Redetermination of the crystal structures of the `Arppe compound' Bi24O31Cl10 and the isomorphous Bi24O31Br10

Eggenweiler, U.; Keller, E.; Krämer, V.

doi:10.1107/S0108768100000550

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Redetermination of the crystal structures of the `Arppe compound' Bi₂₄O₃₁Cl₁₀ and the isomorphous Bi₂₄O₃₁Br₁₀

U. Eggenweiler, E. Keller and V. Krämer

The crystal structures of Bi₂₄O₃₁X₁₀ (X = Cl, Br; 24-bismuth 31-oxide decachloride/-bromide) have been redetermined. The structure models obtained resemble the model described in the literature about 60 years ago, but differ from it in some details of the O substructure and in the fact that the structure for X = Cl is a twofold superstructure of the literature model. A fictional mechanism is given by which the formerly described incorrect O substructure is transferred into the correct one.

Keywords: Arppe compound; Isomorphous; Superstructures.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100000550/jz0008sup1.cif Contains datablocks bi24ocl, bi24obr, global
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100000550/jz0008bi24oclsup2.hkl Contains datablock bi24ocl
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100000550/jz0008bi24obrsup3.hkl Contains datablock bi24obr

Computing details top

For both compounds, data collection: Bruker SMART; cell refinement: Bruker SMART; data reduction: Bruker SHELXTL; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: SCHAKAL 97 (Keller 1997) for bi24ocl; SCHAKAL 97 (Keller, 1997) for bi24obr. For both compounds, software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top

(bi24ocl) top

Crystal data top

Bi₂₄Cl₁₀O₃₁	F(000) = 4820
M_r = 5866.02	D_x = 8.242 Mg m⁻³
Monoclinic, P2/c	Mo Kα radiation, λ = 0.71073 Å
a = 10.033 (2) Å	Cell parameters from 15924 reflections
b = 7.9745 (16) Å	θ = 1.4–28.3°
c = 29.552 (6) Å	µ = 89.60 mm⁻¹
β = 88.742 (4)°	T = 293 K
V = 2363.8 (8) Å³	Needle, pale green
Z = 2	0.22 × 0.02 × 0.01 mm

Data collection top

CCD area detector diffractometer	5546 independent reflections
Radiation source: fine-focus sealed tube	3184 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.130
phi and ω scans	θ_max = 28.3°, θ_min = 1.4°
Absorption correction: integration XPREP / Bruker SHELXTL	h = −13→13
T_min = 0.029, T_max = 0.404	k = −10→0
15924 measured reflections	l = 0→39

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.063	w = 1/[σ²(F_o²) + (0.0599P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.146	(Δ/σ)_max = 0.001
S = 0.90	Δρ_max = 5.98 e Å⁻³
5546 reflections	Δρ_min = −6.16 e Å⁻³
218 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.000152 (8)

Crystal data top

Bi₂₄Cl₁₀O₃₁	V = 2363.8 (8) Å³
M_r = 5866.02	Z = 2
Monoclinic, P2/c	Mo Kα radiation
a = 10.033 (2) Å	µ = 89.60 mm⁻¹
b = 7.9745 (16) Å	T = 293 K
c = 29.552 (6) Å	0.22 × 0.02 × 0.01 mm
β = 88.742 (4)°

Data collection top

CCD area detector diffractometer	5546 independent reflections
Absorption correction: integration XPREP / Bruker SHELXTL	3184 reflections with I > 2σ(I)
T_min = 0.029, T_max = 0.404	R_int = 0.130
15924 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.063	218 parameters
wR(F²) = 0.146	0 restraints
S = 0.90	Δρ_max = 5.98 e Å⁻³
5546 reflections	Δρ_min = −6.16 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. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
Bi1	0.08954 (12)	0.15098 (13)	0.31393 (4)	0.0160 (3)
Bi1A	0.07898 (12)	0.65569 (13)	0.30449 (3)	0.0142 (3)
Bi2	0.24586 (11)	0.11927 (12)	0.42714 (3)	0.0108 (2)
Bi2A	0.25409 (11)	0.65391 (13)	0.42667 (3)	0.0119 (3)
Bi3	0.42866 (11)	0.12419 (11)	0.54524 (3)	0.0091 (2)
Bi3A	0.43899 (11)	0.62388 (11)	0.54670 (3)	0.0092 (2)
Bi4	0.59455 (11)	0.12297 (12)	0.66644 (3)	0.0094 (2)
Bi4A	0.60071 (11)	0.61913 (12)	0.66265 (3)	0.0089 (2)
Bi5	0.79200 (12)	0.10376 (13)	0.78250 (3)	0.0129 (2)
Bi5A	0.75409 (11)	0.62361 (11)	0.78521 (3)	0.0105 (2)
Bi6	0.93266 (12)	0.15522 (12)	0.90838 (3)	0.0132 (3)
Bi6A	0.90338 (12)	0.62165 (11)	0.90284 (3)	0.0114 (2)
Cl1	0.5000	0.1151 (13)	0.2500	0.024 (2)
Cl1A	0.5000	0.6313 (11)	0.2500	0.017 (2)
Cl2	0.6551 (8)	0.1233 (8)	0.3684 (2)	0.0234 (18)
Cl2A	0.6619 (8)	0.6269 (8)	0.3700 (2)	0.0213 (18)
Cl3	0.8110 (9)	0.1264 (9)	0.4870 (2)	0.027 (2)
Cl3A	0.8037 (9)	0.6202 (8)	0.4909 (2)	0.0229 (18)
O1	0.1392 (19)	0.153 (2)	0.2342 (6)	0.011 (4)*
O1A	0.140 (2)	0.602 (2)	0.2317 (6)	0.016 (4)*
O2	0.3093 (19)	0.1240 (19)	0.3542 (5)	0.008 (4)*
O2A	0.3074 (18)	0.6324 (18)	0.3546 (5)	0.007 (4)*
O3	0.4777 (19)	0.124 (2)	0.4723 (6)	0.013 (4)*
O3A	0.4688 (19)	0.6244 (19)	0.4718 (6)	0.010 (4)*
O4	0.6054 (19)	0.130 (2)	0.5863 (6)	0.013 (4)*
O4A	0.620 (2)	0.624 (2)	0.5881 (6)	0.014 (4)*
O5	0.773 (2)	0.126 (2)	0.7046 (6)	0.016 (4)*
O5A	0.7797 (19)	0.628 (2)	0.7017 (6)	0.013 (4)*
O6	0.939 (2)	0.122 (2)	0.8389 (6)	0.015 (4)*
O6A	0.918 (2)	0.631 (2)	0.8317 (6)	0.018 (4)*
O7	1.138 (2)	0.116 (2)	0.9048 (6)	0.019 (4)*
O8	1.071 (3)	0.769 (3)	0.8941 (7)	0.038 (6)*
O8A	1.0152 (18)	0.3990 (19)	0.8992 (5)	0.009 (4)*
O9	1.0000	0.143 (3)	0.7500	0.019 (6)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Bi1	0.0195 (7)	0.0129 (5)	0.0156 (6)	−0.0032 (5)	0.0011 (5)	0.0030 (4)
Bi1A	0.0183 (6)	0.0138 (5)	0.0104 (5)	−0.0020 (5)	0.0011 (5)	−0.0003 (4)
Bi2	0.0115 (6)	0.0108 (5)	0.0100 (5)	0.0009 (4)	0.0003 (5)	−0.0002 (4)
Bi2A	0.0150 (6)	0.0105 (5)	0.0103 (5)	−0.0019 (4)	0.0008 (5)	0.0010 (4)
Bi3	0.0083 (6)	0.0097 (5)	0.0093 (5)	−0.0005 (4)	−0.0005 (4)	0.0001 (4)
Bi3A	0.0096 (6)	0.0091 (5)	0.0089 (5)	−0.0003 (4)	0.0001 (4)	0.0004 (3)
Bi4	0.0092 (6)	0.0090 (5)	0.0101 (5)	0.0004 (4)	−0.0005 (4)	−0.0002 (3)
Bi4A	0.0081 (5)	0.0103 (5)	0.0082 (5)	0.0004 (4)	0.0001 (4)	−0.0005 (4)
Bi5	0.0128 (6)	0.0142 (5)	0.0118 (5)	−0.0008 (5)	−0.0004 (4)	0.0006 (4)
Bi5A	0.0079 (5)	0.0083 (5)	0.0153 (5)	0.0007 (4)	0.0014 (4)	−0.0006 (4)
Bi6	0.0133 (6)	0.0154 (5)	0.0109 (5)	−0.0022 (4)	0.0016 (4)	0.0012 (4)
Bi6A	0.0105 (6)	0.0095 (5)	0.0140 (5)	−0.0004 (4)	0.0034 (4)	−0.0008 (4)
Cl1	0.026 (7)	0.026 (5)	0.021 (6)	0.000	−0.001 (5)	0.000
Cl1A	0.017 (6)	0.013 (5)	0.021 (5)	0.000	0.007 (4)	0.000
Cl2	0.024 (5)	0.019 (4)	0.027 (4)	0.001 (3)	0.002 (4)	−0.001 (3)
Cl2A	0.034 (5)	0.013 (3)	0.017 (4)	0.010 (3)	0.003 (4)	−0.002 (3)
Cl3	0.040 (6)	0.023 (4)	0.017 (4)	−0.001 (4)	0.006 (4)	−0.002 (3)
Cl3A	0.033 (5)	0.016 (3)	0.019 (4)	0.000 (3)	0.014 (4)	−0.001 (3)

Geometric parameters (Å, º) top

Bi1—O1	2.398 (17)	Bi4—O2ⁱⁱ	2.270 (16)
Bi1—O1ⁱ	2.726 (19)	Bi4—O2Aⁱⁱⁱ	2.266 (16)
Bi1—O2	2.538 (19)	Bi4—O4	2.368 (17)
Bi1—O5ⁱⁱ	2.656 (17)	Bi4—O5	2.13 (2)
Bi1—O5Aⁱⁱⁱ	2.240 (17)	Bi4A—Cl1ⁱⁱⁱ	3.473 (6)
Bi1—O6^iv	2.741 (17)	Bi4A—Cl1Aⁱⁱⁱ	3.400 (5)
Bi1—O6A^v	2.492 (19)	Bi4A—Cl2ⁱⁱⁱ	3.427 (8)
Bi1—O8^v	2.46 (2)	Bi4A—Cl2Aⁱⁱⁱ	3.440 (8)
Bi1A—O1A	2.264 (17)	Bi4A—O2ⁱⁱⁱ	2.289 (16)
Bi1A—O1Aⁱ	2.50 (2)	Bi4A—O2Aⁱⁱⁱ	2.261 (15)
Bi1A—O2A	2.763 (18)	Bi4A—O4A	2.207 (17)
Bi1A—O5ⁱⁱⁱ	2.303 (18)	Bi4A—O5A	2.16 (2)
Bi1A—O5Aⁱⁱⁱ	2.673 (17)	Bi5—Cl1ⁱⁱ	3.560 (5)
Bi1A—O6^v	2.469 (17)	Bi5—Cl1Aⁱⁱⁱ	3.754 (5)
Bi1A—O6A^v	2.898 (18)	Bi5—Cl2^vi	3.385 (7)
Bi1A—O8A^v	2.891 (16)	Bi5—Cl2A^vii	3.586 (7)
Bi1A—O9ⁱⁱⁱ	2.419 (16)	Bi5—O1ⁱⁱ	2.214 (16)
Bi2—Cl3ⁱⁱ	3.247 (7)	Bi5—O1Aⁱⁱⁱ	2.479 (18)
Bi2—Cl3Aⁱⁱⁱ	3.222 (7)	Bi5—O5	2.322 (18)
Bi2—O2	2.235 (16)	Bi5—O6	2.254 (19)
Bi2—O3	2.707 (19)	Bi5—O9	2.300 (4)
Bi2—O4ⁱⁱ	2.511 (17)	Bi5A—Cl1ⁱⁱⁱ	3.470 (6)
Bi2—O4Aⁱⁱⁱ	2.488 (17)	Bi5A—Cl1Aⁱⁱⁱ	3.439 (5)
Bi2—O7^iv	2.267 (18)	Bi5A—Cl2^vii	3.316 (7)
Bi2—O8^v	2.21 (2)	Bi5A—Cl2A^vii	3.320 (6)
Bi2A—Cl3ⁱⁱⁱ	3.152 (7)	Bi5A—O1ⁱⁱⁱ	2.149 (17)
Bi2A—Cl3Aⁱⁱⁱ	3.315 (7)	Bi5A—O1Aⁱⁱⁱ	2.142 (18)
Bi2A—O2A	2.190 (16)	Bi5A—O6A	2.17 (2)
Bi2A—O3A	2.569 (19)	Bi5A—O5A	2.476 (17)
Bi2A—O4ⁱⁱⁱ	2.256 (17)	Bi6—O6	2.070 (17)
Bi2A—O4Aⁱⁱⁱ	2.583 (17)	Bi6—O7	2.09 (2)
Bi2A—O7^v	2.275 (18)	Bi6—O8A	2.128 (16)
Bi2A—O8A^v	2.581 (18)	Bi6—Cl3A^vii	3.269 (7)
Bi3—Cl2ⁱⁱ	3.320 (7)	Bi6—Cl3^vi	3.436 (7)
Bi3—Cl2Aⁱⁱⁱ	3.307 (6)	Bi6—Cl2A^vii	3.438 (8)
Bi3—Cl3ⁱⁱ	3.284 (9)	Bi6—Cl2^vi	3.773 (8)
Bi3—Cl3Aⁱⁱⁱ	3.292 (8)	Bi6A—Cl2^vii	3.390 (8)
Bi3—O3	2.201 (17)	Bi6A—Cl2A^vii	3.292 (8)
Bi3—O3ⁱⁱ	2.244 (17)	Bi6A—Cl3^vii	3.313 (7)
Bi3—O3Aⁱⁱⁱ	2.304 (16)	Bi6A—Cl3A^vii	3.373 (7)
Bi3—O4	2.171 (19)	Bi6A—O8	2.07 (2)
Bi3A—Cl2ⁱⁱⁱ	3.339 (7)	Bi6A—O8A	2.102 (16)
Bi3A—Cl2Aⁱⁱⁱ	3.312 (7)	Bi6A—O6A	2.107 (18)
Bi3A—Cl3ⁱⁱⁱ	3.370 (9)	O1—O6Aⁱⁱⁱ	2.67 (2)
Bi3A—Cl3Aⁱⁱⁱ	3.327 (8)	O1A—O9ⁱⁱⁱ	2.52 (3)
Bi3A—O3ⁱⁱⁱ	2.247 (17)	O3—O3ⁱⁱ	2.61 (3)
Bi3A—O3A	2.227 (16)	O3—O3Aⁱⁱⁱ	2.66 (2)
Bi3A—O3Aⁱⁱⁱ	2.248 (16)	O4—O7^viii	2.59 (3)
Bi3A—O4A	2.21 (2)	O5—O9	2.68 (2)
Bi4—Cl1ⁱⁱ	3.240 (6)	O6—O9	2.690 (17)
Bi4—Cl1Aⁱⁱⁱ	3.276 (5)	O6A—O8	2.66 (3)
Bi4—Cl2ⁱⁱ	3.362 (8)	O7—O8A	2.58 (2)
Bi4—Cl2Aⁱⁱⁱ	3.447 (8)

O5Aⁱⁱⁱ—Bi1—O1	71.6 (6)	O5A—Bi5A—Cl2A^vii	141.4 (4)
O5Aⁱⁱⁱ—Bi1—O8^v	91.4 (7)	Cl2^vii—Bi5A—Cl2A^vii	74.49 (17)
O1—Bi1—O8^v	162.8 (7)	O1Aⁱⁱⁱ—Bi5A—Cl1Aⁱⁱⁱ	78.5 (5)
O5Aⁱⁱⁱ—Bi1—O6A^v	83.7 (6)	O1ⁱⁱⁱ—Bi5A—Cl1Aⁱⁱⁱ	141.0 (5)
O1—Bi1—O6A^v	109.2 (6)	O6A—Bi5A—Cl1Aⁱⁱⁱ	141.8 (5)
O8^v—Bi1—O6A^v	65.1 (7)	O5A—Bi5A—Cl1Aⁱⁱⁱ	76.6 (4)
O5Aⁱⁱⁱ—Bi1—O2	69.7 (6)	Cl2^vii—Bi5A—Cl1Aⁱⁱⁱ	111.83 (16)
O1—Bi1—O2	107.3 (6)	Cl2A^vii—Bi5A—Cl1Aⁱⁱⁱ	71.15 (15)
O8^v—Bi1—O2	67.5 (7)	O1Aⁱⁱⁱ—Bi5A—Cl1ⁱⁱⁱ	142.9 (5)
O6A^v—Bi1—O2	124.2 (6)	O1ⁱⁱⁱ—Bi5A—Cl1ⁱⁱⁱ	77.7 (5)
O5Aⁱⁱⁱ—Bi1—O5ⁱⁱ	108.2 (6)	O6A—Bi5A—Cl1ⁱⁱⁱ	138.4 (5)
O1—Bi1—O5ⁱⁱ	73.0 (6)	O5A—Bi5A—Cl1ⁱⁱⁱ	75.7 (4)
O8^v—Bi1—O5ⁱⁱ	116.2 (6)	Cl2^vii—Bi5A—Cl1ⁱⁱⁱ	69.31 (16)
O6A^v—Bi1—O5ⁱⁱ	167.7 (6)	Cl2A^vii—Bi5A—Cl1ⁱⁱⁱ	113.16 (17)
O2—Bi1—O5ⁱⁱ	64.7 (5)	Cl1Aⁱⁱⁱ—Bi5A—Cl1ⁱⁱⁱ	73.13 (18)
O5Aⁱⁱⁱ—Bi1—O1ⁱ	112.5 (6)	O6—Bi6—O7	85.5 (8)
O1—Bi1—O1ⁱ	69.3 (7)	O6—Bi6—O8A	89.4 (6)
O8^v—Bi1—O1ⁱ	117.1 (7)	O7—Bi6—O8A	75.5 (7)
O6A^v—Bi1—O1ⁱ	61.4 (6)	O6—Bi6—Cl3A^vii	144.4 (5)
O2—Bi1—O1ⁱ	174.4 (5)	O7—Bi6—Cl3A^vii	119.7 (5)
O5ⁱⁱ—Bi1—O1ⁱ	109.8 (5)	O8A—Bi6—Cl3A^vii	75.0 (4)
O5Aⁱⁱⁱ—Bi1—O6^iv	175.8 (6)	O6—Bi6—Cl3^vi	126.1 (5)
O1—Bi1—O6^iv	111.8 (5)	O7—Bi6—Cl3^vi	105.7 (5)
O8^v—Bi1—O6^iv	85.3 (6)	O8A—Bi6—Cl3^vi	144.5 (4)
O6A^v—Bi1—O6^iv	97.1 (6)	Cl3A^vii—Bi6—Cl3^vi	74.03 (17)
O2—Bi1—O6^iv	106.6 (5)	O6—Bi6—Cl2A^vii	75.2 (5)
O5ⁱⁱ—Bi1—O6^iv	71.2 (6)	O7—Bi6—Cl2A^vii	147.9 (5)
O1ⁱ—Bi1—O6^iv	71.3 (5)	O8A—Bi6—Cl2A^vii	78.7 (5)
O5Aⁱⁱⁱ—Bi1—O9ⁱⁱ	129.4 (5)	Cl3A^vii—Bi6—Cl2A^vii	70.51 (18)
O1—Bi1—O9ⁱⁱ	58.2 (5)	Cl3^vi—Bi6—Cl2A^vii	106.4 (2)
O8^v—Bi1—O9ⁱⁱ	139.0 (6)	O6—Bi6—Cl2^vi	67.7 (5)
O6A^v—Bi1—O9ⁱⁱ	116.2 (5)	O7—Bi6—Cl2^vi	129.1 (5)
O2—Bi1—O9ⁱⁱ	118.6 (4)	O8A—Bi6—Cl2^vi	141.8 (5)
O5ⁱⁱ—Bi1—O9ⁱⁱ	54.0 (5)	Cl3A^vii—Bi6—Cl2^vi	105.9 (2)
O1ⁱ—Bi1—O9ⁱⁱ	55.8 (4)	Cl3^vi—Bi6—Cl2^vi	64.74 (18)
O6^iv—Bi1—O9ⁱⁱ	53.8 (4)	Cl2A^vii—Bi6—Cl2^vi	66.44 (16)
O1A—Bi1A—O5ⁱⁱⁱ	82.7 (6)	O8—Bi6A—O8A	92.3 (8)
O1A—Bi1A—O9ⁱⁱⁱ	65.1 (5)	O8—Bi6A—O6A	79.3 (8)
O5ⁱⁱⁱ—Bi1A—O9ⁱⁱⁱ	69.0 (6)	O8A—Bi6A—O6A	87.3 (7)
O1A—Bi1A—O6^v	131.9 (6)	O8—Bi6A—Cl2A^vii	155.3 (6)
O5ⁱⁱⁱ—Bi1A—O6^v	82.3 (6)	O8A—Bi6A—Cl2A^vii	82.7 (5)
O9ⁱⁱⁱ—Bi1A—O6^v	66.8 (5)	O6A—Bi6A—Cl2A^vii	76.4 (5)
O1A—Bi1A—O1Aⁱ	77.4 (7)	O8—Bi6A—Cl3^vii	87.9 (6)
O5ⁱⁱⁱ—Bi1A—O1Aⁱ	130.7 (6)	O8A—Bi6A—Cl3^vii	133.7 (5)
O9ⁱⁱⁱ—Bi1A—O1Aⁱ	61.7 (5)	O6A—Bi6A—Cl3^vii	137.8 (5)
O6^v—Bi1A—O1Aⁱ	78.6 (6)	Cl2A^vii—Bi6A—Cl3^vii	113.0 (2)
O1A—Bi1A—O5Aⁱⁱⁱ	69.0 (6)	O8—Bi6A—Cl3A^vii	130.5 (6)
O5ⁱⁱⁱ—Bi1A—O5Aⁱⁱⁱ	106.9 (6)	O8A—Bi6A—Cl3A^vii	72.8 (4)
O9ⁱⁱⁱ—Bi1A—O5Aⁱⁱⁱ	134.1 (5)	O6A—Bi6A—Cl3A^vii	143.5 (5)
O6^v—Bi1A—O5Aⁱⁱⁱ	158.8 (5)	Cl2A^vii—Bi6A—Cl3A^vii	71.06 (18)
O1Aⁱ—Bi1A—O5Aⁱⁱⁱ	107.1 (6)	Cl3^vii—Bi6A—Cl3A^vii	72.21 (17)
O1A—Bi1A—O2A	106.7 (6)	O8—Bi6A—Cl2^vii	102.9 (7)
O5ⁱⁱⁱ—Bi1A—O2A	64.6 (6)	O8A—Bi6A—Cl2^vii	152.5 (5)
O9ⁱⁱⁱ—Bi1A—O2A	133.6 (4)	O6A—Bi6A—Cl2^vii	73.5 (5)
O6^v—Bi1A—O2A	107.4 (6)	Cl2A^vii—Bi6A—Cl2^vii	73.88 (19)
O1Aⁱ—Bi1A—O2A	164.7 (5)	Cl3^vii—Bi6A—Cl2^vii	70.51 (18)
O5Aⁱⁱⁱ—Bi1A—O2A	62.3 (5)	Cl3A^vii—Bi6A—Cl2^vii	111.6 (2)
O1A—Bi1A—O8A^v	160.1 (5)	Bi4ⁱⁱ—Cl1—Bi4^ix	108.3 (3)
O5ⁱⁱⁱ—Bi1A—O8A^v	110.8 (6)	Bi4ⁱⁱ—Cl1—Bi5A^x	109.15 (3)
O9ⁱⁱⁱ—Bi1A—O8A^v	132.5 (4)	Bi4^ix—Cl1—Bi5A^x	112.07 (3)
O6^v—Bi1A—O8A^v	66.3 (5)	Bi4ⁱⁱ—Cl1—Bi5Aⁱⁱⁱ	112.07 (3)
O1Aⁱ—Bi1A—O8A^v	102.2 (5)	Bi4^ix—Cl1—Bi5Aⁱⁱⁱ	109.15 (3)
O5Aⁱⁱⁱ—Bi1A—O8A^v	92.5 (5)	Bi5A^x—Cl1—Bi5Aⁱⁱⁱ	106.2 (3)
O2A—Bi1A—O8A^v	68.8 (5)	Bi4ⁱⁱ—Cl1—Bi4Aⁱⁱⁱ	73.48 (3)
O1A—Bi1A—O6A^v	104.5 (6)	Bi4^ix—Cl1—Bi4Aⁱⁱⁱ	178.2 (3)
O5ⁱⁱⁱ—Bi1A—O6A^v	169.2 (6)	Bi5A^x—Cl1—Bi4Aⁱⁱⁱ	67.31 (14)
O9ⁱⁱⁱ—Bi1A—O6A^v	121.3 (5)	Bi5Aⁱⁱⁱ—Cl1—Bi4Aⁱⁱⁱ	69.68 (14)
O6^v—Bi1A—O6A^v	98.3 (6)	Bi4ⁱⁱ—Cl1—Bi4A^x	178.2 (3)
O1Aⁱ—Bi1A—O6A^v	59.7 (6)	Bi4^ix—Cl1—Bi4A^x	73.48 (3)
O5Aⁱⁱⁱ—Bi1A—O6A^v	69.1 (5)	Bi5A^x—Cl1—Bi4A^x	69.68 (14)
O2A—Bi1A—O6A^v	105.1 (5)	Bi5Aⁱⁱⁱ—Cl1—Bi4A^x	67.31 (14)
O8A^v—Bi1A—O6A^v	60.2 (5)	Bi4Aⁱⁱⁱ—Cl1—Bi4A^x	104.8 (3)
O8^v—Bi2—O2	77.2 (7)	Bi4ⁱⁱ—Cl1—Bi5^ix	74.69 (14)
O8^v—Bi2—O7^iv	79.5 (8)	Bi4^ix—Cl1—Bi5^ix	71.91 (14)
O2—Bi2—O7^iv	82.0 (6)	Bi5A^x—Cl1—Bi5^ix	66.37 (3)
O8^v—Bi2—O4Aⁱⁱⁱ	91.1 (7)	Bi5Aⁱⁱⁱ—Cl1—Bi5^ix	171.7 (3)
O2—Bi2—O4Aⁱⁱⁱ	70.7 (6)	Bi4Aⁱⁱⁱ—Cl1—Bi5^ix	109.05 (4)
O7^iv—Bi2—O4Aⁱⁱⁱ	152.5 (6)	Bi4A^x—Cl1—Bi5^ix	105.78 (4)
O8^v—Bi2—O4ⁱⁱ	136.2 (7)	Bi4ⁱⁱ—Cl1—Bi5ⁱⁱ	71.91 (14)
O2—Bi2—O4ⁱⁱ	72.8 (6)	Bi4^ix—Cl1—Bi5ⁱⁱ	74.69 (14)
O7^iv—Bi2—O4ⁱⁱ	65.5 (7)	Bi5A^x—Cl1—Bi5ⁱⁱ	171.7 (3)
O4Aⁱⁱⁱ—Bi2—O4ⁱⁱ	107.8 (6)	Bi5Aⁱⁱⁱ—Cl1—Bi5ⁱⁱ	66.37 (3)
O8^v—Bi2—O3	155.5 (7)	Bi4Aⁱⁱⁱ—Cl1—Bi5ⁱⁱ	105.78 (4)
O2—Bi2—O3	104.2 (6)	Bi4A^x—Cl1—Bi5ⁱⁱ	109.05 (4)
O7^iv—Bi2—O3	125.0 (6)	Bi5^ix—Cl1—Bi5ⁱⁱ	121.3 (3)
O4Aⁱⁱⁱ—Bi2—O3	67.1 (6)	Bi4ⁱⁱⁱ—Cl1A—Bi4^x	106.5 (2)
O4ⁱⁱ—Bi2—O3	64.8 (6)	Bi4ⁱⁱⁱ—Cl1A—Bi4Aⁱⁱⁱ	72.71 (3)
O8^v—Bi2—Cl3Aⁱⁱⁱ	87.8 (6)	Bi4^x—Cl1A—Bi4Aⁱⁱⁱ	179.2 (2)
O2—Bi2—Cl3Aⁱⁱⁱ	138.6 (4)	Bi4ⁱⁱⁱ—Cl1A—Bi4A^x	179.2 (2)
O7^iv—Bi2—Cl3Aⁱⁱⁱ	133.2 (5)	Bi4^x—Cl1A—Bi4A^x	72.71 (3)
O4Aⁱⁱⁱ—Bi2—Cl3Aⁱⁱⁱ	71.3 (4)	Bi4Aⁱⁱⁱ—Cl1A—Bi4A^x	108.1 (2)
O4ⁱⁱ—Bi2—Cl3Aⁱⁱⁱ	135.3 (4)	Bi4ⁱⁱⁱ—Cl1A—Bi5A^x	109.25 (3)
O3—Bi2—Cl3Aⁱⁱⁱ	75.0 (4)	Bi4^x—Cl1A—Bi5A^x	112.16 (3)
O8^v—Bi2—Cl3ⁱⁱ	117.5 (6)	Bi4Aⁱⁱⁱ—Cl1A—Bi5A^x	68.47 (12)
O2—Bi2—Cl3ⁱⁱ	143.7 (4)	Bi4A^x—Cl1A—Bi5A^x	70.89 (12)
O7^iv—Bi2—Cl3ⁱⁱ	69.7 (5)	Bi4ⁱⁱⁱ—Cl1A—Bi5Aⁱⁱⁱ	112.16 (3)
O4Aⁱⁱⁱ—Bi2—Cl3ⁱⁱ	136.4 (4)	Bi4^x—Cl1A—Bi5Aⁱⁱⁱ	109.25 (3)
O4ⁱⁱ—Bi2—Cl3ⁱⁱ	75.0 (4)	Bi4Aⁱⁱⁱ—Cl1A—Bi5Aⁱⁱⁱ	70.89 (12)
O3—Bi2—Cl3ⁱⁱ	76.2 (4)	Bi4A^x—Cl1A—Bi5Aⁱⁱⁱ	68.47 (12)
Cl3Aⁱⁱⁱ—Bi2—Cl3ⁱⁱ	77.28 (17)	Bi5A^x—Cl1A—Bi5Aⁱⁱⁱ	107.5 (2)
O2A—Bi2A—O4ⁱⁱⁱ	75.9 (6)	Bi4ⁱⁱⁱ—Cl1A—Bi5^x	71.65 (12)
O2A—Bi2A—O7^v	84.4 (6)	Bi4^x—Cl1A—Bi5^x	69.00 (12)
O4ⁱⁱⁱ—Bi2A—O7^v	69.8 (7)	Bi4Aⁱⁱⁱ—Cl1A—Bi5^x	110.91 (3)
O2A—Bi2A—O3A	107.9 (6)	Bi4A^x—Cl1A—Bi5^x	107.71 (3)
O4ⁱⁱⁱ—Bi2A—O3A	68.3 (6)	Bi5A^x—Cl1A—Bi5^x	70.58 (3)
O7^v—Bi2A—O3A	131.3 (6)	Bi5Aⁱⁱⁱ—Cl1A—Bi5^x	176.18 (12)
O2A—Bi2A—O8A^v	83.7 (6)	Bi4ⁱⁱⁱ—Cl1A—Bi5ⁱⁱⁱ	69.00 (12)
O4ⁱⁱⁱ—Bi2A—O8A^v	130.7 (6)	Bi4^x—Cl1A—Bi5ⁱⁱⁱ	71.65 (12)
O7^v—Bi2A—O8A^v	63.9 (6)	Bi4Aⁱⁱⁱ—Cl1A—Bi5ⁱⁱⁱ	107.71 (3)
O3A—Bi2A—O8A^v	160.5 (5)	Bi4A^x—Cl1A—Bi5ⁱⁱⁱ	110.91 (3)
O2A—Bi2A—O4Aⁱⁱⁱ	70.1 (6)	Bi5A^x—Cl1A—Bi5ⁱⁱⁱ	176.18 (12)
O4ⁱⁱⁱ—Bi2A—O4Aⁱⁱⁱ	109.0 (6)	Bi5Aⁱⁱⁱ—Cl1A—Bi5ⁱⁱⁱ	70.58 (3)
O7^v—Bi2A—O4Aⁱⁱⁱ	153.6 (6)	Bi5^x—Cl1A—Bi5ⁱⁱⁱ	111.5 (2)
O3A—Bi2A—O4Aⁱⁱⁱ	66.2 (6)	Bi5A^x—Cl2—Bi3ⁱⁱ	176.8 (3)
O8A^v—Bi2A—O4Aⁱⁱⁱ	105.1 (6)	Bi5A^x—Cl2—Bi3Aⁱⁱⁱ	105.36 (18)
O2A—Bi2A—Cl3ⁱⁱⁱ	150.7 (4)	Bi3ⁱⁱ—Cl2—Bi3Aⁱⁱⁱ	73.66 (15)
O4ⁱⁱⁱ—Bi2A—Cl3ⁱⁱⁱ	80.3 (4)	Bi5A^x—Cl2—Bi4ⁱⁱ	110.0 (2)
O7^v—Bi2A—Cl3ⁱⁱⁱ	71.5 (5)	Bi3ⁱⁱ—Cl2—Bi4ⁱⁱ	73.17 (15)
O3A—Bi2A—Cl3ⁱⁱⁱ	78.0 (4)	Bi3Aⁱⁱⁱ—Cl2—Bi4ⁱⁱ	112.5 (2)
O8A^v—Bi2A—Cl3ⁱⁱⁱ	99.7 (4)	Bi5A^x—Cl2—Bi5^ix	70.10 (14)
O4Aⁱⁱⁱ—Bi2A—Cl3ⁱⁱⁱ	134.9 (4)	Bi3ⁱⁱ—Cl2—Bi5^ix	110.49 (18)
O2A—Bi2A—Cl3Aⁱⁱⁱ	134.2 (4)	Bi3Aⁱⁱⁱ—Cl2—Bi5^ix	171.9 (3)
O4ⁱⁱⁱ—Bi2A—Cl3Aⁱⁱⁱ	136.7 (5)	Bi4ⁱⁱ—Cl2—Bi5^ix	75.56 (15)
O7^v—Bi2A—Cl3Aⁱⁱⁱ	131.2 (5)	Bi5A^x—Cl2—Bi6A^x	69.34 (14)
O3A—Bi2A—Cl3Aⁱⁱⁱ	72.1 (4)	Bi3ⁱⁱ—Cl2—Bi6A^x	107.5 (2)
O8A^v—Bi2A—Cl3Aⁱⁱⁱ	88.5 (4)	Bi3Aⁱⁱⁱ—Cl2—Bi6A^x	67.01 (14)
O4Aⁱⁱⁱ—Bi2A—Cl3Aⁱⁱⁱ	68.7 (4)	Bi4ⁱⁱ—Cl2—Bi6A^x	178.9 (2)
Cl3ⁱⁱⁱ—Bi2A—Cl3Aⁱⁱⁱ	75.03 (17)	Bi5^ix—Cl2—Bi6A^x	104.9 (2)
O4—Bi3—O3	112.4 (7)	Bi5A^x—Cl2—Bi4Aⁱⁱⁱ	69.57 (14)
O4—Bi3—O3ⁱⁱ	78.7 (6)	Bi3ⁱⁱ—Cl2—Bi4Aⁱⁱⁱ	112.6 (2)
O3—Bi3—O3ⁱⁱ	71.9 (7)	Bi3Aⁱⁱⁱ—Cl2—Bi4Aⁱⁱⁱ	68.80 (14)
O4—Bi3—O3Aⁱⁱⁱ	74.8 (6)	Bi4ⁱⁱ—Cl2—Bi4Aⁱⁱⁱ	72.61 (17)
O3—Bi3—O3Aⁱⁱⁱ	72.5 (6)	Bi5^ix—Cl2—Bi4Aⁱⁱⁱ	114.5 (2)
O3ⁱⁱ—Bi3—O3Aⁱⁱⁱ	122.2 (7)	Bi6A^x—Cl2—Bi4Aⁱⁱⁱ	106.28 (18)
O4—Bi3—Cl3ⁱⁱ	141.9 (4)	Bi5A^x—Cl2—Bi6^ix	112.3 (2)
O3—Bi3—Cl3ⁱⁱ	82.2 (5)	Bi3ⁱⁱ—Cl2—Bi6^ix	65.49 (13)
O3ⁱⁱ—Bi3—Cl3ⁱⁱ	72.7 (5)	Bi3Aⁱⁱⁱ—Cl2—Bi6^ix	108.6 (2)
O3Aⁱⁱⁱ—Bi3—Cl3ⁱⁱ	142.4 (5)	Bi4ⁱⁱ—Cl2—Bi6^ix	108.18 (17)
O4—Bi3—Cl3Aⁱⁱⁱ	139.6 (4)	Bi5^ix—Cl2—Bi6^ix	68.25 (13)
O3—Bi3—Cl3Aⁱⁱⁱ	80.1 (5)	Bi6A^x—Cl2—Bi6^ix	72.94 (16)
O3ⁱⁱ—Bi3—Cl3Aⁱⁱⁱ	140.0 (5)	Bi4Aⁱⁱⁱ—Cl2—Bi6^ix	177.3 (2)
O3Aⁱⁱⁱ—Bi3—Cl3Aⁱⁱⁱ	72.9 (5)	Bi6A^x—Cl2A—Bi3ⁱⁱⁱ	109.3 (2)
Cl3ⁱⁱ—Bi3—Cl3Aⁱⁱⁱ	75.78 (19)	Bi6A^x—Cl2A—Bi3Aⁱⁱⁱ	68.45 (13)
O4—Bi3—Cl2Aⁱⁱⁱ	77.2 (5)	Bi3ⁱⁱⁱ—Cl2A—Bi3Aⁱⁱⁱ	74.06 (14)
O3—Bi3—Cl2Aⁱⁱⁱ	142.6 (4)	Bi6A^x—Cl2A—Bi5A^x	70.47 (13)
O3ⁱⁱ—Bi3—Cl2Aⁱⁱⁱ	144.1 (5)	Bi3ⁱⁱⁱ—Cl2A—Bi5A^x	179.7 (3)
O3Aⁱⁱⁱ—Bi3—Cl2Aⁱⁱⁱ	76.0 (4)	Bi3Aⁱⁱⁱ—Cl2A—Bi5A^x	105.85 (17)
Cl3ⁱⁱ—Bi3—Cl2Aⁱⁱⁱ	113.2 (2)	Bi6A^x—Cl2A—Bi6^x	67.38 (16)
Cl3Aⁱⁱⁱ—Bi3—Cl2Aⁱⁱⁱ	71.89 (17)	Bi3ⁱⁱⁱ—Cl2A—Bi6^x	69.69 (14)
O4—Bi3—Cl2ⁱⁱ	77.2 (5)	Bi3Aⁱⁱⁱ—Cl2A—Bi6^x	106.9 (2)
O3—Bi3—Cl2ⁱⁱ	143.1 (4)	Bi5A^x—Cl2A—Bi6^x	110.1 (2)
O3ⁱⁱ—Bi3—Cl2ⁱⁱ	75.6 (4)	Bi6A^x—Cl2A—Bi4Aⁱⁱⁱ	108.21 (17)
O3Aⁱⁱⁱ—Bi3—Cl2ⁱⁱ	142.2 (4)	Bi3ⁱⁱⁱ—Cl2A—Bi4Aⁱⁱⁱ	110.8 (2)
Cl3ⁱⁱ—Bi3—Cl2ⁱⁱ	71.74 (18)	Bi3Aⁱⁱⁱ—Cl2A—Bi4Aⁱⁱⁱ	68.95 (14)
Cl3Aⁱⁱⁱ—Bi3—Cl2ⁱⁱ	116.6 (2)	Bi5A^x—Cl2A—Bi4Aⁱⁱⁱ	69.35 (13)
Cl2Aⁱⁱⁱ—Bi3—Cl2ⁱⁱ	73.39 (17)	Bi6^x—Cl2A—Bi4Aⁱⁱⁱ	175.1 (2)
O4A—Bi3A—O3A	117.1 (7)	Bi6A^x—Cl2A—Bi4ⁱⁱⁱ	178.2 (2)
O4A—Bi3A—O3ⁱⁱⁱ	80.4 (6)	Bi3ⁱⁱⁱ—Cl2A—Bi4ⁱⁱⁱ	72.22 (14)
O3A—Bi3A—O3ⁱⁱⁱ	73.1 (6)	Bi3Aⁱⁱⁱ—Cl2A—Bi4ⁱⁱⁱ	111.3 (2)
O4A—Bi3A—O3Aⁱⁱⁱ	78.2 (6)	Bi5A^x—Cl2A—Bi4ⁱⁱⁱ	108.0 (2)
O3A—Bi3A—O3Aⁱⁱⁱ	73.4 (7)	Bi6^x—Cl2A—Bi4ⁱⁱⁱ	114.28 (17)
O3ⁱⁱⁱ—Bi3A—O3Aⁱⁱⁱ	125.4 (7)	Bi4Aⁱⁱⁱ—Cl2A—Bi4ⁱⁱⁱ	70.16 (16)
O4A—Bi3A—Cl2Aⁱⁱⁱ	80.2 (5)	Bi6A^x—Cl2A—Bi5^x	108.3 (2)
O3A—Bi3A—Cl2Aⁱⁱⁱ	140.5 (4)	Bi3ⁱⁱⁱ—Cl2A—Bi5^x	106.03 (17)
O3ⁱⁱⁱ—Bi3A—Cl2Aⁱⁱⁱ	146.4 (5)	Bi3Aⁱⁱⁱ—Cl2A—Bi5^x	176.4 (3)
O3Aⁱⁱⁱ—Bi3A—Cl2Aⁱⁱⁱ	76.5 (4)	Bi5A^x—Cl2A—Bi5^x	74.04 (13)
O4A—Bi3A—Cl3Aⁱⁱⁱ	143.2 (4)	Bi6^x—Cl2A—Bi5^x	69.96 (14)
O3A—Bi3A—Cl3Aⁱⁱⁱ	75.7 (5)	Bi4Aⁱⁱⁱ—Cl2A—Bi5^x	114.1 (2)
O3ⁱⁱⁱ—Bi3A—Cl3Aⁱⁱⁱ	135.4 (5)	Bi4ⁱⁱⁱ—Cl2A—Bi5^x	71.96 (13)
O3Aⁱⁱⁱ—Bi3A—Cl3Aⁱⁱⁱ	72.8 (5)	Bi2Aⁱⁱⁱ—Cl3—Bi2ⁱⁱ	70.90 (15)
Cl2Aⁱⁱⁱ—Bi3A—Cl3Aⁱⁱⁱ	71.39 (18)	Bi2Aⁱⁱⁱ—Cl3—Bi3ⁱⁱ	115.6 (3)
O4A—Bi3A—Cl2ⁱⁱⁱ	78.8 (5)	Bi2ⁱⁱ—Cl3—Bi3ⁱⁱ	75.06 (17)
O3A—Bi3A—Cl2ⁱⁱⁱ	140.8 (4)	Bi2Aⁱⁱⁱ—Cl3—Bi6A^x	108.7 (2)
O3ⁱⁱⁱ—Bi3A—Cl2ⁱⁱⁱ	75.2 (4)	Bi2ⁱⁱ—Cl3—Bi6A^x	173.8 (3)
O3Aⁱⁱⁱ—Bi3A—Cl2ⁱⁱⁱ	145.4 (4)	Bi3ⁱⁱ—Cl3—Bi6A^x	110.2 (2)
Cl2Aⁱⁱⁱ—Bi3A—Cl2ⁱⁱⁱ	74.30 (16)	Bi2Aⁱⁱⁱ—Cl3—Bi3Aⁱⁱⁱ	76.60 (17)
Cl3Aⁱⁱⁱ—Bi3A—Cl2ⁱⁱⁱ	114.0 (2)	Bi2ⁱⁱ—Cl3—Bi3Aⁱⁱⁱ	117.9 (3)
O4A—Bi3A—Cl3ⁱⁱⁱ	142.1 (4)	Bi3ⁱⁱ—Cl3—Bi3Aⁱⁱⁱ	73.70 (19)
O3A—Bi3A—Cl3ⁱⁱⁱ	77.9 (5)	Bi6A^x—Cl3—Bi3Aⁱⁱⁱ	67.52 (15)
O3ⁱⁱⁱ—Bi3A—Cl3ⁱⁱⁱ	70.9 (5)	Bi2Aⁱⁱⁱ—Cl3—Bi6^ix	167.2 (3)
O3Aⁱⁱⁱ—Bi3A—Cl3ⁱⁱⁱ	138.9 (5)	Bi2ⁱⁱ—Cl3—Bi6^ix	100.82 (19)
Cl2Aⁱⁱⁱ—Bi3A—Cl3ⁱⁱⁱ	111.0 (2)	Bi3ⁱⁱ—Cl3—Bi6^ix	69.98 (14)
Cl3Aⁱⁱⁱ—Bi3A—Cl3ⁱⁱⁱ	72.07 (19)	Bi6A^x—Cl3—Bi6^ix	78.44 (15)
Cl2ⁱⁱⁱ—Bi3A—Cl3ⁱⁱⁱ	70.45 (18)	Bi3Aⁱⁱⁱ—Cl3—Bi6^ix	116.2 (2)
O5—Bi4—O2Aⁱⁱⁱ	76.8 (6)	Bi2ⁱⁱⁱ—Cl3A—Bi6^x	105.05 (19)
O5—Bi4—O2ⁱⁱ	78.2 (6)	Bi2ⁱⁱⁱ—Cl3A—Bi3ⁱⁱⁱ	75.28 (15)
O2Aⁱⁱⁱ—Bi4—O2ⁱⁱ	119.6 (6)	Bi6^x—Cl3A—Bi3ⁱⁱⁱ	71.97 (15)
O5—Bi4—O4	120.5 (7)	Bi2ⁱⁱⁱ—Cl3A—Bi2Aⁱⁱⁱ	81.43 (15)
O2Aⁱⁱⁱ—Bi4—O4	72.3 (6)	Bi6^x—Cl3A—Bi2Aⁱⁱⁱ	165.8 (3)
O2ⁱⁱ—Bi4—O4	75.0 (6)	Bi3ⁱⁱⁱ—Cl3A—Bi2Aⁱⁱⁱ	122.2 (2)
O5—Bi4—Cl1ⁱⁱ	80.7 (5)	Bi2ⁱⁱⁱ—Cl3A—Bi3Aⁱⁱⁱ	121.8 (2)
O2Aⁱⁱⁱ—Bi4—Cl1ⁱⁱ	146.3 (4)	Bi6^x—Cl3A—Bi3Aⁱⁱⁱ	110.6 (2)
O2ⁱⁱ—Bi4—Cl1ⁱⁱ	79.2 (4)	Bi3ⁱⁱⁱ—Cl3A—Bi3Aⁱⁱⁱ	74.05 (19)
O4—Bi4—Cl1ⁱⁱ	141.4 (4)	Bi2Aⁱⁱⁱ—Cl3A—Bi3Aⁱⁱⁱ	75.05 (15)
O5—Bi4—Cl1Aⁱⁱⁱ	80.0 (5)	Bi2ⁱⁱⁱ—Cl3A—Bi6A^x	170.8 (3)
O2Aⁱⁱⁱ—Bi4—Cl1Aⁱⁱⁱ	79.0 (4)	Bi6^x—Cl3A—Bi6A^x	68.41 (13)
O2ⁱⁱ—Bi4—Cl1Aⁱⁱⁱ	146.7 (4)	Bi3ⁱⁱⁱ—Cl3A—Bi6A^x	107.7 (2)
O4—Bi4—Cl1Aⁱⁱⁱ	138.2 (4)	Bi2Aⁱⁱⁱ—Cl3A—Bi6A^x	103.53 (18)
Cl1ⁱⁱ—Bi4—Cl1Aⁱⁱⁱ	72.60 (19)	Bi3Aⁱⁱⁱ—Cl3A—Bi6A^x	67.33 (14)
O5—Bi4—Cl2ⁱⁱ	143.7 (5)	Bi5Aⁱⁱⁱ—O1—Bi5ⁱⁱ	123.8 (8)
O2Aⁱⁱⁱ—Bi4—Cl2ⁱⁱ	137.8 (5)	Bi5Aⁱⁱⁱ—O1—Bi1	111.1 (7)
O2ⁱⁱ—Bi4—Cl2ⁱⁱ	74.1 (5)	Bi5ⁱⁱ—O1—Bi1	105.6 (6)
O4—Bi4—Cl2ⁱⁱ	74.1 (5)	Bi5Aⁱⁱⁱ—O1—Bi1ⁱ	106.6 (6)
Cl1ⁱⁱ—Bi4—Cl2ⁱⁱ	71.54 (14)	Bi5ⁱⁱ—O1—Bi1ⁱ	98.1 (6)
Cl1Aⁱⁱⁱ—Bi4—Cl2ⁱⁱ	112.02 (14)	Bi1—O1—Bi1ⁱ	110.7 (7)
O5—Bi4—Cl2Aⁱⁱⁱ	143.0 (5)	Bi5Aⁱⁱⁱ—O1A—Bi1A	120.3 (8)
O2Aⁱⁱⁱ—Bi4—Cl2Aⁱⁱⁱ	74.8 (5)	Bi5Aⁱⁱⁱ—O1A—Bi5ⁱⁱⁱ	128.4 (9)
O2ⁱⁱ—Bi4—Cl2Aⁱⁱⁱ	137.2 (5)	Bi1A—O1A—Bi5ⁱⁱⁱ	92.8 (6)
O4—Bi4—Cl2Aⁱⁱⁱ	72.1 (5)	Bi5Aⁱⁱⁱ—O1A—Bi1Aⁱ	118.7 (8)
Cl1ⁱⁱ—Bi4—Cl2Aⁱⁱⁱ	111.67 (14)	Bi1A—O1A—Bi1Aⁱ	98.8 (7)
Cl1Aⁱⁱⁱ—Bi4—Cl2Aⁱⁱⁱ	71.56 (12)	Bi5ⁱⁱⁱ—O1A—Bi1Aⁱ	90.3 (6)
Cl2ⁱⁱ—Bi4—Cl2Aⁱⁱⁱ	71.11 (18)	Bi2—O2—Bi4ⁱⁱ	110.8 (7)
O5A—Bi4A—O4A	118.6 (7)	Bi2—O2—Bi4Aⁱⁱⁱ	109.1 (6)
O5A—Bi4A—O2Aⁱⁱⁱ	79.0 (6)	Bi4ⁱⁱ—O2—Bi4Aⁱⁱⁱ	123.7 (8)
O4A—Bi4A—O2Aⁱⁱⁱ	76.3 (6)	Bi2—O2—Bi1	102.8 (7)
O5A—Bi4A—O2ⁱⁱⁱ	76.0 (6)	Bi4ⁱⁱ—O2—Bi1	108.4 (6)
O4A—Bi4A—O2ⁱⁱⁱ	75.1 (6)	Bi4Aⁱⁱⁱ—O2—Bi1	99.5 (6)
O2Aⁱⁱⁱ—Bi4A—O2ⁱⁱⁱ	126.0 (6)	Bi2A—O2A—Bi4Aⁱⁱⁱ	112.3 (7)
O5A—Bi4A—Cl1Aⁱⁱⁱ	81.3 (4)	Bi2A—O2A—Bi4ⁱⁱⁱ	107.2 (6)
O4A—Bi4A—Cl1Aⁱⁱⁱ	141.8 (5)	Bi4Aⁱⁱⁱ—O2A—Bi4ⁱⁱⁱ	121.9 (8)
O2Aⁱⁱⁱ—Bi4A—Cl1Aⁱⁱⁱ	76.3 (4)	Bi2A—O2A—Bi1A	109.2 (7)
O2ⁱⁱⁱ—Bi4A—Cl1Aⁱⁱⁱ	143.1 (4)	Bi4Aⁱⁱⁱ—O2A—Bi1A	106.1 (6)
O5A—Bi4A—Cl2ⁱⁱⁱ	139.5 (4)	Bi4ⁱⁱⁱ—O2A—Bi1A	98.9 (6)
O4A—Bi4A—Cl2ⁱⁱⁱ	76.8 (5)	Bi3—O3—Bi3ⁱⁱ	108.1 (7)
O2Aⁱⁱⁱ—Bi4A—Cl2ⁱⁱⁱ	140.8 (5)	Bi3—O3—Bi3Aⁱⁱⁱ	108.4 (7)
O2ⁱⁱⁱ—Bi4A—Cl2ⁱⁱⁱ	72.5 (5)	Bi3ⁱⁱ—O3—Bi3Aⁱⁱⁱ	125.5 (8)
Cl1Aⁱⁱⁱ—Bi4A—Cl2ⁱⁱⁱ	110.08 (14)	Bi3—O3—Bi2	107.9 (7)
O5A—Bi4A—Cl2Aⁱⁱⁱ	145.1 (4)	Bi3ⁱⁱ—O3—Bi2	103.6 (6)
O4A—Bi4A—Cl2Aⁱⁱⁱ	77.3 (5)	Bi3Aⁱⁱⁱ—O3—Bi2	102.0 (6)
O2Aⁱⁱⁱ—Bi4A—Cl2Aⁱⁱⁱ	75.0 (5)	Bi3A—O3A—Bi3Aⁱⁱⁱ	106.6 (7)
O2ⁱⁱⁱ—Bi4A—Cl2Aⁱⁱⁱ	138.6 (5)	Bi3A—O3A—Bi3ⁱⁱⁱ	105.6 (7)
Cl1Aⁱⁱⁱ—Bi4A—Cl2Aⁱⁱⁱ	70.21 (12)	Bi3Aⁱⁱⁱ—O3A—Bi3ⁱⁱⁱ	122.2 (8)
Cl2ⁱⁱⁱ—Bi4A—Cl2Aⁱⁱⁱ	71.58 (17)	Bi3A—O3A—Bi2A	114.9 (7)
O5A—Bi4A—Cl1ⁱⁱⁱ	79.3 (4)	Bi3Aⁱⁱⁱ—O3A—Bi2A	107.4 (6)
O4A—Bi4A—Cl1ⁱⁱⁱ	138.5 (5)	Bi3ⁱⁱⁱ—O3A—Bi2A	100.5 (6)
O2Aⁱⁱⁱ—Bi4A—Cl1ⁱⁱⁱ	145.1 (4)	Bi3—O4—Bi2Aⁱⁱⁱ	115.8 (7)
O2ⁱⁱⁱ—Bi4A—Cl1ⁱⁱⁱ	73.9 (4)	Bi3—O4—Bi4	122.6 (8)
Cl1Aⁱⁱⁱ—Bi4A—Cl1ⁱⁱⁱ	73.58 (18)	Bi2Aⁱⁱⁱ—O4—Bi4	101.7 (7)
Cl2ⁱⁱⁱ—Bi4A—Cl1ⁱⁱⁱ	68.03 (14)	Bi3—O4—Bi2ⁱⁱ	112.6 (7)
Cl2Aⁱⁱⁱ—Bi4A—Cl1ⁱⁱⁱ	110.15 (13)	Bi2Aⁱⁱⁱ—O4—Bi2ⁱⁱ	102.2 (7)
O1ⁱⁱ—Bi5—O6	91.0 (6)	Bi4—O4—Bi2ⁱⁱ	98.9 (6)
O1ⁱⁱ—Bi5—O9	76.0 (8)	Bi4A—O4A—Bi3A	119.9 (8)
O6—Bi5—O9	72.4 (5)	Bi4A—O4A—Bi2ⁱⁱⁱ	103.3 (7)
O1ⁱⁱ—Bi5—O5	83.2 (6)	Bi3A—O4A—Bi2ⁱⁱⁱ	110.3 (7)
O6—Bi5—O5	143.0 (7)	Bi4A—O4A—Bi2Aⁱⁱⁱ	100.7 (6)
O9—Bi5—O5	70.8 (5)	Bi3A—O4A—Bi2Aⁱⁱⁱ	108.1 (7)
O1ⁱⁱ—Bi5—O1Aⁱⁱⁱ	139.1 (6)	Bi2ⁱⁱⁱ—O4A—Bi2Aⁱⁱⁱ	114.5 (7)
O6—Bi5—O1Aⁱⁱⁱ	83.3 (6)	Bi4—O5—Bi1Aⁱⁱⁱ	119.6 (8)
O9—Bi5—O1Aⁱⁱⁱ	63.6 (7)	Bi4—O5—Bi5	127.8 (9)
O5—Bi5—O1Aⁱⁱⁱ	77.8 (6)	Bi1Aⁱⁱⁱ—O5—Bi5	96.0 (7)
O1ⁱⁱ—Bi5—Cl2^vi	78.0 (5)	Bi4—O5—Bi1ⁱⁱ	108.7 (7)
O6—Bi5—Cl2^vi	75.0 (5)	Bi1Aⁱⁱⁱ—O5—Bi1ⁱⁱ	105.8 (7)
O9—Bi5—Cl2^vi	137.4 (4)	Bi5—O5—Bi1ⁱⁱ	95.0 (6)
O5—Bi5—Cl2^vi	138.0 (5)	Bi4A—O5A—Bi1ⁱⁱⁱ	113.9 (7)
O1Aⁱⁱⁱ—Bi5—Cl2^vi	137.7 (4)	Bi4A—O5A—Bi5A	117.6 (8)
O1ⁱⁱ—Bi5—Cl1ⁱⁱ	75.0 (5)	Bi1ⁱⁱⁱ—O5A—Bi5A	105.3 (7)
O6—Bi5—Cl1ⁱⁱ	141.8 (4)	Bi4A—O5A—Bi1Aⁱⁱⁱ	112.5 (7)
O9—Bi5—Cl1ⁱⁱ	134.3 (3)	Bi1ⁱⁱⁱ—O5A—Bi1Aⁱⁱⁱ	110.2 (7)
O5—Bi5—Cl1ⁱⁱ	71.5 (5)	Bi5A—O5A—Bi1Aⁱⁱⁱ	95.8 (6)
O1Aⁱⁱⁱ—Bi5—Cl1ⁱⁱ	130.1 (5)	Bi6—O6—Bi5	137.4 (10)
Cl2^vi—Bi5—Cl1ⁱⁱ	67.49 (15)	Bi6—O6—Bi1A^xi	108.7 (7)
O1ⁱⁱ—Bi5—Cl2A^vii	145.3 (4)	Bi5—O6—Bi1A^xi	96.7 (6)
O6—Bi5—Cl2A^vii	70.2 (5)	Bi6—O6—Bi1^xii	112.0 (7)
O9—Bi5—Cl2A^vii	122.1 (5)	Bi5—O6—Bi1^xii	96.7 (6)
O5—Bi5—Cl2A^vii	129.2 (4)	Bi1A^xi—O6—Bi1^xii	98.9 (6)
O1Aⁱⁱⁱ—Bi5—Cl2A^vii	69.5 (4)	Bi6A—O6A—Bi5A	126.3 (9)
Cl2^vi—Bi5—Cl2A^vii	69.16 (16)	Bi6A—O6A—Bi1^xi	105.6 (8)
Cl1ⁱⁱ—Bi5—Cl2A^vii	101.52 (16)	Bi5A—O6A—Bi1^xi	114.5 (7)
O1ⁱⁱ—Bi5—Cl1Aⁱⁱⁱ	134.8 (5)	Bi6A—O6A—Bi1A^xi	106.1 (7)
O6—Bi5—Cl1Aⁱⁱⁱ	132.8 (4)	Bi5A—O6A—Bi1A^xi	103.3 (6)
O9—Bi5—Cl1Aⁱⁱⁱ	121.5 (5)	Bi1^xi—O6A—Bi1A^xi	96.7 (6)
O5—Bi5—Cl1Aⁱⁱⁱ	67.7 (5)	Bi6—O7—Bi2^xii	125.9 (8)
O1Aⁱⁱⁱ—Bi5—Cl1Aⁱⁱⁱ	68.7 (5)	Bi6—O7—Bi2A^xi	111.9 (8)
Cl2^vi—Bi5—Cl1Aⁱⁱⁱ	100.76 (16)	Bi2^xii—O7—Bi2A^xi	109.6 (8)
Cl1ⁱⁱ—Bi5—Cl1Aⁱⁱⁱ	63.61 (18)	Bi6A—O8A—Bi6	124.0 (8)
Cl2A^vii—Bi5—Cl1Aⁱⁱⁱ	64.77 (14)	Bi6A—O8A—Bi2A^xi	128.4 (7)
O1Aⁱⁱⁱ—Bi5A—O1ⁱⁱⁱ	113.0 (7)	Bi6—O8A—Bi2A^xi	99.9 (6)
O1Aⁱⁱⁱ—Bi5A—O6A	77.9 (7)	Bi6A—O8A—Bi1A^xi	106.4 (6)
O1ⁱⁱⁱ—Bi5A—O6A	76.4 (7)	Bi6—O8A—Bi1A^xi	93.6 (5)
O1Aⁱⁱⁱ—Bi5A—O5A	74.8 (6)	Bi2A^xi—O8A—Bi1A^xi	95.3 (5)
O1ⁱⁱⁱ—Bi5A—O5A	71.5 (6)	Bi6A—O8—Bi2^xi	145.6 (11)
O6A—Bi5A—O5A	124.5 (7)	Bi6A—O8—Bi1^xi	108.2 (10)
O1Aⁱⁱⁱ—Bi5A—Cl2^vii	145.4 (5)	Bi5—O9—Bi5^viii	164.3 (12)
O1ⁱⁱⁱ—Bi5A—Cl2^vii	80.4 (5)	Bi5—O9—Bi1A^xi	96.9 (4)
O6A—Bi5A—Cl2^vii	74.6 (5)	Bi5^viii—O9—Bi1A^xi	93.5 (3)
O5A—Bi5A—Cl2^vii	138.9 (4)	Bi5—O9—Bi1Aⁱⁱⁱ	93.5 (3)
O1Aⁱⁱⁱ—Bi5A—Cl2A^vii	78.5 (5)	Bi5^viii—O9—Bi1Aⁱⁱⁱ	96.9 (4)
O1ⁱⁱⁱ—Bi5A—Cl2A^vii	146.0 (5)	Bi1A^xi—O9—Bi1Aⁱⁱⁱ	96.9 (9)
O6A—Bi5A—Cl2A^vii	75.0 (5)

Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1, −y, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x−1, −y, z−1/2; (v) x−1, −y+1, z−1/2; (vi) x, −y, z+1/2; (vii) x, −y+1, z+1/2; (viii) −x+2, y, −z+3/2; (ix) x, −y, z−1/2; (x) x, −y+1, z−1/2; (xi) x+1, −y+1, z+1/2; (xii) x+1, −y, z+1/2.

(bi24obr) top

Crystal data top

Bi₂₄Br₁₀O₃₁	F(000) = 2590
M_r = 6310.62	D_x = 8.607 Mg m⁻³
Monoclinic, A2/m	Mo Kα radiation, λ = 0.71073 Å
a = 10.141 (7) Å	Cell parameters from 8153 reflections
b = 4.005 (3) Å	θ = 1.4–28.0°
c = 29.977 (19) Å	µ = 94.64 mm⁻¹
β = 90.197 (12)°	T = 293 K
V = 1217.5 (14) Å³	Needle, pale brown
Z = 1	0.25 × 0.04 × 0.02 mm

Data collection top

CCD area detector diffractometer	1627 independent reflections
Radiation source: fine-focus sealed tube	882 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.128
phi and ω scans	θ_max = 28.3°, θ_min = 1.4°
Absorption correction: integration XPREP / Bruker SHELXTL	h = −13→13
T_min = 0.020, T_max = 0.269	k = 0→5
8153 measured reflections	l = 0→39

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.064	w = 1/[σ²(F_o²) + (0.1089P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.186	(Δ/σ)_max < 0.001
S = 0.91	Δρ_max = 6.08 e Å⁻³
1627 reflections	Δρ_min = −5.92 e Å⁻³
84 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00025 (4)

Crystal data top

Bi₂₄Br₁₀O₃₁	V = 1217.5 (14) Å³
M_r = 6310.62	Z = 1
Monoclinic, A2/m	Mo Kα radiation
a = 10.141 (7) Å	µ = 94.64 mm⁻¹
b = 4.005 (3) Å	T = 293 K
c = 29.977 (19) Å	0.25 × 0.04 × 0.02 mm
β = 90.197 (12)°

Data collection top

CCD area detector diffractometer	1627 independent reflections
Absorption correction: integration XPREP / Bruker SHELXTL	882 reflections with I > 2σ(I)
T_min = 0.020, T_max = 0.269	R_int = 0.128
8153 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.064	84 parameters
wR(F²) = 0.186	0 restraints
S = 0.91	Δρ_max = 6.08 e Å⁻³
1627 reflections	Δρ_min = −5.92 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Bi1	0.08569 (15)	0.0000	0.05880 (6)	0.0480 (6)
Bi2	0.25344 (12)	0.0000	0.17509 (4)	0.0228 (4)
Bi3	0.43453 (12)	0.0000	0.29464 (4)	0.0108 (3)
Bi4	0.60015 (11)	0.0000	0.41348 (4)	0.0114 (3)
Bi5	0.77636 (17)	0.0000	0.53264 (5)	0.0309 (5)
Bi6	0.92640 (17)	0.0000	0.65308 (5)	0.0317 (5)
Br1	0.5000	0.0000	0.0000	0.0151 (10)
Br2	0.6637 (3)	0.0000	0.11904 (11)	0.0190 (8)
Br3	0.8179 (4)	0.0000	0.24020 (13)	0.0234 (8)
O1	0.138 (2)	0.0000	−0.0158 (8)	0.027 (6)*
O2	0.3097 (19)	0.0000	0.1043 (7)	0.011 (4)*
O3	0.478 (2)	0.0000	0.2228 (8)	0.020 (5)*
O4	0.6112 (19)	0.0000	0.3378 (7)	0.013 (4)*
O5	0.778 (2)	0.0000	0.4542 (7)	0.019 (5)*
O6	0.931 (2)	0.0000	0.5837 (8)	0.021 (5)*
O7	1.146 (4)	0.0000	0.6472 (15)	0.024 (11)*	0.50
O8	1.083 (7)	1.309 (19)	0.643 (2)	0.036 (18)*	0.25
O8A	1.021 (5)	0.45 (2)	0.6458 (18)	0.024 (17)*	0.25
O9	1.0000	0.0000	0.5000	0.021 (14)*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Bi1	0.0223 (9)	0.0802 (15)	0.0414 (11)	0.000	0.0109 (8)	0.000
Bi2	0.0167 (7)	0.0407 (10)	0.0109 (7)	0.000	−0.0004 (6)	0.000
Bi3	0.0137 (6)	0.0070 (6)	0.0116 (6)	0.000	0.0014 (5)	0.000
Bi4	0.0103 (6)	0.0085 (6)	0.0153 (7)	0.000	−0.0020 (5)	0.000
Bi5	0.0493 (10)	0.0245 (9)	0.0187 (8)	0.000	−0.0097 (7)	0.000
Bi6	0.0351 (9)	0.0383 (9)	0.0217 (8)	0.000	0.0122 (6)	0.000
Br1	0.016 (2)	0.009 (2)	0.021 (3)	0.000	0.0009 (19)	0.000
Br2	0.0213 (18)	0.0160 (16)	0.0196 (19)	0.000	0.0004 (14)	0.000
Br3	0.026 (2)	0.0184 (18)	0.026 (2)	0.000	0.0012 (16)	0.000

Geometric parameters (Å, º) top

Bi1—O1	2.30 (3)	Bi3—O3ⁱⁱⁱ	2.254 (11)
Bi1—O1ⁱ	2.61 (2)	Bi3—O4	2.207 (19)
Bi1—O2	2.645 (19)	Bi4—Br1^ix	3.4330 (18)
Bi1—O5ⁱⁱ	2.463 (13)	Bi4—Br1^x	3.4330 (18)
Bi1—O5ⁱⁱⁱ	2.463 (13)	Bi4—Br2ⁱⁱⁱ	3.479 (3)
Bi1—O6^iv	2.654 (16)	Bi4—Br2ⁱⁱ	3.479 (3)
Bi1—O6^v	2.654 (16)	Bi4—O2ⁱⁱ	2.266 (10)
Bi1—O8^vi	2.63 (7)	Bi4—O2ⁱⁱⁱ	2.266 (10)
Bi1—O8^vii	2.63 (7)	Bi4—O4	2.27 (2)
Bi1—O8A^viii	2.70 (6)	Bi4—O5	2.18 (2)
Bi1—O8A^iv	2.70 (6)	Bi4—O7^xi	3.15 (5)
Bi1—O9^iv	2.8039 (17)	Bi5—Br1^x	3.578 (2)
Bi2—Br3ⁱⁱ	3.316 (4)	Bi5—Br1^ix	3.578 (2)
Bi2—Br3ⁱⁱⁱ	3.316 (4)	Bi5—Br2^ix	3.470 (4)
Bi2—O2	2.20 (2)	Bi5—Br2^x	3.470 (4)
Bi2—O3	2.68 (2)	Bi5—O1ⁱⁱ	2.240 (12)
Bi2—O4ⁱⁱ	2.459 (12)	Bi5—O1ⁱⁱⁱ	2.240 (12)
Bi2—O4ⁱⁱⁱ	2.459 (12)	Bi5—O5	2.35 (2)
Bi2—O7^iv	2.43 (2)	Bi5—O6	2.19 (2)
Bi2—O7^v	2.43 (2)	Bi5—O9	2.473 (2)
Bi2—O8^vii	2.12 (7)	Bi6—Br3^ix	3.473 (4)
Bi2—O8^vi	2.12 (7)	Bi6—Br3^x	3.473 (4)
Bi2—O8A^iv	2.52 (5)	Bi6—O6	2.08 (2)
Bi2—O8A^viii	2.52 (5)	Bi6—O7	2.24 (5)
Bi3—Br2ⁱⁱ	3.423 (3)	Bi6—O8^xii	2.04 (7)
Bi3—Br2ⁱⁱⁱ	3.423 (3)	Bi6—O8^xiii	2.04 (7)
Bi3—Br3ⁱⁱⁱ	3.412 (3)	Bi6—O8^xiv	3.21 (8)
Bi3—Br3ⁱⁱ	3.412 (3)	Bi6—O8^xv	3.21 (8)
Bi3—Bi3ⁱⁱⁱ	3.600 (3)	Bi6—O8A	2.04 (8)
Bi3—Bi3ⁱⁱ	3.600 (3)	Bi6—O8A^xvi	2.04 (8)
Bi3—O3	2.20 (2)	Bi6—O8A^xiii	2.43 (8)
Bi3—O3ⁱⁱ	2.254 (11)	Bi6—O8A^xii	2.43 (8)

O1—Bi1—O5ⁱⁱ	73.4 (6)	O5—Bi5—Br1^ix	74.7 (4)
O1—Bi1—O5ⁱⁱⁱ	73.4 (6)	O9—Bi5—Br1^ix	127.61 (5)
O5ⁱⁱ—Bi1—O5ⁱⁱⁱ	108.8 (8)	Br2^ix—Bi5—Br1^ix	67.77 (6)
O1—Bi1—O1ⁱ	74.0 (9)	Br2^x—Bi5—Br1^ix	105.52 (8)
O5ⁱⁱ—Bi1—O1ⁱ	114.1 (5)	Br1^x—Bi5—Br1^ix	68.06 (5)
O5ⁱⁱⁱ—Bi1—O1ⁱ	114.1 (5)	O8^xii—Bi6—O8^xiii	75 (4)
O1—Bi1—O8^vi	158.9 (17)	O8^xii—Bi6—O8A	24 (2)
O5ⁱⁱ—Bi1—O8^vi	85.6 (17)	O8^xiii—Bi6—O8A	99 (3)
O5ⁱⁱⁱ—Bi1—O8^vi	113.3 (16)	O8^xii—Bi6—O8A^xvi	99 (3)
O1ⁱ—Bi1—O8^vi	117.4 (17)	O8^xiii—Bi6—O8A^xvi	24 (2)
O1—Bi1—O8^vii	158.9 (17)	O8A—Bi6—O8A^xvi	122 (4)
O5ⁱⁱ—Bi1—O8^vii	113.3 (16)	O8^xii—Bi6—O6	80 (2)
O5ⁱⁱⁱ—Bi1—O8^vii	85.6 (17)	O8^xiii—Bi6—O6	80 (2)
O1ⁱ—Bi1—O8^vii	117.4 (17)	O8A—Bi6—O6	83.2 (15)
O8^vi—Bi1—O8^vii	34 (3)	O8A^xvi—Bi6—O6	83.2 (15)
O1—Bi1—O2	107.4 (8)	O8^xii—Bi6—O7	38 (2)
O5ⁱⁱ—Bi1—O2	66.5 (5)	O8^xiii—Bi6—O7	38 (2)
O5ⁱⁱⁱ—Bi1—O2	66.5 (5)	O8A—Bi6—O7	61.5 (18)
O1ⁱ—Bi1—O2	178.6 (7)	O8A^xvi—Bi6—O7	61.5 (18)
O8^vi—Bi1—O2	61.2 (16)	O6—Bi6—O7	84.0 (13)
O8^vii—Bi1—O2	61.2 (16)	O8^xii—Bi6—O8A^xiii	29 (2)
O1—Bi1—O6^iv	114.4 (6)	O8^xiii—Bi6—O8A^xiii	104 (3)
O5ⁱⁱ—Bi1—O6^iv	172.0 (7)	O8A—Bi6—O8A^xiii	5 (2)
O5ⁱⁱⁱ—Bi1—O6^iv	76.3 (6)	O8A^xvi—Bi6—O8A^xiii	127 (3)
O1ⁱ—Bi1—O6^iv	67.9 (6)	O6—Bi6—O8A^xiii	84.3 (13)
O8^vi—Bi1—O6^iv	86.7 (17)	O7—Bi6—O8A^xiii	66.4 (15)
O8^vii—Bi1—O6^iv	60.2 (16)	O8^xii—Bi6—O8A^xii	104 (3)
O2—Bi1—O6^iv	111.3 (5)	O8^xiii—Bi6—O8A^xii	29 (2)
O1—Bi1—O6^v	114.4 (6)	O8A—Bi6—O8A^xii	127 (3)
O5ⁱⁱ—Bi1—O6^v	76.3 (6)	O8A^xvi—Bi6—O8A^xii	5 (2)
O5ⁱⁱⁱ—Bi1—O6^v	172.0 (7)	O6—Bi6—O8A^xii	84.3 (13)
O1ⁱ—Bi1—O6^v	67.9 (6)	O7—Bi6—O8A^xii	66.4 (14)
O8^vi—Bi1—O6^v	60.2 (16)	O8A^xiii—Bi6—O8A^xii	132 (3)
O8^vii—Bi1—O6^v	86.7 (17)	O8^xii—Bi6—O8^xiv	22 (2)
O2—Bi1—O6^v	111.3 (5)	O8^xiii—Bi6—O8^xiv	97 (3)
O6^iv—Bi1—O6^v	98.0 (8)	O8A—Bi6—O8^xiv	2 (2)
O1—Bi1—O8A^viii	175.3 (18)	O8A^xvi—Bi6—O8^xiv	121 (2)
O5ⁱⁱ—Bi1—O8A^viii	103.1 (17)	O6—Bi6—O8^xiv	83.7 (13)
O5ⁱⁱⁱ—Bi1—O8A^viii	110.9 (17)	O7—Bi6—O8^xiv	59.9 (13)
O1ⁱ—Bi1—O8A^viii	105.2 (13)	O8A^xiii—Bi6—O8^xiv	7 (2)
O8^vi—Bi1—O8A^viii	18.1 (19)	O8A^xii—Bi6—O8^xiv	125.9 (18)
O8^vii—Bi1—O8A^viii	25 (2)	O8^xii—Bi6—O8^xv	97 (3)
O2—Bi1—O8A^viii	73.4 (12)	O8^xiii—Bi6—O8^xv	22 (2)
O6^iv—Bi1—O8A^viii	69.0 (17)	O8A—Bi6—O8^xv	121 (2)
O6^v—Bi1—O8A^viii	61.4 (17)	O8A^xvi—Bi6—O8^xv	2 (2)
O1—Bi1—O8A^iv	175.3 (18)	O6—Bi6—O8^xv	83.7 (13)
O5ⁱⁱ—Bi1—O8A^iv	110.9 (17)	O7—Bi6—O8^xv	59.9 (13)
O5ⁱⁱⁱ—Bi1—O8A^iv	103.1 (17)	O8A^xiii—Bi6—O8^xv	125.9 (17)
O1ⁱ—Bi1—O8A^iv	105.2 (13)	O8A^xii—Bi6—O8^xv	7 (2)
O8^vi—Bi1—O8A^iv	25 (2)	O8^xiv—Bi6—O8^xv	119 (3)
O8^vii—Bi1—O8A^iv	18.1 (19)	O8^xii—Bi6—Br3^ix	91 (2)
O2—Bi1—O8A^iv	73.4 (12)	O8^xiii—Bi6—Br3^ix	135.5 (19)
O6^iv—Bi1—O8A^iv	61.4 (17)	O8A—Bi6—Br3^ix	74.0 (17)
O6^v—Bi1—O8A^iv	69.0 (17)	O8A^xvi—Bi6—Br3^ix	137.4 (15)
O8A^viii—Bi1—O8A^iv	9 (4)	O6—Bi6—Br3^ix	139.4 (3)
O1—Bi1—O9^iv	57.4 (3)	O7—Bi6—Br3^ix	112.2 (9)
O5ⁱⁱ—Bi1—O9^iv	130.8 (5)	O8A^xiii—Bi6—Br3^ix	70.5 (14)
O5ⁱⁱⁱ—Bi1—O9^iv	59.5 (4)	O8A^xii—Bi6—Br3^ix	136.1 (13)
O1ⁱ—Bi1—O9^iv	54.7 (3)	O8^xiv—Bi6—Br3^ix	74.5 (14)
O8^vi—Bi1—O9^iv	143.6 (17)	O8^xv—Bi6—Br3^ix	136.8 (13)
O8^vii—Bi1—O9^iv	112.9 (16)	O8^xii—Bi6—Br3^x	135.5 (19)
O2—Bi1—O9^iv	126.0 (2)	O8^xiii—Bi6—Br3^x	91 (2)
O6^iv—Bi1—O9^iv	57.0 (5)	O8A—Bi6—Br3^x	137.4 (15)
O6^v—Bi1—O9^iv	122.2 (4)	O8A^xvi—Bi6—Br3^x	74.0 (17)
O8A^viii—Bi1—O9^iv	126.0 (16)	O6—Bi6—Br3^x	139.4 (3)
O8A^iv—Bi1—O9^iv	118.3 (16)	O7—Bi6—Br3^x	112.2 (9)
O8^vii—Bi2—O8^vi	42 (4)	O8A^xiii—Bi6—Br3^x	136.1 (13)
O8^vii—Bi2—O2	77 (2)	O8A^xii—Bi6—Br3^x	70.5 (14)
O8^vi—Bi2—O2	77 (2)	O8^xiv—Bi6—Br3^x	136.8 (13)
O8^vii—Bi2—O7^iv	35 (2)	O8^xv—Bi6—Br3^x	74.5 (14)
O8^vi—Bi2—O7^iv	77 (2)	Br3^ix—Bi6—Br3^x	70.42 (9)
O2—Bi2—O7^iv	77.5 (11)	Bi4^xvii—Br1—Bi4^xviii	71.37 (5)
O8^vii—Bi2—O7^v	77 (2)	Bi4^xvii—Br1—Bi4ⁱⁱ	180.00 (5)
O8^vi—Bi2—O7^v	35 (2)	Bi4^xviii—Br1—Bi4ⁱⁱ	108.63 (5)
O2—Bi2—O7^v	77.5 (11)	Bi4^xvii—Br1—Bi4ⁱⁱⁱ	108.63 (5)
O7^iv—Bi2—O7^v	111.3 (16)	Bi4^xviii—Br1—Bi4ⁱⁱⁱ	180.00 (3)
O8^vii—Bi2—O4ⁱⁱ	133 (2)	Bi4ⁱⁱ—Br1—Bi4ⁱⁱⁱ	71.37 (5)
O8^vi—Bi2—O4ⁱⁱ	95 (2)	Bi4^xvii—Br1—Bi5ⁱⁱⁱ	72.57 (5)
O2—Bi2—O4ⁱⁱ	72.6 (5)	Bi4^xviii—Br1—Bi5ⁱⁱⁱ	110.69 (4)
O7^iv—Bi2—O4ⁱⁱ	150.2 (12)	Bi4ⁱⁱ—Br1—Bi5ⁱⁱⁱ	107.43 (5)
O7^v—Bi2—O4ⁱⁱ	61.5 (10)	Bi4ⁱⁱⁱ—Br1—Bi5ⁱⁱⁱ	69.31 (4)
O8^vii—Bi2—O4ⁱⁱⁱ	95 (2)	Bi4^xvii—Br1—Bi5^xviii	107.43 (5)
O8^vi—Bi2—O4ⁱⁱⁱ	133 (2)	Bi4^xviii—Br1—Bi5^xviii	69.31 (4)
O2—Bi2—O4ⁱⁱⁱ	72.6 (5)	Bi4ⁱⁱ—Br1—Bi5^xviii	72.57 (5)
O7^iv—Bi2—O4ⁱⁱⁱ	61.5 (10)	Bi4ⁱⁱⁱ—Br1—Bi5^xviii	110.69 (4)
O7^v—Bi2—O4ⁱⁱⁱ	150.2 (12)	Bi5ⁱⁱⁱ—Br1—Bi5^xviii	180.00 (4)
O4ⁱⁱ—Bi2—O4ⁱⁱⁱ	109.0 (8)	Bi4^xvii—Br1—Bi5ⁱⁱ	110.69 (4)
O8^vii—Bi2—O8A^iv	18 (3)	Bi4^xviii—Br1—Bi5ⁱⁱ	72.57 (5)
O8^vi—Bi2—O8A^iv	28 (3)	Bi4ⁱⁱ—Br1—Bi5ⁱⁱ	69.31 (4)
O2—Bi2—O8A^iv	84.8 (14)	Bi4ⁱⁱⁱ—Br1—Bi5ⁱⁱ	107.43 (5)
O7^iv—Bi2—O8A^iv	53 (2)	Bi5ⁱⁱⁱ—Br1—Bi5ⁱⁱ	68.06 (5)
O7^v—Bi2—O8A^iv	62 (2)	Bi5^xviii—Br1—Bi5ⁱⁱ	111.94 (5)
O4ⁱⁱ—Bi2—O8A^iv	122.5 (19)	Bi4^xvii—Br1—Bi5^xvii	69.31 (4)
O4ⁱⁱⁱ—Bi2—O8A^iv	113.4 (19)	Bi4^xviii—Br1—Bi5^xvii	107.43 (5)
O8^vii—Bi2—O8A^viii	28 (3)	Bi4ⁱⁱ—Br1—Bi5^xvii	110.69 (4)
O8^vi—Bi2—O8A^viii	18 (3)	Bi4ⁱⁱⁱ—Br1—Bi5^xvii	72.57 (5)
O2—Bi2—O8A^viii	84.8 (14)	Bi5ⁱⁱⁱ—Br1—Bi5^xvii	111.94 (5)
O7^iv—Bi2—O8A^viii	62 (2)	Bi5^xviii—Br1—Bi5^xvii	68.06 (5)
O7^v—Bi2—O8A^viii	53 (2)	Bi5ⁱⁱ—Br1—Bi5^xvii	180.00 (4)
O4ⁱⁱ—Bi2—O8A^viii	113.4 (19)	Bi3ⁱⁱ—Br2—Bi3ⁱⁱⁱ	71.61 (9)
O4ⁱⁱⁱ—Bi2—O8A^viii	122.5 (19)	Bi3ⁱⁱ—Br2—Bi5^xvii	177.71 (11)
O8A^iv—Bi2—O8A^viii	10 (4)	Bi3ⁱⁱⁱ—Br2—Bi5^xvii	108.91 (5)
O8^vii—Bi2—O3	159 (2)	Bi3ⁱⁱ—Br2—Bi5^xviii	108.91 (5)
O8^vi—Bi2—O3	159 (2)	Bi3ⁱⁱⁱ—Br2—Bi5^xviii	177.71 (11)
O2—Bi2—O3	107.0 (8)	Bi5^xvii—Br2—Bi5^xviii	70.49 (9)
O7^iv—Bi2—O3	124.2 (8)	Bi3ⁱⁱ—Br2—Bi4ⁱⁱⁱ	108.84 (10)
O7^v—Bi2—O3	124.2 (8)	Bi3ⁱⁱⁱ—Br2—Bi4ⁱⁱⁱ	69.48 (6)
O4ⁱⁱ—Bi2—O3	67.1 (5)	Bi5^xvii—Br2—Bi4ⁱⁱⁱ	73.35 (6)
O4ⁱⁱⁱ—Bi2—O3	67.1 (5)	Bi5^xviii—Br2—Bi4ⁱⁱⁱ	112.20 (10)
O8A^iv—Bi2—O3	167.2 (15)	Bi3ⁱⁱ—Br2—Bi4ⁱⁱ	69.48 (6)
O8A^viii—Bi2—O3	167.2 (14)	Bi3ⁱⁱⁱ—Br2—Bi4ⁱⁱ	108.84 (10)
O8^vii—Bi2—Br3ⁱⁱ	113 (2)	Bi5^xvii—Br2—Bi4ⁱⁱ	112.20 (10)
O8^vi—Bi2—Br3ⁱⁱ	87 (2)	Bi5^xviii—Br2—Bi4ⁱⁱ	73.35 (6)
O2—Bi2—Br3ⁱⁱ	142.84 (5)	Bi4ⁱⁱⁱ—Br2—Bi4ⁱⁱ	70.28 (8)
O7^iv—Bi2—Br3ⁱⁱ	131.6 (11)	Bi3ⁱⁱ—Br2—Bi6^xviii	70.52 (6)
O7^v—Bi2—Br3ⁱⁱ	70.5 (10)	Bi3ⁱⁱⁱ—Br2—Bi6^xviii	109.83 (10)
O4ⁱⁱ—Bi2—Br3ⁱⁱ	75.6 (5)	Bi5^xvii—Br2—Bi6^xviii	107.28 (10)
O4ⁱⁱⁱ—Bi2—Br3ⁱⁱ	137.4 (5)	Bi5^xviii—Br2—Bi6^xviii	68.50 (6)
O8A^iv—Bi2—Br3ⁱⁱ	96.4 (16)	Bi4ⁱⁱⁱ—Br2—Bi6^xviii	179.23 (12)
O8A^viii—Bi2—Br3ⁱⁱ	90.5 (15)	Bi4ⁱⁱ—Br2—Bi6^xviii	109.75 (5)
O3—Bi2—Br3ⁱⁱ	77.2 (4)	Bi3ⁱⁱ—Br2—Bi6^xvii	109.83 (10)
O8^vii—Bi2—Br3ⁱⁱⁱ	87 (2)	Bi3ⁱⁱⁱ—Br2—Bi6^xvii	70.52 (6)
O8^vi—Bi2—Br3ⁱⁱⁱ	113 (2)	Bi5^xvii—Br2—Bi6^xvii	68.50 (6)
O2—Bi2—Br3ⁱⁱⁱ	142.84 (5)	Bi5^xviii—Br2—Bi6^xvii	107.28 (10)
O7^iv—Bi2—Br3ⁱⁱⁱ	70.5 (10)	Bi4ⁱⁱⁱ—Br2—Bi6^xvii	109.75 (5)
O7^v—Bi2—Br3ⁱⁱⁱ	131.6 (11)	Bi4ⁱⁱ—Br2—Bi6^xvii	179.23 (12)
O4ⁱⁱ—Bi2—Br3ⁱⁱⁱ	137.4 (5)	Bi6^xviii—Br2—Bi6^xvii	70.20 (8)
O4ⁱⁱⁱ—Bi2—Br3ⁱⁱⁱ	75.6 (5)	Bi3ⁱⁱ—Br2—O6^xviii	96.9 (3)
O8A^iv—Bi2—Br3ⁱⁱⁱ	90.5 (15)	Bi3ⁱⁱⁱ—Br2—O6^xviii	141.6 (4)
O8A^viii—Bi2—Br3ⁱⁱⁱ	96.4 (16)	Bi5^xvii—Br2—O6^xviii	81.3 (3)
O3—Bi2—Br3ⁱⁱⁱ	77.2 (4)	Bi5^xviii—Br2—O6^xviii	36.4 (3)
Br3ⁱⁱ—Bi2—Br3ⁱⁱⁱ	74.31 (10)	Bi4ⁱⁱⁱ—Br2—O6^xviii	146.3 (4)
O3—Bi3—O4	114.2 (8)	Bi4ⁱⁱ—Br2—O6^xviii	100.3 (3)
O3—Bi3—O3ⁱⁱ	72.1 (6)	Bi6^xviii—Br2—O6^xviii	34.5 (4)
O4—Bi3—O3ⁱⁱ	79.4 (6)	Bi6^xvii—Br2—O6^xviii	80.0 (3)
O3—Bi3—O3ⁱⁱⁱ	72.1 (6)	Bi3ⁱⁱ—Br2—O6^xvii	141.6 (4)
O4—Bi3—O3ⁱⁱⁱ	79.4 (6)	Bi3ⁱⁱⁱ—Br2—O6^xvii	96.9 (3)
O3ⁱⁱ—Bi3—O3ⁱⁱⁱ	125.4 (11)	Bi5^xvii—Br2—O6^xvii	36.4 (3)
O3—Bi3—Br3ⁱⁱⁱ	81.5 (4)	Bi5^xviii—Br2—O6^xvii	81.3 (3)
O4—Bi3—Br3ⁱⁱⁱ	141.87 (18)	Bi4ⁱⁱⁱ—Br2—O6^xvii	100.3 (3)
O3ⁱⁱ—Bi3—Br3ⁱⁱⁱ	138.3 (5)	Bi4ⁱⁱ—Br2—O6^xvii	146.3 (4)
O3ⁱⁱⁱ—Bi3—Br3ⁱⁱⁱ	72.8 (5)	Bi6^xviii—Br2—O6^xvii	80.0 (3)
O3—Bi3—Br3ⁱⁱ	81.5 (4)	Bi6^xvii—Br2—O6^xvii	34.5 (4)
O4—Bi3—Br3ⁱⁱ	141.87 (18)	Bi2ⁱⁱ—Br3—Bi2ⁱⁱⁱ	74.31 (10)
O3ⁱⁱ—Bi3—Br3ⁱⁱ	72.8 (5)	Bi2ⁱⁱ—Br3—O7^xi	42.4 (3)
O3ⁱⁱⁱ—Bi3—Br3ⁱⁱ	138.3 (5)	Bi2ⁱⁱⁱ—Br3—O7^xi	42.4 (3)
Br3ⁱⁱⁱ—Bi3—Br3ⁱⁱ	71.89 (9)	Bi2ⁱⁱ—Br3—Bi3ⁱⁱⁱ	115.05 (12)
O3—Bi3—Br2ⁱⁱ	143.11 (13)	Bi2ⁱⁱⁱ—Br3—Bi3ⁱⁱⁱ	73.40 (7)
O4—Bi3—Br2ⁱⁱ	78.1 (5)	Bi2ⁱⁱ—Br3—Bi3ⁱⁱ	73.40 (7)
O3ⁱⁱ—Bi3—Br2ⁱⁱ	76.8 (6)	Bi2ⁱⁱⁱ—Br3—Bi3ⁱⁱ	115.05 (12)
O3ⁱⁱⁱ—Bi3—Br2ⁱⁱ	144.3 (6)	Bi3ⁱⁱⁱ—Br3—Bi3ⁱⁱ	71.89 (9)
Br3ⁱⁱⁱ—Bi3—Br2ⁱⁱ	110.78 (10)	Bi2ⁱⁱ—Br3—Bi6^xvii	174.10 (12)
Br3ⁱⁱ—Bi3—Br2ⁱⁱ	70.61 (9)	Bi2ⁱⁱⁱ—Br3—Bi6^xvii	107.35 (5)
O3—Bi3—Br2ⁱⁱⁱ	143.11 (13)	Bi3ⁱⁱⁱ—Br3—Bi6^xvii	70.76 (7)
O4—Bi3—Br2ⁱⁱⁱ	78.1 (5)	Bi3ⁱⁱ—Br3—Bi6^xvii	110.33 (11)
O3ⁱⁱ—Bi3—Br2ⁱⁱⁱ	144.3 (6)	Bi2ⁱⁱ—Br3—Bi6^xviii	107.35 (5)
O3ⁱⁱⁱ—Bi3—Br2ⁱⁱⁱ	76.8 (6)	Bi2ⁱⁱⁱ—Br3—Bi6^xviii	174.10 (12)
Br3ⁱⁱⁱ—Bi3—Br2ⁱⁱⁱ	70.61 (9)	Bi3ⁱⁱⁱ—Br3—Bi6^xviii	110.33 (11)
Br3ⁱⁱ—Bi3—Br2ⁱⁱⁱ	110.78 (10)	Bi3ⁱⁱ—Br3—Bi6^xviii	70.76 (7)
Br2ⁱⁱ—Bi3—Br2ⁱⁱⁱ	71.61 (9)	Bi6^xvii—Br3—Bi6^xviii	70.42 (9)
O5—Bi4—O2ⁱⁱ	78.3 (5)	Bi5ⁱⁱ—O1—Bi5ⁱⁱⁱ	126.8 (12)
O5—Bi4—O2ⁱⁱⁱ	78.3 (5)	Bi5ⁱⁱ—O1—Bi1	108.1 (6)
O2ⁱⁱ—Bi4—O2ⁱⁱⁱ	124.2 (10)	Bi5ⁱⁱⁱ—O1—Bi1	108.1 (6)
O5—Bi4—O4	121.1 (8)	Bi5ⁱⁱ—O1—Bi1ⁱ	103.0 (6)
O2ⁱⁱ—Bi4—O4	75.2 (5)	Bi5ⁱⁱⁱ—O1—Bi1ⁱ	103.0 (6)
O2ⁱⁱⁱ—Bi4—O4	75.2 (5)	Bi1—O1—Bi1ⁱ	106.0 (10)
O5—Bi4—O7^xi	69.3 (10)	Bi2—O2—Bi4ⁱⁱ	109.5 (5)
O2ⁱⁱ—Bi4—O7^xi	62.2 (5)	Bi2—O2—Bi4ⁱⁱⁱ	109.5 (5)
O2ⁱⁱⁱ—Bi4—O7^xi	62.2 (5)	Bi4ⁱⁱ—O2—Bi4ⁱⁱⁱ	124.2 (9)
O4—Bi4—O7^xi	51.8 (9)	Bi2—O2—Bi1	105.8 (8)
O5—Bi4—Br1^ix	79.8 (5)	Bi4ⁱⁱ—O2—Bi1	103.0 (5)
O2ⁱⁱ—Bi4—Br1^ix	77.5 (5)	Bi4ⁱⁱⁱ—O2—Bi1	103.0 (5)
O2ⁱⁱⁱ—Bi4—Br1^ix	144.5 (5)	Bi3—O3—Bi3ⁱⁱ	107.9 (6)
O4—Bi4—Br1^ix	140.4 (2)	Bi3—O3—Bi3ⁱⁱⁱ	107.9 (6)
O7^xi—Bi4—Br1^ix	132.8 (5)	Bi3ⁱⁱ—O3—Bi3ⁱⁱⁱ	125.4 (11)
O5—Bi4—Br1^x	79.8 (5)	Bi3—O3—Bi2	110.5 (9)
O2ⁱⁱ—Bi4—Br1^x	144.5 (5)	Bi3ⁱⁱ—O3—Bi2	102.1 (6)
O2ⁱⁱⁱ—Bi4—Br1^x	77.5 (5)	Bi3ⁱⁱⁱ—O3—Bi2	102.1 (6)
O4—Bi4—Br1^x	140.4 (2)	Bi3—O3—Br3	93.1 (6)
O7^xi—Bi4—Br1^x	132.8 (5)	Bi3ⁱⁱ—O3—Br3	69.1 (5)
Br1^ix—Bi4—Br1^x	71.37 (5)	Bi3ⁱⁱⁱ—O3—Br3	69.1 (5)
O5—Bi4—Br2ⁱⁱⁱ	142.5 (2)	Bi2—O3—Br3	156.4 (9)
O2ⁱⁱ—Bi4—Br2ⁱⁱⁱ	138.9 (5)	Bi3—O4—Bi4	122.9 (9)
O2ⁱⁱⁱ—Bi4—Br2ⁱⁱⁱ	74.7 (5)	Bi3—O4—Bi2ⁱⁱ	111.1 (6)
O4—Bi4—Br2ⁱⁱⁱ	76.2 (4)	Bi4—O4—Bi2ⁱⁱ	100.8 (5)
O7^xi—Bi4—Br2ⁱⁱⁱ	117.8 (6)	Bi3—O4—Bi2ⁱⁱⁱ	111.1 (6)
Br1^ix—Bi4—Br2ⁱⁱⁱ	108.55 (7)	Bi4—O4—Bi2ⁱⁱⁱ	100.8 (5)
Br1^x—Bi4—Br2ⁱⁱⁱ	69.31 (6)	Bi2ⁱⁱ—O4—Bi2ⁱⁱⁱ	109.0 (8)
O5—Bi4—Br2ⁱⁱ	142.5 (2)	Bi4—O5—Bi5	123.4 (10)
O2ⁱⁱ—Bi4—Br2ⁱⁱ	74.7 (5)	Bi4—O5—Bi1ⁱⁱ	112.0 (6)
O2ⁱⁱⁱ—Bi4—Br2ⁱⁱ	138.9 (5)	Bi5—O5—Bi1ⁱⁱ	99.5 (6)
O4—Bi4—Br2ⁱⁱ	76.2 (4)	Bi4—O5—Bi1ⁱⁱⁱ	112.0 (6)
O7^xi—Bi4—Br2ⁱⁱ	117.8 (6)	Bi5—O5—Bi1ⁱⁱⁱ	99.5 (6)
Br1^ix—Bi4—Br2ⁱⁱ	69.31 (6)	Bi1ⁱⁱ—O5—Bi1ⁱⁱⁱ	108.8 (8)
Br1^x—Bi4—Br2ⁱⁱ	108.55 (7)	Bi6—O6—Bi1^xix	107.2 (6)
Br2ⁱⁱⁱ—Bi4—Br2ⁱⁱ	70.28 (8)	Bi5—O6—Bi1^xix	103.1 (7)
O5—Bi4—Bi2ⁱⁱⁱ	94.0 (5)	Bi6—O6—Bi1^xx	107.2 (6)
O2ⁱⁱ—Bi4—Bi2ⁱⁱⁱ	98.5 (5)	Bi5—O6—Bi1^xx	103.1 (7)
O2ⁱⁱⁱ—Bi4—Bi2ⁱⁱⁱ	34.7 (5)	Bi1^xix—O6—Bi1^xx	98.0 (8)
O4—Bi4—Bi2ⁱⁱⁱ	41.5 (3)	Bi6—O6—Br2^x	71.4 (6)
O7^xi—Bi4—Bi2ⁱⁱⁱ	41.0 (4)	Bi5—O6—Br2^x	70.2 (5)
O6—Bi5—O1ⁱⁱ	83.2 (6)	Bi1^xix—O6—Br2^x	165.2 (6)
O6—Bi5—O1ⁱⁱⁱ	83.2 (6)	Bi1^xx—O6—Br2^x	96.41 (18)
O1ⁱⁱ—Bi5—O1ⁱⁱⁱ	126.8 (12)	Bi6—O6—Br2^ix	71.4 (6)
O6—Bi5—O5	133.8 (9)	Bi5—O6—Br2^ix	70.2 (5)
O1ⁱⁱ—Bi5—O5	76.7 (6)	Bi1^xix—O6—Br2^ix	96.41 (18)
O1ⁱⁱⁱ—Bi5—O5	76.7 (6)	Bi1^xx—O6—Br2^ix	165.2 (6)
O6—Bi5—O9	67.8 (6)	Bi6—O7—Bi2^xix	114.7 (13)
O1ⁱⁱ—Bi5—O9	63.6 (6)	Bi6—O7—Bi2^xx	114.7 (13)
O1ⁱⁱⁱ—Bi5—O9	63.6 (6)	Bi2^xix—O7—Bi2^xx	111.3 (16)
O5—Bi5—O9	66.0 (5)	Bi6—O7—Bi4^xi	149.3 (19)
O6—Bi5—Br2^ix	73.4 (5)	Bi2^xix—O7—Bi4^xi	80.5 (11)
O1ⁱⁱ—Bi5—Br2^ix	77.4 (6)	Bi2^xx—O7—Bi4^xi	80.5 (11)
O1ⁱⁱⁱ—Bi5—Br2^ix	144.4 (6)	Bi6—O8A—Bi6^xxi	127 (3)
O5—Bi5—Br2^ix	138.6 (3)	Bi6—O8A—Bi2^xix	118 (3)
O9—Bi5—Br2^ix	126.87 (6)	Bi6^xxi—O8A—Bi2^xix	105 (3)
O6—Bi5—Br2^x	73.4 (5)	Bi6—O8A—Bi1^xix	107 (3)
O1ⁱⁱ—Bi5—Br2^x	144.4 (6)	Bi6^xxi—O8A—Bi1^xix	96 (2)
O1ⁱⁱⁱ—Bi5—Br2^x	77.4 (6)	Bi2^xix—O8A—Bi1^xix	95.6 (18)
O5—Bi5—Br2^x	138.6 (3)	Bi6^xxi—O8—Bi2^xxii	142 (4)
O9—Bi5—Br2^x	126.87 (6)	Bi6^xxi—O8—Bi1^xxii	109 (3)
Br2^ix—Bi5—Br2^x	70.49 (9)	Bi2^xxii—O8—Bi1^xxii	109 (3)
O6—Bi5—Br1^x	138.6 (3)	Bi6^xxi—O8—Bi6^xxiii	97 (3)
O1ⁱⁱ—Bi5—Br1^x	137.8 (6)	Bi2^xxii—O8—Bi6^xxiii	93 (2)
O1ⁱⁱⁱ—Bi5—Br1^x	74.9 (6)	Bi1^xxii—O8—Bi6^xxiii	81.3 (19)
O5—Bi5—Br1^x	74.7 (4)	Bi5—O9—Bi5^xi	180.00 (6)
O9—Bi5—Br1^x	127.61 (5)	Bi5—O9—Bi1ⁱⁱⁱ	88.06 (5)
Br2^ix—Bi5—Br1^x	105.52 (8)	Bi5^xi—O9—Bi1ⁱⁱⁱ	91.94 (5)
Br2^x—Bi5—Br1^x	67.77 (6)	Bi5—O9—Bi1ⁱⁱ	88.06 (5)
O6—Bi5—Br1^ix	138.6 (3)	Bi5^xi—O9—Bi1ⁱⁱ	91.94 (5)
O1ⁱⁱ—Bi5—Br1^ix	74.9 (6)	Bi1ⁱⁱⁱ—O9—Bi1ⁱⁱ	91.15 (7)
O1ⁱⁱⁱ—Bi5—Br1^ix	137.8 (6)

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

Experimental details

	(bi24ocl)	(bi24obr)
Crystal data
Chemical formula	Bi₂₄Cl₁₀O₃₁	Bi₂₄Br₁₀O₃₁
M_r	5866.02	6310.62
Crystal system, space group	Monoclinic, P2/c	Monoclinic, A2/m
Temperature (K)	293	293
a, b, c (Å)	10.033 (2), 7.9745 (16), 29.552 (6)	10.141 (7), 4.005 (3), 29.977 (19)
β (°)	88.742 (4)	90.197 (12)
V (Å³)	2363.8 (8)	1217.5 (14)
Z	2	1
Radiation type	Mo Kα	Mo Kα
µ (mm⁻¹)	89.60	94.64
Crystal size (mm)	0.22 × 0.02 × 0.01	0.25 × 0.04 × 0.02

Data collection
Diffractometer	CCD area detector diffractometer	CCD area detector diffractometer
Absorption correction	Integration XPREP / Bruker SHELXTL	Integration XPREP / Bruker SHELXTL
T_min, T_max	0.029, 0.404	0.020, 0.269
No. of measured, independent and observed [I > 2σ(I)] reflections	15924, 5546, 3184	8153, 1627, 882
R_int	0.130	0.128
(sin θ/λ)_max (Å⁻¹)	0.668	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.063, 0.146, 0.90	0.064, 0.186, 0.91
No. of reflections	5546	1627
No. of parameters	218	84
Δρ_max, Δρ_min (e Å⁻³)	5.98, −6.16	6.08, −5.92

Computer programs: Bruker SMART, Bruker SHELXTL, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SCHAKAL 97 (Keller 1997), SCHAKAL 97 (Keller, 1997).

Selected bond lengths (Å) for (bi24ocl) top

Bi1—O1	2.398 (17)	Bi4—O2ⁱⁱ	2.270 (16)
Bi1—O1ⁱ	2.726 (19)	Bi4—O2Aⁱⁱⁱ	2.266 (16)
Bi1—O2	2.538 (19)	Bi4—O4	2.368 (17)
Bi1—O5ⁱⁱ	2.656 (17)	Bi4—O5	2.13 (2)
Bi1—O5Aⁱⁱⁱ	2.240 (17)	Bi4A—Cl1ⁱⁱⁱ	3.473 (6)
Bi1—O6^iv	2.741 (17)	Bi4A—Cl1Aⁱⁱⁱ	3.400 (5)
Bi1—O6A^v	2.492 (19)	Bi4A—Cl2ⁱⁱⁱ	3.427 (8)
Bi1—O8^v	2.46 (2)	Bi4A—Cl2Aⁱⁱⁱ	3.440 (8)
Bi1A—O1A	2.264 (17)	Bi4A—O2ⁱⁱⁱ	2.289 (16)
Bi1A—O1Aⁱ	2.50 (2)	Bi4A—O2Aⁱⁱⁱ	2.261 (15)
Bi1A—O2A	2.763 (18)	Bi4A—O4A	2.207 (17)
Bi1A—O5ⁱⁱⁱ	2.303 (18)	Bi4A—O5A	2.16 (2)
Bi1A—O5Aⁱⁱⁱ	2.673 (17)	Bi5—Cl1ⁱⁱ	3.560 (5)
Bi1A—O6^v	2.469 (17)	Bi5—Cl1Aⁱⁱⁱ	3.754 (5)
Bi1A—O6A^v	2.898 (18)	Bi5—Cl2^vi	3.385 (7)
Bi1A—O8A^v	2.891 (16)	Bi5—Cl2A^vii	3.586 (7)
Bi1A—O9ⁱⁱⁱ	2.419 (16)	Bi5—O1ⁱⁱ	2.214 (16)
Bi2—Cl3ⁱⁱ	3.247 (7)	Bi5—O1Aⁱⁱⁱ	2.479 (18)
Bi2—Cl3Aⁱⁱⁱ	3.222 (7)	Bi5—O5	2.322 (18)
Bi2—O2	2.235 (16)	Bi5—O6	2.254 (19)
Bi2—O3	2.707 (19)	Bi5—O9	2.300 (4)
Bi2—O4ⁱⁱ	2.511 (17)	Bi5A—Cl1ⁱⁱⁱ	3.470 (6)
Bi2—O4Aⁱⁱⁱ	2.488 (17)	Bi5A—Cl1Aⁱⁱⁱ	3.439 (5)
Bi2—O7^iv	2.267 (18)	Bi5A—Cl2^vii	3.316 (7)
Bi2—O8^v	2.21 (2)	Bi5A—Cl2A^vii	3.320 (6)
Bi2A—Cl3ⁱⁱⁱ	3.152 (7)	Bi5A—O1ⁱⁱⁱ	2.149 (17)
Bi2A—Cl3Aⁱⁱⁱ	3.315 (7)	Bi5A—O1Aⁱⁱⁱ	2.142 (18)
Bi2A—O2A	2.190 (16)	Bi5A—O6A	2.17 (2)
Bi2A—O3A	2.569 (19)	Bi5A—O5A	2.476 (17)
Bi2A—O4ⁱⁱⁱ	2.256 (17)	Bi6—O6	2.070 (17)
Bi2A—O4Aⁱⁱⁱ	2.583 (17)	Bi6—O7	2.09 (2)
Bi2A—O7^v	2.275 (18)	Bi6—O8A	2.128 (16)
Bi2A—O8A^v	2.581 (18)	Bi6—Cl3A^vii	3.269 (7)
Bi3—Cl2ⁱⁱ	3.320 (7)	Bi6—Cl3^vi	3.436 (7)
Bi3—Cl2Aⁱⁱⁱ	3.307 (6)	Bi6—Cl2A^vii	3.438 (8)
Bi3—Cl3ⁱⁱ	3.284 (9)	Bi6—Cl2^vi	3.773 (8)
Bi3—Cl3Aⁱⁱⁱ	3.292 (8)	Bi6A—Cl2^vii	3.390 (8)
Bi3—O3	2.201 (17)	Bi6A—Cl2A^vii	3.292 (8)
Bi3—O3ⁱⁱ	2.244 (17)	Bi6A—Cl3^vii	3.313 (7)
Bi3—O3Aⁱⁱⁱ	2.304 (16)	Bi6A—Cl3A^vii	3.373 (7)
Bi3—O4	2.171 (19)	Bi6A—O8	2.07 (2)
Bi3A—Cl2ⁱⁱⁱ	3.339 (7)	Bi6A—O8A	2.102 (16)
Bi3A—Cl2Aⁱⁱⁱ	3.312 (7)	Bi6A—O6A	2.107 (18)
Bi3A—Cl3ⁱⁱⁱ	3.370 (9)	O1—O6Aⁱⁱⁱ	2.67 (2)
Bi3A—Cl3Aⁱⁱⁱ	3.327 (8)	O1A—O9ⁱⁱⁱ	2.52 (3)
Bi3A—O3ⁱⁱⁱ	2.247 (17)	O3—O3ⁱⁱ	2.61 (3)
Bi3A—O3A	2.227 (16)	O3—O3Aⁱⁱⁱ	2.66 (2)
Bi3A—O3Aⁱⁱⁱ	2.248 (16)	O4—O7^viii	2.59 (3)
Bi3A—O4A	2.21 (2)	O5—O9	2.68 (2)
Bi4—Cl1ⁱⁱ	3.240 (6)	O6—O9	2.690 (17)
Bi4—Cl1Aⁱⁱⁱ	3.276 (5)	O6A—O8	2.66 (3)
Bi4—Cl2ⁱⁱ	3.362 (8)	O7—O8A	2.58 (2)
Bi4—Cl2Aⁱⁱⁱ	3.447 (8)

Selected bond lengths (Å) for (bi24obr) top

Bi1—O1	2.30 (3)	Bi3—O3ⁱⁱ	2.254 (11)
Bi1—O1ⁱ	2.61 (2)	Bi3—O4	2.207 (19)
Bi1—O2	2.645 (19)	Bi4—Br1^viii	3.4330 (18)
Bi1—O5ⁱⁱ	2.463 (13)	Bi4—Br2^vii	3.479 (3)
Bi1—O6ⁱⁱⁱ	2.654 (16)	Bi4—O2ⁱⁱ	2.266 (10)
Bi1—O8^iv	2.63 (7)	Bi4—O4	2.27 (2)
Bi1—O8A^v	2.70 (6)	Bi4—O5	2.18 (2)
Bi1—O9ⁱⁱⁱ	2.8039 (17)	Bi5—Br1^viii	3.578 (2)
Bi2—Br3ⁱⁱ	3.316 (4)	Bi5—Br2^ix	3.470 (4)
Bi2—O2	2.20 (2)	Bi5—O1ⁱⁱ	2.240 (12)
Bi2—O3	2.68 (2)	Bi5—O5	2.35 (2)
Bi2—O4ⁱⁱ	2.459 (12)	Bi5—O6	2.19 (2)
Bi2—O7ⁱⁱⁱ	2.43 (2)	Bi5—O9	2.473 (2)
Bi2—O8^vi	2.12 (7)	Bi6—Br3^ix	3.473 (4)
Bi2—O8Aⁱⁱⁱ	2.52 (5)	Bi6—O6	2.08 (2)
Bi3—Br2ⁱⁱ	3.423 (3)	Bi6—O7	2.24 (5)
Bi3—Br3^vii	3.412 (3)	Bi6—O8^x	2.04 (7)
Bi3—Bi3^vii	3.600 (3)	Bi6—O8A	2.04 (8)
Bi3—O3	2.20 (2)	Bi6—O8A^x	2.43 (8)

Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y+1/2, −z+1/2; (iii) x−1, y−1/2, z−1/2; (iv) x−1, −y+3/2, z−1/2; (v) x−1, −y+1/2, z−1/2; (vi) x−1, y−3/2, z−1/2; (vii) −x+1, −y−1/2, −z+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) x, −y+1, z.

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