Download citation
Download citation
link to html
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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100000550/jz0008sup1.cif
Contains datablocks bi24ocl, bi24obr, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100000550/jz0008bi24oclsup2.hkl
Contains datablock bi24ocl

hkl

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
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
(bi24ocl) top
Crystal data top
Bi24Cl10O31F(000) = 4820
Mr = 5866.02Dx = 8.242 Mg m3
Monoclinic, P2/cMo Kα radiation, λ = 0.71073 Å
a = 10.033 (2) ÅCell parameters from 15924 reflections
b = 7.9745 (16) Åθ = 1.4–28.3°
c = 29.552 (6) ŵ = 89.60 mm1
β = 88.742 (4)°T = 293 K
V = 2363.8 (8) Å3Needle, pale green
Z = 20.22 × 0.02 × 0.01 mm
Data collection top
CCD area detector
diffractometer
5546 independent reflections
Radiation source: fine-focus sealed tube3184 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.130
phi and ω scansθmax = 28.3°, θmin = 1.4°
Absorption correction: integration
XPREP / Bruker SHELXTL
h = 1313
Tmin = 0.029, Tmax = 0.404k = 100
15924 measured reflectionsl = 039
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.063 w = 1/[σ2(Fo2) + (0.0599P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.146(Δ/σ)max = 0.001
S = 0.90Δρmax = 5.98 e Å3
5546 reflectionsΔρmin = 6.16 e Å3
218 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.000152 (8)
Crystal data top
Bi24Cl10O31V = 2363.8 (8) Å3
Mr = 5866.02Z = 2
Monoclinic, P2/cMo Kα radiation
a = 10.033 (2) ŵ = 89.60 mm1
b = 7.9745 (16) ÅT = 293 K
c = 29.552 (6) Å0.22 × 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)
Tmin = 0.029, Tmax = 0.404Rint = 0.130
15924 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.063218 parameters
wR(F2) = 0.1460 restraints
S = 0.90Δρmax = 5.98 e Å3
5546 reflectionsΔρmin = 6.16 e Å3
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
xyzUiso*/Ueq
Bi10.08954 (12)0.15098 (13)0.31393 (4)0.0160 (3)
Bi1A0.07898 (12)0.65569 (13)0.30449 (3)0.0142 (3)
Bi20.24586 (11)0.11927 (12)0.42714 (3)0.0108 (2)
Bi2A0.25409 (11)0.65391 (13)0.42667 (3)0.0119 (3)
Bi30.42866 (11)0.12419 (11)0.54524 (3)0.0091 (2)
Bi3A0.43899 (11)0.62388 (11)0.54670 (3)0.0092 (2)
Bi40.59455 (11)0.12297 (12)0.66644 (3)0.0094 (2)
Bi4A0.60071 (11)0.61913 (12)0.66265 (3)0.0089 (2)
Bi50.79200 (12)0.10376 (13)0.78250 (3)0.0129 (2)
Bi5A0.75409 (11)0.62361 (11)0.78521 (3)0.0105 (2)
Bi60.93266 (12)0.15522 (12)0.90838 (3)0.0132 (3)
Bi6A0.90338 (12)0.62165 (11)0.90284 (3)0.0114 (2)
Cl10.50000.1151 (13)0.25000.024 (2)
Cl1A0.50000.6313 (11)0.25000.017 (2)
Cl20.6551 (8)0.1233 (8)0.3684 (2)0.0234 (18)
Cl2A0.6619 (8)0.6269 (8)0.3700 (2)0.0213 (18)
Cl30.8110 (9)0.1264 (9)0.4870 (2)0.027 (2)
Cl3A0.8037 (9)0.6202 (8)0.4909 (2)0.0229 (18)
O10.1392 (19)0.153 (2)0.2342 (6)0.011 (4)*
O1A0.140 (2)0.602 (2)0.2317 (6)0.016 (4)*
O20.3093 (19)0.1240 (19)0.3542 (5)0.008 (4)*
O2A0.3074 (18)0.6324 (18)0.3546 (5)0.007 (4)*
O30.4777 (19)0.124 (2)0.4723 (6)0.013 (4)*
O3A0.4688 (19)0.6244 (19)0.4718 (6)0.010 (4)*
O40.6054 (19)0.130 (2)0.5863 (6)0.013 (4)*
O4A0.620 (2)0.624 (2)0.5881 (6)0.014 (4)*
O50.773 (2)0.126 (2)0.7046 (6)0.016 (4)*
O5A0.7797 (19)0.628 (2)0.7017 (6)0.013 (4)*
O60.939 (2)0.122 (2)0.8389 (6)0.015 (4)*
O6A0.918 (2)0.631 (2)0.8317 (6)0.018 (4)*
O71.138 (2)0.116 (2)0.9048 (6)0.019 (4)*
O81.071 (3)0.769 (3)0.8941 (7)0.038 (6)*
O8A1.0152 (18)0.3990 (19)0.8992 (5)0.009 (4)*
O91.00000.143 (3)0.75000.019 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.0195 (7)0.0129 (5)0.0156 (6)0.0032 (5)0.0011 (5)0.0030 (4)
Bi1A0.0183 (6)0.0138 (5)0.0104 (5)0.0020 (5)0.0011 (5)0.0003 (4)
Bi20.0115 (6)0.0108 (5)0.0100 (5)0.0009 (4)0.0003 (5)0.0002 (4)
Bi2A0.0150 (6)0.0105 (5)0.0103 (5)0.0019 (4)0.0008 (5)0.0010 (4)
Bi30.0083 (6)0.0097 (5)0.0093 (5)0.0005 (4)0.0005 (4)0.0001 (4)
Bi3A0.0096 (6)0.0091 (5)0.0089 (5)0.0003 (4)0.0001 (4)0.0004 (3)
Bi40.0092 (6)0.0090 (5)0.0101 (5)0.0004 (4)0.0005 (4)0.0002 (3)
Bi4A0.0081 (5)0.0103 (5)0.0082 (5)0.0004 (4)0.0001 (4)0.0005 (4)
Bi50.0128 (6)0.0142 (5)0.0118 (5)0.0008 (5)0.0004 (4)0.0006 (4)
Bi5A0.0079 (5)0.0083 (5)0.0153 (5)0.0007 (4)0.0014 (4)0.0006 (4)
Bi60.0133 (6)0.0154 (5)0.0109 (5)0.0022 (4)0.0016 (4)0.0012 (4)
Bi6A0.0105 (6)0.0095 (5)0.0140 (5)0.0004 (4)0.0034 (4)0.0008 (4)
Cl10.026 (7)0.026 (5)0.021 (6)0.0000.001 (5)0.000
Cl1A0.017 (6)0.013 (5)0.021 (5)0.0000.007 (4)0.000
Cl20.024 (5)0.019 (4)0.027 (4)0.001 (3)0.002 (4)0.001 (3)
Cl2A0.034 (5)0.013 (3)0.017 (4)0.010 (3)0.003 (4)0.002 (3)
Cl30.040 (6)0.023 (4)0.017 (4)0.001 (4)0.006 (4)0.002 (3)
Cl3A0.033 (5)0.016 (3)0.019 (4)0.000 (3)0.014 (4)0.001 (3)
Geometric parameters (Å, º) top
Bi1—O12.398 (17)Bi4—O2ii2.270 (16)
Bi1—O1i2.726 (19)Bi4—O2Aiii2.266 (16)
Bi1—O22.538 (19)Bi4—O42.368 (17)
Bi1—O5ii2.656 (17)Bi4—O52.13 (2)
Bi1—O5Aiii2.240 (17)Bi4A—Cl1iii3.473 (6)
Bi1—O6iv2.741 (17)Bi4A—Cl1Aiii3.400 (5)
Bi1—O6Av2.492 (19)Bi4A—Cl2iii3.427 (8)
Bi1—O8v2.46 (2)Bi4A—Cl2Aiii3.440 (8)
Bi1A—O1A2.264 (17)Bi4A—O2iii2.289 (16)
Bi1A—O1Ai2.50 (2)Bi4A—O2Aiii2.261 (15)
Bi1A—O2A2.763 (18)Bi4A—O4A2.207 (17)
Bi1A—O5iii2.303 (18)Bi4A—O5A2.16 (2)
Bi1A—O5Aiii2.673 (17)Bi5—Cl1ii3.560 (5)
Bi1A—O6v2.469 (17)Bi5—Cl1Aiii3.754 (5)
Bi1A—O6Av2.898 (18)Bi5—Cl2vi3.385 (7)
Bi1A—O8Av2.891 (16)Bi5—Cl2Avii3.586 (7)
Bi1A—O9iii2.419 (16)Bi5—O1ii2.214 (16)
Bi2—Cl3ii3.247 (7)Bi5—O1Aiii2.479 (18)
Bi2—Cl3Aiii3.222 (7)Bi5—O52.322 (18)
Bi2—O22.235 (16)Bi5—O62.254 (19)
Bi2—O32.707 (19)Bi5—O92.300 (4)
Bi2—O4ii2.511 (17)Bi5A—Cl1iii3.470 (6)
Bi2—O4Aiii2.488 (17)Bi5A—Cl1Aiii3.439 (5)
Bi2—O7iv2.267 (18)Bi5A—Cl2vii3.316 (7)
Bi2—O8v2.21 (2)Bi5A—Cl2Avii3.320 (6)
Bi2A—Cl3iii3.152 (7)Bi5A—O1iii2.149 (17)
Bi2A—Cl3Aiii3.315 (7)Bi5A—O1Aiii2.142 (18)
Bi2A—O2A2.190 (16)Bi5A—O6A2.17 (2)
Bi2A—O3A2.569 (19)Bi5A—O5A2.476 (17)
Bi2A—O4iii2.256 (17)Bi6—O62.070 (17)
Bi2A—O4Aiii2.583 (17)Bi6—O72.09 (2)
Bi2A—O7v2.275 (18)Bi6—O8A2.128 (16)
Bi2A—O8Av2.581 (18)Bi6—Cl3Avii3.269 (7)
Bi3—Cl2ii3.320 (7)Bi6—Cl3vi3.436 (7)
Bi3—Cl2Aiii3.307 (6)Bi6—Cl2Avii3.438 (8)
Bi3—Cl3ii3.284 (9)Bi6—Cl2vi3.773 (8)
Bi3—Cl3Aiii3.292 (8)Bi6A—Cl2vii3.390 (8)
Bi3—O32.201 (17)Bi6A—Cl2Avii3.292 (8)
Bi3—O3ii2.244 (17)Bi6A—Cl3vii3.313 (7)
Bi3—O3Aiii2.304 (16)Bi6A—Cl3Avii3.373 (7)
Bi3—O42.171 (19)Bi6A—O82.07 (2)
Bi3A—Cl2iii3.339 (7)Bi6A—O8A2.102 (16)
Bi3A—Cl2Aiii3.312 (7)Bi6A—O6A2.107 (18)
Bi3A—Cl3iii3.370 (9)O1—O6Aiii2.67 (2)
Bi3A—Cl3Aiii3.327 (8)O1A—O9iii2.52 (3)
Bi3A—O3iii2.247 (17)O3—O3ii2.61 (3)
Bi3A—O3A2.227 (16)O3—O3Aiii2.66 (2)
Bi3A—O3Aiii2.248 (16)O4—O7viii2.59 (3)
Bi3A—O4A2.21 (2)O5—O92.68 (2)
Bi4—Cl1ii3.240 (6)O6—O92.690 (17)
Bi4—Cl1Aiii3.276 (5)O6A—O82.66 (3)
Bi4—Cl2ii3.362 (8)O7—O8A2.58 (2)
Bi4—Cl2Aiii3.447 (8)
O5Aiii—Bi1—O171.6 (6)O5A—Bi5A—Cl2Avii141.4 (4)
O5Aiii—Bi1—O8v91.4 (7)Cl2vii—Bi5A—Cl2Avii74.49 (17)
O1—Bi1—O8v162.8 (7)O1Aiii—Bi5A—Cl1Aiii78.5 (5)
O5Aiii—Bi1—O6Av83.7 (6)O1iii—Bi5A—Cl1Aiii141.0 (5)
O1—Bi1—O6Av109.2 (6)O6A—Bi5A—Cl1Aiii141.8 (5)
O8v—Bi1—O6Av65.1 (7)O5A—Bi5A—Cl1Aiii76.6 (4)
O5Aiii—Bi1—O269.7 (6)Cl2vii—Bi5A—Cl1Aiii111.83 (16)
O1—Bi1—O2107.3 (6)Cl2Avii—Bi5A—Cl1Aiii71.15 (15)
O8v—Bi1—O267.5 (7)O1Aiii—Bi5A—Cl1iii142.9 (5)
O6Av—Bi1—O2124.2 (6)O1iii—Bi5A—Cl1iii77.7 (5)
O5Aiii—Bi1—O5ii108.2 (6)O6A—Bi5A—Cl1iii138.4 (5)
O1—Bi1—O5ii73.0 (6)O5A—Bi5A—Cl1iii75.7 (4)
O8v—Bi1—O5ii116.2 (6)Cl2vii—Bi5A—Cl1iii69.31 (16)
O6Av—Bi1—O5ii167.7 (6)Cl2Avii—Bi5A—Cl1iii113.16 (17)
O2—Bi1—O5ii64.7 (5)Cl1Aiii—Bi5A—Cl1iii73.13 (18)
O5Aiii—Bi1—O1i112.5 (6)O6—Bi6—O785.5 (8)
O1—Bi1—O1i69.3 (7)O6—Bi6—O8A89.4 (6)
O8v—Bi1—O1i117.1 (7)O7—Bi6—O8A75.5 (7)
O6Av—Bi1—O1i61.4 (6)O6—Bi6—Cl3Avii144.4 (5)
O2—Bi1—O1i174.4 (5)O7—Bi6—Cl3Avii119.7 (5)
O5ii—Bi1—O1i109.8 (5)O8A—Bi6—Cl3Avii75.0 (4)
O5Aiii—Bi1—O6iv175.8 (6)O6—Bi6—Cl3vi126.1 (5)
O1—Bi1—O6iv111.8 (5)O7—Bi6—Cl3vi105.7 (5)
O8v—Bi1—O6iv85.3 (6)O8A—Bi6—Cl3vi144.5 (4)
O6Av—Bi1—O6iv97.1 (6)Cl3Avii—Bi6—Cl3vi74.03 (17)
O2—Bi1—O6iv106.6 (5)O6—Bi6—Cl2Avii75.2 (5)
O5ii—Bi1—O6iv71.2 (6)O7—Bi6—Cl2Avii147.9 (5)
O1i—Bi1—O6iv71.3 (5)O8A—Bi6—Cl2Avii78.7 (5)
O5Aiii—Bi1—O9ii129.4 (5)Cl3Avii—Bi6—Cl2Avii70.51 (18)
O1—Bi1—O9ii58.2 (5)Cl3vi—Bi6—Cl2Avii106.4 (2)
O8v—Bi1—O9ii139.0 (6)O6—Bi6—Cl2vi67.7 (5)
O6Av—Bi1—O9ii116.2 (5)O7—Bi6—Cl2vi129.1 (5)
O2—Bi1—O9ii118.6 (4)O8A—Bi6—Cl2vi141.8 (5)
O5ii—Bi1—O9ii54.0 (5)Cl3Avii—Bi6—Cl2vi105.9 (2)
O1i—Bi1—O9ii55.8 (4)Cl3vi—Bi6—Cl2vi64.74 (18)
O6iv—Bi1—O9ii53.8 (4)Cl2Avii—Bi6—Cl2vi66.44 (16)
O1A—Bi1A—O5iii82.7 (6)O8—Bi6A—O8A92.3 (8)
O1A—Bi1A—O9iii65.1 (5)O8—Bi6A—O6A79.3 (8)
O5iii—Bi1A—O9iii69.0 (6)O8A—Bi6A—O6A87.3 (7)
O1A—Bi1A—O6v131.9 (6)O8—Bi6A—Cl2Avii155.3 (6)
O5iii—Bi1A—O6v82.3 (6)O8A—Bi6A—Cl2Avii82.7 (5)
O9iii—Bi1A—O6v66.8 (5)O6A—Bi6A—Cl2Avii76.4 (5)
O1A—Bi1A—O1Ai77.4 (7)O8—Bi6A—Cl3vii87.9 (6)
O5iii—Bi1A—O1Ai130.7 (6)O8A—Bi6A—Cl3vii133.7 (5)
O9iii—Bi1A—O1Ai61.7 (5)O6A—Bi6A—Cl3vii137.8 (5)
O6v—Bi1A—O1Ai78.6 (6)Cl2Avii—Bi6A—Cl3vii113.0 (2)
O1A—Bi1A—O5Aiii69.0 (6)O8—Bi6A—Cl3Avii130.5 (6)
O5iii—Bi1A—O5Aiii106.9 (6)O8A—Bi6A—Cl3Avii72.8 (4)
O9iii—Bi1A—O5Aiii134.1 (5)O6A—Bi6A—Cl3Avii143.5 (5)
O6v—Bi1A—O5Aiii158.8 (5)Cl2Avii—Bi6A—Cl3Avii71.06 (18)
O1Ai—Bi1A—O5Aiii107.1 (6)Cl3vii—Bi6A—Cl3Avii72.21 (17)
O1A—Bi1A—O2A106.7 (6)O8—Bi6A—Cl2vii102.9 (7)
O5iii—Bi1A—O2A64.6 (6)O8A—Bi6A—Cl2vii152.5 (5)
O9iii—Bi1A—O2A133.6 (4)O6A—Bi6A—Cl2vii73.5 (5)
O6v—Bi1A—O2A107.4 (6)Cl2Avii—Bi6A—Cl2vii73.88 (19)
O1Ai—Bi1A—O2A164.7 (5)Cl3vii—Bi6A—Cl2vii70.51 (18)
O5Aiii—Bi1A—O2A62.3 (5)Cl3Avii—Bi6A—Cl2vii111.6 (2)
O1A—Bi1A—O8Av160.1 (5)Bi4ii—Cl1—Bi4ix108.3 (3)
O5iii—Bi1A—O8Av110.8 (6)Bi4ii—Cl1—Bi5Ax109.15 (3)
O9iii—Bi1A—O8Av132.5 (4)Bi4ix—Cl1—Bi5Ax112.07 (3)
O6v—Bi1A—O8Av66.3 (5)Bi4ii—Cl1—Bi5Aiii112.07 (3)
O1Ai—Bi1A—O8Av102.2 (5)Bi4ix—Cl1—Bi5Aiii109.15 (3)
O5Aiii—Bi1A—O8Av92.5 (5)Bi5Ax—Cl1—Bi5Aiii106.2 (3)
O2A—Bi1A—O8Av68.8 (5)Bi4ii—Cl1—Bi4Aiii73.48 (3)
O1A—Bi1A—O6Av104.5 (6)Bi4ix—Cl1—Bi4Aiii178.2 (3)
O5iii—Bi1A—O6Av169.2 (6)Bi5Ax—Cl1—Bi4Aiii67.31 (14)
O9iii—Bi1A—O6Av121.3 (5)Bi5Aiii—Cl1—Bi4Aiii69.68 (14)
O6v—Bi1A—O6Av98.3 (6)Bi4ii—Cl1—Bi4Ax178.2 (3)
O1Ai—Bi1A—O6Av59.7 (6)Bi4ix—Cl1—Bi4Ax73.48 (3)
O5Aiii—Bi1A—O6Av69.1 (5)Bi5Ax—Cl1—Bi4Ax69.68 (14)
O2A—Bi1A—O6Av105.1 (5)Bi5Aiii—Cl1—Bi4Ax67.31 (14)
O8Av—Bi1A—O6Av60.2 (5)Bi4Aiii—Cl1—Bi4Ax104.8 (3)
O8v—Bi2—O277.2 (7)Bi4ii—Cl1—Bi5ix74.69 (14)
O8v—Bi2—O7iv79.5 (8)Bi4ix—Cl1—Bi5ix71.91 (14)
O2—Bi2—O7iv82.0 (6)Bi5Ax—Cl1—Bi5ix66.37 (3)
O8v—Bi2—O4Aiii91.1 (7)Bi5Aiii—Cl1—Bi5ix171.7 (3)
O2—Bi2—O4Aiii70.7 (6)Bi4Aiii—Cl1—Bi5ix109.05 (4)
O7iv—Bi2—O4Aiii152.5 (6)Bi4Ax—Cl1—Bi5ix105.78 (4)
O8v—Bi2—O4ii136.2 (7)Bi4ii—Cl1—Bi5ii71.91 (14)
O2—Bi2—O4ii72.8 (6)Bi4ix—Cl1—Bi5ii74.69 (14)
O7iv—Bi2—O4ii65.5 (7)Bi5Ax—Cl1—Bi5ii171.7 (3)
O4Aiii—Bi2—O4ii107.8 (6)Bi5Aiii—Cl1—Bi5ii66.37 (3)
O8v—Bi2—O3155.5 (7)Bi4Aiii—Cl1—Bi5ii105.78 (4)
O2—Bi2—O3104.2 (6)Bi4Ax—Cl1—Bi5ii109.05 (4)
O7iv—Bi2—O3125.0 (6)Bi5ix—Cl1—Bi5ii121.3 (3)
O4Aiii—Bi2—O367.1 (6)Bi4iii—Cl1A—Bi4x106.5 (2)
O4ii—Bi2—O364.8 (6)Bi4iii—Cl1A—Bi4Aiii72.71 (3)
O8v—Bi2—Cl3Aiii87.8 (6)Bi4x—Cl1A—Bi4Aiii179.2 (2)
O2—Bi2—Cl3Aiii138.6 (4)Bi4iii—Cl1A—Bi4Ax179.2 (2)
O7iv—Bi2—Cl3Aiii133.2 (5)Bi4x—Cl1A—Bi4Ax72.71 (3)
O4Aiii—Bi2—Cl3Aiii71.3 (4)Bi4Aiii—Cl1A—Bi4Ax108.1 (2)
O4ii—Bi2—Cl3Aiii135.3 (4)Bi4iii—Cl1A—Bi5Ax109.25 (3)
O3—Bi2—Cl3Aiii75.0 (4)Bi4x—Cl1A—Bi5Ax112.16 (3)
O8v—Bi2—Cl3ii117.5 (6)Bi4Aiii—Cl1A—Bi5Ax68.47 (12)
O2—Bi2—Cl3ii143.7 (4)Bi4Ax—Cl1A—Bi5Ax70.89 (12)
O7iv—Bi2—Cl3ii69.7 (5)Bi4iii—Cl1A—Bi5Aiii112.16 (3)
O4Aiii—Bi2—Cl3ii136.4 (4)Bi4x—Cl1A—Bi5Aiii109.25 (3)
O4ii—Bi2—Cl3ii75.0 (4)Bi4Aiii—Cl1A—Bi5Aiii70.89 (12)
O3—Bi2—Cl3ii76.2 (4)Bi4Ax—Cl1A—Bi5Aiii68.47 (12)
Cl3Aiii—Bi2—Cl3ii77.28 (17)Bi5Ax—Cl1A—Bi5Aiii107.5 (2)
O2A—Bi2A—O4iii75.9 (6)Bi4iii—Cl1A—Bi5x71.65 (12)
O2A—Bi2A—O7v84.4 (6)Bi4x—Cl1A—Bi5x69.00 (12)
O4iii—Bi2A—O7v69.8 (7)Bi4Aiii—Cl1A—Bi5x110.91 (3)
O2A—Bi2A—O3A107.9 (6)Bi4Ax—Cl1A—Bi5x107.71 (3)
O4iii—Bi2A—O3A68.3 (6)Bi5Ax—Cl1A—Bi5x70.58 (3)
O7v—Bi2A—O3A131.3 (6)Bi5Aiii—Cl1A—Bi5x176.18 (12)
O2A—Bi2A—O8Av83.7 (6)Bi4iii—Cl1A—Bi5iii69.00 (12)
O4iii—Bi2A—O8Av130.7 (6)Bi4x—Cl1A—Bi5iii71.65 (12)
O7v—Bi2A—O8Av63.9 (6)Bi4Aiii—Cl1A—Bi5iii107.71 (3)
O3A—Bi2A—O8Av160.5 (5)Bi4Ax—Cl1A—Bi5iii110.91 (3)
O2A—Bi2A—O4Aiii70.1 (6)Bi5Ax—Cl1A—Bi5iii176.18 (12)
O4iii—Bi2A—O4Aiii109.0 (6)Bi5Aiii—Cl1A—Bi5iii70.58 (3)
O7v—Bi2A—O4Aiii153.6 (6)Bi5x—Cl1A—Bi5iii111.5 (2)
O3A—Bi2A—O4Aiii66.2 (6)Bi5Ax—Cl2—Bi3ii176.8 (3)
O8Av—Bi2A—O4Aiii105.1 (6)Bi5Ax—Cl2—Bi3Aiii105.36 (18)
O2A—Bi2A—Cl3iii150.7 (4)Bi3ii—Cl2—Bi3Aiii73.66 (15)
O4iii—Bi2A—Cl3iii80.3 (4)Bi5Ax—Cl2—Bi4ii110.0 (2)
O7v—Bi2A—Cl3iii71.5 (5)Bi3ii—Cl2—Bi4ii73.17 (15)
O3A—Bi2A—Cl3iii78.0 (4)Bi3Aiii—Cl2—Bi4ii112.5 (2)
O8Av—Bi2A—Cl3iii99.7 (4)Bi5Ax—Cl2—Bi5ix70.10 (14)
O4Aiii—Bi2A—Cl3iii134.9 (4)Bi3ii—Cl2—Bi5ix110.49 (18)
O2A—Bi2A—Cl3Aiii134.2 (4)Bi3Aiii—Cl2—Bi5ix171.9 (3)
O4iii—Bi2A—Cl3Aiii136.7 (5)Bi4ii—Cl2—Bi5ix75.56 (15)
O7v—Bi2A—Cl3Aiii131.2 (5)Bi5Ax—Cl2—Bi6Ax69.34 (14)
O3A—Bi2A—Cl3Aiii72.1 (4)Bi3ii—Cl2—Bi6Ax107.5 (2)
O8Av—Bi2A—Cl3Aiii88.5 (4)Bi3Aiii—Cl2—Bi6Ax67.01 (14)
O4Aiii—Bi2A—Cl3Aiii68.7 (4)Bi4ii—Cl2—Bi6Ax178.9 (2)
Cl3iii—Bi2A—Cl3Aiii75.03 (17)Bi5ix—Cl2—Bi6Ax104.9 (2)
O4—Bi3—O3112.4 (7)Bi5Ax—Cl2—Bi4Aiii69.57 (14)
O4—Bi3—O3ii78.7 (6)Bi3ii—Cl2—Bi4Aiii112.6 (2)
O3—Bi3—O3ii71.9 (7)Bi3Aiii—Cl2—Bi4Aiii68.80 (14)
O4—Bi3—O3Aiii74.8 (6)Bi4ii—Cl2—Bi4Aiii72.61 (17)
O3—Bi3—O3Aiii72.5 (6)Bi5ix—Cl2—Bi4Aiii114.5 (2)
O3ii—Bi3—O3Aiii122.2 (7)Bi6Ax—Cl2—Bi4Aiii106.28 (18)
O4—Bi3—Cl3ii141.9 (4)Bi5Ax—Cl2—Bi6ix112.3 (2)
O3—Bi3—Cl3ii82.2 (5)Bi3ii—Cl2—Bi6ix65.49 (13)
O3ii—Bi3—Cl3ii72.7 (5)Bi3Aiii—Cl2—Bi6ix108.6 (2)
O3Aiii—Bi3—Cl3ii142.4 (5)Bi4ii—Cl2—Bi6ix108.18 (17)
O4—Bi3—Cl3Aiii139.6 (4)Bi5ix—Cl2—Bi6ix68.25 (13)
O3—Bi3—Cl3Aiii80.1 (5)Bi6Ax—Cl2—Bi6ix72.94 (16)
O3ii—Bi3—Cl3Aiii140.0 (5)Bi4Aiii—Cl2—Bi6ix177.3 (2)
O3Aiii—Bi3—Cl3Aiii72.9 (5)Bi6Ax—Cl2A—Bi3iii109.3 (2)
Cl3ii—Bi3—Cl3Aiii75.78 (19)Bi6Ax—Cl2A—Bi3Aiii68.45 (13)
O4—Bi3—Cl2Aiii77.2 (5)Bi3iii—Cl2A—Bi3Aiii74.06 (14)
O3—Bi3—Cl2Aiii142.6 (4)Bi6Ax—Cl2A—Bi5Ax70.47 (13)
O3ii—Bi3—Cl2Aiii144.1 (5)Bi3iii—Cl2A—Bi5Ax179.7 (3)
O3Aiii—Bi3—Cl2Aiii76.0 (4)Bi3Aiii—Cl2A—Bi5Ax105.85 (17)
Cl3ii—Bi3—Cl2Aiii113.2 (2)Bi6Ax—Cl2A—Bi6x67.38 (16)
Cl3Aiii—Bi3—Cl2Aiii71.89 (17)Bi3iii—Cl2A—Bi6x69.69 (14)
O4—Bi3—Cl2ii77.2 (5)Bi3Aiii—Cl2A—Bi6x106.9 (2)
O3—Bi3—Cl2ii143.1 (4)Bi5Ax—Cl2A—Bi6x110.1 (2)
O3ii—Bi3—Cl2ii75.6 (4)Bi6Ax—Cl2A—Bi4Aiii108.21 (17)
O3Aiii—Bi3—Cl2ii142.2 (4)Bi3iii—Cl2A—Bi4Aiii110.8 (2)
Cl3ii—Bi3—Cl2ii71.74 (18)Bi3Aiii—Cl2A—Bi4Aiii68.95 (14)
Cl3Aiii—Bi3—Cl2ii116.6 (2)Bi5Ax—Cl2A—Bi4Aiii69.35 (13)
Cl2Aiii—Bi3—Cl2ii73.39 (17)Bi6x—Cl2A—Bi4Aiii175.1 (2)
O4A—Bi3A—O3A117.1 (7)Bi6Ax—Cl2A—Bi4iii178.2 (2)
O4A—Bi3A—O3iii80.4 (6)Bi3iii—Cl2A—Bi4iii72.22 (14)
O3A—Bi3A—O3iii73.1 (6)Bi3Aiii—Cl2A—Bi4iii111.3 (2)
O4A—Bi3A—O3Aiii78.2 (6)Bi5Ax—Cl2A—Bi4iii108.0 (2)
O3A—Bi3A—O3Aiii73.4 (7)Bi6x—Cl2A—Bi4iii114.28 (17)
O3iii—Bi3A—O3Aiii125.4 (7)Bi4Aiii—Cl2A—Bi4iii70.16 (16)
O4A—Bi3A—Cl2Aiii80.2 (5)Bi6Ax—Cl2A—Bi5x108.3 (2)
O3A—Bi3A—Cl2Aiii140.5 (4)Bi3iii—Cl2A—Bi5x106.03 (17)
O3iii—Bi3A—Cl2Aiii146.4 (5)Bi3Aiii—Cl2A—Bi5x176.4 (3)
O3Aiii—Bi3A—Cl2Aiii76.5 (4)Bi5Ax—Cl2A—Bi5x74.04 (13)
O4A—Bi3A—Cl3Aiii143.2 (4)Bi6x—Cl2A—Bi5x69.96 (14)
O3A—Bi3A—Cl3Aiii75.7 (5)Bi4Aiii—Cl2A—Bi5x114.1 (2)
O3iii—Bi3A—Cl3Aiii135.4 (5)Bi4iii—Cl2A—Bi5x71.96 (13)
O3Aiii—Bi3A—Cl3Aiii72.8 (5)Bi2Aiii—Cl3—Bi2ii70.90 (15)
Cl2Aiii—Bi3A—Cl3Aiii71.39 (18)Bi2Aiii—Cl3—Bi3ii115.6 (3)
O4A—Bi3A—Cl2iii78.8 (5)Bi2ii—Cl3—Bi3ii75.06 (17)
O3A—Bi3A—Cl2iii140.8 (4)Bi2Aiii—Cl3—Bi6Ax108.7 (2)
O3iii—Bi3A—Cl2iii75.2 (4)Bi2ii—Cl3—Bi6Ax173.8 (3)
O3Aiii—Bi3A—Cl2iii145.4 (4)Bi3ii—Cl3—Bi6Ax110.2 (2)
Cl2Aiii—Bi3A—Cl2iii74.30 (16)Bi2Aiii—Cl3—Bi3Aiii76.60 (17)
Cl3Aiii—Bi3A—Cl2iii114.0 (2)Bi2ii—Cl3—Bi3Aiii117.9 (3)
O4A—Bi3A—Cl3iii142.1 (4)Bi3ii—Cl3—Bi3Aiii73.70 (19)
O3A—Bi3A—Cl3iii77.9 (5)Bi6Ax—Cl3—Bi3Aiii67.52 (15)
O3iii—Bi3A—Cl3iii70.9 (5)Bi2Aiii—Cl3—Bi6ix167.2 (3)
O3Aiii—Bi3A—Cl3iii138.9 (5)Bi2ii—Cl3—Bi6ix100.82 (19)
Cl2Aiii—Bi3A—Cl3iii111.0 (2)Bi3ii—Cl3—Bi6ix69.98 (14)
Cl3Aiii—Bi3A—Cl3iii72.07 (19)Bi6Ax—Cl3—Bi6ix78.44 (15)
Cl2iii—Bi3A—Cl3iii70.45 (18)Bi3Aiii—Cl3—Bi6ix116.2 (2)
O5—Bi4—O2Aiii76.8 (6)Bi2iii—Cl3A—Bi6x105.05 (19)
O5—Bi4—O2ii78.2 (6)Bi2iii—Cl3A—Bi3iii75.28 (15)
O2Aiii—Bi4—O2ii119.6 (6)Bi6x—Cl3A—Bi3iii71.97 (15)
O5—Bi4—O4120.5 (7)Bi2iii—Cl3A—Bi2Aiii81.43 (15)
O2Aiii—Bi4—O472.3 (6)Bi6x—Cl3A—Bi2Aiii165.8 (3)
O2ii—Bi4—O475.0 (6)Bi3iii—Cl3A—Bi2Aiii122.2 (2)
O5—Bi4—Cl1ii80.7 (5)Bi2iii—Cl3A—Bi3Aiii121.8 (2)
O2Aiii—Bi4—Cl1ii146.3 (4)Bi6x—Cl3A—Bi3Aiii110.6 (2)
O2ii—Bi4—Cl1ii79.2 (4)Bi3iii—Cl3A—Bi3Aiii74.05 (19)
O4—Bi4—Cl1ii141.4 (4)Bi2Aiii—Cl3A—Bi3Aiii75.05 (15)
O5—Bi4—Cl1Aiii80.0 (5)Bi2iii—Cl3A—Bi6Ax170.8 (3)
O2Aiii—Bi4—Cl1Aiii79.0 (4)Bi6x—Cl3A—Bi6Ax68.41 (13)
O2ii—Bi4—Cl1Aiii146.7 (4)Bi3iii—Cl3A—Bi6Ax107.7 (2)
O4—Bi4—Cl1Aiii138.2 (4)Bi2Aiii—Cl3A—Bi6Ax103.53 (18)
Cl1ii—Bi4—Cl1Aiii72.60 (19)Bi3Aiii—Cl3A—Bi6Ax67.33 (14)
O5—Bi4—Cl2ii143.7 (5)Bi5Aiii—O1—Bi5ii123.8 (8)
O2Aiii—Bi4—Cl2ii137.8 (5)Bi5Aiii—O1—Bi1111.1 (7)
O2ii—Bi4—Cl2ii74.1 (5)Bi5ii—O1—Bi1105.6 (6)
O4—Bi4—Cl2ii74.1 (5)Bi5Aiii—O1—Bi1i106.6 (6)
Cl1ii—Bi4—Cl2ii71.54 (14)Bi5ii—O1—Bi1i98.1 (6)
Cl1Aiii—Bi4—Cl2ii112.02 (14)Bi1—O1—Bi1i110.7 (7)
O5—Bi4—Cl2Aiii143.0 (5)Bi5Aiii—O1A—Bi1A120.3 (8)
O2Aiii—Bi4—Cl2Aiii74.8 (5)Bi5Aiii—O1A—Bi5iii128.4 (9)
O2ii—Bi4—Cl2Aiii137.2 (5)Bi1A—O1A—Bi5iii92.8 (6)
O4—Bi4—Cl2Aiii72.1 (5)Bi5Aiii—O1A—Bi1Ai118.7 (8)
Cl1ii—Bi4—Cl2Aiii111.67 (14)Bi1A—O1A—Bi1Ai98.8 (7)
Cl1Aiii—Bi4—Cl2Aiii71.56 (12)Bi5iii—O1A—Bi1Ai90.3 (6)
Cl2ii—Bi4—Cl2Aiii71.11 (18)Bi2—O2—Bi4ii110.8 (7)
O5A—Bi4A—O4A118.6 (7)Bi2—O2—Bi4Aiii109.1 (6)
O5A—Bi4A—O2Aiii79.0 (6)Bi4ii—O2—Bi4Aiii123.7 (8)
O4A—Bi4A—O2Aiii76.3 (6)Bi2—O2—Bi1102.8 (7)
O5A—Bi4A—O2iii76.0 (6)Bi4ii—O2—Bi1108.4 (6)
O4A—Bi4A—O2iii75.1 (6)Bi4Aiii—O2—Bi199.5 (6)
O2Aiii—Bi4A—O2iii126.0 (6)Bi2A—O2A—Bi4Aiii112.3 (7)
O5A—Bi4A—Cl1Aiii81.3 (4)Bi2A—O2A—Bi4iii107.2 (6)
O4A—Bi4A—Cl1Aiii141.8 (5)Bi4Aiii—O2A—Bi4iii121.9 (8)
O2Aiii—Bi4A—Cl1Aiii76.3 (4)Bi2A—O2A—Bi1A109.2 (7)
O2iii—Bi4A—Cl1Aiii143.1 (4)Bi4Aiii—O2A—Bi1A106.1 (6)
O5A—Bi4A—Cl2iii139.5 (4)Bi4iii—O2A—Bi1A98.9 (6)
O4A—Bi4A—Cl2iii76.8 (5)Bi3—O3—Bi3ii108.1 (7)
O2Aiii—Bi4A—Cl2iii140.8 (5)Bi3—O3—Bi3Aiii108.4 (7)
O2iii—Bi4A—Cl2iii72.5 (5)Bi3ii—O3—Bi3Aiii125.5 (8)
Cl1Aiii—Bi4A—Cl2iii110.08 (14)Bi3—O3—Bi2107.9 (7)
O5A—Bi4A—Cl2Aiii145.1 (4)Bi3ii—O3—Bi2103.6 (6)
O4A—Bi4A—Cl2Aiii77.3 (5)Bi3Aiii—O3—Bi2102.0 (6)
O2Aiii—Bi4A—Cl2Aiii75.0 (5)Bi3A—O3A—Bi3Aiii106.6 (7)
O2iii—Bi4A—Cl2Aiii138.6 (5)Bi3A—O3A—Bi3iii105.6 (7)
Cl1Aiii—Bi4A—Cl2Aiii70.21 (12)Bi3Aiii—O3A—Bi3iii122.2 (8)
Cl2iii—Bi4A—Cl2Aiii71.58 (17)Bi3A—O3A—Bi2A114.9 (7)
O5A—Bi4A—Cl1iii79.3 (4)Bi3Aiii—O3A—Bi2A107.4 (6)
O4A—Bi4A—Cl1iii138.5 (5)Bi3iii—O3A—Bi2A100.5 (6)
O2Aiii—Bi4A—Cl1iii145.1 (4)Bi3—O4—Bi2Aiii115.8 (7)
O2iii—Bi4A—Cl1iii73.9 (4)Bi3—O4—Bi4122.6 (8)
Cl1Aiii—Bi4A—Cl1iii73.58 (18)Bi2Aiii—O4—Bi4101.7 (7)
Cl2iii—Bi4A—Cl1iii68.03 (14)Bi3—O4—Bi2ii112.6 (7)
Cl2Aiii—Bi4A—Cl1iii110.15 (13)Bi2Aiii—O4—Bi2ii102.2 (7)
O1ii—Bi5—O691.0 (6)Bi4—O4—Bi2ii98.9 (6)
O1ii—Bi5—O976.0 (8)Bi4A—O4A—Bi3A119.9 (8)
O6—Bi5—O972.4 (5)Bi4A—O4A—Bi2iii103.3 (7)
O1ii—Bi5—O583.2 (6)Bi3A—O4A—Bi2iii110.3 (7)
O6—Bi5—O5143.0 (7)Bi4A—O4A—Bi2Aiii100.7 (6)
O9—Bi5—O570.8 (5)Bi3A—O4A—Bi2Aiii108.1 (7)
O1ii—Bi5—O1Aiii139.1 (6)Bi2iii—O4A—Bi2Aiii114.5 (7)
O6—Bi5—O1Aiii83.3 (6)Bi4—O5—Bi1Aiii119.6 (8)
O9—Bi5—O1Aiii63.6 (7)Bi4—O5—Bi5127.8 (9)
O5—Bi5—O1Aiii77.8 (6)Bi1Aiii—O5—Bi596.0 (7)
O1ii—Bi5—Cl2vi78.0 (5)Bi4—O5—Bi1ii108.7 (7)
O6—Bi5—Cl2vi75.0 (5)Bi1Aiii—O5—Bi1ii105.8 (7)
O9—Bi5—Cl2vi137.4 (4)Bi5—O5—Bi1ii95.0 (6)
O5—Bi5—Cl2vi138.0 (5)Bi4A—O5A—Bi1iii113.9 (7)
O1Aiii—Bi5—Cl2vi137.7 (4)Bi4A—O5A—Bi5A117.6 (8)
O1ii—Bi5—Cl1ii75.0 (5)Bi1iii—O5A—Bi5A105.3 (7)
O6—Bi5—Cl1ii141.8 (4)Bi4A—O5A—Bi1Aiii112.5 (7)
O9—Bi5—Cl1ii134.3 (3)Bi1iii—O5A—Bi1Aiii110.2 (7)
O5—Bi5—Cl1ii71.5 (5)Bi5A—O5A—Bi1Aiii95.8 (6)
O1Aiii—Bi5—Cl1ii130.1 (5)Bi6—O6—Bi5137.4 (10)
Cl2vi—Bi5—Cl1ii67.49 (15)Bi6—O6—Bi1Axi108.7 (7)
O1ii—Bi5—Cl2Avii145.3 (4)Bi5—O6—Bi1Axi96.7 (6)
O6—Bi5—Cl2Avii70.2 (5)Bi6—O6—Bi1xii112.0 (7)
O9—Bi5—Cl2Avii122.1 (5)Bi5—O6—Bi1xii96.7 (6)
O5—Bi5—Cl2Avii129.2 (4)Bi1Axi—O6—Bi1xii98.9 (6)
O1Aiii—Bi5—Cl2Avii69.5 (4)Bi6A—O6A—Bi5A126.3 (9)
Cl2vi—Bi5—Cl2Avii69.16 (16)Bi6A—O6A—Bi1xi105.6 (8)
Cl1ii—Bi5—Cl2Avii101.52 (16)Bi5A—O6A—Bi1xi114.5 (7)
O1ii—Bi5—Cl1Aiii134.8 (5)Bi6A—O6A—Bi1Axi106.1 (7)
O6—Bi5—Cl1Aiii132.8 (4)Bi5A—O6A—Bi1Axi103.3 (6)
O9—Bi5—Cl1Aiii121.5 (5)Bi1xi—O6A—Bi1Axi96.7 (6)
O5—Bi5—Cl1Aiii67.7 (5)Bi6—O7—Bi2xii125.9 (8)
O1Aiii—Bi5—Cl1Aiii68.7 (5)Bi6—O7—Bi2Axi111.9 (8)
Cl2vi—Bi5—Cl1Aiii100.76 (16)Bi2xii—O7—Bi2Axi109.6 (8)
Cl1ii—Bi5—Cl1Aiii63.61 (18)Bi6A—O8A—Bi6124.0 (8)
Cl2Avii—Bi5—Cl1Aiii64.77 (14)Bi6A—O8A—Bi2Axi128.4 (7)
O1Aiii—Bi5A—O1iii113.0 (7)Bi6—O8A—Bi2Axi99.9 (6)
O1Aiii—Bi5A—O6A77.9 (7)Bi6A—O8A—Bi1Axi106.4 (6)
O1iii—Bi5A—O6A76.4 (7)Bi6—O8A—Bi1Axi93.6 (5)
O1Aiii—Bi5A—O5A74.8 (6)Bi2Axi—O8A—Bi1Axi95.3 (5)
O1iii—Bi5A—O5A71.5 (6)Bi6A—O8—Bi2xi145.6 (11)
O6A—Bi5A—O5A124.5 (7)Bi6A—O8—Bi1xi108.2 (10)
O1Aiii—Bi5A—Cl2vii145.4 (5)Bi5—O9—Bi5viii164.3 (12)
O1iii—Bi5A—Cl2vii80.4 (5)Bi5—O9—Bi1Axi96.9 (4)
O6A—Bi5A—Cl2vii74.6 (5)Bi5viii—O9—Bi1Axi93.5 (3)
O5A—Bi5A—Cl2vii138.9 (4)Bi5—O9—Bi1Aiii93.5 (3)
O1Aiii—Bi5A—Cl2Avii78.5 (5)Bi5viii—O9—Bi1Aiii96.9 (4)
O1iii—Bi5A—Cl2Avii146.0 (5)Bi1Axi—O9—Bi1Aiii96.9 (9)
O6A—Bi5A—Cl2Avii75.0 (5)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1, y, z+1; (iii) x+1, y+1, z+1; (iv) x1, y, z1/2; (v) x1, y+1, z1/2; (vi) x, y, z+1/2; (vii) x, y+1, z+1/2; (viii) x+2, y, z+3/2; (ix) x, y, z1/2; (x) x, y+1, z1/2; (xi) x+1, y+1, z+1/2; (xii) x+1, y, z+1/2.
(bi24obr) top
Crystal data top
Bi24Br10O31F(000) = 2590
Mr = 6310.62Dx = 8.607 Mg m3
Monoclinic, A2/mMo Kα radiation, λ = 0.71073 Å
a = 10.141 (7) ÅCell parameters from 8153 reflections
b = 4.005 (3) Åθ = 1.4–28.0°
c = 29.977 (19) ŵ = 94.64 mm1
β = 90.197 (12)°T = 293 K
V = 1217.5 (14) Å3Needle, pale brown
Z = 10.25 × 0.04 × 0.02 mm
Data collection top
CCD area detector
diffractometer
1627 independent reflections
Radiation source: fine-focus sealed tube882 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.128
phi and ω scansθmax = 28.3°, θmin = 1.4°
Absorption correction: integration
XPREP / Bruker SHELXTL
h = 1313
Tmin = 0.020, Tmax = 0.269k = 05
8153 measured reflectionsl = 039
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.064 w = 1/[σ2(Fo2) + (0.1089P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.186(Δ/σ)max < 0.001
S = 0.91Δρmax = 6.08 e Å3
1627 reflectionsΔρmin = 5.92 e Å3
84 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00025 (4)
Crystal data top
Bi24Br10O31V = 1217.5 (14) Å3
Mr = 6310.62Z = 1
Monoclinic, A2/mMo Kα radiation
a = 10.141 (7) ŵ = 94.64 mm1
b = 4.005 (3) ÅT = 293 K
c = 29.977 (19) Å0.25 × 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)
Tmin = 0.020, Tmax = 0.269Rint = 0.128
8153 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.06484 parameters
wR(F2) = 0.1860 restraints
S = 0.91Δρmax = 6.08 e Å3
1627 reflectionsΔρmin = 5.92 e Å3
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
xyzUiso*/UeqOcc. (<1)
Bi10.08569 (15)0.00000.05880 (6)0.0480 (6)
Bi20.25344 (12)0.00000.17509 (4)0.0228 (4)
Bi30.43453 (12)0.00000.29464 (4)0.0108 (3)
Bi40.60015 (11)0.00000.41348 (4)0.0114 (3)
Bi50.77636 (17)0.00000.53264 (5)0.0309 (5)
Bi60.92640 (17)0.00000.65308 (5)0.0317 (5)
Br10.50000.00000.00000.0151 (10)
Br20.6637 (3)0.00000.11904 (11)0.0190 (8)
Br30.8179 (4)0.00000.24020 (13)0.0234 (8)
O10.138 (2)0.00000.0158 (8)0.027 (6)*
O20.3097 (19)0.00000.1043 (7)0.011 (4)*
O30.478 (2)0.00000.2228 (8)0.020 (5)*
O40.6112 (19)0.00000.3378 (7)0.013 (4)*
O50.778 (2)0.00000.4542 (7)0.019 (5)*
O60.931 (2)0.00000.5837 (8)0.021 (5)*
O71.146 (4)0.00000.6472 (15)0.024 (11)*0.50
O81.083 (7)1.309 (19)0.643 (2)0.036 (18)*0.25
O8A1.021 (5)0.45 (2)0.6458 (18)0.024 (17)*0.25
O91.00000.00000.50000.021 (14)*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.0223 (9)0.0802 (15)0.0414 (11)0.0000.0109 (8)0.000
Bi20.0167 (7)0.0407 (10)0.0109 (7)0.0000.0004 (6)0.000
Bi30.0137 (6)0.0070 (6)0.0116 (6)0.0000.0014 (5)0.000
Bi40.0103 (6)0.0085 (6)0.0153 (7)0.0000.0020 (5)0.000
Bi50.0493 (10)0.0245 (9)0.0187 (8)0.0000.0097 (7)0.000
Bi60.0351 (9)0.0383 (9)0.0217 (8)0.0000.0122 (6)0.000
Br10.016 (2)0.009 (2)0.021 (3)0.0000.0009 (19)0.000
Br20.0213 (18)0.0160 (16)0.0196 (19)0.0000.0004 (14)0.000
Br30.026 (2)0.0184 (18)0.026 (2)0.0000.0012 (16)0.000
Geometric parameters (Å, º) top
Bi1—O12.30 (3)Bi3—O3iii2.254 (11)
Bi1—O1i2.61 (2)Bi3—O42.207 (19)
Bi1—O22.645 (19)Bi4—Br1ix3.4330 (18)
Bi1—O5ii2.463 (13)Bi4—Br1x3.4330 (18)
Bi1—O5iii2.463 (13)Bi4—Br2iii3.479 (3)
Bi1—O6iv2.654 (16)Bi4—Br2ii3.479 (3)
Bi1—O6v2.654 (16)Bi4—O2ii2.266 (10)
Bi1—O8vi2.63 (7)Bi4—O2iii2.266 (10)
Bi1—O8vii2.63 (7)Bi4—O42.27 (2)
Bi1—O8Aviii2.70 (6)Bi4—O52.18 (2)
Bi1—O8Aiv2.70 (6)Bi4—O7xi3.15 (5)
Bi1—O9iv2.8039 (17)Bi5—Br1x3.578 (2)
Bi2—Br3ii3.316 (4)Bi5—Br1ix3.578 (2)
Bi2—Br3iii3.316 (4)Bi5—Br2ix3.470 (4)
Bi2—O22.20 (2)Bi5—Br2x3.470 (4)
Bi2—O32.68 (2)Bi5—O1ii2.240 (12)
Bi2—O4ii2.459 (12)Bi5—O1iii2.240 (12)
Bi2—O4iii2.459 (12)Bi5—O52.35 (2)
Bi2—O7iv2.43 (2)Bi5—O62.19 (2)
Bi2—O7v2.43 (2)Bi5—O92.473 (2)
Bi2—O8vii2.12 (7)Bi6—Br3ix3.473 (4)
Bi2—O8vi2.12 (7)Bi6—Br3x3.473 (4)
Bi2—O8Aiv2.52 (5)Bi6—O62.08 (2)
Bi2—O8Aviii2.52 (5)Bi6—O72.24 (5)
Bi3—Br2ii3.423 (3)Bi6—O8xii2.04 (7)
Bi3—Br2iii3.423 (3)Bi6—O8xiii2.04 (7)
Bi3—Br3iii3.412 (3)Bi6—O8xiv3.21 (8)
Bi3—Br3ii3.412 (3)Bi6—O8xv3.21 (8)
Bi3—Bi3iii3.600 (3)Bi6—O8A2.04 (8)
Bi3—Bi3ii3.600 (3)Bi6—O8Axvi2.04 (8)
Bi3—O32.20 (2)Bi6—O8Axiii2.43 (8)
Bi3—O3ii2.254 (11)Bi6—O8Axii2.43 (8)
O1—Bi1—O5ii73.4 (6)O5—Bi5—Br1ix74.7 (4)
O1—Bi1—O5iii73.4 (6)O9—Bi5—Br1ix127.61 (5)
O5ii—Bi1—O5iii108.8 (8)Br2ix—Bi5—Br1ix67.77 (6)
O1—Bi1—O1i74.0 (9)Br2x—Bi5—Br1ix105.52 (8)
O5ii—Bi1—O1i114.1 (5)Br1x—Bi5—Br1ix68.06 (5)
O5iii—Bi1—O1i114.1 (5)O8xii—Bi6—O8xiii75 (4)
O1—Bi1—O8vi158.9 (17)O8xii—Bi6—O8A24 (2)
O5ii—Bi1—O8vi85.6 (17)O8xiii—Bi6—O8A99 (3)
O5iii—Bi1—O8vi113.3 (16)O8xii—Bi6—O8Axvi99 (3)
O1i—Bi1—O8vi117.4 (17)O8xiii—Bi6—O8Axvi24 (2)
O1—Bi1—O8vii158.9 (17)O8A—Bi6—O8Axvi122 (4)
O5ii—Bi1—O8vii113.3 (16)O8xii—Bi6—O680 (2)
O5iii—Bi1—O8vii85.6 (17)O8xiii—Bi6—O680 (2)
O1i—Bi1—O8vii117.4 (17)O8A—Bi6—O683.2 (15)
O8vi—Bi1—O8vii34 (3)O8Axvi—Bi6—O683.2 (15)
O1—Bi1—O2107.4 (8)O8xii—Bi6—O738 (2)
O5ii—Bi1—O266.5 (5)O8xiii—Bi6—O738 (2)
O5iii—Bi1—O266.5 (5)O8A—Bi6—O761.5 (18)
O1i—Bi1—O2178.6 (7)O8Axvi—Bi6—O761.5 (18)
O8vi—Bi1—O261.2 (16)O6—Bi6—O784.0 (13)
O8vii—Bi1—O261.2 (16)O8xii—Bi6—O8Axiii29 (2)
O1—Bi1—O6iv114.4 (6)O8xiii—Bi6—O8Axiii104 (3)
O5ii—Bi1—O6iv172.0 (7)O8A—Bi6—O8Axiii5 (2)
O5iii—Bi1—O6iv76.3 (6)O8Axvi—Bi6—O8Axiii127 (3)
O1i—Bi1—O6iv67.9 (6)O6—Bi6—O8Axiii84.3 (13)
O8vi—Bi1—O6iv86.7 (17)O7—Bi6—O8Axiii66.4 (15)
O8vii—Bi1—O6iv60.2 (16)O8xii—Bi6—O8Axii104 (3)
O2—Bi1—O6iv111.3 (5)O8xiii—Bi6—O8Axii29 (2)
O1—Bi1—O6v114.4 (6)O8A—Bi6—O8Axii127 (3)
O5ii—Bi1—O6v76.3 (6)O8Axvi—Bi6—O8Axii5 (2)
O5iii—Bi1—O6v172.0 (7)O6—Bi6—O8Axii84.3 (13)
O1i—Bi1—O6v67.9 (6)O7—Bi6—O8Axii66.4 (14)
O8vi—Bi1—O6v60.2 (16)O8Axiii—Bi6—O8Axii132 (3)
O8vii—Bi1—O6v86.7 (17)O8xii—Bi6—O8xiv22 (2)
O2—Bi1—O6v111.3 (5)O8xiii—Bi6—O8xiv97 (3)
O6iv—Bi1—O6v98.0 (8)O8A—Bi6—O8xiv2 (2)
O1—Bi1—O8Aviii175.3 (18)O8Axvi—Bi6—O8xiv121 (2)
O5ii—Bi1—O8Aviii103.1 (17)O6—Bi6—O8xiv83.7 (13)
O5iii—Bi1—O8Aviii110.9 (17)O7—Bi6—O8xiv59.9 (13)
O1i—Bi1—O8Aviii105.2 (13)O8Axiii—Bi6—O8xiv7 (2)
O8vi—Bi1—O8Aviii18.1 (19)O8Axii—Bi6—O8xiv125.9 (18)
O8vii—Bi1—O8Aviii25 (2)O8xii—Bi6—O8xv97 (3)
O2—Bi1—O8Aviii73.4 (12)O8xiii—Bi6—O8xv22 (2)
O6iv—Bi1—O8Aviii69.0 (17)O8A—Bi6—O8xv121 (2)
O6v—Bi1—O8Aviii61.4 (17)O8Axvi—Bi6—O8xv2 (2)
O1—Bi1—O8Aiv175.3 (18)O6—Bi6—O8xv83.7 (13)
O5ii—Bi1—O8Aiv110.9 (17)O7—Bi6—O8xv59.9 (13)
O5iii—Bi1—O8Aiv103.1 (17)O8Axiii—Bi6—O8xv125.9 (17)
O1i—Bi1—O8Aiv105.2 (13)O8Axii—Bi6—O8xv7 (2)
O8vi—Bi1—O8Aiv25 (2)O8xiv—Bi6—O8xv119 (3)
O8vii—Bi1—O8Aiv18.1 (19)O8xii—Bi6—Br3ix91 (2)
O2—Bi1—O8Aiv73.4 (12)O8xiii—Bi6—Br3ix135.5 (19)
O6iv—Bi1—O8Aiv61.4 (17)O8A—Bi6—Br3ix74.0 (17)
O6v—Bi1—O8Aiv69.0 (17)O8Axvi—Bi6—Br3ix137.4 (15)
O8Aviii—Bi1—O8Aiv9 (4)O6—Bi6—Br3ix139.4 (3)
O1—Bi1—O9iv57.4 (3)O7—Bi6—Br3ix112.2 (9)
O5ii—Bi1—O9iv130.8 (5)O8Axiii—Bi6—Br3ix70.5 (14)
O5iii—Bi1—O9iv59.5 (4)O8Axii—Bi6—Br3ix136.1 (13)
O1i—Bi1—O9iv54.7 (3)O8xiv—Bi6—Br3ix74.5 (14)
O8vi—Bi1—O9iv143.6 (17)O8xv—Bi6—Br3ix136.8 (13)
O8vii—Bi1—O9iv112.9 (16)O8xii—Bi6—Br3x135.5 (19)
O2—Bi1—O9iv126.0 (2)O8xiii—Bi6—Br3x91 (2)
O6iv—Bi1—O9iv57.0 (5)O8A—Bi6—Br3x137.4 (15)
O6v—Bi1—O9iv122.2 (4)O8Axvi—Bi6—Br3x74.0 (17)
O8Aviii—Bi1—O9iv126.0 (16)O6—Bi6—Br3x139.4 (3)
O8Aiv—Bi1—O9iv118.3 (16)O7—Bi6—Br3x112.2 (9)
O8vii—Bi2—O8vi42 (4)O8Axiii—Bi6—Br3x136.1 (13)
O8vii—Bi2—O277 (2)O8Axii—Bi6—Br3x70.5 (14)
O8vi—Bi2—O277 (2)O8xiv—Bi6—Br3x136.8 (13)
O8vii—Bi2—O7iv35 (2)O8xv—Bi6—Br3x74.5 (14)
O8vi—Bi2—O7iv77 (2)Br3ix—Bi6—Br3x70.42 (9)
O2—Bi2—O7iv77.5 (11)Bi4xvii—Br1—Bi4xviii71.37 (5)
O8vii—Bi2—O7v77 (2)Bi4xvii—Br1—Bi4ii180.00 (5)
O8vi—Bi2—O7v35 (2)Bi4xviii—Br1—Bi4ii108.63 (5)
O2—Bi2—O7v77.5 (11)Bi4xvii—Br1—Bi4iii108.63 (5)
O7iv—Bi2—O7v111.3 (16)Bi4xviii—Br1—Bi4iii180.00 (3)
O8vii—Bi2—O4ii133 (2)Bi4ii—Br1—Bi4iii71.37 (5)
O8vi—Bi2—O4ii95 (2)Bi4xvii—Br1—Bi5iii72.57 (5)
O2—Bi2—O4ii72.6 (5)Bi4xviii—Br1—Bi5iii110.69 (4)
O7iv—Bi2—O4ii150.2 (12)Bi4ii—Br1—Bi5iii107.43 (5)
O7v—Bi2—O4ii61.5 (10)Bi4iii—Br1—Bi5iii69.31 (4)
O8vii—Bi2—O4iii95 (2)Bi4xvii—Br1—Bi5xviii107.43 (5)
O8vi—Bi2—O4iii133 (2)Bi4xviii—Br1—Bi5xviii69.31 (4)
O2—Bi2—O4iii72.6 (5)Bi4ii—Br1—Bi5xviii72.57 (5)
O7iv—Bi2—O4iii61.5 (10)Bi4iii—Br1—Bi5xviii110.69 (4)
O7v—Bi2—O4iii150.2 (12)Bi5iii—Br1—Bi5xviii180.00 (4)
O4ii—Bi2—O4iii109.0 (8)Bi4xvii—Br1—Bi5ii110.69 (4)
O8vii—Bi2—O8Aiv18 (3)Bi4xviii—Br1—Bi5ii72.57 (5)
O8vi—Bi2—O8Aiv28 (3)Bi4ii—Br1—Bi5ii69.31 (4)
O2—Bi2—O8Aiv84.8 (14)Bi4iii—Br1—Bi5ii107.43 (5)
O7iv—Bi2—O8Aiv53 (2)Bi5iii—Br1—Bi5ii68.06 (5)
O7v—Bi2—O8Aiv62 (2)Bi5xviii—Br1—Bi5ii111.94 (5)
O4ii—Bi2—O8Aiv122.5 (19)Bi4xvii—Br1—Bi5xvii69.31 (4)
O4iii—Bi2—O8Aiv113.4 (19)Bi4xviii—Br1—Bi5xvii107.43 (5)
O8vii—Bi2—O8Aviii28 (3)Bi4ii—Br1—Bi5xvii110.69 (4)
O8vi—Bi2—O8Aviii18 (3)Bi4iii—Br1—Bi5xvii72.57 (5)
O2—Bi2—O8Aviii84.8 (14)Bi5iii—Br1—Bi5xvii111.94 (5)
O7iv—Bi2—O8Aviii62 (2)Bi5xviii—Br1—Bi5xvii68.06 (5)
O7v—Bi2—O8Aviii53 (2)Bi5ii—Br1—Bi5xvii180.00 (4)
O4ii—Bi2—O8Aviii113.4 (19)Bi3ii—Br2—Bi3iii71.61 (9)
O4iii—Bi2—O8Aviii122.5 (19)Bi3ii—Br2—Bi5xvii177.71 (11)
O8Aiv—Bi2—O8Aviii10 (4)Bi3iii—Br2—Bi5xvii108.91 (5)
O8vii—Bi2—O3159 (2)Bi3ii—Br2—Bi5xviii108.91 (5)
O8vi—Bi2—O3159 (2)Bi3iii—Br2—Bi5xviii177.71 (11)
O2—Bi2—O3107.0 (8)Bi5xvii—Br2—Bi5xviii70.49 (9)
O7iv—Bi2—O3124.2 (8)Bi3ii—Br2—Bi4iii108.84 (10)
O7v—Bi2—O3124.2 (8)Bi3iii—Br2—Bi4iii69.48 (6)
O4ii—Bi2—O367.1 (5)Bi5xvii—Br2—Bi4iii73.35 (6)
O4iii—Bi2—O367.1 (5)Bi5xviii—Br2—Bi4iii112.20 (10)
O8Aiv—Bi2—O3167.2 (15)Bi3ii—Br2—Bi4ii69.48 (6)
O8Aviii—Bi2—O3167.2 (14)Bi3iii—Br2—Bi4ii108.84 (10)
O8vii—Bi2—Br3ii113 (2)Bi5xvii—Br2—Bi4ii112.20 (10)
O8vi—Bi2—Br3ii87 (2)Bi5xviii—Br2—Bi4ii73.35 (6)
O2—Bi2—Br3ii142.84 (5)Bi4iii—Br2—Bi4ii70.28 (8)
O7iv—Bi2—Br3ii131.6 (11)Bi3ii—Br2—Bi6xviii70.52 (6)
O7v—Bi2—Br3ii70.5 (10)Bi3iii—Br2—Bi6xviii109.83 (10)
O4ii—Bi2—Br3ii75.6 (5)Bi5xvii—Br2—Bi6xviii107.28 (10)
O4iii—Bi2—Br3ii137.4 (5)Bi5xviii—Br2—Bi6xviii68.50 (6)
O8Aiv—Bi2—Br3ii96.4 (16)Bi4iii—Br2—Bi6xviii179.23 (12)
O8Aviii—Bi2—Br3ii90.5 (15)Bi4ii—Br2—Bi6xviii109.75 (5)
O3—Bi2—Br3ii77.2 (4)Bi3ii—Br2—Bi6xvii109.83 (10)
O8vii—Bi2—Br3iii87 (2)Bi3iii—Br2—Bi6xvii70.52 (6)
O8vi—Bi2—Br3iii113 (2)Bi5xvii—Br2—Bi6xvii68.50 (6)
O2—Bi2—Br3iii142.84 (5)Bi5xviii—Br2—Bi6xvii107.28 (10)
O7iv—Bi2—Br3iii70.5 (10)Bi4iii—Br2—Bi6xvii109.75 (5)
O7v—Bi2—Br3iii131.6 (11)Bi4ii—Br2—Bi6xvii179.23 (12)
O4ii—Bi2—Br3iii137.4 (5)Bi6xviii—Br2—Bi6xvii70.20 (8)
O4iii—Bi2—Br3iii75.6 (5)Bi3ii—Br2—O6xviii96.9 (3)
O8Aiv—Bi2—Br3iii90.5 (15)Bi3iii—Br2—O6xviii141.6 (4)
O8Aviii—Bi2—Br3iii96.4 (16)Bi5xvii—Br2—O6xviii81.3 (3)
O3—Bi2—Br3iii77.2 (4)Bi5xviii—Br2—O6xviii36.4 (3)
Br3ii—Bi2—Br3iii74.31 (10)Bi4iii—Br2—O6xviii146.3 (4)
O3—Bi3—O4114.2 (8)Bi4ii—Br2—O6xviii100.3 (3)
O3—Bi3—O3ii72.1 (6)Bi6xviii—Br2—O6xviii34.5 (4)
O4—Bi3—O3ii79.4 (6)Bi6xvii—Br2—O6xviii80.0 (3)
O3—Bi3—O3iii72.1 (6)Bi3ii—Br2—O6xvii141.6 (4)
O4—Bi3—O3iii79.4 (6)Bi3iii—Br2—O6xvii96.9 (3)
O3ii—Bi3—O3iii125.4 (11)Bi5xvii—Br2—O6xvii36.4 (3)
O3—Bi3—Br3iii81.5 (4)Bi5xviii—Br2—O6xvii81.3 (3)
O4—Bi3—Br3iii141.87 (18)Bi4iii—Br2—O6xvii100.3 (3)
O3ii—Bi3—Br3iii138.3 (5)Bi4ii—Br2—O6xvii146.3 (4)
O3iii—Bi3—Br3iii72.8 (5)Bi6xviii—Br2—O6xvii80.0 (3)
O3—Bi3—Br3ii81.5 (4)Bi6xvii—Br2—O6xvii34.5 (4)
O4—Bi3—Br3ii141.87 (18)Bi2ii—Br3—Bi2iii74.31 (10)
O3ii—Bi3—Br3ii72.8 (5)Bi2ii—Br3—O7xi42.4 (3)
O3iii—Bi3—Br3ii138.3 (5)Bi2iii—Br3—O7xi42.4 (3)
Br3iii—Bi3—Br3ii71.89 (9)Bi2ii—Br3—Bi3iii115.05 (12)
O3—Bi3—Br2ii143.11 (13)Bi2iii—Br3—Bi3iii73.40 (7)
O4—Bi3—Br2ii78.1 (5)Bi2ii—Br3—Bi3ii73.40 (7)
O3ii—Bi3—Br2ii76.8 (6)Bi2iii—Br3—Bi3ii115.05 (12)
O3iii—Bi3—Br2ii144.3 (6)Bi3iii—Br3—Bi3ii71.89 (9)
Br3iii—Bi3—Br2ii110.78 (10)Bi2ii—Br3—Bi6xvii174.10 (12)
Br3ii—Bi3—Br2ii70.61 (9)Bi2iii—Br3—Bi6xvii107.35 (5)
O3—Bi3—Br2iii143.11 (13)Bi3iii—Br3—Bi6xvii70.76 (7)
O4—Bi3—Br2iii78.1 (5)Bi3ii—Br3—Bi6xvii110.33 (11)
O3ii—Bi3—Br2iii144.3 (6)Bi2ii—Br3—Bi6xviii107.35 (5)
O3iii—Bi3—Br2iii76.8 (6)Bi2iii—Br3—Bi6xviii174.10 (12)
Br3iii—Bi3—Br2iii70.61 (9)Bi3iii—Br3—Bi6xviii110.33 (11)
Br3ii—Bi3—Br2iii110.78 (10)Bi3ii—Br3—Bi6xviii70.76 (7)
Br2ii—Bi3—Br2iii71.61 (9)Bi6xvii—Br3—Bi6xviii70.42 (9)
O5—Bi4—O2ii78.3 (5)Bi5ii—O1—Bi5iii126.8 (12)
O5—Bi4—O2iii78.3 (5)Bi5ii—O1—Bi1108.1 (6)
O2ii—Bi4—O2iii124.2 (10)Bi5iii—O1—Bi1108.1 (6)
O5—Bi4—O4121.1 (8)Bi5ii—O1—Bi1i103.0 (6)
O2ii—Bi4—O475.2 (5)Bi5iii—O1—Bi1i103.0 (6)
O2iii—Bi4—O475.2 (5)Bi1—O1—Bi1i106.0 (10)
O5—Bi4—O7xi69.3 (10)Bi2—O2—Bi4ii109.5 (5)
O2ii—Bi4—O7xi62.2 (5)Bi2—O2—Bi4iii109.5 (5)
O2iii—Bi4—O7xi62.2 (5)Bi4ii—O2—Bi4iii124.2 (9)
O4—Bi4—O7xi51.8 (9)Bi2—O2—Bi1105.8 (8)
O5—Bi4—Br1ix79.8 (5)Bi4ii—O2—Bi1103.0 (5)
O2ii—Bi4—Br1ix77.5 (5)Bi4iii—O2—Bi1103.0 (5)
O2iii—Bi4—Br1ix144.5 (5)Bi3—O3—Bi3ii107.9 (6)
O4—Bi4—Br1ix140.4 (2)Bi3—O3—Bi3iii107.9 (6)
O7xi—Bi4—Br1ix132.8 (5)Bi3ii—O3—Bi3iii125.4 (11)
O5—Bi4—Br1x79.8 (5)Bi3—O3—Bi2110.5 (9)
O2ii—Bi4—Br1x144.5 (5)Bi3ii—O3—Bi2102.1 (6)
O2iii—Bi4—Br1x77.5 (5)Bi3iii—O3—Bi2102.1 (6)
O4—Bi4—Br1x140.4 (2)Bi3—O3—Br393.1 (6)
O7xi—Bi4—Br1x132.8 (5)Bi3ii—O3—Br369.1 (5)
Br1ix—Bi4—Br1x71.37 (5)Bi3iii—O3—Br369.1 (5)
O5—Bi4—Br2iii142.5 (2)Bi2—O3—Br3156.4 (9)
O2ii—Bi4—Br2iii138.9 (5)Bi3—O4—Bi4122.9 (9)
O2iii—Bi4—Br2iii74.7 (5)Bi3—O4—Bi2ii111.1 (6)
O4—Bi4—Br2iii76.2 (4)Bi4—O4—Bi2ii100.8 (5)
O7xi—Bi4—Br2iii117.8 (6)Bi3—O4—Bi2iii111.1 (6)
Br1ix—Bi4—Br2iii108.55 (7)Bi4—O4—Bi2iii100.8 (5)
Br1x—Bi4—Br2iii69.31 (6)Bi2ii—O4—Bi2iii109.0 (8)
O5—Bi4—Br2ii142.5 (2)Bi4—O5—Bi5123.4 (10)
O2ii—Bi4—Br2ii74.7 (5)Bi4—O5—Bi1ii112.0 (6)
O2iii—Bi4—Br2ii138.9 (5)Bi5—O5—Bi1ii99.5 (6)
O4—Bi4—Br2ii76.2 (4)Bi4—O5—Bi1iii112.0 (6)
O7xi—Bi4—Br2ii117.8 (6)Bi5—O5—Bi1iii99.5 (6)
Br1ix—Bi4—Br2ii69.31 (6)Bi1ii—O5—Bi1iii108.8 (8)
Br1x—Bi4—Br2ii108.55 (7)Bi6—O6—Bi1xix107.2 (6)
Br2iii—Bi4—Br2ii70.28 (8)Bi5—O6—Bi1xix103.1 (7)
O5—Bi4—Bi2iii94.0 (5)Bi6—O6—Bi1xx107.2 (6)
O2ii—Bi4—Bi2iii98.5 (5)Bi5—O6—Bi1xx103.1 (7)
O2iii—Bi4—Bi2iii34.7 (5)Bi1xix—O6—Bi1xx98.0 (8)
O4—Bi4—Bi2iii41.5 (3)Bi6—O6—Br2x71.4 (6)
O7xi—Bi4—Bi2iii41.0 (4)Bi5—O6—Br2x70.2 (5)
O6—Bi5—O1ii83.2 (6)Bi1xix—O6—Br2x165.2 (6)
O6—Bi5—O1iii83.2 (6)Bi1xx—O6—Br2x96.41 (18)
O1ii—Bi5—O1iii126.8 (12)Bi6—O6—Br2ix71.4 (6)
O6—Bi5—O5133.8 (9)Bi5—O6—Br2ix70.2 (5)
O1ii—Bi5—O576.7 (6)Bi1xix—O6—Br2ix96.41 (18)
O1iii—Bi5—O576.7 (6)Bi1xx—O6—Br2ix165.2 (6)
O6—Bi5—O967.8 (6)Bi6—O7—Bi2xix114.7 (13)
O1ii—Bi5—O963.6 (6)Bi6—O7—Bi2xx114.7 (13)
O1iii—Bi5—O963.6 (6)Bi2xix—O7—Bi2xx111.3 (16)
O5—Bi5—O966.0 (5)Bi6—O7—Bi4xi149.3 (19)
O6—Bi5—Br2ix73.4 (5)Bi2xix—O7—Bi4xi80.5 (11)
O1ii—Bi5—Br2ix77.4 (6)Bi2xx—O7—Bi4xi80.5 (11)
O1iii—Bi5—Br2ix144.4 (6)Bi6—O8A—Bi6xxi127 (3)
O5—Bi5—Br2ix138.6 (3)Bi6—O8A—Bi2xix118 (3)
O9—Bi5—Br2ix126.87 (6)Bi6xxi—O8A—Bi2xix105 (3)
O6—Bi5—Br2x73.4 (5)Bi6—O8A—Bi1xix107 (3)
O1ii—Bi5—Br2x144.4 (6)Bi6xxi—O8A—Bi1xix96 (2)
O1iii—Bi5—Br2x77.4 (6)Bi2xix—O8A—Bi1xix95.6 (18)
O5—Bi5—Br2x138.6 (3)Bi6xxi—O8—Bi2xxii142 (4)
O9—Bi5—Br2x126.87 (6)Bi6xxi—O8—Bi1xxii109 (3)
Br2ix—Bi5—Br2x70.49 (9)Bi2xxii—O8—Bi1xxii109 (3)
O6—Bi5—Br1x138.6 (3)Bi6xxi—O8—Bi6xxiii97 (3)
O1ii—Bi5—Br1x137.8 (6)Bi2xxii—O8—Bi6xxiii93 (2)
O1iii—Bi5—Br1x74.9 (6)Bi1xxii—O8—Bi6xxiii81.3 (19)
O5—Bi5—Br1x74.7 (4)Bi5—O9—Bi5xi180.00 (6)
O9—Bi5—Br1x127.61 (5)Bi5—O9—Bi1iii88.06 (5)
Br2ix—Bi5—Br1x105.52 (8)Bi5xi—O9—Bi1iii91.94 (5)
Br2x—Bi5—Br1x67.77 (6)Bi5—O9—Bi1ii88.06 (5)
O6—Bi5—Br1ix138.6 (3)Bi5xi—O9—Bi1ii91.94 (5)
O1ii—Bi5—Br1ix74.9 (6)Bi1iii—O9—Bi1ii91.15 (7)
O1iii—Bi5—Br1ix137.8 (6)
Symmetry codes: (i) x, y, z; (ii) x+1, y+1/2, z+1/2; (iii) x+1, y1/2, z+1/2; (iv) x1, y1/2, z1/2; (v) x1, y+1/2, z1/2; (vi) x1, y+3/2, z1/2; (vii) x1, y3/2, z1/2; (viii) x1, y+1/2, z1/2; (ix) x, y+1/2, z+1/2; (x) x, y1/2, z+1/2; (xi) x+2, y, z+1; (xii) x, y1, z; (xiii) x, y+1, z; (xiv) x, y+2, z; (xv) x, y2, z; (xvi) x, y, z; (xvii) x, y1/2, z1/2; (xviii) x, y+1/2, z1/2; (xix) x+1, y+1/2, z+1/2; (xx) x+1, y1/2, 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 formulaBi24Cl10O31Bi24Br10O31
Mr5866.026310.62
Crystal system, space groupMonoclinic, P2/cMonoclinic, A2/m
Temperature (K)293293
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)
V3)2363.8 (8)1217.5 (14)
Z21
Radiation typeMo KαMo Kα
µ (mm1)89.6094.64
Crystal size (mm)0.22 × 0.02 × 0.010.25 × 0.04 × 0.02
Data collection
DiffractometerCCD area detector
diffractometer
CCD area detector
diffractometer
Absorption correctionIntegration
XPREP / Bruker SHELXTL
Integration
XPREP / Bruker SHELXTL
Tmin, Tmax0.029, 0.4040.020, 0.269
No. of measured, independent and
observed [I > 2σ(I)] reflections
15924, 5546, 3184 8153, 1627, 882
Rint0.1300.128
(sin θ/λ)max1)0.6680.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.063, 0.146, 0.90 0.064, 0.186, 0.91
No. of reflections55461627
No. of parameters21884
Δρmax, Δρmin (e Å3)5.98, 6.166.08, 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—O12.398 (17)Bi4—O2ii2.270 (16)
Bi1—O1i2.726 (19)Bi4—O2Aiii2.266 (16)
Bi1—O22.538 (19)Bi4—O42.368 (17)
Bi1—O5ii2.656 (17)Bi4—O52.13 (2)
Bi1—O5Aiii2.240 (17)Bi4A—Cl1iii3.473 (6)
Bi1—O6iv2.741 (17)Bi4A—Cl1Aiii3.400 (5)
Bi1—O6Av2.492 (19)Bi4A—Cl2iii3.427 (8)
Bi1—O8v2.46 (2)Bi4A—Cl2Aiii3.440 (8)
Bi1A—O1A2.264 (17)Bi4A—O2iii2.289 (16)
Bi1A—O1Ai2.50 (2)Bi4A—O2Aiii2.261 (15)
Bi1A—O2A2.763 (18)Bi4A—O4A2.207 (17)
Bi1A—O5iii2.303 (18)Bi4A—O5A2.16 (2)
Bi1A—O5Aiii2.673 (17)Bi5—Cl1ii3.560 (5)
Bi1A—O6v2.469 (17)Bi5—Cl1Aiii3.754 (5)
Bi1A—O6Av2.898 (18)Bi5—Cl2vi3.385 (7)
Bi1A—O8Av2.891 (16)Bi5—Cl2Avii3.586 (7)
Bi1A—O9iii2.419 (16)Bi5—O1ii2.214 (16)
Bi2—Cl3ii3.247 (7)Bi5—O1Aiii2.479 (18)
Bi2—Cl3Aiii3.222 (7)Bi5—O52.322 (18)
Bi2—O22.235 (16)Bi5—O62.254 (19)
Bi2—O32.707 (19)Bi5—O92.300 (4)
Bi2—O4ii2.511 (17)Bi5A—Cl1iii3.470 (6)
Bi2—O4Aiii2.488 (17)Bi5A—Cl1Aiii3.439 (5)
Bi2—O7iv2.267 (18)Bi5A—Cl2vii3.316 (7)
Bi2—O8v2.21 (2)Bi5A—Cl2Avii3.320 (6)
Bi2A—Cl3iii3.152 (7)Bi5A—O1iii2.149 (17)
Bi2A—Cl3Aiii3.315 (7)Bi5A—O1Aiii2.142 (18)
Bi2A—O2A2.190 (16)Bi5A—O6A2.17 (2)
Bi2A—O3A2.569 (19)Bi5A—O5A2.476 (17)
Bi2A—O4iii2.256 (17)Bi6—O62.070 (17)
Bi2A—O4Aiii2.583 (17)Bi6—O72.09 (2)
Bi2A—O7v2.275 (18)Bi6—O8A2.128 (16)
Bi2A—O8Av2.581 (18)Bi6—Cl3Avii3.269 (7)
Bi3—Cl2ii3.320 (7)Bi6—Cl3vi3.436 (7)
Bi3—Cl2Aiii3.307 (6)Bi6—Cl2Avii3.438 (8)
Bi3—Cl3ii3.284 (9)Bi6—Cl2vi3.773 (8)
Bi3—Cl3Aiii3.292 (8)Bi6A—Cl2vii3.390 (8)
Bi3—O32.201 (17)Bi6A—Cl2Avii3.292 (8)
Bi3—O3ii2.244 (17)Bi6A—Cl3vii3.313 (7)
Bi3—O3Aiii2.304 (16)Bi6A—Cl3Avii3.373 (7)
Bi3—O42.171 (19)Bi6A—O82.07 (2)
Bi3A—Cl2iii3.339 (7)Bi6A—O8A2.102 (16)
Bi3A—Cl2Aiii3.312 (7)Bi6A—O6A2.107 (18)
Bi3A—Cl3iii3.370 (9)O1—O6Aiii2.67 (2)
Bi3A—Cl3Aiii3.327 (8)O1A—O9iii2.52 (3)
Bi3A—O3iii2.247 (17)O3—O3ii2.61 (3)
Bi3A—O3A2.227 (16)O3—O3Aiii2.66 (2)
Bi3A—O3Aiii2.248 (16)O4—O7viii2.59 (3)
Bi3A—O4A2.21 (2)O5—O92.68 (2)
Bi4—Cl1ii3.240 (6)O6—O92.690 (17)
Bi4—Cl1Aiii3.276 (5)O6A—O82.66 (3)
Bi4—Cl2ii3.362 (8)O7—O8A2.58 (2)
Bi4—Cl2Aiii3.447 (8)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1, y, z+1; (iii) x+1, y+1, z+1; (iv) x1, y, z1/2; (v) x1, y+1, z1/2; (vi) x, y, z+1/2; (vii) x, y+1, z+1/2; (viii) x+2, y, z+3/2.
Selected bond lengths (Å) for (bi24obr) top
Bi1—O12.30 (3)Bi3—O3ii2.254 (11)
Bi1—O1i2.61 (2)Bi3—O42.207 (19)
Bi1—O22.645 (19)Bi4—Br1viii3.4330 (18)
Bi1—O5ii2.463 (13)Bi4—Br2vii3.479 (3)
Bi1—O6iii2.654 (16)Bi4—O2ii2.266 (10)
Bi1—O8iv2.63 (7)Bi4—O42.27 (2)
Bi1—O8Av2.70 (6)Bi4—O52.18 (2)
Bi1—O9iii2.8039 (17)Bi5—Br1viii3.578 (2)
Bi2—Br3ii3.316 (4)Bi5—Br2ix3.470 (4)
Bi2—O22.20 (2)Bi5—O1ii2.240 (12)
Bi2—O32.68 (2)Bi5—O52.35 (2)
Bi2—O4ii2.459 (12)Bi5—O62.19 (2)
Bi2—O7iii2.43 (2)Bi5—O92.473 (2)
Bi2—O8vi2.12 (7)Bi6—Br3ix3.473 (4)
Bi2—O8Aiii2.52 (5)Bi6—O62.08 (2)
Bi3—Br2ii3.423 (3)Bi6—O72.24 (5)
Bi3—Br3vii3.412 (3)Bi6—O8x2.04 (7)
Bi3—Bi3vii3.600 (3)Bi6—O8A2.04 (8)
Bi3—O32.20 (2)Bi6—O8Ax2.43 (8)
Symmetry codes: (i) x, y, z; (ii) x+1, y+1/2, z+1/2; (iii) x1, y1/2, z1/2; (iv) x1, y+3/2, z1/2; (v) x1, y+1/2, z1/2; (vi) x1, y3/2, z1/2; (vii) x+1, y1/2, z+1/2; (viii) x, y1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) x, y+1, z.
 

Follow Acta Cryst. B
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds