x—I6—O12—Ba5^vii	−139.85 (11)
Ba4^vi—I7—O13—Ba3^vi	4.55 (18)	O13—I7—O9—Ba1	143.25 (11)
Ba4^vi—I7—O13—Ba3ⁱⁱ	−172.541 (16)	O13—I7—O9—Ba2	68.51 (12)
Ba4ⁱⁱ—I7—O13—Ba3ⁱⁱ	−4.55 (18)	O13—I7—O9—Ba3^vi	−46.23 (11)
Ba4ⁱⁱ—I7—O13—Ba3^vi	172.541 (16)	O13—I7—O9—Ba4^vi	−137.85 (12)
Ba4^vi—I7—O13—Ba4	−83.99 (9)	O13—I7—O10—Ba3^vi	47.94 (12)
Ba4ⁱⁱ—I7—O13—Ba4	83.99 (9)	O13—I7—O10—Ba4^vi	132.17 (11)
Ba4ⁱⁱ—I7—O13—Ba5	−96.01 (9)	O13—I7—O10—Ba5	−40.52 (11)
Ba4^vi—I7—O13—Ba5	96.01 (9)	O15^iv—I7—O9—Ba1	−35.05 (10)
Ba5^vii—I6—O12—Ba2	−86.03 (8)	O15^iv—I7—O9—Ba2	−109.79 (12)
Ba5^viii—I6—O12—Ba2	86.03 (8)	O15^iv—I7—O9—Ba3^vi	135.47 (11)
Ba5^viii—I6—O12—Ba3	−93.97 (8)	O15^iv—I7—O9—Ba4^vi	43.85 (11)
Ba5^vii—I6—O12—Ba3	93.97 (8)	O15^iv—I7—O10—Ba3^vi	−130.35 (11)
Ba5^viii—I6—O12—Ba5^vii	172.07 (17)	O15^iv—I7—O10—Ba4^vi	−46.12 (10)
Ba5^vii—I6—O12—Ba5^viii	−172.07 (17)	O15^iv—I7—O10—Ba5	141.19 (10)

Symmetry codes: (i) x, −y+1/2, z; (ii) −x+1/2, −y+1, z−1/2; (iii) −x+1/2, y−1/2, z−1/2; (iv) x−1/2, y, −z+1/2; (v) x−1/2, −y+1/2, −z+1/2; (vi) −x+1/2, −y, z−1/2; (vii) −x+1/2, −y+1, z+1/2; (viii) −x+1/2, −y, 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−1/2, y, −z+3/2; (xii) −x+1, −y+1, −z+1; (xiii) −x+1, −y, −z+1; (xiv) x+1/2, y, −z+1/2; (xv) x+1/2, −y+1/2, −z+1/2; (xvi) −x, −y+1, −z+1; (xvii) −x, y−1/2, −z+1; (xviii) −x, −y, −z+1; (xix) x, y, z+1; (xx) x+1/2, y, −z+3/2.

(80K) top

Crystal data top

Ba₅I₂O₁₂	D_x = 6.132 Mg m⁻³
M_r = 1132.50	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pnma	Cell parameters from 13815 reflections
a = 19.7361 (3) Å	θ = 1.9–36.2°
b = 5.8779 (1) Å	µ = 20.90 mm⁻¹
c = 10.5749 (1) Å	T = 80 K
V = 1226.76 (3) Å³	Prism, brown
Z = 4	0.22 × 0.12 × 0.08 mm
F(000) = 1928

Data collection top

XtaLAB Synergy-I with HyPix3000 diffractometer	2462 reflections with I > 2σ(I)
Detector resolution: 10.0000 pixels mm^-1	R_int = 0.033
ω scans	θ_max = 33.1°, θ_min = 2.1°
Absorption correction: gaussian (CrysAlisPro; Rigaku OD, 2020)	h = −27→30
T_min = 0.150, T_max = 0.750	k = −8→9
16187 measured reflections	l = −16→14
2529 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0092P)² + 7.6239P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.022	(Δ/σ)_max = 0.001
wR(F²) = 0.043	Δρ_max = 1.90 e Å⁻³
S = 1.25	Δρ_min = −1.60 e Å⁻³
2529 reflections	Extinction correction: SHELXL2018/3 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
104 parameters	Extinction coefficient: 0.00060 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ba1	0.04800 (2)	0.250000	0.08951 (3)	0.00409 (6)
Ba2	0.14082 (2)	0.250000	0.38331 (3)	0.00342 (6)
Ba3	0.19966 (2)	0.250000	0.74015 (3)	0.00461 (6)
Ba4	0.34267 (2)	0.250000	0.47535 (3)	0.00355 (6)
Ba5	0.42748 (2)	0.250000	0.08947 (3)	0.00448 (6)
I6	0.01359 (2)	0.250000	0.74889 (3)	0.00249 (6)
I7	0.23871 (2)	0.250000	0.10166 (3)	0.00307 (6)
O8	0.03691 (13)	0.5213 (4)	0.3330 (2)	0.0056 (5)
O9	0.18812 (14)	0.0229 (5)	0.1838 (2)	0.0074 (5)
O10	0.28798 (14)	0.0228 (5)	0.0181 (3)	0.0083 (5)
O11	0.43517 (13)	0.5187 (5)	0.3288 (3)	0.0067 (5)
O12	0.07588 (19)	0.250000	0.6120 (4)	0.0062 (7)
O13	0.3025 (2)	0.250000	0.2342 (4)	0.0079 (7)
O14	0.45602 (18)	0.250000	0.6070 (3)	0.0048 (6)
O15	0.67265 (19)	0.250000	0.5245 (4)	0.0081 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba1	0.00457 (12)	0.00427 (12)	0.00343 (11)	0.000	0.00003 (9)	0.000
Ba2	0.00324 (11)	0.00415 (12)	0.00288 (11)	0.000	−0.00054 (9)	0.000
Ba3	0.00566 (12)	0.00425 (12)	0.00394 (12)	0.000	0.00160 (9)	0.000
Ba4	0.00339 (11)	0.00438 (12)	0.00288 (11)	0.000	−0.00051 (9)	0.000
Ba5	0.00447 (12)	0.00409 (12)	0.00487 (12)	0.000	−0.00101 (9)	0.000
I6	0.00238 (12)	0.00310 (13)	0.00198 (12)	0.000	0.00006 (9)	0.000
I7	0.00310 (12)	0.00381 (13)	0.00229 (12)	0.000	0.00011 (10)	0.000
O8	0.0048 (10)	0.0055 (12)	0.0065 (11)	0.0025 (9)	−0.0006 (9)	0.0025 (9)
O9	0.0106 (12)	0.0054 (12)	0.0063 (11)	−0.0019 (10)	0.0028 (9)	0.0004 (9)
O10	0.0112 (12)	0.0053 (12)	0.0084 (11)	0.0030 (10)	0.0031 (10)	−0.0012 (9)
O11	0.0065 (11)	0.0059 (11)	0.0077 (11)	−0.0022 (9)	0.0013 (9)	0.0025 (9)
O12	0.0051 (15)	0.0077 (17)	0.0056 (15)	0.000	0.0047 (13)	0.000
O13	0.0104 (17)	0.0101 (17)	0.0033 (15)	0.000	−0.0040 (13)	0.000
O14	0.0044 (14)	0.0063 (16)	0.0038 (15)	0.000	−0.0009 (12)	0.000
O15	0.0065 (15)	0.0112 (18)	0.0066 (16)	0.000	0.0015 (13)	0.000

Geometric parameters (Å, º) top

Ba1—O8	3.037 (3)	Ba4—I7^viii	3.6057 (2)
Ba1—O8ⁱ	3.037 (3)	Ba4—O9^ix	2.793 (3)
Ba1—O9	3.229 (3)	Ba4—O9^viii	2.793 (3)
Ba1—O9ⁱ	3.229 (3)	Ba4—O10^ix	3.070 (3)
Ba1—O11ⁱⁱ	3.092 (3)	Ba4—O10^viii	3.070 (3)
Ba1—O11ⁱⁱⁱ	3.092 (3)	Ba4—O11ⁱ	2.869 (3)
Ba1—O11^iv	2.864 (3)	Ba4—O11	2.869 (3)
Ba1—O11^v	2.864 (3)	Ba4—O13	2.670 (4)
Ba1—O14ⁱⁱ	2.9458 (3)	Ba4—O14	2.635 (4)
Ba1—O14^vi	2.9458 (3)	Ba4—O15^xii	2.9545 (4)
Ba1—O14^iv	2.759 (4)	Ba4—O15^xiii	2.9545 (4)
Ba1—O15^iv	2.740 (4)	Ba5—I6ⁱⁱ	3.5822 (2)
Ba2—Ba3	3.9482 (4)	Ba5—O8ⁱⁱ	3.107 (3)
Ba2—Ba5^vii	3.8997 (3)	Ba5—O8^xiv	2.807 (3)
Ba2—Ba5^viii	3.8997 (3)	Ba5—O8^xv	2.807 (3)
Ba2—I7	3.5501 (4)	Ba5—O8ⁱⁱⁱ	3.107 (3)
Ba2—O8ⁱ	2.652 (3)	Ba5—O10	3.152 (3)
Ba2—O8	2.652 (3)	Ba5—O10ⁱ	3.152 (3)
Ba2—O9ⁱ	2.665 (3)	Ba5—O11ⁱ	2.987 (3)
Ba2—O9	2.665 (3)	Ba5—O11	2.987 (3)
Ba2—O10^viii	2.565 (3)	Ba5—O12^vi	2.9494 (3)
Ba2—O10^ix	2.565 (3)	Ba5—O12ⁱⁱ	2.9494 (3)
Ba2—O12	2.737 (4)	Ba5—O13	2.903 (4)
Ba3—I7^viii	3.5016 (2)	I6—O8^xvi	1.884 (3)
Ba3—I7^vii	3.5016 (2)	I6—O8^xvii	1.884 (3)
Ba3—O9^viii	2.799 (3)	I6—O11^vii	1.893 (3)
Ba3—O9^ix	2.799 (3)	I6—O11^x	1.893 (3)
Ba3—O10^ix	2.854 (3)	I6—O12	1.899 (4)
Ba3—O10^viii	2.854 (3)	I6—O14^xi	1.901 (4)
Ba3—O11^vii	3.132 (3)	I7—O9ⁱ	1.880 (3)
Ba3—O11^x	3.132 (3)	I7—O9	1.880 (3)
Ba3—O12	2.794 (4)	I7—O10	1.873 (3)
Ba3—O13^vii	2.9399 (1)	I7—O10ⁱ	1.873 (3)
Ba3—O13^viii	2.9399 (1)	I7—O13	1.884 (4)
Ba3—O15^xi	2.545 (4)	I7—O15^iv	1.866 (4)
Ba4—I7^vii	3.6057 (2)

O8ⁱ—Ba1—O8	63.36 (10)	O8ⁱⁱⁱ—Ba5—O10ⁱ	99.90 (7)
O8ⁱ—Ba1—O9ⁱ	90.97 (7)	O8^xv—Ba5—O10ⁱ	169.34 (7)
O8—Ba1—O9ⁱ	65.33 (7)	O8ⁱⁱ—Ba5—O10ⁱ	78.78 (7)
O8ⁱ—Ba1—O9	65.33 (7)	O8^xiv—Ba5—O10ⁱ	120.09 (7)
O8—Ba1—O9	90.97 (7)	O8ⁱⁱⁱ—Ba5—O10	78.77 (7)
O8ⁱ—Ba1—O11ⁱⁱⁱ	122.21 (7)	O8ⁱⁱ—Ba5—O10	99.90 (7)
O8—Ba1—O11ⁱⁱⁱ	174.14 (7)	O8^xv—Ba5—O10	120.09 (7)
O8ⁱ—Ba1—O11ⁱⁱ	174.14 (7)	O8^xiv—Ba5—O10	169.35 (7)
O8—Ba1—O11ⁱⁱ	122.21 (7)	O8^xiv—Ba5—O11ⁱ	90.80 (8)
O9ⁱ—Ba1—O9	48.85 (10)	O8^xv—Ba5—O11	90.80 (7)
O11^v—Ba1—O8ⁱ	53.02 (7)	O8^xv—Ba5—O11ⁱ	54.06 (7)
O11^iv—Ba1—O8ⁱ	88.73 (7)	O8^xiv—Ba5—O11	54.06 (7)
O11^v—Ba1—O8	88.73 (7)	O8^xiv—Ba5—O12ⁱⁱ	55.08 (9)
O11^iv—Ba1—O8	53.02 (7)	O8^xv—Ba5—O12^vi	55.08 (9)
O11^v—Ba1—O9ⁱ	143.22 (7)	O8^xv—Ba5—O12ⁱⁱ	124.04 (9)
O11^v—Ba1—O9	110.17 (7)	O8^xiv—Ba5—O12^vi	124.04 (9)
O11ⁱⁱⁱ—Ba1—O9	90.10 (7)	O8^xv—Ba5—O13	119.99 (8)
O11^iv—Ba1—O9ⁱ	110.17 (7)	O8^xiv—Ba5—O13	119.99 (8)
O11^iv—Ba1—O9	143.22 (7)	O10—Ba5—I6ⁱⁱ	138.07 (5)
O11ⁱⁱⁱ—Ba1—O9ⁱ	111.43 (7)	O10ⁱ—Ba5—I6ⁱⁱ	92.79 (5)
O11ⁱⁱ—Ba1—O9	111.43 (7)	O10—Ba5—O10ⁱ	50.13 (10)
O11ⁱⁱ—Ba1—O9ⁱ	90.10 (7)	O11—Ba5—I6ⁱⁱ	31.89 (5)
O11ⁱⁱⁱ—Ba1—O11ⁱⁱ	52.17 (10)	O11ⁱ—Ba5—I6ⁱⁱ	91.07 (5)
O11^v—Ba1—O11^iv	66.95 (10)	O11ⁱ—Ba5—O8ⁱⁱ	163.07 (7)
O11^v—Ba1—O11ⁱⁱ	126.52 (4)	O11—Ba5—O8ⁱⁱ	119.95 (7)
O11^v—Ba1—O11ⁱⁱⁱ	96.32 (7)	O11—Ba5—O8ⁱⁱⁱ	163.07 (7)
O11^iv—Ba1—O11ⁱⁱⁱ	126.52 (4)	O11ⁱ—Ba5—O8ⁱⁱⁱ	119.95 (7)
O11^iv—Ba1—O11ⁱⁱ	96.32 (7)	O11—Ba5—O10ⁱ	91.33 (7)
O11^iv—Ba1—O14ⁱⁱ	53.83 (9)	O11ⁱ—Ba5—O10ⁱ	118.12 (7)
O11^v—Ba1—O14ⁱⁱ	120.69 (9)	O11—Ba5—O10	118.12 (7)
O11^v—Ba1—O14^vi	53.83 (9)	O11ⁱ—Ba5—O10	91.33 (7)
O11^iv—Ba1—O14^vi	120.69 (9)	O11—Ba5—O11ⁱ	63.85 (10)
O14^iv—Ba1—O8	126.24 (7)	O12ⁱⁱ—Ba5—I6ⁱⁱ	31.97 (7)
O14^vi—Ba1—O8	117.95 (9)	O12^vi—Ba5—I6ⁱⁱ	141.89 (7)
O14ⁱⁱ—Ba1—O8	54.61 (9)	O12ⁱⁱ—Ba5—O8ⁱⁱ	69.18 (9)
O14ⁱⁱ—Ba1—O8ⁱ	117.95 (9)	O12^vi—Ba5—O8ⁱⁱ	120.45 (9)
O14^vi—Ba1—O8ⁱ	54.61 (9)	O12^vi—Ba5—O8ⁱⁱⁱ	69.18 (9)
O14^iv—Ba1—O8ⁱ	126.24 (7)	O12ⁱⁱ—Ba5—O8ⁱⁱⁱ	120.45 (9)
O14^iv—Ba1—O9	142.76 (7)	O12^vi—Ba5—O10ⁱ	114.95 (9)
O14ⁱⁱ—Ba1—O9ⁱ	65.87 (9)	O12ⁱⁱ—Ba5—O10ⁱ	65.01 (9)
O14^iv—Ba1—O9ⁱ	142.76 (7)	O12ⁱⁱ—Ba5—O10	114.95 (9)
O14ⁱⁱ—Ba1—O9	114.60 (9)	O12^vi—Ba5—O10	65.01 (9)
O14^vi—Ba1—O9	65.87 (9)	O12^vi—Ba5—O11ⁱ	53.54 (9)
O14^vi—Ba1—O9ⁱ	114.60 (9)	O12ⁱⁱ—Ba5—O11	53.54 (9)
O14^iv—Ba1—O11^iv	73.48 (8)	O12^vi—Ba5—O11	117.36 (9)
O14^iv—Ba1—O11^v	73.48 (8)	O12ⁱⁱ—Ba5—O11ⁱ	117.36 (9)
O14^vi—Ba1—O11ⁱⁱ	119.83 (9)	O12ⁱⁱ—Ba5—O12^vi	170.37 (15)
O14^iv—Ba1—O11ⁱⁱⁱ	53.07 (8)	O13—Ba5—I6ⁱⁱ	91.59 (4)
O14ⁱⁱ—Ba1—O11ⁱⁱ	67.68 (9)	O13—Ba5—O8ⁱⁱⁱ	130.72 (8)
O14ⁱⁱ—Ba1—O11ⁱⁱⁱ	119.83 (9)	O13—Ba5—O8ⁱⁱ	130.72 (8)
O14^iv—Ba1—O11ⁱⁱ	53.07 (8)	O13—Ba5—O10	51.97 (8)
O14^vi—Ba1—O11ⁱⁱⁱ	67.68 (9)	O13—Ba5—O10ⁱ	51.97 (8)
O14^iv—Ba1—O14ⁱⁱ	91.69 (7)	O13—Ba5—O11ⁱ	66.20 (8)
O14^iv—Ba1—O14^vi	91.69 (7)	O13—Ba5—O11	66.20 (8)
O14ⁱⁱ—Ba1—O14^vi	172.17 (14)	O13—Ba5—O12ⁱⁱ	86.46 (8)
O15^iv—Ba1—O8ⁱ	115.98 (8)	O13—Ba5—O12^vi	86.46 (8)
O15^iv—Ba1—O8	115.98 (8)	Ba1^xvi—I6—Ba1^xviii	108.979 (11)
O15^iv—Ba1—O9ⁱ	50.72 (8)	Ba1^xvi—I6—Ba1^xix	66.249 (7)
O15^iv—Ba1—O9	50.72 (8)	Ba1^xviii—I6—Ba1^xix	66.249 (7)
O15^iv—Ba1—O11ⁱⁱ	60.73 (8)	Ba1^xvi—I6—Ba3	110.393 (7)
O15^iv—Ba1—O11^v	146.21 (5)	Ba1^xix—I6—Ba3	80.763 (9)
O15^iv—Ba1—O11^iv	146.21 (5)	Ba1^xviii—I6—Ba3	110.393 (7)
O15^iv—Ba1—O11ⁱⁱⁱ	60.73 (8)	Ba5^viii—I6—Ba1^xvi	179.206 (10)
O15^iv—Ba1—O14^iv	105.02 (11)	Ba5^vii—I6—Ba1^xviii	179.206 (10)
O15^iv—Ba1—O14ⁱⁱ	92.97 (7)	Ba5^viii—I6—Ba1^xviii	70.380 (5)
O15^iv—Ba1—O14^vi	92.97 (7)	Ba5^viii—I6—Ba1^xix	113.722 (7)
Ba1—Ba2—Ba3	166.582 (11)	Ba5^vii—I6—Ba1^xix	113.722 (7)
Ba1—Ba2—Ba5^vii	107.819 (7)	Ba5^vii—I6—Ba1^xvi	70.380 (5)
Ba1—Ba2—Ba5^viii	107.819 (7)	Ba5^viii—I6—Ba3	70.341 (7)
Ba5^viii—Ba2—Ba3	64.364 (6)	Ba5^vii—I6—Ba3	70.341 (7)
Ba5^vii—Ba2—Ba3	64.364 (6)	Ba5^viii—I6—Ba5^vii	110.256 (11)
Ba5^vii—Ba2—Ba5^viii	97.813 (9)	O8^xvi—I6—Ba1^xviii	128.33 (8)
I7—Ba2—Ba1	63.494 (8)	O8^xvi—I6—Ba1^xix	123.35 (8)
I7—Ba2—Ba3	129.924 (10)	O8^xvii—I6—Ba1^xviii	57.24 (8)
I7—Ba2—Ba5^vii	131.082 (5)	O8^xvii—I6—Ba1^xix	123.35 (8)
I7—Ba2—Ba5^viii	131.082 (5)	O8^xvii—I6—Ba1^xvi	128.33 (8)
O8ⁱ—Ba2—Ba1	55.56 (6)	O8^xvi—I6—Ba1^xvi	57.24 (8)
O8—Ba2—Ba1	55.56 (6)	O8^xvi—I6—Ba3	121.15 (8)
O8—Ba2—Ba3	114.78 (6)	O8^xvii—I6—Ba3	121.15 (8)
O8ⁱ—Ba2—Ba3	114.78 (6)	O8^xvi—I6—Ba5^vii	50.96 (8)
O8ⁱ—Ba2—Ba5^vii	107.34 (6)	O8^xvii—I6—Ba5^vii	122.73 (8)
O8ⁱ—Ba2—Ba5^viii	52.52 (6)	O8^xvii—I6—Ba5^viii	50.96 (8)
O8—Ba2—Ba5^viii	107.34 (6)	O8^xvi—I6—Ba5^viii	122.73 (8)
O8—Ba2—Ba5^vii	52.52 (6)	O8^xvii—I6—O8^xvi	91.01 (16)
O8ⁱ—Ba2—I7	104.63 (6)	O8^xvi—I6—O11^vii	88.60 (12)
O8—Ba2—I7	104.63 (6)	O8^xvii—I6—O11^vii	179.13 (12)
O8ⁱ—Ba2—O8	73.95 (11)	O8^xvii—I6—O11^x	88.60 (12)
O8ⁱ—Ba2—O9ⁱ	114.42 (8)	O8^xvi—I6—O11^x	179.13 (12)
O8—Ba2—O9ⁱ	79.10 (8)	O8^xvii—I6—O12	89.54 (11)
O8ⁱ—Ba2—O9	79.10 (8)	O8^xvi—I6—O12	89.54 (11)
O8—Ba2—O9	114.42 (8)	O8^xvii—I6—O14^xi	93.01 (11)
O8ⁱ—Ba2—O12	79.34 (8)	O8^xvi—I6—O14^xi	93.01 (11)
O8—Ba2—O12	79.34 (8)	O11^vii—I6—Ba1^xix	57.49 (8)
O9ⁱ—Ba2—Ba1	59.74 (6)	O11^x—I6—Ba1^xviii	51.98 (8)
O9—Ba2—Ba1	59.74 (6)	O11^x—I6—Ba1^xvi	123.58 (8)
O9ⁱ—Ba2—Ba3	130.80 (6)	O11^vii—I6—Ba1^xviii	123.58 (8)
O9—Ba2—Ba3	130.80 (6)	O11^vii—I6—Ba1^xvi	51.98 (8)
O9ⁱ—Ba2—Ba5^viii	160.23 (6)	O11^x—I6—Ba1^xix	57.49 (8)
O9—Ba2—Ba5^vii	160.23 (6)	O11^x—I6—Ba3	58.48 (8)
O9ⁱ—Ba2—Ba5^vii	100.72 (6)	O11^vii—I6—Ba3	58.48 (8)
O9—Ba2—Ba5^viii	100.72 (6)	O11^vii—I6—Ba5^viii	128.73 (8)
O9ⁱ—Ba2—I7	31.28 (6)	O11^vii—I6—Ba5^vii	56.46 (8)
O9—Ba2—I7	31.28 (6)	O11^x—I6—Ba5^vii	128.73 (8)
O9ⁱ—Ba2—O9	60.12 (11)	O11^x—I6—Ba5^viii	56.46 (8)
O9ⁱ—Ba2—O12	149.69 (6)	O11^vii—I6—O11^x	91.78 (16)
O9—Ba2—O12	149.69 (6)	O11^x—I6—O12	89.67 (11)
O10^ix—Ba2—Ba1	139.20 (6)	O11^vii—I6—O12	89.67 (12)
O10^viii—Ba2—Ba1	139.20 (6)	O11^x—I6—O14^xi	87.79 (11)
O10^viii—Ba2—Ba3	46.18 (6)	O11^vii—I6—O14^xi	87.79 (11)
O10^ix—Ba2—Ba3	46.18 (6)	O12—I6—Ba1^xvi	125.360 (9)
O10^ix—Ba2—Ba5^viii	110.48 (6)	O12—I6—Ba1^xix	128.98 (12)
O10^viii—Ba2—Ba5^vii	110.48 (6)	O12—I6—Ba1^xviii	125.360 (9)
O10^viii—Ba2—Ba5^viii	53.66 (6)	O12—I6—Ba3	48.21 (12)
O10^ix—Ba2—Ba5^vii	53.66 (6)	O12—I6—Ba5^viii	55.328 (10)
O10^ix—Ba2—I7	99.68 (6)	O12—I6—Ba5^vii	55.328 (10)
O10^viii—Ba2—I7	99.68 (6)	O12—I6—O14^xi	176.36 (16)
O10^viii—Ba2—O8ⁱ	99.15 (9)	O14^xi—I6—Ba1^xviii	54.500 (6)
O10^viii—Ba2—O8	155.67 (8)	O14^xi—I6—Ba1^xix	47.38 (11)
O10^ix—Ba2—O8	99.15 (9)	O14^xi—I6—Ba1^xvi	54.500 (6)
O10^ix—Ba2—O8ⁱ	155.67 (8)	O14^xi—I6—Ba3	128.15 (11)
O10^viii—Ba2—O9ⁱ	124.14 (9)	O14^xi—I6—Ba5^viii	124.845 (7)
O10^ix—Ba2—O9ⁱ	86.26 (9)	O14^xi—I6—Ba5^vii	124.845 (6)
O10^viii—Ba2—O9	86.26 (9)	Ba2—I7—Ba4^vi	93.922 (8)
O10^ix—Ba2—O9	124.14 (9)	Ba2—I7—Ba4ⁱⁱ	93.922 (8)
O10^ix—Ba2—O10^viii	77.40 (12)	Ba2—I7—Ba5	124.951 (11)
O10^ix—Ba2—O12	76.43 (9)	Ba3^vi—I7—Ba2	80.685 (8)
O10^viii—Ba2—O12	76.43 (9)	Ba3ⁱⁱ—I7—Ba2	80.685 (8)
O12—Ba2—Ba1	121.56 (8)	Ba3ⁱⁱ—I7—Ba3^vi	114.135 (12)
O12—Ba2—Ba3	45.03 (8)	Ba3^vi—I7—Ba4ⁱⁱ	173.593 (12)
O12—Ba2—Ba5^vii	49.017 (7)	Ba3ⁱⁱ—I7—Ba4^vi	173.593 (12)
O12—Ba2—Ba5^viii	49.017 (7)	Ba3ⁱⁱ—I7—Ba4ⁱⁱ	68.009 (6)
O12—Ba2—I7	174.95 (8)	Ba3^vi—I7—Ba4^vi	68.009 (6)
I7^viii—Ba3—I7^vii	114.134 (12)	Ba3^vi—I7—Ba5	70.569 (7)
O9^viii—Ba3—I7^viii	32.34 (5)	Ba3ⁱⁱ—I7—Ba5	70.569 (7)
O9^ix—Ba3—I7^viii	96.73 (6)	Ba4^vi—I7—Ba4ⁱⁱ	109.191 (11)
O9^viii—Ba3—I7^vii	96.73 (6)	Ba4ⁱⁱ—I7—Ba5	115.616 (7)
O9^ix—Ba3—I7^vii	32.34 (5)	Ba4^vi—I7—Ba5	115.616 (7)
O9^ix—Ba3—O9^viii	69.93 (11)	O9—I7—Ba2	47.41 (8)
O9^ix—Ba3—O10^ix	55.61 (8)	O9ⁱ—I7—Ba2	47.41 (8)
O9^viii—Ba3—O10^viii	55.61 (8)	O9—I7—Ba3ⁱⁱ	125.96 (8)
O9^ix—Ba3—O10^viii	94.55 (8)	O9ⁱ—I7—Ba3^vi	125.96 (8)
O9^viii—Ba3—O10^ix	94.55 (8)	O9—I7—Ba3^vi	52.78 (8)
O9^viii—Ba3—O11^x	119.17 (7)	O9ⁱ—I7—Ba3ⁱⁱ	52.78 (8)
O9^ix—Ba3—O11^x	170.03 (8)	O9—I7—Ba4ⁱⁱ	120.90 (8)
O9^ix—Ba3—O11^vii	119.17 (7)	O9—I7—Ba4^vi	49.90 (8)
O9^viii—Ba3—O11^vii	170.03 (8)	O9ⁱ—I7—Ba4ⁱⁱ	49.90 (8)
O9^ix—Ba3—O13^vii	55.53 (9)	O9ⁱ—I7—Ba4^vi	120.90 (9)
O9^viii—Ba3—O13^vii	125.44 (10)	O9ⁱ—I7—Ba5	123.14 (8)
O9^ix—Ba3—O13^viii	125.44 (10)	O9—I7—Ba5	123.14 (8)
O9^viii—Ba3—O13^viii	55.53 (9)	O9—I7—O9ⁱ	90.50 (16)
O10^viii—Ba3—I7^vii	95.62 (6)	O9—I7—O13	90.63 (12)
O10^ix—Ba3—I7^viii	95.62 (6)	O9ⁱ—I7—O13	90.63 (12)
O10^viii—Ba3—I7^viii	32.28 (5)	O10ⁱ—I7—Ba2	132.70 (8)
O10^ix—Ba3—I7^vii	32.28 (5)	O10—I7—Ba2	132.70 (8)
O10^viii—Ba3—O10^ix	68.38 (11)	O10ⁱ—I7—Ba3^vi	127.97 (9)
O10^ix—Ba3—O11^x	124.25 (7)	O10—I7—Ba3ⁱⁱ	127.97 (9)
O10^ix—Ba3—O11^vii	94.30 (7)	O10ⁱ—I7—Ba3ⁱⁱ	54.46 (8)
O10^viii—Ba3—O11^x	94.30 (7)	O10—I7—Ba3^vi	54.46 (8)
O10^viii—Ba3—O11^vii	124.25 (7)	O10ⁱ—I7—Ba4ⁱⁱ	58.37 (9)
O10^viii—Ba3—O13^vii	123.06 (9)	O10—I7—Ba4^vi	58.37 (9)
O10^ix—Ba3—O13^vii	54.68 (9)	O10—I7—Ba4ⁱⁱ	129.60 (8)
O10^viii—Ba3—O13^viii	54.68 (9)	O10ⁱ—I7—Ba4^vi	129.60 (8)
O10^ix—Ba3—O13^viii	123.06 (9)	O10—I7—Ba5	57.65 (9)
O11^vii—Ba3—I7^viii	141.69 (5)	O10ⁱ—I7—Ba5	57.65 (9)
O11^vii—Ba3—I7^vii	93.21 (5)	O10ⁱ—I7—O9ⁱ	89.28 (12)
O11^x—Ba3—I7^vii	141.69 (5)	O10—I7—O9ⁱ	179.11 (12)
O11^x—Ba3—I7^viii	93.21 (5)	O10—I7—O9	89.28 (12)
O11^x—Ba3—O11^vii	51.45 (10)	O10ⁱ—I7—O9	179.11 (12)
O12—Ba3—I7^vii	95.79 (4)	O10ⁱ—I7—O10	90.92 (17)
O12—Ba3—I7^viii	95.79 (4)	O10ⁱ—I7—O13	90.23 (12)
O12—Ba3—O9^ix	126.07 (7)	O10—I7—O13	90.23 (12)
O12—Ba3—O9^viii	126.07 (7)	O13—I7—Ba2	74.90 (12)
O12—Ba3—O10^ix	71.08 (8)	O13—I7—Ba3ⁱⁱ	57.095 (7)
O12—Ba3—O10^viii	71.08 (8)	O13—I7—Ba3^vi	57.095 (7)
O12—Ba3—O11^vii	53.28 (8)	O13—I7—Ba4ⁱⁱ	124.977 (14)
O12—Ba3—O11^x	53.28 (8)	O13—I7—Ba4^vi	124.977 (14)
O12—Ba3—O13^viii	88.68 (8)	O13—I7—Ba5	50.05 (12)
O12—Ba3—O13^vii	88.68 (8)	O15^iv—I7—Ba2	102.70 (12)
O13^vii—Ba3—I7^viii	146.63 (7)	O15^iv—I7—Ba3^vi	122.812 (9)
O13^vii—Ba3—I7^vii	32.55 (7)	O15^iv—I7—Ba3ⁱⁱ	122.812 (9)
O13^viii—Ba3—I7^viii	32.55 (7)	O15^iv—I7—Ba4ⁱⁱ	54.813 (10)
O13^viii—Ba3—I7^vii	146.63 (7)	O15^iv—I7—Ba4^vi	54.813 (10)
O13^viii—Ba3—O11^x	63.90 (9)	O15^iv—I7—Ba5	132.35 (12)
O13^vii—Ba3—O11^x	115.34 (9)	O15^iv—I7—O9ⁱ	87.68 (12)
O13^vii—Ba3—O11^vii	63.90 (9)	O15^iv—I7—O9	87.68 (12)
O13^viii—Ba3—O11^vii	115.34 (9)	O15^iv—I7—O10	91.45 (12)
O13^viii—Ba3—O13^vii	177.04 (16)	O15^iv—I7—O10ⁱ	91.45 (12)
O15^xi—Ba3—I7^vii	118.80 (3)	O15^iv—I7—O13	177.60 (17)
O15^xi—Ba3—I7^viii	118.80 (3)	Ba1—O8—Ba5^vii	161.98 (9)
O15^xi—Ba3—O9^viii	111.96 (9)	Ba2—O8—Ba1	78.37 (7)
O15^xi—Ba3—O9^ix	111.96 (9)	Ba2—O8—Ba5^iv	101.23 (8)
O15^xi—Ba3—O10^ix	145.32 (6)	Ba2—O8—Ba5^vii	84.85 (7)
O15^xi—Ba3—O10^viii	145.32 (6)	Ba5^iv—O8—Ba1	90.26 (7)
O15^xi—Ba3—O11^x	61.92 (9)	Ba5^iv—O8—Ba5^vii	99.50 (8)
O15^xi—Ba3—O11^vii	61.92 (9)	I6^xvi—O8—Ba1	91.31 (9)
O15^xi—Ba3—O12	106.92 (11)	I6^xvi—O8—Ba2	158.48 (13)
O15^xi—Ba3—O13^viii	91.02 (7)	I6^xvi—O8—Ba5^iv	97.62 (10)
O15^xi—Ba3—O13^vii	91.02 (7)	I6^xvi—O8—Ba5^vii	102.26 (10)
I7^viii—Ba4—I7^vii	109.190 (11)	Ba2—O9—Ba1	74.77 (7)
O9^viii—Ba4—I7^viii	30.98 (5)	Ba2—O9—Ba3^vi	113.32 (9)
O9^ix—Ba4—I7^vii	30.98 (5)	Ba2—O9—Ba4^vi	146.73 (11)
O9^ix—Ba4—I7^viii	94.51 (6)	Ba3^vi—O9—Ba1	168.67 (10)
O9^viii—Ba4—I7^vii	94.51 (6)	Ba4^vi—O9—Ba1	78.89 (7)
O9^ix—Ba4—O9^viii	70.09 (11)	Ba4^vi—O9—Ba3^vi	90.63 (8)
O9^viii—Ba4—O10^viii	53.21 (7)	I7—O9—Ba1	91.06 (10)
O9^ix—Ba4—O10^viii	90.05 (8)	I7—O9—Ba2	101.31 (11)
O9^ix—Ba4—O10^ix	53.21 (7)	I7—O9—Ba3^vi	94.88 (10)
O9^viii—Ba4—O10^ix	90.05 (8)	I7—O9—Ba4^vi	99.12 (10)
O9^viii—Ba4—O11ⁱ	104.40 (8)	Ba2^vi—O10—Ba3^vi	93.39 (8)
O9^ix—Ba4—O11ⁱ	151.76 (8)	Ba2^vi—O10—Ba4^vi	92.96 (8)
O9^viii—Ba4—O11	151.76 (8)	Ba2^vi—O10—Ba5	85.38 (7)
O9^ix—Ba4—O11	104.40 (8)	Ba3^vi—O10—Ba4^vi	84.23 (7)
O9^ix—Ba4—O15^xiii	123.27 (9)	Ba3^vi—O10—Ba5	88.08 (7)
O9^viii—Ba4—O15^xii	123.27 (9)	Ba4^vi—O10—Ba5	172.02 (10)
O9^viii—Ba4—O15^xiii	53.58 (9)	I7—O10—Ba2^vi	172.85 (15)
O9^ix—Ba4—O15^xii	53.58 (9)	I7—O10—Ba3^vi	93.26 (10)
O10^ix—Ba4—I7^viii	89.83 (5)	I7—O10—Ba4^vi	90.33 (10)
O10^ix—Ba4—I7^vii	31.30 (5)	I7—O10—Ba5	92.21 (10)
O10^viii—Ba4—I7^vii	89.83 (5)	Ba1^xiv—O11—Ba1^vii	83.68 (7)
O10^viii—Ba4—I7^viii	31.30 (5)	Ba1^vii—O11—Ba3ⁱⁱ	99.63 (8)
O10^viii—Ba4—O10^ix	62.98 (10)	Ba1^xiv—O11—Ba3ⁱⁱ	172.10 (10)
O11ⁱ—Ba4—I7^vii	158.81 (5)	Ba1^xiv—O11—Ba4	91.61 (8)
O11ⁱ—Ba4—I7^viii	92.00 (5)	Ba1^xiv—O11—Ba5	90.20 (7)
O11—Ba4—I7^vii	92.00 (5)	Ba4—O11—Ba1^vii	80.14 (7)
O11—Ba4—I7^viii	158.81 (5)	Ba4—O11—Ba3ⁱⁱ	81.95 (6)
O11ⁱ—Ba4—O10^ix	154.38 (7)	Ba4—O11—Ba5	97.72 (8)
O11—Ba4—O10^viii	154.38 (7)	Ba5—O11—Ba1^vii	173.43 (10)
O11ⁱ—Ba4—O10^viii	109.05 (7)	Ba5—O11—Ba3ⁱⁱ	86.15 (7)
O11—Ba4—O10^ix	109.05 (7)	I6ⁱⁱ—O11—Ba1^xiv	96.62 (10)
O11—Ba4—O11ⁱ	66.81 (11)	I6ⁱⁱ—O11—Ba1^vii	91.42 (10)
O11—Ba4—O15^xiii	127.81 (9)	I6ⁱⁱ—O11—Ba3ⁱⁱ	90.50 (9)
O11ⁱ—Ba4—O15^xiii	61.16 (9)	I6ⁱⁱ—O11—Ba4	167.51 (13)
O11ⁱ—Ba4—O15^xii	127.81 (9)	I6ⁱⁱ—O11—Ba5	91.65 (10)
O11—Ba4—O15^xii	61.16 (9)	Ba2—O12—Ba3	91.09 (11)
O13—Ba4—I7^vii	102.80 (5)	Ba2—O12—Ba5^viii	86.51 (7)
O13—Ba4—I7^viii	102.80 (5)	Ba2—O12—Ba5^vii	86.51 (7)
O13—Ba4—O9^ix	133.56 (8)	Ba3—O12—Ba5^viii	93.38 (7)
O13—Ba4—O9^viii	133.56 (8)	Ba3—O12—Ba5^vii	93.38 (7)
O13—Ba4—O10^ix	83.76 (9)	Ba5^viii—O12—Ba5^vii	170.37 (15)
O13—Ba4—O10^viii	83.76 (9)	I6—O12—Ba2	167.6 (2)
O13—Ba4—O11ⁱ	70.92 (9)	I6—O12—Ba3	101.33 (15)
O13—Ba4—O11	70.91 (9)	I6—O12—Ba5^viii	92.70 (7)
O13—Ba4—O15^xii	88.28 (8)	I6—O12—Ba5^vii	92.70 (7)
O13—Ba4—O15^xiii	88.28 (8)	Ba3^vi—O13—Ba3ⁱⁱ	177.04 (16)
O14—Ba4—I7^viii	100.51 (4)	Ba4—O13—Ba3ⁱⁱ	89.08 (7)
O14—Ba4—I7^vii	100.51 (4)	Ba4—O13—Ba3^vi	89.08 (7)
O14—Ba4—O9^viii	76.57 (8)	Ba4—O13—Ba5	104.55 (13)
O14—Ba4—O9^ix	76.57 (8)	Ba5—O13—Ba3ⁱⁱ	91.35 (8)
O14—Ba4—O10^ix	129.44 (8)	Ba5—O13—Ba3^vi	91.35 (8)
O14—Ba4—O10^viii	129.44 (8)	I7—O13—Ba3ⁱⁱ	90.35 (7)
O14—Ba4—O11	75.24 (8)	I7—O13—Ba3^vi	90.35 (7)
O14—Ba4—O11ⁱ	75.24 (8)	I7—O13—Ba4	155.3 (2)
O14—Ba4—O13	139.17 (12)	I7—O13—Ba5	100.11 (15)
O14—Ba4—O15^xii	94.97 (8)	Ba1^xiv—O14—Ba1^vii	88.31 (7)
O14—Ba4—O15^xiii	94.97 (8)	Ba1^xiv—O14—Ba1^viii	88.31 (7)
O15^xiii—Ba4—I7^viii	31.07 (7)	Ba1^viii—O14—Ba1^vii	172.17 (14)
O15^xii—Ba4—I7^vii	31.07 (7)	Ba4—O14—Ba1^vii	86.79 (7)
O15^xii—Ba4—I7^viii	139.91 (7)	Ba4—O14—Ba1^xiv	99.25 (12)
O15^xiii—Ba4—I7^vii	139.91 (7)	Ba4—O14—Ba1^viii	86.79 (7)
O15^xiii—Ba4—O10^viii	52.72 (9)	I6^xx—O14—Ba1^viii	93.81 (7)
O15^xii—Ba4—O10^viii	115.70 (9)	I6^xx—O14—Ba1^vii	93.81 (7)
O15^xiii—Ba4—O10^ix	115.70 (9)	I6^xx—O14—Ba1^xiv	102.16 (15)
O15^xii—Ba4—O10^ix	52.72 (9)	I6^xx—O14—Ba4	158.60 (19)
O15^xiii—Ba4—O15^xii	168.25 (15)	Ba1^xiv—O15—Ba4^xiii	84.74 (7)
O8ⁱⁱ—Ba5—I6ⁱⁱ	88.99 (5)	Ba1^xiv—O15—Ba4^xii	84.74 (7)
O8^xiv—Ba5—I6ⁱⁱ	31.42 (5)	Ba3^xx—O15—Ba1^xiv	128.21 (15)
O8^xv—Ba5—I6ⁱⁱ	94.53 (5)	Ba3^xx—O15—Ba4^xii	91.21 (8)
O8ⁱⁱⁱ—Ba5—I6ⁱⁱ	133.80 (5)	Ba3^xx—O15—Ba4^xiii	91.21 (8)
O8^xiv—Ba5—O8ⁱⁱ	80.50 (8)	Ba4^xiii—O15—Ba4^xii	168.26 (15)
O8^xiv—Ba5—O8ⁱⁱⁱ	109.06 (5)	I7^xiv—O15—Ba1^xiv	108.21 (17)
O8^xv—Ba5—O8ⁱⁱⁱ	80.50 (8)	I7^xiv—O15—Ba3^xx	123.57 (18)
O8^xv—Ba5—O8ⁱⁱ	109.06 (5)	I7^xiv—O15—Ba4^xii	94.12 (7)
O8ⁱⁱⁱ—Ba5—O8ⁱⁱ	51.26 (10)	I7^xiv—O15—Ba4^xiii	94.12 (7)
O8^xiv—Ba5—O8^xv	69.24 (11)

Ba1^xviii—I6—O12—Ba2	93.51 (9)	Ba5—I7—O9—Ba1	−176.105 (13)
Ba1^xix—I6—O12—Ba2	180.000 (1)	Ba5—I7—O9—Ba2	109.21 (8)
Ba1^xvi—I6—O12—Ba2	−93.51 (9)	Ba5—I7—O9—Ba3^vi	−5.76 (12)
Ba1^xvi—I6—O12—Ba3	86.49 (8)	Ba5—I7—O9—Ba4^vi	−97.19 (8)
Ba1^xviii—I6—O12—Ba3	−86.49 (8)	Ba5—I7—O10—Ba3^vi	88.20 (8)
Ba1^xix—I6—O12—Ba3	0.000 (1)	Ba5—I7—O10—Ba4^vi	172.43 (10)
Ba1^xix—I6—O12—Ba5^vii	−93.99 (8)	Ba5—I7—O13—Ba3ⁱⁱ	91.44 (8)
Ba1^xviii—I6—O12—Ba5^vii	179.517 (15)	Ba5—I7—O13—Ba3^vi	−91.44 (8)
Ba1^xvi—I6—O12—Ba5^vii	−7.49 (16)	Ba5—I7—O13—Ba4	180.000 (1)
Ba1^xvi—I6—O12—Ba5^viii	−179.517 (15)	O8^xvi—I6—O12—Ba2	−45.51 (8)
Ba1^xix—I6—O12—Ba5^viii	93.99 (8)	O8^xvii—I6—O12—Ba2	45.51 (8)
Ba1^xviii—I6—O12—Ba5^viii	7.49 (16)	O8^xvi—I6—O12—Ba3	134.49 (8)
Ba2—I7—O9—Ba1	74.68 (8)	O8^xvii—I6—O12—Ba3	−134.49 (8)
Ba2—I7—O9—Ba3^vi	−114.97 (12)	O8^xvi—I6—O12—Ba5^viii	−131.52 (11)
Ba2—I7—O9—Ba4^vi	153.60 (14)	O8^xvii—I6—O12—Ba5^viii	−40.50 (11)
Ba2—I7—O10—Ba3^vi	−21.57 (14)	O8^xvi—I6—O12—Ba5^vii	40.50 (11)
Ba2—I7—O10—Ba4^vi	62.67 (11)	O8^xvii—I6—O12—Ba5^vii	131.52 (11)
Ba2—I7—O10—Ba5	−109.77 (8)	O9ⁱ—I7—O9—Ba1	52.70 (12)
Ba2—I7—O13—Ba3ⁱⁱ	−88.56 (8)	O9ⁱ—I7—O9—Ba2	−21.98 (16)
Ba2—I7—O13—Ba3^vi	88.56 (8)	O9ⁱ—I7—O9—Ba3^vi	−136.96 (6)
Ba2—I7—O13—Ba4	0.0	O9ⁱ—I7—O9—Ba4^vi	131.61 (6)
Ba2—I7—O13—Ba5	180.0	O9—I7—O10—Ba3^vi	−42.73 (10)
Ba3—I6—O12—Ba2	180.000 (2)	O9—I7—O10—Ba4^vi	41.50 (10)
Ba3—I6—O12—Ba5^vii	−93.99 (8)	O9—I7—O10—Ba5	−130.93 (10)
Ba3—I6—O12—Ba5^viii	93.99 (8)	O9—I7—O13—Ba3^vi	43.31 (12)
Ba3^vi—I7—O9—Ba1	−170.35 (11)	O9ⁱ—I7—O13—Ba3ⁱⁱ	−43.31 (12)
Ba3ⁱⁱ—I7—O9—Ba1	94.88 (8)	O9ⁱ—I7—O13—Ba3^vi	133.82 (11)
Ba3ⁱⁱ—I7—O9—Ba2	20.20 (14)	O9—I7—O13—Ba3ⁱⁱ	−133.82 (11)
Ba3^vi—I7—O9—Ba2	114.97 (12)	O9ⁱ—I7—O13—Ba4	45.25 (8)
Ba3ⁱⁱ—I7—O9—Ba3^vi	−94.78 (8)	O9—I7—O13—Ba4	−45.25 (8)
Ba3ⁱⁱ—I7—O9—Ba4^vi	173.793 (17)	O9—I7—O13—Ba5	134.75 (8)
Ba3^vi—I7—O9—Ba4^vi	−91.43 (9)	O9ⁱ—I7—O13—Ba5	−134.75 (8)
Ba3ⁱⁱ—I7—O10—Ba3^vi	94.58 (9)	O10—I7—O9—Ba1	−126.44 (10)
Ba3ⁱⁱ—I7—O10—Ba4^vi	178.820 (19)	O10—I7—O9—Ba2	158.88 (12)
Ba3^vi—I7—O10—Ba4^vi	84.24 (8)	O10—I7—O9—Ba3^vi	43.90 (11)
Ba3ⁱⁱ—I7—O10—Ba5	6.39 (12)	O10—I7—O9—Ba4^vi	−47.53 (11)
Ba3^vi—I7—O10—Ba5	−88.20 (8)	O10ⁱ—I7—O10—Ba3^vi	138.13 (6)
Ba3^vi—I7—O13—Ba3ⁱⁱ	−177.13 (16)	O10ⁱ—I7—O10—Ba4^vi	−137.64 (6)
Ba3ⁱⁱ—I7—O13—Ba3^vi	177.13 (16)	O10ⁱ—I7—O10—Ba5	49.93 (13)
Ba3ⁱⁱ—I7—O13—Ba4	88.56 (8)	O10ⁱ—I7—O13—Ba3^vi	−136.90 (12)
Ba3^vi—I7—O13—Ba4	−88.56 (8)	O10ⁱ—I7—O13—Ba3ⁱⁱ	45.97 (12)
Ba3^vi—I7—O13—Ba5	91.44 (8)	O10—I7—O13—Ba3ⁱⁱ	136.90 (12)
Ba3ⁱⁱ—I7—O13—Ba5	−91.44 (8)	O10—I7—O13—Ba3^vi	−45.97 (12)
Ba4ⁱⁱ—I7—O9—Ba1	10.90 (10)	O10—I7—O13—Ba4	−134.54 (8)
Ba4^vi—I7—O9—Ba1	−78.92 (8)	O10ⁱ—I7—O13—Ba4	134.54 (8)
Ba4^vi—I7—O9—Ba2	−153.60 (14)	O10ⁱ—I7—O13—Ba5	−45.46 (8)
Ba4ⁱⁱ—I7—O9—Ba2	−63.78 (11)	O10—I7—O13—Ba5	45.46 (8)
Ba4ⁱⁱ—I7—O9—Ba3^vi	−178.751 (17)	O11^vii—I6—O12—Ba2	−134.11 (8)
Ba4^vi—I7—O9—Ba3^vi	91.43 (9)	O11^x—I6—O12—Ba2	134.11 (8)
Ba4ⁱⁱ—I7—O9—Ba4^vi	89.82 (9)	O11^vii—I6—O12—Ba3	45.89 (8)
Ba4ⁱⁱ—I7—O10—Ba3^vi	−173.745 (18)	O11^x—I6—O12—Ba3	−45.89 (8)
Ba4^vi—I7—O10—Ba3^vi	−84.24 (8)	O11^vii—I6—O12—Ba5^viii	139.88 (12)
Ba4ⁱⁱ—I7—O10—Ba4^vi	−89.51 (9)	O11^vii—I6—O12—Ba5^vii	−48.10 (11)
Ba4^vi—I7—O10—Ba5	−172.43 (10)	O11^x—I6—O12—Ba5^viii	48.10 (11)
Ba4ⁱⁱ—I7—O10—Ba5	98.06 (8)	O11^x—I6—O12—Ba5^vii	−139.88 (12)
Ba4^vi—I7—O13—Ba3^vi	4.44 (17)	O13—I7—O9—Ba1	143.33 (10)
Ba4^vi—I7—O13—Ba3ⁱⁱ	−172.690 (16)	O13—I7—O9—Ba2	68.65 (12)
Ba4ⁱⁱ—I7—O13—Ba3ⁱⁱ	−4.44 (17)	O13—I7—O9—Ba3^vi	−46.32 (11)
Ba4ⁱⁱ—I7—O13—Ba3^vi	172.690 (16)	O13—I7—O9—Ba4^vi	−137.75 (11)
Ba4^vi—I7—O13—Ba4	−84.13 (9)	O13—I7—O10—Ba3^vi	47.89 (11)
Ba4ⁱⁱ—I7—O13—Ba4	84.13 (9)	O13—I7—O10—Ba4^vi	132.13 (10)
Ba4ⁱⁱ—I7—O13—Ba5	−95.87 (9)	O13—I7—O10—Ba5	−40.31 (10)
Ba4^vi—I7—O13—Ba5	95.87 (9)	O15^iv—I7—O9—Ba1	−34.96 (10)
Ba5^vii—I6—O12—Ba2	−86.01 (8)	O15^iv—I7—O9—Ba2	−109.64 (12)
Ba5^viii—I6—O12—Ba2	86.01 (8)	O15^iv—I7—O9—Ba3^vi	135.39 (11)
Ba5^viii—I6—O12—Ba3	−93.99 (8)	O15^iv—I7—O9—Ba4^vi	43.96 (11)
Ba5^vii—I6—O12—Ba3	93.99 (8)	O15^iv—I7—O10—Ba3^vi	−130.39 (10)
Ba5^viii—I6—O12—Ba5^vii	172.02 (16)	O15^iv—I7—O10—Ba4^vi	−46.16 (10)
Ba5^vii—I6—O12—Ba5^viii	−172.02 (16)	O15^iv—I7—O10—Ba5	141.41 (10)

Acknowledgements

DWB is grateful for the help of Dr Rosario Scopelliti in ISIC of EPFL.

Funding information

Funding for this research was provided by: Swiss National Science Foundation (SNSF) Sinergia network `NanoSkyrmionics' (grant No. CRSII5-171003).

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