Download citation
Download citation
link to html
The crystal structures of two new natural Bi oxysulfates with the formula Bi14O16(SO4)5 [labelled new phase I; monoclinic, space group C2, a = 21.658 (4), b = 5.6648 (9), c = 15.092 (3) Å, β = 119.433 (11)° and Z = 2] and Bi30O33(SO4)9(AsO4)2 [labelled new phase II; triclinic, space group P1, a = 5.670 (3), b = 13.9408 (9), c = 22.7908 (18) Å, α = 80.903 (5), β = 82.854 (14), γ = 78.27 (2)° and Z = 1] from the high-temperature fumarole deposit of the La Fossa crater at Vulcano (Aeolian Islands, Italy) are reported. The structures are built up by a combination of fluorite-related Bi—O units and isolated (SO4)2− tetrahedra (new phase I) or both (SO4)2− and (AsO4)3− tetrahedra (new phase II). Owing to the effect of stereoactive lone pairs of Bi3+, Bi—O units in both the structures can be suitably described in terms of oxo-centered OBi4 tetrahedra. The structure of Bi14O16(SO4)5 is based upon one-dimensional [O16Bi14]10+ ribbons formed by six chains of edge-sharing OBi4 tetrahedra extending along [010]. In the structure of Bi30O33(SO4)9(AsO4)2 the same ribbon type coexists with another one-dimensional ribbon formed by seven chains of edge-sharing OBi4 tetrahedra and with the composition [O17Bi16]14+. Ribbons of the same type are joined by (SO4)2− and (AsO4)3− tetrahedra along [010] – if a reduced triclinic unit-cell setting is considered – so forming two different (001) slabs which alternate to each other along [001] and are joined by additional (SO4)2− tetrahedra. New phase I represents the natural analogues of synthetic Bi14O16(SO4)5, but with an ordered structure model.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S205252061501358X/dk5037sup1.cif
Contains datablocks I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252061501358X/dk5037Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252061501358X/dk5037IIsup3.hkl
Contains datablock II

CCDC reference: 1413155

Computing details top

For both compounds, data reduction: SAINT-IRIX (Bruker, 2003); program(s) used to solve structure: SIR 2014 (Burla et al., 2014); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(I) Bi-sulfate top
Crystal data top
Bi14O36S5F(000) = 3028
Mr = 3630.02Dx = 7.54 Mg m3
Monoclinic, C2Melting point: Bi14 O36 S5 K
a = 21.658 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 5.6648 (9) ŵ = 76.52 mm1
c = 15.092 (3) ÅT = 293 K
β = 119.433 (11)°Needle, white
V = 1612.7 (5) Å30.53 × 0.04 × 0.02 mm
Z = 2
Data collection top
Bruker AXS X8 APEX2 with 2K-CCD detector
diffractometer
3034 independent reflections
Radiation source: fine-focus sealed tube2234 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.057
integration of the spots scansθmax = 26.4°, θmin = 1.6°
Absorption correction: numerical - needle
program WinGX (Farrugia, 2012)
h = 2626
Tmin = 0.062, Tmax = 0.309k = 67
5991 measured reflectionsl = 1818
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)] = 0.124 w = 1/[σ2(Fo2) + (0.1584P)2 + 1159.5515P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.342(Δ/σ)max = 0.001
S = 1.19Δρmax = 5.84 e Å3
3034 reflectionsΔρmin = 5.21 e Å3
143 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
10 restraintsAbsolute structure parameter: 0.72 (11)
Crystal data top
Bi14O36S5V = 1612.7 (5) Å3
Mr = 3630.02Z = 2
Monoclinic, C2Mo Kα radiation
a = 21.658 (4) ŵ = 76.52 mm1
b = 5.6648 (9) ÅT = 293 K
c = 15.092 (3) Å0.53 × 0.04 × 0.02 mm
β = 119.433 (11)°
Data collection top
Bruker AXS X8 APEX2 with 2K-CCD detector
diffractometer
3034 independent reflections
Absorption correction: numerical - needle
program WinGX (Farrugia, 2012)
2234 reflections with I > 2σ(I)
Tmin = 0.062, Tmax = 0.309Rint = 0.057
5991 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.124 w = 1/[σ2(Fo2) + (0.1584P)2 + 1159.5515P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.342Δρmax = 5.84 e Å3
S = 1.19Δρmin = 5.21 e Å3
3034 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
143 parametersAbsolute structure parameter: 0.72 (11)
10 restraints
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
Bi10.32061 (16)0.6216 (6)0.0357 (2)0.0215 (7)
Bi20.21038 (18)0.6834 (8)0.1551 (2)0.0349 (11)
Bi30.46302 (16)0.2140 (9)0.1037 (3)0.0305 (8)
Bi40.37244 (17)0.7054 (8)0.4221 (2)0.0280 (8)
Bi50.74335 (19)0.7158 (10)0.3680 (3)0.0387 (9)
Bi60.34840 (19)0.1510 (7)0.2310 (3)0.0328 (10)
Bi70.49262 (19)0.7215 (10)0.2911 (3)0.0367 (9)
S10.50000.229 (9)0.50000.032 (7)*
O170.556 (3)0.185 (16)0.473 (5)0.049 (18)*
S20.0837 (8)0.207 (4)0.1133 (11)0.012 (3)*
O90.085 (7)0.422 (14)0.059 (9)0.09 (4)*
O100.061 (9)0.03 (2)0.029 (9)0.13 (6)*
O110.1629 (14)0.21 (2)0.182 (5)0.06 (2)*
O120.021 (5)0.14 (3)0.123 (11)0.13 (5)*
S30.6270 (15)0.198 (7)0.376 (2)0.053 (7)*
O130.675 (7)0.25 (5)0.333 (11)0.16 (6)*
O140.667 (12)0.39 (3)0.448 (16)0.23 (12)*
O150.654 (6)0.015 (14)0.442 (8)0.08 (3)*
O160.566 (4)0.24 (3)0.392 (7)0.08 (3)*
O10.269 (3)0.930 (12)0.110 (5)0.024 (13)*
O20.269 (3)0.457 (10)0.112 (4)0.014 (11)*
O30.795 (4)0.470 (14)0.329 (6)0.035 (17)*
O40.305 (3)0.457 (10)0.327 (4)0.018 (12)*
O50.438 (4)0.948 (13)0.181 (5)0.034 (16)*
O60.351 (3)0.231 (15)0.017 (4)0.033 (12)*
O70.428 (3)0.452 (12)0.180 (5)0.027 (14)*
O80.397 (5)0.670 (18)0.303 (7)0.07 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.0207 (13)0.0169 (16)0.0315 (16)0.0000 (13)0.0163 (12)0.0061 (13)
Bi20.0314 (16)0.051 (3)0.0250 (15)0.0128 (17)0.0157 (13)0.0169 (17)
Bi30.0275 (15)0.0284 (18)0.0438 (18)0.0033 (17)0.0238 (14)0.0064 (19)
Bi40.0325 (16)0.0245 (19)0.0252 (14)0.0017 (16)0.0128 (12)0.0016 (16)
Bi50.0385 (18)0.030 (2)0.052 (2)0.0001 (19)0.0260 (16)0.009 (2)
Bi60.0308 (17)0.043 (3)0.0294 (16)0.0174 (14)0.0185 (14)0.0141 (14)
Bi70.0395 (18)0.036 (2)0.0355 (17)0.006 (2)0.0194 (15)0.000 (2)
Geometric parameters (Å, º) top
Bi1—O22.17 (5)Bi6—O5iii2.65 (7)
Bi1—O1i2.36 (6)Bi6—O42.71 (6)
Bi1—O62.36 (8)Bi6—Bi4iii3.672 (6)
Bi1—O72.46 (6)Bi7—O51.97 (7)
Bi1—O12.60 (7)Bi7—O72.19 (6)
Bi1—Bi33.576 (5)Bi7—O82.20 (9)
Bi1—Bi2i3.606 (6)S1—O17ix1.47 (2)
Bi1—Bi23.646 (4)S1—O171.47 (2)
Bi2—O22.12 (5)O17—O161.38 (10)
Bi2—O12.21 (6)S2—O91.48 (2)
Bi2—O6ii2.28 (6)S2—O101.48 (2)
Bi2—O42.72 (6)S2—O121.48 (2)
Bi2—Bi1ii3.606 (6)S2—O111.51 (2)
Bi3—O62.13 (6)O9—Bi3ii2.71 (6)
Bi3—O72.14 (6)O10—Bi3i2.56 (4)
Bi3—O5iii2.14 (7)O11—Bi5viii2.47 (6)
Bi3—O10ii2.56 (4)O12—Bi3viii2.66 (13)
Bi3—O12iv2.66 (13)S3—O161.47 (2)
Bi3—O9i2.71 (6)S3—O131.49 (2)
Bi4—O42.02 (6)S3—O141.49 (2)
Bi4—O82.11 (8)S3—O151.49 (2)
Bi4—O3v2.17 (7)O14—Bi5x2.7 (3)
Bi4—Bi6vi3.672 (6)O1—Bi6vi2.19 (7)
Bi5—O32.04 (8)O1—Bi1ii2.36 (6)
Bi5—O4iv2.20 (6)O3—Bi4xi2.17 (7)
Bi5—O11iv2.47 (6)O3—Bi6iv2.51 (7)
Bi5—O14vii2.7 (3)O4—Bi5viii2.20 (6)
Bi6—O1iii2.19 (7)O5—Bi3vi2.14 (7)
Bi6—O22.48 (5)O5—Bi6vi2.65 (7)
Bi6—O3viii2.51 (7)O6—Bi2i2.28 (6)
O2—Bi1—O1i83.9 (19)O3—Bi5—O11iv81 (3)
O2—Bi1—O684 (2)O4iv—Bi5—O11iv83 (3)
O1i—Bi1—O667 (2)O3—Bi5—O14vii109 (5)
O2—Bi1—O783 (2)O4iv—Bi5—O14vii80 (5)
O1i—Bi1—O7129 (2)O11iv—Bi5—O14vii158 (4)
O6—Bi1—O763 (2)O1iii—Bi6—O279 (2)
O2—Bi1—O167.6 (19)O1iii—Bi6—O3viii82 (2)
O1i—Bi1—O1112.1 (13)O2—Bi6—O3viii111 (2)
O6—Bi1—O1152 (2)O1iii—Bi6—O5iii84 (2)
O7—Bi1—O1107 (2)O2—Bi6—O5iii116 (2)
O2—Bi1—Bi399.5 (14)O3viii—Bi6—O5iii127 (2)
O1i—Bi1—Bi399.7 (16)O1iii—Bi6—O4119 (2)
O6—Bi1—Bi335.0 (14)O2—Bi6—O469.0 (17)
O7—Bi1—Bi335.9 (15)O3viii—Bi6—O464.0 (19)
O1—Bi1—Bi3143.4 (14)O5iii—Bi6—O4157.1 (19)
O2—Bi1—Bi2i100.8 (15)O1iii—Bi6—Bi4iii90.8 (17)
O1i—Bi1—Bi2i36.5 (15)O2—Bi6—Bi4iii146.0 (12)
O6—Bi1—Bi2i38.2 (14)O3viii—Bi6—Bi4iii35.1 (17)
O7—Bi1—Bi2i99.3 (15)O5iii—Bi6—Bi4iii94.7 (16)
O1—Bi1—Bi2i148.6 (14)O4—Bi6—Bi4iii88.3 (12)
Bi3—Bi1—Bi2i65.20 (10)O5—Bi7—O785 (2)
O2—Bi1—Bi231.4 (15)O5—Bi7—O887 (3)
O1i—Bi1—Bi293.7 (15)O7—Bi7—O872 (3)
O6—Bi1—Bi2115.7 (14)O17ix—S1—O17161 (8)
O7—Bi1—Bi299.4 (15)O16—O17—S1137 (6)
O1—Bi1—Bi236.9 (14)O9—S2—O1099 (7)
Bi3—Bi1—Bi2127.02 (12)O9—S2—O12123 (8)
Bi2i—Bi1—Bi2123.40 (13)O10—S2—O1288 (9)
O2—Bi2—O176 (2)O9—S2—O1192 (7)
O2—Bi2—O6ii80 (2)O10—S2—O11113 (8)
O1—Bi2—O6ii71 (2)O12—S2—O11136 (7)
O2—Bi2—O473.8 (18)S2—O9—Bi3ii154 (8)
O1—Bi2—O4108 (2)S2—O10—Bi3i173 (10)
O6ii—Bi2—O4153 (2)S2—O11—Bi5viii135 (4)
O2—Bi2—Bi1ii94.5 (15)S2—O12—Bi3viii130 (9)
O1—Bi2—Bi1ii39.4 (16)O16—S3—O13156 (10)
O6ii—Bi2—Bi1ii40 (2)O16—S3—O1490 (10)
O4—Bi2—Bi1ii147.8 (12)O13—S3—O1485 (10)
O2—Bi2—Bi132.3 (15)O16—S3—O1596 (7)
O1—Bi2—Bi144.9 (17)O13—S3—O15108 (10)
O6ii—Bi2—Bi166.5 (14)O14—S3—O15102 (10)
O4—Bi2—Bi193.3 (12)S3—O14—Bi5x110 (10)
Bi1ii—Bi2—Bi165.28 (8)O17—O16—S3132 (8)
O6—Bi3—O772 (3)Bi6vi—O1—Bi2116 (3)
O6—Bi3—O5iii81 (3)Bi6vi—O1—Bi1ii118 (3)
O7—Bi3—O5iii84 (2)Bi2—O1—Bi1ii104 (2)
O6—Bi3—O10ii76 (4)Bi6vi—O1—Bi1115 (3)
O7—Bi3—O10ii89 (4)Bi2—O1—Bi198 (2)
O5iii—Bi3—O10ii157 (4)Bi1ii—O1—Bi1104 (2)
O6—Bi3—O12iv111 (4)Bi2—O2—Bi1116 (3)
O7—Bi3—O12iv69 (3)Bi2—O2—Bi6121 (2)
O5iii—Bi3—O12iv144 (4)Bi1—O2—Bi6109 (2)
O10ii—Bi3—O12iv49 (5)Bi5—O3—Bi4xi130 (4)
O6—Bi3—O9i70 (3)Bi5—O3—Bi6iv111 (3)
O7—Bi3—O9i142 (3)Bi4xi—O3—Bi6iv103 (3)
O5iii—Bi3—O9i89 (3)Bi4—O4—Bi5viii124 (3)
O10ii—Bi3—O9i83 (4)Bi4—O4—Bi6120 (2)
O12iv—Bi3—O9i127 (4)Bi5viii—O4—Bi6100 (2)
O6—Bi3—Bi139 (2)Bi4—O4—Bi2107 (2)
O7—Bi3—Bi142.4 (17)Bi5viii—O4—Bi2106 (2)
O5iii—Bi3—Bi1101.2 (19)Bi6—O4—Bi294.9 (18)
O10ii—Bi3—Bi160 (4)Bi7—O5—Bi3vi135 (4)
O12iv—Bi3—Bi175 (3)Bi7—O5—Bi6vi106 (3)
O9i—Bi3—Bi1104 (2)Bi3vi—O5—Bi6vi106 (3)
O4—Bi4—O874 (3)Bi3—O6—Bi2i123 (3)
O4—Bi4—O3v88 (2)Bi3—O6—Bi1106 (3)
O8—Bi4—O3v87 (3)Bi2i—O6—Bi1102 (3)
O4—Bi4—Bi6vi98.6 (17)Bi3—O7—Bi7126 (3)
O8—Bi4—Bi6vi53 (3)Bi3—O7—Bi1102 (2)
O3v—Bi4—Bi6vi41.7 (19)Bi7—O7—Bi1112 (3)
O3—Bi5—O4iv81 (2)Bi4—O8—Bi7134 (4)
Symmetry codes: (i) x+1/2, y1/2, z; (ii) x+1/2, y+1/2, z; (iii) x, y1, z; (iv) x+1/2, y+1/2, z; (v) x1/2, y+1/2, z; (vi) x, y+1, z; (vii) x+3/2, y+1/2, z+1; (viii) x1/2, y1/2, z; (ix) x+1, y, z+1; (x) x+3/2, y1/2, z+1; (xi) x+1/2, y1/2, z.
(II) top
Crystal data top
As2Bi30O77S9Z = 4
Mr = 7939.87F(000) = 3290
Triclinic, P1Dx = 7.538 Mg m3
a = 5.670 (3) ÅMelting point: As2 Bi30 O77 S9 K
b = 13.9408 (9) ÅMo Kα radiation, λ = 0.71073 Å
c = 22.7908 (18) ŵ = 76.27 mm1
α = 80.903 (5)°T = 293 K
β = 82.854 (14)°Needle, white
γ = 78.27 (2)°0.22 × 0.01 × 0.01 mm
V = 1733.8 (10) Å3
Data collection top
Bruker AXS X8 APEX2 with 2K-CCD detector
diffractometer
10496 independent reflections
Radiation source: fine-focus sealed tube4123 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
integration of the spots scansθmax = 30.5°, θmin = 2.9°
Absorption correction: numerical - needle
program WinGX (Farrugia, 2012)
h = 68
Tmin = 0.355, Tmax = 0.474k = 1419
11765 measured reflectionsl = 3223
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)] = 0.119 w = 1/[σ2(Fo2) + (0.1967P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.374(Δ/σ)max = 0.006
S = 0.97Δρmax = 21.57 e Å3
10496 reflectionsΔρmin = 4.61 e Å3
567 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
3 restraintsAbsolute structure parameter: 0.00 (5)
Crystal data top
As2Bi30O77S9γ = 78.27 (2)°
Mr = 7939.87V = 1733.8 (10) Å3
Triclinic, P1Z = 4
a = 5.670 (3) ÅMo Kα radiation
b = 13.9408 (9) ŵ = 76.27 mm1
c = 22.7908 (18) ÅT = 293 K
α = 80.903 (5)°0.22 × 0.01 × 0.01 mm
β = 82.854 (14)°
Data collection top
Bruker AXS X8 APEX2 with 2K-CCD detector
diffractometer
10496 independent reflections
Absorption correction: numerical - needle
program WinGX (Farrugia, 2012)
4123 reflections with I > 2σ(I)
Tmin = 0.355, Tmax = 0.474Rint = 0.047
11765 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.1193 restraints
wR(F2) = 0.374Δρmax = 21.57 e Å3
S = 0.97Δρmin = 4.61 e Å3
10496 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
567 parametersAbsolute structure parameter: 0.00 (5)
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)
Bi10.9141 (11)0.7182 (5)0.4117 (3)0.0384 (14)
Bi20.0535 (8)0.2771 (4)0.5889 (3)0.0307 (11)
Bi30.8933 (9)0.0878 (5)0.2832 (2)0.0400 (13)
Bi40.2633 (8)0.9135 (4)0.7164 (2)0.0331 (11)
Bi50.5110 (8)0.6427 (4)0.3150 (3)0.0283 (11)
Bi60.4736 (8)0.3581 (4)0.6854 (2)0.0287 (11)
Bi70.6855 (8)0.4516 (4)0.1507 (2)0.0283 (11)
Bi80.2943 (9)0.5458 (4)0.8501 (3)0.0319 (12)
Bi90.0263 (10)0.8156 (4)0.2489 (2)0.0347 (11)
Bi100.1037 (8)0.1817 (4)0.7514 (2)0.0287 (10)
Bi110.4813 (8)0.0007 (4)0.1842 (2)0.0325 (11)
Bi120.6679 (8)0.9999 (4)0.8151 (2)0.0295 (10)
Bi130.2620 (9)0.3802 (5)0.0572 (2)0.0326 (12)
Bi140.7028 (8)0.6179 (4)0.9439 (2)0.0260 (10)
Bi150.8505 (9)0.1779 (4)0.1235 (3)0.0322 (11)
Bi160.1467 (8)0.8196 (4)0.8765 (2)0.0218 (9)
Bi170.1969 (11)0.1776 (7)0.3850 (3)0.0509 (19)
Bi180.7571 (8)0.8308 (7)0.6131 (3)0.0476 (18)
Bi190.9836 (7)0.9104 (4)0.0835 (2)0.0222 (9)
Bi200.9795 (8)0.0885 (4)0.9165 (2)0.0270 (10)
Bi210.5359 (9)0.7397 (4)0.1421 (3)0.0321 (12)
Bi220.4202 (7)0.2601 (4)0.8566 (2)0.0240 (9)
Bi230.2812 (11)0.2743 (6)0.2183 (3)0.0509 (19)
Bi240.7551 (14)0.7328 (6)0.7821 (3)0.0455 (16)
Bi250.4006 (17)0.9138 (6)0.3428 (3)0.060 (2)
Bi260.6882 (12)0.0926 (5)0.6538 (3)0.0504 (18)
Bi270.2042 (13)0.0121 (8)0.5500 (4)0.066 (2)
Bi280.6337 (14)0.3568 (7)0.3233 (4)0.064 (2)
Bi290.9137 (12)0.5526 (7)0.6128 (5)0.069 (3)
Bi300.4831 (12)0.4807 (6)0.5206 (4)0.0565 (18)
S10.148 (4)0.6229 (18)0.0487 (11)0.014 (4)*
O340.39 (2)0.594 (10)0.055 (6)0.07 (3)*
O350.125 (12)0.670 (6)0.988 (3)0.029 (15)*
O360.92 (2)0.535 (11)0.068 (7)0.08 (4)*
S20.815 (6)0.375 (3)0.9528 (17)0.036 (7)*
O370.95 (3)0.434 (12)0.921 (7)0.08 (4)*
O380.830 (12)0.310 (6)0.909 (3)0.025 (14)*
O390.71 (4)0.352 (19)0.017 (11)0.14 (8)*
O400.525 (16)0.441 (8)0.934 (4)0.04 (2)*
S30.070 (5)0.559 (2)0.2365 (14)0.023 (5)*
O410.98 (2)0.581 (11)0.290 (6)0.08 (4)*
O420.88 (2)0.631 (9)0.216 (5)0.06 (3)*
O430.301 (12)0.576 (6)0.195 (3)0.026 (14)*
O440.014 (14)0.456 (6)0.222 (4)0.035 (17)*
S40.864 (5)0.438 (3)0.7748 (15)0.029 (6)*
O450.73 (3)0.375 (12)0.788 (7)0.09 (4)*
O460.888 (17)0.445 (8)0.692 (5)0.05 (2)*
S50.558 (7)0.870 (3)0.972 (2)0.044 (9)*
O470.322 (14)0.914 (7)0.954 (4)0.037 (17)*
O480.617 (17)0.788 (8)0.927 (5)0.05 (2)*
O490.79 (3)0.916 (12)0.953 (7)0.08 (4)*
O500.42 (2)0.808 (11)0.036 (6)0.07 (3)*
S60.604 (6)0.240 (3)0.4964 (17)0.036 (7)*
O510.534 (15)0.312 (7)0.527 (4)0.036 (18)*
O520.46 (3)0.147 (13)0.525 (7)0.09 (4)*
As70.077 (2)0.4437 (11)0.3858 (6)0.005 (4)*0.25 (8)
S70.077 (2)0.4437 (11)0.3858 (6)0.005 (4)*0.75 (8)
O530.232 (19)0.519 (9)0.409 (5)0.05 (2)*
O540.825 (17)0.533 (8)0.401 (4)0.04 (2)*
S80.400 (4)0.1251 (18)0.0310 (11)0.012 (4)*
O550.314 (17)0.192 (8)0.064 (5)0.05 (2)*
O560.367 (14)0.153 (7)0.967 (4)0.035 (17)*
O570.201 (14)0.069 (7)0.055 (4)0.033 (17)*
As90.770 (2)0.9817 (10)0.4510 (6)0.019 (4)*0.71 (10)
S90.770 (2)0.9817 (10)0.4510 (6)0.019 (4)*0.29 (10)
O580.586 (16)0.030 (7)0.405 (4)0.04 (2)*
O590.823 (16)0.888 (8)0.391 (5)0.04 (2)*
As100.3156 (17)0.6413 (8)0.6790 (5)0.007 (3)*0.72 (8)
S100.3156 (17)0.6413 (8)0.6790 (5)0.007 (3)*0.28 (8)
O600.10 (3)0.722 (12)0.687 (7)0.09 (4)*
S110.367 (10)0.734 (5)0.513 (3)0.070 (14)*
O610.188 (14)0.661 (7)0.525 (4)0.034 (17)*
O620.37 (2)0.740 (9)0.455 (5)0.06 (3)*
O10.683 (16)0.440 (7)0.590 (4)0.04 (2)*
O20.428 (13)0.240 (6)0.318 (4)0.027 (15)*
O30.252 (12)0.139 (6)0.853 (3)0.022 (14)*
O40.556 (12)0.162 (6)0.195 (4)0.023 (15)*
O50.849 (11)0.058 (5)0.735 (3)0.019 (13)*
O60.380 (11)0.844 (6)0.804 (3)0.020 (14)*
O70.781 (14)0.254 (7)0.664 (4)0.029 (17)*
O80.725 (10)0.843 (5)0.148 (3)0.013 (11)*
O90.726 (11)0.147 (5)0.857 (3)0.017 (12)*
O100.19 (2)0.450 (9)0.586 (6)0.06 (3)*
O110.965 (17)0.953 (8)0.607 (5)0.05 (2)*
O120.950 (10)0.650 (5)0.870 (3)0.016 (12)*
O130.230 (11)0.850 (5)0.151 (3)0.018 (13)*
O140.150 (15)0.945 (7)0.274 (4)0.04 (2)*
O150.325 (12)0.059 (6)0.731 (4)0.025 (15)*
O160.199 (11)0.745 (6)0.339 (3)0.018 (13)*
O170.917 (11)0.839 (5)0.805 (3)0.019 (13)*
O180.281 (10)0.253 (5)0.666 (3)0.015 (12)*
O190.960 (17)0.248 (8)0.318 (5)0.04 (2)*
O200.456 (16)0.954 (8)0.616 (5)0.04 (2)*
O210.021 (18)0.353 (8)0.115 (5)0.05 (2)*
O220.466 (12)0.638 (6)0.873 (3)0.025 (14)*
O230.689 (13)0.748 (7)0.339 (4)0.029 (17)*
O240.635 (15)0.960 (7)0.272 (4)0.04 (2)*
O250.076 (16)0.156 (8)0.195 (5)0.04 (2)*
O260.097 (11)0.108 (5)0.614 (3)0.019 (12)*
O270.431 (14)0.747 (7)0.231 (4)0.037 (18)*
O280.422 (13)0.251 (6)0.763 (3)0.030 (15)*
O290.849 (14)0.011 (6)0.145 (4)0.033 (17)*
O300.982 (15)0.977 (7)0.853 (4)0.040 (19)*
O310.63 (2)0.343 (10)0.232 (6)0.07 (3)*
O320.62 (3)0.853 (12)0.708 (7)0.04 (3)*0.60
O330.23 (3)1.092 (12)0.324 (7)0.04 (3)*0.60
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.041 (3)0.043 (3)0.029 (3)0.009 (2)0.002 (2)0.003 (2)
Bi20.031 (2)0.033 (3)0.031 (3)0.0108 (19)0.0056 (18)0.004 (2)
Bi30.030 (2)0.062 (4)0.029 (2)0.013 (2)0.0007 (18)0.004 (2)
Bi40.0223 (18)0.050 (3)0.029 (2)0.0082 (19)0.0061 (16)0.007 (2)
Bi50.0229 (19)0.030 (3)0.036 (3)0.0116 (18)0.0031 (17)0.007 (2)
Bi60.0222 (18)0.024 (2)0.037 (3)0.0080 (16)0.0047 (17)0.007 (2)
Bi70.0238 (18)0.028 (2)0.031 (3)0.0028 (17)0.0007 (16)0.002 (2)
Bi80.036 (2)0.022 (2)0.039 (3)0.0045 (19)0.009 (2)0.005 (2)
Bi90.036 (2)0.030 (2)0.036 (3)0.0058 (19)0.0003 (19)0.0031 (19)
Bi100.029 (2)0.0235 (19)0.036 (2)0.0049 (16)0.0086 (17)0.0064 (17)
Bi110.023 (2)0.045 (3)0.029 (2)0.0062 (18)0.0026 (16)0.005 (2)
Bi120.0255 (19)0.034 (2)0.031 (2)0.0079 (17)0.0001 (16)0.0085 (18)
Bi130.034 (2)0.039 (3)0.022 (2)0.002 (2)0.0068 (17)0.001 (2)
Bi140.0196 (17)0.028 (2)0.030 (3)0.0063 (16)0.0038 (15)0.0073 (19)
Bi150.032 (2)0.037 (3)0.025 (2)0.000 (2)0.0051 (17)0.002 (2)
Bi160.0207 (18)0.021 (2)0.022 (2)0.0022 (15)0.0019 (14)0.0028 (16)
Bi170.038 (2)0.094 (6)0.031 (3)0.025 (3)0.001 (2)0.025 (3)
Bi180.0206 (18)0.089 (5)0.036 (3)0.007 (2)0.0035 (18)0.025 (3)
Bi190.0213 (15)0.025 (2)0.020 (2)0.0020 (15)0.0020 (13)0.0059 (17)
Bi200.0231 (18)0.034 (3)0.025 (2)0.0090 (17)0.0003 (15)0.003 (2)
Bi210.035 (2)0.030 (3)0.034 (3)0.015 (2)0.0029 (19)0.004 (2)
Bi220.0178 (15)0.026 (2)0.029 (2)0.0030 (15)0.0018 (14)0.0075 (18)
Bi230.042 (3)0.071 (4)0.026 (3)0.023 (3)0.002 (2)0.010 (3)
Bi240.067 (4)0.057 (4)0.027 (3)0.040 (3)0.001 (2)0.015 (2)
Bi250.090 (5)0.064 (4)0.040 (3)0.057 (4)0.030 (3)0.026 (3)
Bi260.062 (4)0.046 (3)0.038 (3)0.022 (3)0.029 (3)0.015 (2)
Bi270.048 (3)0.093 (7)0.056 (5)0.013 (4)0.012 (3)0.001 (4)
Bi280.060 (4)0.060 (5)0.072 (6)0.009 (4)0.012 (3)0.010 (4)
Bi290.040 (3)0.061 (5)0.106 (7)0.011 (3)0.005 (3)0.011 (5)
Bi300.052 (3)0.062 (4)0.058 (4)0.013 (3)0.010 (3)0.011 (3)
Geometric parameters (Å, º) top
Bi1—O232.16 (8)Bi24—O322.26 (15)
Bi1—O16i2.21 (7)Bi24—O62.41 (7)
Bi1—O592.30 (11)Bi24—O122.41 (6)
Bi2—O7ii2.18 (8)Bi24—O60i2.74 (16)
Bi2—O182.25 (6)Bi25—O242.07 (9)
Bi2—O262.30 (7)Bi25—O142.19 (9)
Bi2—O102.68 (13)Bi25—O332.46 (16)
Bi2—Bi26ii3.646 (11)Bi25—O232.56 (8)
Bi3—O33iii2.22 (15)Bi25—O592.70 (10)
Bi3—O14iii2.24 (9)Bi25—O58v2.75 (10)
Bi3—O25i2.31 (10)Bi25—Bi3vii3.619 (12)
Bi3—O192.59 (11)Bi25—Bi11v3.629 (9)
Bi3—O24iv2.59 (10)Bi26—O52.10 (7)
Bi3—Bi17i3.565 (8)Bi26—O26i2.43 (6)
Bi3—Bi25iii3.619 (13)Bi26—O72.47 (9)
Bi3—Bi153.679 (8)Bi26—O11iv2.52 (10)
Bi4—O322.04 (14)Bi26—O152.61 (8)
Bi4—O62.19 (7)Bi26—Bi27i3.633 (11)
Bi4—O15v2.21 (8)Bi26—Bi2i3.646 (11)
Bi4—O202.44 (10)Bi26—Bi12iv3.694 (8)
Bi4—Bi183.553 (7)Bi27—O11viii1.97 (10)
Bi4—Bi243.654 (10)Bi27—O262.08 (7)
Bi5—O232.11 (9)Bi27—O20iv2.16 (10)
Bi5—O162.11 (7)Bi27—O522.54 (17)
Bi5—O272.24 (9)Bi27—Bi26ii3.633 (11)
Bi5—O412.64 (13)Bi28—O312.12 (14)
Bi5—Bi93.579 (8)Bi28—O192.15 (9)
Bi6—O72.09 (8)Bi28—O22.21 (8)
Bi6—O182.12 (7)Bi29—O10i2.01 (12)
Bi6—O282.16 (8)Bi29—O462.17 (11)
Bi6—O12.57 (10)Bi29—O12.39 (10)
Bi6—Bi103.586 (8)Bi29—Bi30i3.675 (11)
Bi7—O312.23 (14)Bi30—O11.99 (10)
Bi7—O21i2.25 (10)Bi30—O102.14 (12)
Bi7—O362.43 (15)Bi30—O512.29 (9)
Bi7—O44i2.63 (8)Bi30—O612.73 (8)
Bi7—O432.69 (7)Bi30—Bi29ii3.675 (11)
Bi8—O221.93 (8)S1—O341.39 (12)
Bi8—O12ii2.23 (6)S1—O35ix1.45 (8)
Bi8—O402.54 (10)S1—O36ii1.93 (15)
Bi9—O142.24 (10)O35—S1x1.45 (8)
Bi9—O272.31 (8)O36—S1i1.93 (15)
Bi9—O162.36 (7)O36—Bi13i2.62 (14)
Bi9—O132.41 (7)S2—O371.30 (16)
Bi9—O24ii2.74 (9)S2—O381.44 (9)
Bi9—Bi213.636 (8)S2—O39x1.5 (2)
Bi10—O151.98 (8)S2—O401.78 (10)
Bi10—O182.26 (7)O39—S2ix1.5 (2)
Bi10—O282.28 (8)S3—O41ii1.33 (14)
Bi10—O32.50 (8)S3—O42ii1.38 (12)
Bi10—O5ii2.57 (7)S3—O431.55 (8)
Bi10—Bi223.586 (7)S3—O441.63 (9)
Bi11—O292.18 (8)O41—S3i1.33 (14)
Bi11—O24iv2.22 (10)O41—O421.83 (18)
Bi11—O42.42 (8)O42—S3i1.38 (12)
Bi11—O8iv2.54 (6)O44—Bi7ii2.63 (8)
Bi11—O14iv2.72 (9)S4—O451.23 (17)
Bi11—Bi153.565 (8)S4—O461.86 (11)
Bi11—Bi19iv3.576 (6)S5—O471.44 (9)
Bi11—Bi25iv3.629 (9)S5—O491.55 (16)
Bi12—O302.02 (9)S5—O481.62 (12)
Bi12—O5v2.11 (7)S5—O50x1.75 (15)
Bi12—O172.43 (7)O50—S5ix1.75 (15)
Bi12—O9v2.49 (7)S6—O511.29 (10)
Bi12—Bi16i3.564 (7)S6—O521.68 (17)
Bi12—Bi20v3.578 (7)As7—O531.68 (12)
Bi12—Bi26v3.694 (8)As7—O54ii1.74 (10)
Bi13—O211.83 (11)O54—S7i1.74 (10)
Bi13—O552.57 (11)O54—As7i1.74 (10)
Bi13—O392.6 (2)S8—O551.27 (11)
Bi13—O36ii2.62 (14)S8—O56ix1.47 (9)
Bi14—O122.11 (7)S8—O571.51 (9)
Bi14—O222.17 (7)O56—S8x1.47 (9)
Bi14—O482.31 (11)O57—Bi19viii2.69 (9)
Bi14—O372.75 (15)O57—Bi15ii2.73 (8)
Bi15—O25i2.13 (10)As9—O58v1.54 (9)
Bi15—O42.21 (7)As9—O591.99 (11)
Bi15—O292.31 (9)O58—S9iv1.54 (9)
Bi15—O57i2.73 (8)O58—As9iv1.54 (9)
Bi16—O62.02 (7)O58—Bi25iv2.75 (10)
Bi16—O17ii2.17 (7)As10—O601.50 (16)
Bi16—O30ii2.22 (9)O60—Bi18ii2.78 (16)
Bi16—O472.74 (9)O60—Bi24ii2.74 (15)
Bi16—Bi12ii3.564 (7)S11—O621.31 (13)
Bi17—O33iv1.94 (16)S11—O611.54 (11)
Bi17—O22.09 (8)O3—Bi20ii2.13 (7)
Bi17—O19ii2.15 (10)O5—Bi12iv2.11 (7)
Bi17—O582.73 (9)O5—Bi10i2.57 (7)
Bi17—Bi3ii3.565 (8)O7—Bi2i2.18 (8)
Bi18—O202.16 (10)O8—Bi11v2.54 (6)
Bi18—O112.24 (11)O9—Bi12iv2.49 (7)
Bi18—O322.26 (15)O10—Bi29ii2.01 (12)
Bi18—O60i2.78 (16)O11—Bi27vi1.97 (10)
Bi19—O29v2.11 (9)O11—Bi26v2.52 (10)
Bi19—O13i2.16 (7)O12—Bi8i2.23 (6)
Bi19—O82.18 (6)O13—Bi19ii2.16 (7)
Bi19—O57vi2.69 (9)O14—Bi3vii2.24 (9)
Bi19—Bi11v3.576 (7)O14—Bi11v2.72 (9)
Bi20—O92.06 (6)O15—Bi4iv2.21 (8)
Bi20—O3i2.13 (7)O16—Bi1ii2.21 (7)
Bi20—O30iv2.28 (10)O17—Bi16i2.17 (7)
Bi20—Bi12iv3.578 (7)O19—Bi17i2.15 (10)
Bi21—O82.00 (6)O19—Bi23i2.75 (10)
Bi21—O272.06 (9)O20—Bi27v2.16 (10)
Bi21—O132.09 (6)O21—Bi7ii2.25 (10)
Bi21—O502.57 (14)O24—Bi11v2.22 (10)
Bi22—O92.09 (6)O24—Bi3v2.59 (10)
Bi22—O32.12 (8)O24—Bi9i2.74 (9)
Bi22—O282.15 (8)O25—Bi15ii2.13 (10)
Bi22—O562.73 (9)O25—Bi3ii2.31 (10)
Bi23—O42.06 (7)O26—Bi26ii2.43 (6)
Bi23—O252.37 (11)O29—Bi19iv2.11 (9)
Bi23—O312.45 (13)O30—Bi16i2.22 (9)
Bi23—O22.46 (8)O30—Bi20v2.28 (10)
Bi23—O442.68 (8)O33—Bi17v1.94 (16)
Bi23—O19ii2.75 (10)O33—Bi3vii2.22 (15)
Bi24—O172.05 (7)
O23—Bi1—O16i83 (3)O25—Bi23—O44115 (3)
O23—Bi1—O5975 (3)O31—Bi23—O4488 (4)
O16i—Bi1—O5979 (3)O2—Bi23—O44101 (3)
O7ii—Bi2—O1880 (3)O4—Bi23—O19ii121 (3)
O7ii—Bi2—O2675 (3)O25—Bi23—O19ii77 (3)
O18—Bi2—O2680 (2)O31—Bi23—O19ii116 (4)
O7ii—Bi2—O10111 (4)O2—Bi23—O19ii61 (3)
O18—Bi2—O1075 (3)O44—Bi23—O19ii77 (3)
O26—Bi2—O10153 (3)O17—Bi24—O3283 (4)
O7ii—Bi2—Bi26ii41 (2)O17—Bi24—O685 (3)
O18—Bi2—Bi26ii95.4 (18)O32—Bi24—O663 (4)
O26—Bi2—Bi26ii40.8 (15)O17—Bi24—O1277 (2)
O10—Bi2—Bi26ii152 (3)O32—Bi24—O12160 (4)
O33iii—Bi3—O14iii72 (5)O6—Bi24—O12114 (2)
O33iii—Bi3—O25i87 (5)O17—Bi24—O60i86 (4)
O14iii—Bi3—O25i88 (3)O32—Bi24—O60i72 (5)
O33iii—Bi3—O1959 (5)O6—Bi24—O60i135 (4)
O14iii—Bi3—O19130 (3)O12—Bi24—O60i107 (4)
O25i—Bi3—O1982 (4)O17—Bi24—Bi493.6 (19)
O33iii—Bi3—O24iv138 (5)O32—Bi24—Bi430 (4)
O14iii—Bi3—O24iv73 (3)O6—Bi24—Bi435.4 (18)
O25i—Bi3—O24iv115 (3)O12—Bi24—Bi4149.2 (15)
O19—Bi3—O24iv154 (3)O60i—Bi24—Bi4101 (3)
O33iii—Bi3—Bi17i29 (4)O24—Bi25—O1482 (4)
O14iii—Bi3—Bi17i99 (2)O24—Bi25—O3379 (4)
O25i—Bi3—Bi17i99 (3)O14—Bi25—O3369 (4)
O19—Bi3—Bi17i37 (2)O24—Bi25—O2383 (3)
O24iv—Bi3—Bi17i145 (2)O14—Bi25—O23112 (3)
O33iii—Bi3—Bi25iii42 (4)O33—Bi25—O23162 (4)
O14iii—Bi3—Bi25iii35 (2)O24—Bi25—O5977 (3)
O25i—Bi3—Bi25iii101 (2)O14—Bi25—O59158 (3)
O19—Bi3—Bi25iii100 (2)O33—Bi25—O59110 (4)
O24iv—Bi3—Bi25iii97 (2)O23—Bi25—O5962 (3)
Bi17i—Bi3—Bi25iii65.0 (2)O24—Bi25—O58v85 (3)
O33iii—Bi3—Bi15120 (4)O14—Bi25—O58v134 (3)
O14iii—Bi3—Bi1598 (2)O33—Bi25—O58v66 (4)
O25i—Bi3—Bi1533 (2)O23—Bi25—O58v110 (3)
O19—Bi3—Bi1599 (2)O59—Bi25—O58v48 (3)
O24iv—Bi3—Bi1588 (2)O24—Bi25—Bi3vii91 (3)
Bi17i—Bi3—Bi15127.7 (2)O14—Bi25—Bi3vii36 (3)
Bi25iii—Bi3—Bi15124.4 (2)O33—Bi25—Bi3vii37 (4)
O32—Bi4—O670 (5)O23—Bi25—Bi3vii147.7 (19)
O32—Bi4—O15v94 (5)O59—Bi25—Bi3vii147 (2)
O6—Bi4—O15v92 (3)O58v—Bi25—Bi3vii101.4 (19)
O32—Bi4—O2067 (5)O24—Bi25—Bi11v34 (3)
O6—Bi4—O20137 (3)O14—Bi25—Bi11v48 (2)
O15v—Bi4—O2085 (3)O33—Bi25—Bi11v71 (4)
O32—Bi4—Bi1836 (4)O23—Bi25—Bi11v95.9 (19)
O6—Bi4—Bi18104.3 (18)O59—Bi25—Bi11v110 (2)
O15v—Bi4—Bi18103.9 (19)O58v—Bi25—Bi11v110 (2)
O20—Bi4—Bi1837 (2)Bi3vii—Bi25—Bi11v64.7 (2)
O32—Bi4—Bi2434 (4)O5—Bi26—O26i82 (2)
O6—Bi4—Bi2439.5 (18)O5—Bi26—O780 (3)
O15v—Bi4—Bi24105.4 (19)O26i—Bi26—O768 (2)
O20—Bi4—Bi24100 (2)O5—Bi26—O11iv94 (3)
Bi18—Bi4—Bi2465.09 (18)O26i—Bi26—O11iv60 (3)
O23—Bi5—O1683 (3)O7—Bi26—O11iv127 (3)
O23—Bi5—O2787 (3)O5—Bi26—O1578 (3)
O16—Bi5—O2774 (3)O26i—Bi26—O15160 (2)
O23—Bi5—O4173 (4)O7—Bi26—O15109 (3)
O16—Bi5—O41155 (4)O11iv—Bi26—O15121 (3)
O27—Bi5—O41100 (4)O5—Bi26—Bi27i100.4 (18)
O23—Bi5—Bi997 (2)O26i—Bi26—Bi27i33.2 (17)
O16—Bi5—Bi939 (2)O7—Bi26—Bi27i98.1 (19)
O27—Bi5—Bi939 (2)O11iv—Bi26—Bi27i31 (2)
O41—Bi5—Bi9138 (3)O15—Bi26—Bi27i152.1 (18)
O7—Bi6—O1884 (3)O5—Bi26—Bi2i95 (2)
O7—Bi6—O2884 (3)O26i—Bi26—Bi2i38.3 (16)
O18—Bi6—O2870 (3)O7—Bi26—Bi2i36 (2)
O7—Bi6—O175 (3)O11iv—Bi26—Bi2i94 (2)
O18—Bi6—O1111 (3)O15—Bi26—Bi2i144.0 (18)
O28—Bi6—O1159 (3)Bi27i—Bi26—Bi2i63.6 (2)
O7—Bi6—Bi1096 (2)O5—Bi26—Bi12iv28.9 (19)
O18—Bi6—Bi1036.5 (18)O26i—Bi26—Bi12iv110.5 (16)
O28—Bi6—Bi1037 (2)O7—Bi26—Bi12iv95 (2)
O1—Bi6—Bi10147 (2)O11iv—Bi26—Bi12iv103 (2)
O31—Bi7—O21i93 (4)O15—Bi26—Bi12iv49.4 (17)
O31—Bi7—O36156 (5)Bi27i—Bi26—Bi12iv122.0 (2)
O21i—Bi7—O3666 (4)Bi2i—Bi26—Bi12iv120.5 (2)
O31—Bi7—O44i73 (4)O11viii—Bi27—O2675 (4)
O21i—Bi7—O44i75 (3)O11viii—Bi27—O20iv86 (4)
O36—Bi7—O44i90 (4)O26—Bi27—O20iv77 (3)
O31—Bi7—O4388 (4)O11viii—Bi27—O52147 (5)
O21i—Bi7—O43177 (3)O26—Bi27—O5272 (4)
O36—Bi7—O43112 (4)O20iv—Bi27—O5283 (5)
O44i—Bi7—O43102 (2)O11viii—Bi27—Bi26ii42 (3)
O22—Bi8—O12ii88 (3)O26—Bi27—Bi26ii39.6 (18)
O22—Bi8—O4078 (3)O20iv—Bi27—Bi26ii96 (3)
O12ii—Bi8—O40121 (3)O52—Bi27—Bi26ii109 (4)
O14—Bi9—O2787 (3)O31—Bi28—O1984 (4)
O14—Bi9—O1679 (3)O31—Bi28—O272 (4)
O27—Bi9—O1668 (3)O19—Bi28—O288 (3)
O14—Bi9—O1388 (3)O10i—Bi29—O4684 (4)
O27—Bi9—O1361 (3)O10i—Bi29—O183 (4)
O16—Bi9—O13128 (2)O46—Bi29—O174 (4)
O14—Bi9—O24ii70 (3)O10i—Bi29—Bi30i29 (4)
O27—Bi9—O24ii157 (3)O46—Bi29—Bi30i110 (3)
O16—Bi9—O24ii110 (3)O1—Bi29—Bi30i100 (2)
O13—Bi9—O24ii112 (3)O1—Bi30—O1083 (4)
O14—Bi9—Bi593 (2)O1—Bi30—O5180 (4)
O27—Bi9—Bi537 (2)O10—Bi30—O5179 (4)
O16—Bi9—Bi534.4 (16)O1—Bi30—O61112 (3)
O13—Bi9—Bi598.2 (15)O10—Bi30—O6176 (4)
O24ii—Bi9—Bi5144 (2)O51—Bi30—O61150 (3)
O14—Bi9—Bi2198 (2)O1—Bi30—Bi29ii95 (3)
O27—Bi9—Bi2132 (2)O10—Bi30—Bi29ii27 (3)
O16—Bi9—Bi2199.6 (16)O51—Bi30—Bi29ii105 (2)
O13—Bi9—Bi2133.1 (16)O61—Bi30—Bi29ii49.6 (18)
O24ii—Bi9—Bi21145 (2)O34—S1—O35ix107 (6)
Bi5—Bi9—Bi2166.45 (16)O34—S1—O36ii124 (7)
O15—Bi10—O1884 (3)O35ix—S1—O36ii108 (5)
O15—Bi10—O2891 (3)S1i—O36—Bi7144 (8)
O18—Bi10—O2865 (3)S1i—O36—Bi13i91 (5)
O15—Bi10—O387 (3)Bi7—O36—Bi13i95 (5)
O18—Bi10—O3129 (2)O37—S2—O3896 (8)
O28—Bi10—O365 (3)O37—S2—O39x138 (10)
O15—Bi10—O5ii71 (3)O38—S2—O39x124 (10)
O18—Bi10—O5ii113 (2)O37—S2—O4099 (8)
O28—Bi10—O5ii162 (2)O38—S2—O4092 (5)
O3—Bi10—O5ii110 (2)O39x—S2—O4091 (10)
O15—Bi10—Bi699 (2)S2—O37—Bi14103 (8)
O18—Bi10—Bi633.8 (17)S2ix—O39—Bi13126 (10)
O28—Bi10—Bi635 (2)S2—O40—Bi8145 (5)
O3—Bi10—Bi699.8 (17)O41ii—S3—O42ii85 (8)
O5ii—Bi10—Bi6147.2 (16)O41ii—S3—O43134 (7)
O15—Bi10—Bi22102 (2)O42ii—S3—O43107 (6)
O18—Bi10—Bi2299.1 (17)O41ii—S3—O44114 (7)
O28—Bi10—Bi2235 (2)O42ii—S3—O44105 (6)
O3—Bi10—Bi2235.4 (18)O43—S3—O44105 (4)
O5ii—Bi10—Bi22145.6 (16)S3i—O41—O4249 (6)
Bi6—Bi10—Bi2266.27 (15)S3i—O41—Bi5121 (8)
O29—Bi11—O24iv87 (3)O42—O41—Bi578 (6)
O29—Bi11—O472 (3)S3i—O42—O4146 (6)
O24iv—Bi11—O482 (3)S3—O43—Bi7133 (4)
O29—Bi11—O8iv65 (3)S3—O44—Bi7ii122 (4)
O24iv—Bi11—O8iv91 (3)S3—O44—Bi23134 (4)
O4—Bi11—O8iv137 (2)Bi7ii—O44—Bi23100 (3)
O29—Bi11—O14iv153 (3)O45—S4—O4698 (8)
O24iv—Bi11—O14iv68 (3)S4—O46—Bi29140 (6)
O4—Bi11—O14iv109 (3)O47—S5—O49124 (8)
O8iv—Bi11—O14iv107 (2)O47—S5—O4896 (6)
O29—Bi11—Bi1539 (2)O49—S5—O4897 (7)
O24iv—Bi11—Bi1596 (2)O47—S5—O50x89 (6)
O4—Bi11—Bi1537.5 (17)O49—S5—O50x139 (8)
O8iv—Bi11—Bi15102.2 (14)O48—S5—O50x102 (7)
O14iv—Bi11—Bi15147 (2)S5—O47—Bi16116 (5)
O29—Bi11—Bi19iv33 (2)S5—O48—Bi14132 (6)
O24iv—Bi11—Bi19iv102 (2)S5ix—O50—Bi21135 (7)
O4—Bi11—Bi19iv102.7 (17)O51—S6—O52110 (7)
O8iv—Bi11—Bi19iv37.2 (14)S6—O51—Bi30144 (6)
O14iv—Bi11—Bi19iv144 (2)S6—O52—Bi27170 (9)
Bi15—Bi11—Bi19iv65.85 (15)O53—As7—O54ii85 (5)
O29—Bi11—Bi25iv117 (2)S7i—O54—As7i0.0 (12)
O24iv—Bi11—Bi25iv31 (2)O55—S8—O56ix116 (6)
O4—Bi11—Bi25iv95.8 (19)O55—S8—O5792 (6)
O8iv—Bi11—Bi25iv99.5 (14)O56ix—S8—O57104 (5)
O14iv—Bi11—Bi25iv36.9 (19)S8—O55—Bi13138 (7)
Bi15—Bi11—Bi25iv122.8 (2)S8x—O56—Bi22155 (5)
Bi19iv—Bi11—Bi25iv125.5 (2)S8—O57—Bi19viii157 (5)
O30—Bi12—O5v88 (3)S8—O57—Bi15ii111 (5)
O30—Bi12—O1767 (3)Bi19viii—O57—Bi15ii91 (2)
O5v—Bi12—O1789 (3)O58v—As9—O5976 (5)
O30—Bi12—O9v67 (3)S9iv—O58—As9iv0.0 (14)
O5v—Bi12—O9v87 (3)S9iv—O58—Bi17144 (5)
O17—Bi12—O9v134 (2)As9iv—O58—Bi17144 (5)
O30—Bi12—Bi16i34 (3)S9iv—O58—Bi25iv120 (5)
O5v—Bi12—Bi16i100.8 (18)As9iv—O58—Bi25iv120 (5)
O17—Bi12—Bi16i36.6 (16)Bi17—O58—Bi25iv90 (3)
O9v—Bi12—Bi16i99.8 (14)As9—O59—Bi1126 (5)
O30—Bi12—Bi20v36 (3)As9—O59—Bi25106 (4)
O5v—Bi12—Bi20v98 (2)Bi1—O59—Bi25101 (4)
O17—Bi12—Bi20v102.0 (16)As10—O60—Bi18ii134 (9)
O9v—Bi12—Bi20v34.0 (15)As10—O60—Bi24ii127 (9)
Bi16i—Bi12—Bi20v66.19 (15)Bi18ii—O60—Bi24ii89 (4)
O30—Bi12—Bi26v117 (3)O62—S11—O6193 (7)
O5v—Bi12—Bi26v28.7 (19)S11—O61—Bi30103 (4)
O17—Bi12—Bi26v96.0 (17)Bi30—O1—Bi29119 (5)
O9v—Bi12—Bi26v101.5 (16)Bi30—O1—Bi6116 (4)
Bi16i—Bi12—Bi26v121.60 (17)Bi29—O1—Bi6111 (4)
Bi20v—Bi12—Bi26v123.2 (2)Bi17—O2—Bi28128 (4)
O21—Bi13—O5578 (4)Bi17—O2—Bi23115 (3)
O21—Bi13—O39150 (6)Bi28—O2—Bi23106 (3)
O55—Bi13—O3984 (6)Bi22—O3—Bi20ii126 (4)
O21—Bi13—O36ii68 (5)Bi22—O3—Bi10101 (3)
O55—Bi13—O36ii140 (4)Bi20ii—O3—Bi10110 (3)
O39—Bi13—O36ii135 (7)Bi23—O4—Bi15125 (4)
O12—Bi14—O2281 (3)Bi23—O4—Bi11122 (3)
O12—Bi14—O4877 (3)Bi15—O4—Bi11100 (3)
O22—Bi14—O4881 (3)Bi26—O5—Bi12iv122 (3)
O12—Bi14—O3777 (4)Bi26—O5—Bi10i114 (3)
O22—Bi14—O3795 (4)Bi12iv—O5—Bi10i112 (3)
O48—Bi14—O37154 (4)Bi16—O6—Bi4123 (3)
O25i—Bi15—O485 (3)Bi16—O6—Bi24124 (3)
O25i—Bi15—O2986 (4)Bi4—O6—Bi24105 (3)
O4—Bi15—O2974 (3)Bi6—O7—Bi2i125 (4)
O25i—Bi15—O57i92 (3)Bi6—O7—Bi26113 (3)
O4—Bi15—O57i141 (3)Bi2i—O7—Bi26103 (3)
O29—Bi15—O57i68 (3)Bi21—O8—Bi19131 (3)
O25i—Bi15—Bi1198 (3)Bi21—O8—Bi11v116 (2)
O4—Bi15—Bi1142 (2)Bi19—O8—Bi11v98 (2)
O29—Bi15—Bi1136.2 (19)Bi20—O9—Bi22134 (4)
O57i—Bi15—Bi11101.1 (19)Bi20—O9—Bi12iv103 (3)
O25i—Bi15—Bi336 (3)Bi22—O9—Bi12iv113 (3)
O4—Bi15—Bi351.2 (19)Bi29ii—O10—Bi30125 (6)
O29—Bi15—Bi368 (2)Bi29ii—O10—Bi2110 (5)
O57i—Bi15—Bi3110.8 (18)Bi30—O10—Bi2116 (5)
Bi11—Bi15—Bi365.48 (16)Bi27vi—O11—Bi18137 (5)
O6—Bi16—O17ii78 (3)Bi27vi—O11—Bi26v107 (5)
O6—Bi16—O30ii85 (3)Bi18—O11—Bi26v107 (4)
O17ii—Bi16—O30ii69 (3)Bi14—O12—Bi8i122 (3)
O6—Bi16—O4799 (3)Bi14—O12—Bi24113 (2)
O17ii—Bi16—O47145 (3)Bi8i—O12—Bi24114 (3)
O30ii—Bi16—O4776 (3)Bi21—O13—Bi19ii125 (3)
O6—Bi16—Bi12ii93 (2)Bi21—O13—Bi9108 (3)
O17ii—Bi16—Bi12ii41.9 (19)Bi19ii—O13—Bi9113 (3)
O30ii—Bi16—Bi12ii31 (2)Bi25—O14—Bi3vii110 (4)
O47—Bi16—Bi12ii104.3 (18)Bi25—O14—Bi9117 (4)
O33iv—Bi17—O278 (5)Bi3vii—O14—Bi9121 (4)
O33iv—Bi17—O19ii71 (5)Bi25—O14—Bi11v95 (3)
O2—Bi17—O19ii77 (3)Bi3vii—O14—Bi11v102 (4)
O33iv—Bi17—O5873 (5)Bi9—O14—Bi11v107 (4)
O2—Bi17—O5885 (3)Bi10—O15—Bi4iv133 (4)
O19ii—Bi17—O58142 (3)Bi10—O15—Bi26113 (4)
O33iv—Bi17—Bi3ii34 (4)Bi4iv—O15—Bi26104 (3)
O2—Bi17—Bi3ii94 (2)Bi5—O16—Bi1ii126 (4)
O19ii—Bi17—Bi3ii46 (3)Bi5—O16—Bi9106 (3)
O58—Bi17—Bi3ii103 (2)Bi1ii—O16—Bi9111 (3)
O20—Bi18—O1181 (4)Bi24—O17—Bi16i126 (4)
O20—Bi18—O3269 (5)Bi24—O17—Bi12118 (3)
O11—Bi18—O3289 (5)Bi16i—O17—Bi12101 (3)
O20—Bi18—O60i138 (4)Bi6—O18—Bi2125 (3)
O11—Bi18—O60i85 (4)Bi6—O18—Bi10110 (3)
O32—Bi18—O60i71 (5)Bi2—O18—Bi10113 (3)
O20—Bi18—Bi442 (3)Bi28—O19—Bi17i130 (5)
O11—Bi18—Bi4100 (3)Bi28—O19—Bi3113 (4)
O32—Bi18—Bi432 (4)Bi17i—O19—Bi397 (4)
O60i—Bi18—Bi4103 (3)Bi28—O19—Bi23i117 (4)
O29v—Bi19—O13i81 (3)Bi17i—O19—Bi23i102 (3)
O29v—Bi19—O873 (3)Bi3—O19—Bi23i89 (3)
O13i—Bi19—O884 (2)Bi27v—O20—Bi18128 (5)
O29v—Bi19—O57vi71 (3)Bi27v—O20—Bi4114 (4)
O13i—Bi19—O57vi90 (3)Bi18—O20—Bi4101 (4)
O8—Bi19—O57vi144 (2)Bi13—O21—Bi7ii131 (6)
O29v—Bi19—Bi11v34 (2)Bi8—O22—Bi14130 (4)
O13i—Bi19—Bi11v96.0 (18)Bi5—O23—Bi1124 (4)
O8—Bi19—Bi11v44.7 (16)Bi5—O23—Bi25111 (3)
O57vi—Bi19—Bi11v101.5 (17)Bi1—O23—Bi25110 (3)
O9—Bi20—O3i90 (3)Bi25—O24—Bi11v116 (4)
O9—Bi20—O30iv71 (3)Bi25—O24—Bi3v120 (4)
O3i—Bi20—O30iv85 (3)Bi11v—O24—Bi3v109 (4)
O9—Bi20—Bi12iv43 (2)Bi25—O24—Bi9i113 (4)
O3i—Bi20—Bi12iv97 (2)Bi11v—O24—Bi9i103 (3)
O30iv—Bi20—Bi12iv31 (2)Bi3v—O24—Bi9i94 (3)
O8—Bi21—O2785 (3)Bi15ii—O25—Bi3ii112 (4)
O8—Bi21—O1386 (3)Bi15ii—O25—Bi23125 (5)
O27—Bi21—O1371 (3)Bi3ii—O25—Bi23107 (4)
O8—Bi21—O5096 (4)Bi27—O26—Bi2122 (3)
O27—Bi21—O50144 (4)Bi27—O26—Bi26ii107 (3)
O13—Bi21—O5074 (4)Bi2—O26—Bi26ii101 (2)
O8—Bi21—Bi997.9 (17)Bi21—O27—Bi5134 (4)
O27—Bi21—Bi936 (2)Bi21—O27—Bi9112 (4)
O13—Bi21—Bi939 (2)Bi5—O27—Bi9104 (3)
O50—Bi21—Bi9109 (3)Bi22—O28—Bi6131 (4)
O9—Bi22—O381 (3)Bi22—O28—Bi10108 (3)
O9—Bi22—O2887 (3)Bi6—O28—Bi10108 (3)
O3—Bi22—O2874 (3)Bi19iv—O29—Bi11113 (4)
O9—Bi22—O5676 (3)Bi19iv—O29—Bi15123 (4)
O3—Bi22—O5669 (3)Bi11—O29—Bi15105 (3)
O28—Bi22—O56142 (3)Bi12—O30—Bi16i114 (4)
O9—Bi22—Bi1098.9 (19)Bi12—O30—Bi20v112 (4)
O3—Bi22—Bi1043 (2)Bi16i—O30—Bi20v120 (4)
O28—Bi22—Bi1037 (2)Bi28—O31—Bi7130 (7)
O56—Bi22—Bi10111.4 (19)Bi28—O31—Bi23110 (5)
O4—Bi23—O2576 (3)Bi7—O31—Bi23106 (5)
O4—Bi23—O3180 (4)Bi4—O32—Bi18111 (7)
O25—Bi23—O31156 (4)Bi4—O32—Bi24116 (7)
O4—Bi23—O286 (3)Bi18—O32—Bi24118 (7)
O25—Bi23—O2115 (3)Bi17v—O33—Bi3vii118 (7)
O31—Bi23—O262 (4)Bi17v—O33—Bi25122 (7)
O4—Bi23—O44161 (3)Bi3vii—O33—Bi25101 (6)
Symmetry codes: (i) x+1, y, z; (ii) x1, y, z; (iii) x+1, y1, z; (iv) x, y1, z; (v) x, y+1, z; (vi) x+1, y+1, z; (vii) x1, y+1, z; (viii) x1, y1, z; (ix) x, y, z1; (x) x, y, z+1.

Experimental details

(I)(II)
Crystal data
Chemical formulaBi14O36S5As2Bi30O77S9
Mr3630.027939.87
Crystal system, space groupMonoclinic, C2Triclinic, P1
Temperature (K)293293
a, b, c (Å)21.658 (4), 5.6648 (9), 15.092 (3)5.670 (3), 13.9408 (9), 22.7908 (18)
α, β, γ (°)90, 119.433 (11), 9080.903 (5), 82.854 (14), 78.27 (2)
V3)1612.7 (5)1733.8 (10)
Z24
Radiation typeMo KαMo Kα
µ (mm1)76.5276.27
Crystal size (mm)0.53 × 0.04 × 0.020.22 × 0.01 × 0.01
Data collection
DiffractometerBruker AXS X8 APEX2 with 2K-CCD detector
diffractometer
Bruker AXS X8 APEX2 with 2K-CCD detector
diffractometer
Absorption correctionNumerical - needle
program WinGX (Farrugia, 2012)
Numerical - needle
program WinGX (Farrugia, 2012)
Tmin, Tmax0.062, 0.3090.355, 0.474
No. of measured, independent and
observed [I > 2σ(I)] reflections
5991, 3034, 2234 11765, 10496, 4123
Rint0.0570.047
(sin θ/λ)max1)0.6260.714
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.124, 0.342, 1.19 0.119, 0.374, 0.97
No. of reflections303410496
No. of parameters143567
No. of restraints103
w = 1/[σ2(Fo2) + (0.1584P)2 + 1159.5515P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.1967P)2]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)5.84, 5.2121.57, 4.61
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0.72 (11)0.00 (5)

Computer programs: SAINT-IRIX (Bruker, 2003), SIR 2014 (Burla et al., 2014), SHELXL97 (Sheldrick, 1997).

 

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