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Iron was inserted into the known crystal structure of the bis­muth phosphate oxide Bi6.67(PO4)4O4 to ascertain its location in the vacancies associated with the bis­muth ion located at the origin of the unit cell. Single-crystal X-ray diffraction refinements converged to a model of composition Bi6(Bi0.32Fe0.68)(PO4)4O4 (hexabismuth iron tetraphosphate tetraoxide), in which Bi and Fe are displaced from the origin giving rise to a random distribution over the 2i sites instead of 1a, the origin of space group P\overline{1}. The isotropic displacement parameter for Bi/Fe has a reasonable value in this model. This structure establishes for the first time that Fe substitutes in the Bi-deficient site in this series of materials and that Fe and Bi are disordered around the center of symmetry. These results enhance understanding of the crystal chemistry of these main group phosphates that are of inter­est in ion transport.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108021045/sq3151sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108021045/sq3151Isup2.hkl
Contains datablock I

Comment top

Recently the crystal structure of a pillared lithium bismuth phosphate, LiBi7.37P3O19, was described in which Li is incorporated in an interstitial tetrahedral site by four O atoms (Arumugam et al., 2007). Preliminary experiments indicated that no Li+ transport occurs in this compound. We attempted to substitute Fe2+ into the structure, hoping that any charge deficiency would be balanced by additional introduction of Li into the structure. The synthesis of a putative Li2Bi7.37-xFexP3O19 from stoichiometric mixtures in the ratio 3:8:6:5 of Li2CO3, NH4H2PO4, Bi2O3 and metallic Fe, respectively, by the standard ceramic technique led to single crystals that were eventually identified as isostructural with Bi6.67(PO4)4O4 (Ketatni et al., 1998; Giraud et al., 2000). The single-crystal X-ray diffraction refinement of the crystal structure of Bi6.67(PO4)4O4 (Ketatni et al., 1998) showed that the site occupancy of the Bi4 atom at the origin, (0 0 0), was less than unity, 0.67 (6), and the equivalent isotropic displacement parameter was large, 3.44 (6) Å2 (Ueq = 0.044 Å2). The authors also reported the unit-cell parameters of phases containing Li, Na, K, Sr, Cd, Ca and Pb, where the substituents were placed into the site containing the vacancy, Bi6.5A+0.5 and Bi6M2+. Giraud et al., (2000) investigated several of these phases, including PbBi6(PO4)4O4, using Rietveld refinement of X-ray diffraction data and reported that Pb completely replaced Bi at the origin. However, its isotropic displacement parameter was large.

A single-crystal was selected from the product and X-ray fluorescence spectroscopy showed the presence of iron. We decided, therefore, to subject this crystal to a complete structure determination to clarify the location of Fe and to see whether the anomalously large displacement parameter of the occupant atom at the origin position could be due to disorder. We report the result here.

The crystal structure of Bi6.67(PO4)4O4 has previously been described by Ketatni et al. (1998) and Giraud et al. (2000). Using the reported atomic parameters, our absorption-corrected intensities and anisotropic displacement parameters except for O atoms, and placing Fe1 together with Bi4 into the (0, 0, 0) position with the sum of the site occupancies for these two atoms restrained to 0.5, the least-squares refinements converged to R1 = 0.093. However, in this final result the restraint failed (disagreeable restraint), the isotropic displacement parameter for Fe1/Bi4 became large, Ueq = 0.060 (4) Å2, and the displacement parameters for P1 and P2 were non-positive definite. Difference electron densities also indicated that these atoms were displaced from the origin. The atomic positions for Fe1 and Bi4 were permitted to vary in the next cycles of refinement, but the isotropic displacement parameters were restrained to remain equal; R1 converged to 0.0364 with a Bi4 occupancy of 0.155 (6) and an Fe1 occupancy of 0.347 (15), leading to the stoichiometry Bi6.32Fe0.68P4O20 or Bi6(Bi0.32Fe0.68)(PO4)4O4. Fig. 1 shows the unit cell with Fe1 displaced slightly from the origin; atom Bi4 that shares a nearby site has been omitted for the sake of clarity. The coordination polyhedron around this site consists of eight O atoms in a distorted cubic arrangement. The two crystallographically distinct PO4 tetrahedra are isolated but share an edge with the oxygen coordination polyhedron around the origin. The Bi2O2 chains that are so characteristic of these structures (Colmont et al., 2008; Arumugam et al., 2008; Abraham et al., 2002) are present here as well. A corrugated chain of Bi2O2 exists in the ac plane (Fig. 2). The substitution of isovalent and aliovalent ions occurs in the Bi4 site containing the vacancies in the parent compound. If this site is completely occupied by Bi or a mixture of cations, it is likely that small oxygen variations in the stoichiometry required for charge balance occur among these O atoms.

Experimental top

The title compound, Bi6(Bi0.32Fe0.68)(PO4)4O4, was synthesized by the ceramic method by reacting a mixture of analytical grade Li2CO3, NH4H2PO4 and Bi2O3 and metallic Fe in the molar ratio 3:8:6:5. Prior to use, Bi2O3 was dried in air at 873 K for 24 h in order to remove any moisture or carbonates associated with it. The mixture was initially heated in air at 468 K for 2 h to decompose NH4H2PO4 and finally at 973 K for 12 h in alumina crucibles. The intermediate product was then ground and reheated in air at 1100 K for 1 h in a gold boat and further heated to 1173 K and annealed at that temperature for about 14 h. Greenish–yellow single crystals of this pure phase were obtained by cooling the reaction mixture from 1173 to 1073 K at a rate of 5 K h-1 and then furnace-cooling to room temperature. The phase purity was determined from the powder diffraction pattern and is nearly 100%. A few very weak reflections barely visible above background were not indexed with the single-crystal lattice parameters.

Computing details top

Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view of the crystal structure of Bi6(Bi0.32Fe0.68)(PO4)4O4, along [001]. The disordered Bi4 site near the origin has been omitted for clarity.
[Figure 2] Fig. 2. A view of the zigzag Bi2O2 infinite chains in the ac plane.
hexabismuth iron tetraphosphate tetraoxide top
Crystal data top
Bi6(Bi0.32Fe0.68)(PO4)4O4Z = 1
Mr = 1801.1F(000) = 761.7
Triclinic, P1Dx = 7.279 Mg m3
Hall symbol: -P_1Mo Kα radiation, λ = 0.71073 Å
a = 9.2097 (18) ÅCell parameters from 6175 reflections
b = 7.5214 (15) Åθ = 1–27.5°
c = 6.9033 (14) ŵ = 67.86 mm1
α = 112.48 (3)°T = 293 K
β = 93.71 (3)°Irregular, green yellow
γ = 106.95 (3)°0.03 × 0.01 × 0.01 mm
V = 414.2 (2) Å3
Data collection top
Nonius KappaCCD
diffractometer
1855 independent reflections
Radiation source: fine-focus sealed tube1600 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
ϕ scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 1°
Absorption correction: numerical
(EUHEDRAL; Spek, 2006; de Meulenaer & Tompa, 1965)
h = 1111
Tmin = 0.053, Tmax = 0.403k = 99
6043 measured reflectionsl = 80
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)] = 0.036 w = 1/[σ2(Fo2) + (0.0555P)2 + 8.9305P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.097(Δ/σ)max < 0.001
S = 1.11Δρmax = 4.10 e Å3
1600 reflectionsΔρmin = 2.90 e Å3
96 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.0094 (5)
Crystal data top
Bi6(Bi0.32Fe0.68)(PO4)4O4γ = 106.95 (3)°
Mr = 1801.1V = 414.2 (2) Å3
Triclinic, P1Z = 1
a = 9.2097 (18) ÅMo Kα radiation
b = 7.5214 (15) ŵ = 67.86 mm1
c = 6.9033 (14) ÅT = 293 K
α = 112.48 (3)°0.03 × 0.01 × 0.01 mm
β = 93.71 (3)°
Data collection top
Nonius KappaCCD
diffractometer
1855 independent reflections
Absorption correction: numerical
(EUHEDRAL; Spek, 2006; de Meulenaer & Tompa, 1965)
1600 reflections with I > 2σ(I)
Tmin = 0.053, Tmax = 0.403Rint = 0.081
6043 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03696 parameters
wR(F2) = 0.0971 restraint
S = 1.11Δρmax = 4.10 e Å3
1600 reflectionsΔρmin = 2.90 e Å3
Special details top

Experimental. Several crystals were examined on a Nonius κ automated CCD diffractometer equipped with a graphite monochromator with Mo Kα radiation, λ = 0.71079 Å. The best crystal displaying the lowest mosaicity was used for the data collection. Data reduction and scaling were performed using DENZO-SMN (Otwinowski & Minor, 1997).Details of crystal data, data collection and structure refinement are listed in Table. The structure was solved with the direct methods program SHELXS(Sheldrick, 1997) in space group P1 that yielded the heavy atom positions. Difference electron density maps revealed the phosphorus and oxygen atoms. The refinement proceeded by least squares using SHELXL (Sheldrick, 1997).

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)
Bi10.32548 (6)0.30567 (7)0.81061 (7)0.00717 (19)
Bi20.08275 (6)0.78373 (7)0.43077 (8)0.0137 (2)
Bi30.48939 (5)0.86838 (7)0.66292 (7)0.00593 (19)
Bi40.0113 (9)0.0042 (12)0.0328 (11)0.0024 (8)*0.155 (6)
Fe10.0271 (14)0.0018 (18)0.0450 (19)0.0024 (8)*0.347 (15)
P10.2369 (4)0.7360 (5)0.9502 (5)0.0065 (7)
P20.2516 (4)0.3906 (5)0.3369 (5)0.0079 (7)
O10.1440 (11)0.8354 (13)1.1151 (14)0.0077 (18)*
O20.2720 (12)0.2446 (15)0.1212 (16)0.018 (2)*
O30.2381 (10)0.8172 (13)0.7757 (14)0.0087 (18)*
O40.1031 (10)0.0917 (13)0.6748 (14)0.0088 (18)*
O50.3117 (11)0.6110 (14)0.3586 (15)0.014 (2)*
O60.0814 (13)0.3243 (17)0.3474 (18)0.025 (2)*
O70.3653 (10)0.0289 (13)0.5526 (14)0.0073 (17)*
O80.3487 (11)0.3783 (14)0.5198 (15)0.0111 (19)*
O90.4103 (10)0.7976 (13)1.0523 (14)0.0069 (17)*
O100.1605 (11)0.5002 (14)0.8541 (15)0.013 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Bi10.0070 (3)0.0038 (3)0.0061 (3)0.00039 (19)0.00193 (19)0.00099 (19)
Bi20.0102 (3)0.0043 (3)0.0207 (3)0.0018 (2)0.0041 (2)0.0004 (2)
Bi30.0066 (3)0.0040 (3)0.0057 (3)0.00143 (19)0.00034 (19)0.00103 (19)
P10.0093 (18)0.0025 (14)0.0071 (15)0.0006 (12)0.0022 (12)0.0024 (12)
P20.0106 (18)0.0038 (14)0.0069 (16)0.0006 (13)0.0005 (13)0.0014 (12)
Geometric parameters (Å, º) top
Bi1—O42.083 (9)O1—O102.532 (13)
Bi1—O82.281 (9)O1—O92.595 (13)
Bi1—O72.310 (8)O1—O4xiv2.852 (12)
Bi1—O102.357 (9)O1—O2viii2.940 (14)
Bi1—O2i2.410 (10)O1—O7viii3.084 (12)
Bi1—O9ii2.965 (9)O2—Fe1xi2.332 (16)
Bi1—O93.242 (9)O2—Bi1vii2.410 (10)
Bi1—O3iii3.432 (8)O2—O62.476 (15)
Bi1—O5iv3.573 (10)O2—O52.509 (14)
Bi1—Bi4i3.624 (7)O2—O82.510 (14)
Bi1—Bi1ii3.648 (2)O2—Bi4xi2.599 (13)
Bi1—Bi2iii3.679 (2)O2—O1xii2.940 (14)
Bi2—O4v2.227 (9)O2—O4vii2.977 (14)
Bi2—O4vi2.374 (9)O2—Bi3iv3.067 (10)
Bi2—O6vi2.414 (11)O3—O92.478 (12)
Bi2—O1vii2.429 (9)O3—O102.556 (12)
Bi2—O7v2.572 (9)O3—O7v2.702 (12)
Bi2—O32.583 (9)O3—O6vi2.770 (15)
Bi2—O10vi2.622 (10)O3—Fe1vi2.779 (15)
Bi2—O52.760 (9)O3—O52.934 (13)
Bi2—O63.275 (11)O3—Bi4viii2.956 (11)
Bi2—Bi4viii3.626 (7)O3—O4v2.963 (12)
Bi2—Bi1v3.679 (2)O4—Bi2iii2.227 (9)
Bi3—O7v2.177 (8)O4—Bi2vi2.374 (9)
Bi3—O7iv2.266 (8)O4—Fe1xiii2.378 (15)
Bi3—O52.332 (10)O4—Bi4i2.477 (10)
Bi3—O9ix2.380 (9)O4—O4xiii2.583 (18)
Bi3—O32.460 (9)O4—O102.704 (13)
Bi3—O8iv2.706 (9)O4—O72.718 (12)
Bi3—O93.026 (8)O4—O1xiv2.852 (12)
Bi3—O2iv3.067 (10)O4—O3iii2.963 (12)
Bi3—O83.242 (9)O4—O2i2.977 (14)
Bi3—O1ix3.323 (9)O4—Bi4xiii2.999 (11)
Bi3—Bi3x3.5009 (12)O5—O82.492 (13)
Bi4—Fe1xi0.181 (18)O5—O62.518 (15)
Bi4—Bi4xi0.528 (12)O5—O7v2.776 (12)
Bi4—Fe10.665 (9)O5—O9vii3.007 (12)
Bi4—O1vi2.291 (11)O5—O8iv3.155 (13)
Bi4—O22.415 (13)O5—O7iv3.218 (13)
Bi4—O1xii2.425 (11)O5—O10vii3.352 (14)
Bi4—O6xi2.445 (14)O6—Bi2vi2.414 (11)
Bi4—O4vii2.477 (10)O6—Bi4xi2.445 (14)
Bi4—O2xi2.599 (13)O6—O82.512 (15)
Bi4—O62.672 (13)O6—Fe1xi2.763 (17)
Bi4—O3xii2.956 (11)O6—O3vi2.770 (15)
Bi4—O4xiii2.999 (11)O6—O4xiii3.033 (14)
Fe1—Bi4xi0.181 (18)O6—O103.176 (14)
Fe1—Fe1xi0.82 (2)O7—Bi3iii2.177 (8)
Fe1—O2xi2.332 (16)O7—Bi3iv2.266 (8)
Fe1—O1vi2.352 (14)O7—Bi2iii2.572 (9)
Fe1—O4xiii2.378 (15)O7—O3iii2.702 (12)
Fe1—O62.384 (16)O7—O7xv2.737 (17)
Fe1—O1xii2.408 (14)O7—O82.769 (12)
Fe1—O22.710 (16)O7—O5iii2.776 (12)
Fe1—O6xi2.763 (17)O7—O9ii2.896 (13)
Fe1—O3vi2.779 (15)O7—O1xii3.084 (12)
Fe1—O4vii3.110 (15)O7—O5iv3.218 (13)
P1—O31.544 (9)O8—Bi3iv2.706 (9)
P1—O101.547 (10)O8—O8iv2.949 (18)
P1—O91.560 (10)O8—O102.999 (13)
P1—O11.560 (9)O8—O5iv3.155 (13)
P2—O61.516 (12)O9—Bi3ix2.380 (9)
P2—O51.530 (9)O9—O102.534 (14)
P2—O21.537 (10)O9—O7ii2.896 (13)
P2—O81.547 (10)O9—Bi1ii2.965 (9)
P2—Bi4xi3.078 (9)O9—O5i3.007 (12)
O1—Bi4vi2.291 (11)O9—O2iv3.286 (13)
O1—Fe1vi2.352 (14)O9—O7viii3.337 (12)
O1—Fe1viii2.408 (14)O10—Bi2vi2.622 (10)
O1—Bi4viii2.425 (11)O10—O1xiv3.262 (13)
O1—Bi2i2.429 (9)O10—O5i3.352 (14)
O1—O32.519 (12)O10—O6vi3.371 (15)
O4—Bi1—O893.6 (3)O7v—O3—Fe1vi104.0 (4)
O4—Bi1—O776.3 (3)O6vi—O3—Fe1vi50.9 (4)
O8—Bi1—O774.2 (3)P1—O3—O5122.4 (5)
O4—Bi1—O1074.7 (3)Bi3—O3—O550.3 (3)
O8—Bi1—O1080.6 (3)O9—O3—O5108.2 (4)
O7—Bi1—O10139.9 (3)O1—O3—O5154.8 (4)
O4—Bi1—O2i82.7 (3)O10—O3—O595.0 (4)
O8—Bi1—O2i172.4 (3)Bi2—O3—O559.6 (3)
O7—Bi1—O2i111.1 (3)O7v—O3—O558.9 (3)
O10—Bi1—O2i92.0 (3)O6vi—O3—O598.5 (4)
O4—Bi1—O9ii123.0 (3)Fe1vi—O3—O5140.8 (5)
O8—Bi1—O9ii112.9 (3)P1—O3—Bi4viii87.3 (4)
O7—Bi1—O9ii65.2 (3)Bi3—O3—Bi4viii147.2 (4)
O10—Bi1—O9ii154.8 (3)O9—O3—Bi4viii110.5 (4)
O2i—Bi1—O9ii74.6 (3)O1—O3—Bi4viii51.9 (3)
O4—Bi1—O9125.5 (3)O10—O3—Bi4viii99.6 (4)
O8—Bi1—O981.8 (3)Bi2—O3—Bi4viii81.5 (3)
O7—Bi1—O9148.9 (3)O7v—O3—Bi4viii104.8 (4)
O10—Bi1—O950.9 (3)O6vi—O3—Bi4viii50.4 (3)
O2i—Bi1—O994.9 (3)Fe1vi—O3—Bi4viii0.8 (4)
O9ii—Bi1—O9108.17 (19)O5—O3—Bi4viii141.0 (4)
O4—Bi1—O3iii59.1 (3)P1—O3—O4v136.5 (5)
O8—Bi1—O3iii122.5 (3)Bi3—O3—O4v106.2 (3)
O7—Bi1—O3iii51.8 (2)O9—O3—O4v143.9 (4)
O10—Bi1—O3iii127.8 (3)O1—O3—O4v100.5 (4)
O2i—Bi1—O3iii61.0 (3)O10—O3—O4v141.1 (5)
O9ii—Bi1—O3iii64.1 (2)Bi2—O3—O4v46.7 (2)
O9—Bi1—O3iii155.7 (2)O7v—O3—O4v57.1 (3)
O4—Bi1—O5iv135.0 (3)O6vi—O3—O4v63.8 (3)
O8—Bi1—O5iv60.6 (3)Fe1vi—O3—O4v48.8 (3)
O7—Bi1—O5iv62.0 (3)O5—O3—O4v98.9 (4)
O10—Bi1—O5iv128.6 (3)Bi4viii—O3—O4v49.5 (2)
O2i—Bi1—O5iv126.5 (3)Bi1—O4—Bi2iii117.2 (4)
O9ii—Bi1—O5iv53.8 (2)Bi1—O4—Bi2vi115.4 (4)
O9—Bi1—O5iv89.1 (2)Bi2iii—O4—Bi2vi111.8 (4)
O3iii—Bi1—O5iv102.1 (2)Bi1—O4—Fe1xiii103.5 (5)
O4—Bi1—Bi4i41.3 (3)Bi2iii—O4—Fe1xiii98.7 (4)
O8—Bi1—Bi4i134.4 (3)Bi2vi—O4—Fe1xiii107.9 (4)
O7—Bi1—Bi4i95.6 (2)Bi1—O4—Bi4i105.0 (4)
O10—Bi1—Bi4i80.2 (3)Bi2iii—O4—Bi4i100.7 (4)
O2i—Bi1—Bi4i41.4 (3)Bi2vi—O4—Bi4i104.4 (4)
O9ii—Bi1—Bi4i101.6 (2)Fe1xiii—O4—Bi4i3.6 (4)
O9—Bi1—Bi4i115.4 (2)Bi1—O4—O4xiii142.1 (6)
O3iii—Bi1—Bi4i49.44 (19)Bi2iii—O4—O4xiii58.6 (3)
O5iv—Bi1—Bi4i151.11 (19)Bi2vi—O4—O4xiii53.2 (3)
O4—Bi1—Bi1ii163.6 (2)Fe1xiii—O4—O4xiii114.4 (6)
O8—Bi1—Bi1ii101.0 (2)Bi4i—O4—O4xiii112.9 (5)
O7—Bi1—Bi1ii114.9 (2)Bi1—O4—O1057.3 (3)
O10—Bi1—Bi1ii100.1 (2)Bi2iii—O4—O10159.2 (4)
O2i—Bi1—Bi1ii82.0 (3)Bi2vi—O4—O1061.8 (3)
O9ii—Bi1—Bi1ii57.62 (17)Fe1xiii—O4—O10102.1 (5)
O9—Bi1—Bi1ii50.55 (16)Bi4i—O4—O10100.1 (4)
O3iii—Bi1—Bi1ii117.08 (15)O4xiii—O4—O10111.8 (5)
O5iv—Bi1—Bi1ii60.38 (16)Bi1—O4—O755.6 (3)
Bi4i—Bi1—Bi1ii122.94 (12)Bi2iii—O4—O761.7 (3)
O4—Bi1—Bi2iii32.6 (2)Bi2vi—O4—O7136.3 (4)
O8—Bi1—Bi2iii86.4 (2)Fe1xiii—O4—O7115.7 (5)
O7—Bi1—Bi2iii43.8 (2)Bi4i—O4—O7119.3 (4)
O10—Bi1—Bi2iii104.8 (2)O4xiii—O4—O7104.8 (5)
O2i—Bi1—Bi2iii93.9 (3)O10—O4—O7107.9 (4)
O9ii—Bi1—Bi2iii97.39 (17)Bi1—O4—O1xiv118.4 (4)
O9—Bi1—Bi2iii154.36 (16)Bi2iii—O4—O1xiv122.2 (4)
O3iii—Bi1—Bi2iii42.42 (15)Bi2vi—O4—O1xiv54.5 (3)
O5iv—Bi1—Bi2iii104.82 (16)Fe1xiii—O4—O1xiv53.9 (4)
Bi4i—Bi1—Bi2iii59.54 (13)Bi4i—O4—O1xiv50.3 (3)
Bi1ii—Bi1—Bi2iii154.92 (3)O4xiii—O4—O1xiv85.7 (5)
O4v—Bi2—O4vi68.2 (4)O10—O4—O1xiv71.9 (3)
O4v—Bi2—O6vi81.5 (3)O7—O4—O1xiv168.3 (4)
O4vi—Bi2—O6vi89.6 (3)Bi1—O4—O3iii83.8 (3)
O4v—Bi2—O1vii105.3 (3)Bi2iii—O4—O3iii57.6 (3)
O4vi—Bi2—O1vii72.8 (3)Bi2vi—O4—O3iii160.5 (4)
O6vi—Bi2—O1vii156.5 (4)Fe1xiii—O4—O3iii61.6 (4)
O4v—Bi2—O7v68.6 (3)Bi4i—O4—O3iii65.1 (3)
O4vi—Bi2—O7v116.3 (3)O4xiii—O4—O3iii113.9 (5)
O6vi—Bi2—O7v126.7 (3)O10—O4—O3iii134.2 (4)
O1vii—Bi2—O7v76.1 (3)O7—O4—O3iii56.6 (3)
O4v—Bi2—O375.6 (3)O1xiv—O4—O3iii114.7 (4)
O4vi—Bi2—O3139.6 (3)Bi1—O4—O2i53.4 (3)
O6vi—Bi2—O367.2 (3)Bi2iii—O4—O2i120.4 (4)
O1vii—Bi2—O3136.1 (3)Bi2vi—O4—O2i125.0 (4)
O7v—Bi2—O363.2 (3)Fe1xiii—O4—O2i50.1 (4)
O4v—Bi2—O10vi128.9 (3)Bi4i—O4—O2i51.6 (3)
O4vi—Bi2—O10vi65.3 (3)O4xiii—O4—O2i164.4 (6)
O6vi—Bi2—O10vi78.1 (3)O10—O4—O2i74.1 (3)
O1vii—Bi2—O10vi80.4 (3)O7—O4—O2i86.1 (4)
O7v—Bi2—O10vi154.2 (3)O1xiv—O4—O2i82.6 (3)
O3—Bi2—O10vi134.1 (3)O3iii—O4—O2i62.8 (3)
O4v—Bi2—O5127.6 (3)Bi1—O4—Bi4xiii104.9 (4)
O4vi—Bi2—O5152.8 (3)Bi2iii—O4—Bi4xiii102.1 (3)
O6vi—Bi2—O5113.2 (3)Bi2vi—O4—Bi4xiii103.0 (3)
O1vii—Bi2—O581.0 (3)Fe1xiii—O4—Bi4xiii5.1 (2)
O7v—Bi2—O562.6 (3)Bi4i—O4—Bi4xiii1.6 (3)
O3—Bi2—O566.5 (3)O4xiii—O4—Bi4xiii112.9 (5)
O10vi—Bi2—O5103.5 (3)O10—O4—Bi4xiii98.7 (4)
O4v—Bi2—O6145.8 (3)O7—O4—Bi4xiii120.6 (4)
O4vi—Bi2—O6133.4 (3)O1xiv—O4—Bi4xiii48.9 (3)
O6vi—Bi2—O673.8 (4)O3iii—O4—Bi4xiii66.7 (3)
O1vii—Bi2—O6106.8 (3)O2i—O4—Bi4xiii51.6 (3)
O7v—Bi2—O6108.3 (3)P2—O5—Bi3120.1 (5)
O3—Bi2—O673.2 (3)P2—O5—O836.2 (3)
O10vi—Bi2—O668.7 (3)Bi3—O5—O884.4 (4)
O5—Bi2—O648.4 (3)P2—O5—O235.2 (3)
O4v—Bi2—Bi4viii42.1 (2)Bi3—O5—O2135.9 (5)
O4vi—Bi2—Bi4viii86.7 (2)O8—O5—O260.2 (4)
O6vi—Bi2—Bi4viii42.0 (3)P2—O5—O634.1 (4)
O1vii—Bi2—Bi4viii147.1 (2)Bi3—O5—O6126.6 (5)
O7v—Bi2—Bi4viii91.1 (2)O8—O5—O660.2 (4)
O3—Bi2—Bi4viii53.7 (2)O2—O5—O659.0 (4)
O10vi—Bi2—Bi4viii114.6 (2)P2—O5—Bi2110.6 (5)
O5—Bi2—Bi4viii120.1 (2)Bi3—O5—Bi294.4 (3)
O6—Bi2—Bi4viii106.0 (2)O8—O5—Bi2122.8 (4)
O4v—Bi2—Bi1v30.2 (2)O2—O5—Bi2125.8 (4)
O4vi—Bi2—Bi1v91.1 (2)O6—O5—Bi276.6 (4)
O6vi—Bi2—Bi1v101.3 (3)P2—O5—O7v155.2 (6)
O1vii—Bi2—Bi1v94.7 (2)Bi3—O5—O7v49.5 (3)
O7v—Bi2—Bi1v38.47 (19)O8—O5—O7v129.6 (5)
O3—Bi2—Bi1v63.67 (19)O2—O5—O7v169.2 (5)
O10vi—Bi2—Bi1v156.3 (2)O6—O5—O7v127.9 (5)
O5—Bi2—Bi1v98.5 (2)Bi2—O5—O7v55.4 (3)
O6—Bi2—Bi1v134.3 (2)P2—O5—O398.9 (5)
Bi4viii—Bi2—Bi1v59.48 (13)Bi3—O5—O354.3 (3)
O7v—Bi3—O7iv76.0 (4)O8—O5—O382.0 (4)
O7v—Bi3—O575.9 (3)O2—O5—O3134.1 (5)
O7iv—Bi3—O588.8 (3)O6—O5—O380.5 (4)
O7v—Bi3—O9ix78.8 (3)Bi2—O5—O353.9 (2)
O7iv—Bi3—O9ix91.8 (3)O7v—O5—O356.4 (3)
O5—Bi3—O9ix153.8 (3)P2—O5—O9vii133.6 (5)
O7v—Bi3—O371.0 (3)Bi3—O5—O9vii97.2 (4)
O7iv—Bi3—O3146.0 (3)O8—O5—O9vii146.0 (5)
O5—Bi3—O375.4 (3)O2—O5—O9vii98.8 (4)
O9ix—Bi3—O389.9 (3)O6—O5—O9vii134.8 (5)
O7v—Bi3—O8iv134.2 (3)Bi2—O5—O9vii91.1 (3)
O7iv—Bi3—O8iv67.0 (3)O7v—O5—O9vii70.4 (3)
O5—Bi3—O8iv77.2 (3)O3—O5—O9vii126.2 (4)
O9ix—Bi3—O8iv126.9 (3)P2—O5—O8iv88.4 (4)
O3—Bi3—O8iv134.9 (3)Bi3—O5—O8iv56.7 (3)
O7v—Bi3—O9117.2 (3)O8—O5—O8iv61.7 (4)
O7iv—Bi3—O9159.2 (3)O2—O5—O8iv82.3 (4)
O5—Bi3—O9109.4 (3)O6—O5—O8iv120.5 (4)
O9ix—Bi3—O976.3 (3)Bi2—O5—O8iv151.1 (4)
O3—Bi3—O952.5 (3)O7v—O5—O8iv98.5 (4)
O8iv—Bi3—O9106.5 (2)O3—O5—O8iv103.1 (4)
O7v—Bi3—O2iv164.9 (3)O9vii—O5—O8iv90.8 (3)
O7iv—Bi3—O2iv97.8 (3)P2—O5—O7iv139.7 (5)
O5—Bi3—O2iv118.1 (3)Bi3—O5—O7iv44.7 (2)
O9ix—Bi3—O2iv87.8 (3)O8—O5—O7iv110.2 (4)
O3—Bi3—O2iv116.3 (3)O2—O5—O7iv121.4 (4)
O8iv—Bi3—O2iv51.1 (3)O6—O5—O7iv169.5 (5)
O9—Bi3—O2iv65.3 (3)Bi2—O5—O7iv108.0 (3)
O7v—Bi3—O8122.0 (3)O7v—O5—O7iv53.7 (3)
O7iv—Bi3—O8116.1 (3)O3—O5—O7iv94.4 (4)
O5—Bi3—O849.9 (3)O9vii—O5—O7iv55.3 (3)
O9ix—Bi3—O8147.6 (3)O8iv—O5—O7iv51.5 (3)
O3—Bi3—O876.3 (3)P2—O5—O10vii95.9 (5)
O8iv—Bi3—O858.6 (3)Bi3—O5—O10vii142.7 (4)
O9—Bi3—O872.0 (2)O8—O5—O10vii129.5 (4)
O2iv—Bi3—O873.1 (3)O2—O5—O10vii70.0 (4)
O7v—Bi3—O1ix110.7 (3)O6—O5—O10vii88.3 (4)
O7iv—Bi3—O1ix63.7 (3)Bi2—O5—O10vii80.1 (3)
O5—Bi3—O1ix147.6 (3)O7v—O5—O10vii100.7 (4)
O9ix—Bi3—O1ix50.9 (3)O3—O5—O10vii133.9 (4)
O3—Bi3—O1ix136.9 (3)O9vii—O5—O10vii46.6 (3)
O8iv—Bi3—O1ix76.4 (3)O8iv—O5—O10vii120.7 (4)
O9—Bi3—O1ix95.8 (2)O7iv—O5—O10vii101.7 (3)
O2iv—Bi3—O1ix54.6 (3)P2—O6—Fe1103.4 (6)
O8—Bi3—O1ix125.7 (2)P2—O6—Bi2vi139.2 (7)
O7v—Bi3—Bi3x38.9 (2)Fe1—O6—Bi2vi93.5 (5)
O7iv—Bi3—Bi3x37.1 (2)P2—O6—Bi4xi99.3 (6)
O5—Bi3—Bi3x80.5 (2)Fe1—O6—Bi4xi4.1 (4)
O9ix—Bi3—Bi3x84.2 (2)Bi2vi—O6—Bi4xi96.6 (4)
O3—Bi3—Bi3x109.5 (2)P2—O6—O236.1 (4)
O8iv—Bi3—Bi3x100.39 (19)Fe1—O6—O267.8 (5)
O9—Bi3—Bi3x152.81 (16)Bi2vi—O6—O2144.5 (5)
O2iv—Bi3—Bi3x133.45 (19)Bi4xi—O6—O263.8 (4)
O8—Bi3—Bi3x127.89 (17)P2—O6—O835.3 (4)
O1ix—Bi3—Bi3x86.17 (15)Fe1—O6—O8111.9 (5)
Fe1xi—Bi4—Bi4xi133 (7)Bi2vi—O6—O8104.0 (5)
Fe1xi—Bi4—Fe1145 (5)Bi4xi—O6—O8108.4 (5)
Bi4xi—Bi4—Fe111.5 (18)O2—O6—O860.4 (4)
Fe1xi—Bi4—O1vi128 (6)P2—O6—O534.4 (3)
Bi4xi—Bi4—O1vi98.4 (17)Fe1—O6—O5123.4 (6)
Fe1—Bi4—O1vi86.9 (7)Bi2vi—O6—O5142.6 (5)
Fe1xi—Bi4—O261 (6)Bi4xi—O6—O5120.0 (5)
Bi4xi—Bi4—O2104.7 (18)O2—O6—O560.3 (4)
Fe1—Bi4—O2109.5 (5)O8—O6—O559.4 (4)
O1vi—Bi4—O2109.6 (4)P2—O6—Bi491.9 (5)
Fe1xi—Bi4—O1xii64 (5)Fe1—O6—Bi413.6 (2)
Bi4xi—Bi4—O1xii69.2 (16)Bi2vi—O6—Bi4107.1 (4)
Fe1—Bi4—O1xii80.6 (6)Bi4xi—O6—Bi410.7 (3)
O1vi—Bi4—O1xii167.6 (3)O2—O6—Bi455.8 (4)
O2—Bi4—O1xii74.8 (4)O8—O6—Bi4106.6 (5)
Fe1xi—Bi4—O6xi68 (6)O5—O6—Bi4109.7 (5)
Bi4xi—Bi4—O6xi110.1 (18)P2—O6—Fe1xi88.6 (5)
Fe1—Bi4—O6xi111.9 (5)Fe1—O6—Fe1xi16.3 (5)
O1vi—Bi4—O6xi100.5 (4)Bi2vi—O6—Fe1xi109.4 (5)
O2—Bi4—O6xi129.4 (5)Bi4xi—O6—Fe1xi12.92 (18)
O1xii—Bi4—O6xi84.4 (4)O2—O6—Fe1xi52.5 (4)
Fe1xi—Bi4—O4vii55 (5)O8—O6—Fe1xi103.5 (5)
Bi4xi—Bi4—O4vii170.8 (18)O5—O6—Fe1xi107.1 (5)
Fe1—Bi4—O4vii160.0 (6)Bi4—O6—Fe1xi3.3 (4)
O1vi—Bi4—O4vii73.3 (3)P2—O6—O3vi160.7 (7)
O2—Bi4—O4vii75.0 (4)Fe1—O6—O3vi64.8 (4)
O1xii—Bi4—O4vii119.1 (4)Bi2vi—O6—O3vi59.3 (3)
O6xi—Bi4—O4vii76.1 (4)Bi4xi—O6—O3vi68.7 (4)
Fe1xi—Bi4—O2xi126 (6)O2—O6—O3vi127.8 (5)
Bi4xi—Bi4—O2xi64.0 (17)O8—O6—O3vi161.5 (5)
Fe1—Bi4—O2xi59.4 (6)O5—O6—O3vi138.6 (5)
O1vi—Bi4—O2xi73.6 (4)Bi4—O6—O3vi74.0 (4)
O2—Bi4—O2xi168.7 (3)Fe1xi—O6—O3vi77.3 (4)
O1xii—Bi4—O2xi99.9 (4)P2—O6—O4xiii124.2 (6)
O6xi—Bi4—O2xi58.7 (4)Fe1—O6—O4xiii50.3 (4)
O4vii—Bi4—O2xi116.2 (4)Bi2vi—O6—O4xiii46.6 (3)
Fe1xi—Bi4—O6118 (6)Bi4xi—O6—O4xiii52.4 (3)
Bi4xi—Bi4—O659.2 (17)O2—O6—O4xiii102.5 (5)
Fe1—Bi4—O657.7 (6)O8—O6—O4xiii102.0 (4)
O1vi—Bi4—O682.1 (4)O5—O6—O4xiii158.6 (5)
O2—Bi4—O658.0 (4)Bi4—O6—O4xiii63.1 (3)
O1xii—Bi4—O691.1 (4)Fe1xi—O6—O4xiii64.7 (4)
O6xi—Bi4—O6169.3 (3)O3vi—O6—O4xiii61.2 (3)
O4vii—Bi4—O6114.5 (4)P2—O6—O1091.7 (5)
O2xi—Bi4—O6112.9 (4)Fe1—O6—O10139.0 (5)
Fe1xi—Bi4—O3xii13 (6)Bi2vi—O6—O1053.9 (3)
Bi4xi—Bi4—O3xii123.4 (17)Bi4xi—O6—O10139.8 (5)
Fe1—Bi4—O3xii134.6 (6)O2—O6—O10122.8 (5)
O1vi—Bi4—O3xii137.5 (4)O8—O6—O1062.4 (4)
O2—Bi4—O3xii69.5 (3)O5—O6—O1090.1 (4)
O1xii—Bi4—O3xii54.8 (3)Bi4—O6—O10148.8 (5)
O6xi—Bi4—O3xii60.9 (4)Fe1xi—O6—O10148.5 (5)
O4vii—Bi4—O3xii65.4 (3)O3vi—O6—O10107.2 (4)
O2xi—Bi4—O3xii115.9 (4)O4xiii—O6—O1089.6 (4)
O6—Bi4—O3xii123.7 (4)Bi3iii—O7—Bi3iv104.0 (4)
Fe1xi—Bi4—O4xiii126 (6)Bi3iii—O7—Bi1117.2 (4)
Bi4xi—Bi4—O4xiii7.6 (15)Bi3iv—O7—Bi1110.0 (3)
Fe1—Bi4—O4xiii18.5 (7)Bi3iii—O7—Bi2iii104.0 (3)
O1vi—Bi4—O4xiii105.2 (4)Bi3iv—O7—Bi2iii124.8 (4)
O2—Bi4—O4xiii105.0 (4)Bi1—O7—Bi2iii97.7 (3)
O1xii—Bi4—O4xiii62.4 (3)Bi3iii—O7—O3iii59.4 (3)
O6xi—Bi4—O4xiii105.0 (4)Bi3iv—O7—O3iii161.6 (4)
O4vii—Bi4—O4xiii178.4 (3)Bi1—O7—O3iii86.1 (3)
O2xi—Bi4—O4xiii63.8 (3)Bi2iii—O7—O3iii58.6 (3)
O6—Bi4—O4xiii64.4 (3)Bi3iii—O7—O4124.9 (4)
O3xii—Bi4—O4xiii116.1 (3)Bi3iv—O7—O4131.1 (4)
Bi4xi—Fe1—Bi435 (5)Bi1—O7—O448.1 (3)
Bi4xi—Fe1—Fe1xi28 (4)Bi2iii—O7—O449.7 (2)
Bi4—Fe1—Fe1xi7.4 (12)O3iii—O7—O466.3 (3)
Bi4xi—Fe1—O2xi115 (6)Bi3iii—O7—O7xv53.5 (3)
Bi4—Fe1—O2xi106.4 (7)Bi3iv—O7—O7xv50.5 (3)
Fe1xi—Fe1—O2xi108.8 (18)Bi1—O7—O7xv130.3 (5)
Bi4xi—Fe1—O1vi112 (6)Bi2iii—O7—O7xv131.7 (5)
Bi4—Fe1—O1vi76.7 (6)O3iii—O7—O7xv112.4 (5)
Fe1xi—Fe1—O1vi84.0 (16)O4—O7—O7xv177.6 (6)
O2xi—Fe1—O1vi77.7 (5)Bi3iii—O7—O8151.5 (4)
Bi4xi—Fe1—O4xiii121 (6)Bi3iv—O7—O864.1 (3)
Bi4—Fe1—O4xiii156.4 (9)Bi1—O7—O852.4 (3)
Fe1xi—Fe1—O4xiii149.2 (18)Bi2iii—O7—O8103.9 (3)
O2xi—Fe1—O4xiii78.4 (5)O3iii—O7—O8134.2 (4)
O1vi—Fe1—O4xiii126.6 (6)O4—O7—O870.9 (3)
Bi4xi—Fe1—O6108 (6)O7xv—O7—O8109.7 (5)
Bi4—Fe1—O6108.7 (7)Bi3iii—O7—O5iii54.6 (3)
Fe1xi—Fe1—O6109.1 (18)Bi3iv—O7—O5iii99.9 (4)
O2xi—Fe1—O6137.3 (7)Bi1—O7—O5iii150.0 (4)
O1vi—Fe1—O687.4 (5)Bi2iii—O7—O5iii62.0 (3)
O4xiii—Fe1—O679.2 (5)O3iii—O7—O5iii64.7 (3)
Bi4xi—Fe1—O1xii48 (5)O4—O7—O5iii109.3 (4)
Bi4—Fe1—O1xii83.6 (7)O7xv—O7—O5iii71.4 (4)
Fe1xi—Fe1—O1xii76.2 (15)O8—O7—O5iii149.0 (4)
O2xi—Fe1—O1xii108.5 (6)Bi3iii—O7—O9ii53.7 (3)
O1vi—Fe1—O1xii160.2 (6)Bi3iv—O7—O9ii102.0 (4)
O4xiii—Fe1—O1xii73.1 (4)Bi1—O7—O9ii68.4 (3)
O6—Fe1—O1xii99.0 (5)Bi2iii—O7—O9ii132.8 (4)
Bi4xi—Fe1—O251 (6)O3iii—O7—O9ii75.2 (3)
Bi4—Fe1—O257.1 (5)O4—O7—O9ii105.0 (4)
Fe1xi—Fe1—O254.5 (16)O7xv—O7—O9ii72.6 (4)
O2xi—Fe1—O2163.4 (6)O8—O7—O9ii101.5 (4)
O1vi—Fe1—O298.7 (5)O5iii—O7—O9ii108.0 (4)
O4xiii—Fe1—O2115.6 (5)Bi3iii—O7—O1xii124.0 (4)
O6—Fe1—O257.7 (4)Bi3iv—O7—O1xii75.1 (3)
O1xii—Fe1—O269.8 (4)Bi1—O7—O1xii115.1 (4)
Bi4xi—Fe1—O6xi59 (6)Bi2iii—O7—O1xii49.9 (2)
Bi4—Fe1—O6xi55.2 (5)O3iii—O7—O1xii106.7 (4)
Fe1xi—Fe1—O6xi54.6 (16)O4—O7—O1xii79.0 (3)
O2xi—Fe1—O6xi57.4 (4)O7xv—O7—O1xii103.4 (5)
O1vi—Fe1—O6xi90.5 (5)O8—O7—O1xii79.8 (3)
O4xiii—Fe1—O6xi114.7 (5)O5iii—O7—O1xii70.2 (3)
O6—Fe1—O6xi163.7 (5)O9ii—O7—O1xii176.0 (4)
O1xii—Fe1—O6xi78.2 (4)Bi3iii—O7—O5iv89.6 (3)
O2—Fe1—O6xi106.8 (5)Bi3iv—O7—O5iv46.4 (2)
Bi4xi—Fe1—O3vi166 (6)Bi1—O7—O5iv78.7 (3)
Bi4—Fe1—O3vi133.9 (8)Bi2iii—O7—O5iv166.0 (4)
Fe1xi—Fe1—O3vi141.1 (17)O3iii—O7—O5iv133.8 (4)
O2xi—Fe1—O3vi73.9 (4)O4—O7—O5iv124.4 (4)
O1vi—Fe1—O3vi58.1 (4)O7xv—O7—O5iv54.8 (3)
O4xiii—Fe1—O3vi69.6 (4)O8—O7—O5iv63.1 (3)
O6—Fe1—O3vi64.4 (4)O5iii—O7—O5iv126.3 (3)
O1xii—Fe1—O3vi141.4 (6)O9ii—O7—O5iv58.6 (3)
O2—Fe1—O3vi118.3 (5)O1xii—O7—O5iv119.3 (4)
O6xi—Fe1—O3vi127.2 (5)P2—O8—Bi1141.6 (6)
Bi4xi—Fe1—O4vii51 (5)P2—O8—O535.7 (3)
Bi4—Fe1—O4vii15.8 (5)Bi1—O8—O5144.2 (5)
Fe1xi—Fe1—O4vii23.1 (14)P2—O8—O235.4 (3)
O2xi—Fe1—O4vii103.8 (5)Bi1—O8—O2146.1 (5)
O1vi—Fe1—O4vii61.1 (4)O5—O8—O260.2 (4)
O4xiii—Fe1—O4vii172.2 (5)P2—O8—O634.5 (4)
O6—Fe1—O4vii103.3 (5)Bi1—O8—O6107.2 (4)
O1xii—Fe1—O4vii99.1 (5)O5—O8—O660.4 (4)
O2—Fe1—O4vii61.1 (4)O2—O8—O659.1 (4)
O6xi—Fe1—O4vii61.9 (4)P2—O8—Bi3iv107.2 (4)
O3vi—Fe1—O4vii118.1 (4)Bi1—O8—Bi3iv97.1 (3)
O3—P1—O10111.6 (5)O5—O8—Bi3iv118.0 (4)
O3—P1—O9105.9 (5)O2—O8—Bi3iv71.9 (3)
O10—P1—O9109.3 (5)O6—O8—Bi3iv123.0 (4)
O3—P1—O1108.4 (5)P2—O8—O7127.5 (5)
O10—P1—O1109.1 (5)Bi1—O8—O753.4 (3)
O9—P1—O1112.5 (5)O5—O8—O7160.4 (5)
O6—P2—O5111.5 (6)O2—O8—O7100.2 (4)
O6—P2—O2108.4 (6)O6—O8—O7111.6 (4)
O5—P2—O2109.8 (5)Bi3iv—O8—O748.9 (2)
O6—P2—O8110.2 (6)P2—O8—O8iv95.9 (5)
O5—P2—O8108.1 (6)Bi1—O8—O8iv120.5 (5)
O2—P2—O8108.9 (5)O5—O8—O8iv70.3 (4)
O6—P2—Bi4xi51.6 (4)O2—O8—O8iv86.6 (5)
O5—P2—Bi4xi135.0 (4)O6—O8—O8iv129.1 (6)
O2—P2—Bi4xi57.5 (4)Bi3iv—O8—O8iv69.8 (3)
O8—P2—Bi4xi116.9 (4)O7—O8—O8iv110.6 (5)
O6—P2—Bi459.0 (4)P2—O8—O1097.9 (5)
O5—P2—Bi4128.8 (4)Bi1—O8—O1050.8 (3)
O2—P2—Bi449.4 (4)O5—O8—O1094.8 (4)
O8—P2—Bi4122.5 (4)O2—O8—O10128.8 (5)
Bi4xi—P2—Bi49.8 (2)O6—O8—O1069.7 (4)
P1—O1—Bi4vi120.3 (5)Bi3iv—O8—O10147.1 (4)
P1—O1—Fe1vi104.5 (5)O7—O8—O1098.8 (4)
Bi4vi—O1—Fe1vi16.4 (2)O8iv—O8—O10129.0 (5)
P1—O1—Fe1viii123.5 (6)P2—O8—O5iv137.5 (5)
Bi4vi—O1—Fe1viii3.4 (4)Bi1—O8—O5iv80.4 (3)
Fe1vi—O1—Fe1viii19.8 (6)O5—O8—O5iv118.3 (4)
P1—O1—Bi4viii108.3 (5)O2—O8—O5iv109.7 (4)
Bi4vi—O1—Bi4viii12.4 (3)O6—O8—O5iv168.3 (5)
Fe1vi—O1—Bi4viii4.0 (4)Bi3iv—O8—O5iv46.1 (2)
Fe1viii—O1—Bi4viii15.8 (2)O7—O8—O5iv65.4 (3)
P1—O1—Bi2i129.4 (5)O8iv—O8—O5iv48.0 (3)
Bi4vi—O1—Bi2i108.6 (4)O10—O8—O5iv121.5 (4)
Fe1vi—O1—Bi2i124.9 (5)P2—O8—O4104.5 (5)
Fe1viii—O1—Bi2i105.2 (4)Bi1—O8—O440.7 (2)
Bi4viii—O1—Bi2i121.0 (4)O5—O8—O4129.3 (4)
P1—O1—O335.6 (3)O2—O8—O4108.2 (4)
Bi4vi—O1—O385.7 (4)O6—O8—O471.5 (4)
Fe1vi—O1—O369.5 (4)Bi3iv—O8—O4100.6 (3)
Fe1viii—O1—O389.0 (4)O7—O8—O453.8 (3)
Bi4viii—O1—O373.4 (3)O8iv—O8—O4159.4 (5)
Bi2i—O1—O3165.0 (4)O10—O8—O451.7 (3)
P1—O1—O1035.3 (3)O5iv—O8—O4112.0 (3)
Bi4vi—O1—O10123.7 (5)P2—O8—Bi381.2 (4)
Fe1vi—O1—O10114.2 (5)Bi1—O8—Bi3111.0 (3)
Fe1viii—O1—O10125.3 (5)O5—O8—Bi345.7 (3)
Bi4viii—O1—O10116.6 (4)O2—O8—Bi3101.8 (4)
Bi2i—O1—O10105.9 (4)O6—O8—Bi396.9 (4)
O3—O1—O1060.8 (3)Bi3iv—O8—Bi3121.4 (3)
P1—O1—O933.7 (3)O7—O8—Bi3150.2 (4)
Bi4vi—O1—O9137.7 (4)O8iv—O8—Bi351.6 (3)
Fe1vi—O1—O9122.1 (5)O10—O8—Bi382.6 (3)
Fe1viii—O1—O9140.9 (5)O5iv—O8—Bi388.3 (3)
Bi4viii—O1—O9126.0 (4)O4—O8—Bi3134.3 (3)
Bi2i—O1—O9110.2 (4)P1—O9—Bi3ix113.2 (5)
O3—O1—O957.9 (3)P1—O9—O336.8 (3)
O10—O1—O959.2 (4)Bi3ix—O9—O3106.6 (4)
P1—O1—O4xiv162.2 (6)P1—O9—O1035.2 (3)
Bi4vi—O1—O4xiv56.3 (3)Bi3ix—O9—O10142.4 (4)
Fe1vi—O1—O4xiv72.7 (4)O3—O9—O1061.3 (4)
Fe1viii—O1—O4xiv52.9 (4)P1—O9—O133.8 (3)
Bi4viii—O1—O4xiv68.7 (3)Bi3ix—O9—O183.7 (3)
Bi2i—O1—O4xiv52.7 (2)O3—O9—O159.5 (3)
O3—O1—O4xiv140.4 (4)O10—O9—O159.2 (4)
O10—O1—O4xiv129.0 (4)P1—O9—O7ii145.6 (5)
O9—O1—O4xiv160.9 (5)Bi3ix—O9—O7ii47.5 (2)
P1—O1—O2viii95.2 (5)O3—O9—O7ii153.9 (4)
Bi4vi—O1—O2viii58.0 (3)O10—O9—O7ii139.4 (4)
Fe1vi—O1—O2viii50.8 (4)O1—O9—O7ii112.6 (4)
Fe1viii—O1—O2viii59.9 (4)P1—O9—Bi1ii151.3 (5)
Bi4viii—O1—O2viii52.4 (3)Bi3ix—O9—Bi1ii90.9 (3)
Bi2i—O1—O2viii122.7 (4)O3—O9—Bi1ii151.7 (4)
O3—O1—O2viii68.6 (4)O10—O9—Bi1ii116.3 (4)
O10—O1—O2viii128.5 (5)O1—O9—Bi1ii146.7 (4)
O9—O1—O2viii86.7 (4)O7ii—O9—Bi1ii46.4 (2)
O4xiv—O1—O2viii96.2 (4)P1—O9—O5i89.9 (4)
P1—O1—O7viii104.7 (5)Bi3ix—O9—O5i91.2 (3)
Bi4vi—O1—O7viii121.7 (4)O3—O9—O5i126.7 (4)
Fe1vi—O1—O7viii128.0 (5)O10—O9—O5i73.9 (4)
Fe1viii—O1—O7viii120.2 (5)O1—O9—O5i73.8 (3)
Bi4viii—O1—O7viii126.9 (4)O7ii—O9—O5i66.0 (3)
Bi2i—O1—O7viii54.0 (2)Bi1ii—O9—O5i73.5 (3)
O3—O1—O7viii122.7 (4)P1—O9—Bi386.9 (4)
O10—O1—O7viii114.6 (4)Bi3ix—O9—Bi3103.7 (3)
O9—O1—O7viii71.4 (3)O3—O9—Bi351.9 (3)
O4xiv—O1—O7viii90.0 (4)O10—O9—Bi395.3 (3)
O2viii—O1—O7viii84.5 (4)O1—O9—Bi3110.3 (4)
P2—O2—Fe1xi105.5 (6)O7ii—O9—Bi3122.5 (3)
P2—O2—Bi1vii129.3 (6)Bi1ii—O9—Bi3103.0 (3)
Fe1xi—O2—Bi1vii95.4 (5)O5i—O9—Bi3164.8 (4)
P2—O2—Bi4101.7 (5)P1—O9—Bi180.8 (4)
Fe1xi—O2—Bi43.9 (4)Bi3ix—O9—Bi1157.8 (4)
Bi1vii—O2—Bi497.4 (4)O3—O9—Bi194.8 (3)
P2—O2—O635.5 (4)O10—O9—Bi146.2 (3)
Fe1xi—O2—O670.1 (5)O1—O9—Bi1103.0 (3)
Bi1vii—O2—O6130.3 (5)O7ii—O9—Bi1111.3 (3)
Bi4—O2—O666.2 (4)Bi1ii—O9—Bi171.83 (19)
P2—O2—O535.0 (3)O5i—O9—Bi170.9 (3)
Fe1xi—O2—O5122.7 (6)Bi3—O9—Bi193.9 (2)
Bi1vii—O2—O595.1 (4)P1—O9—O2iv136.5 (5)
Bi4—O2—O5119.1 (5)Bi3ix—O9—O2iv100.4 (4)
O6—O2—O560.7 (4)O3—O9—O2iv108.6 (4)
P2—O2—O835.7 (3)O10—O9—O2iv117.1 (4)
Fe1xi—O2—O8117.8 (5)O1—O9—O2iv168.1 (4)
Bi1vii—O2—O8145.4 (5)O7ii—O9—O2iv77.8 (3)
Bi4—O2—O8115.2 (5)Bi1ii—O9—O2iv45.0 (2)
O6—O2—O860.5 (4)O5i—O9—O2iv117.0 (4)
O5—O2—O859.5 (4)Bi3—O9—O2iv58.0 (2)
P2—O2—Bi4xi92.5 (5)Bi1—O9—O2iv77.4 (3)
Fe1xi—O2—Bi4xi14.2 (2)P1—O9—O7viii94.5 (4)
Bi1vii—O2—Bi4xi108.5 (4)Bi3ix—O9—O7viii42.7 (2)
Bi4—O2—Bi4xi11.3 (3)O3—O9—O7viii114.9 (4)
O6—O2—Bi4xi57.5 (4)O10—O9—O7viii106.7 (4)
O5—O2—Bi4xi114.5 (5)O1—O9—O7viii61.1 (3)
O8—O2—Bi4xi103.8 (4)O7ii—O9—O7viii51.5 (3)
P2—O2—Fe189.6 (5)Bi1ii—O9—O7viii93.1 (3)
Fe1xi—O2—Fe116.6 (6)O5i—O9—O7viii51.6 (3)
Bi1vii—O2—Fe1109.7 (5)Bi3—O9—O7viii143.5 (3)
Bi4—O2—Fe113.38 (18)Bi1—O9—O7viii122.4 (3)
O6—O2—Fe154.5 (4)O2iv—O9—O7viii128.9 (4)
O5—O2—Fe1111.5 (5)P1—O10—Bi1117.6 (5)
O8—O2—Fe1101.9 (5)P1—O10—O135.6 (3)
Bi4xi—O2—Fe13.1 (4)Bi1—O10—O1139.3 (5)
P2—O2—O1xii104.5 (5)P1—O10—O935.5 (3)
Fe1xi—O2—O1xii51.4 (4)Bi1—O10—O983.0 (4)
Bi1vii—O2—O1xii124.2 (5)O1—O10—O961.6 (4)
Bi4—O2—O1xii52.8 (3)P1—O10—O334.2 (3)
O6—O2—O1xii84.1 (4)Bi1—O10—O3119.4 (4)
O5—O2—O1xii139.5 (5)O1—O10—O359.3 (3)
O8—O2—O1xii86.9 (4)O9—O10—O358.3 (3)
Bi4xi—O2—O1xii48.4 (3)P1—O10—Bi2vi137.9 (5)
Fe1—O2—O1xii50.3 (4)Bi1—O10—Bi2vi98.3 (3)
P2—O2—O4vii132.0 (6)O1—O10—Bi2vi121.1 (4)
Fe1xi—O2—O4vii51.5 (4)O9—O10—Bi2vi165.7 (4)
Bi1vii—O2—O4vii43.9 (2)O3—O10—Bi2vi109.7 (4)
Bi4—O2—O4vii53.5 (3)P1—O10—O4165.0 (6)
O6—O2—O4vii104.8 (5)Bi1—O10—O448.0 (3)
O5—O2—O4vii115.4 (4)O1—O10—O4156.6 (5)
O8—O2—O4vii165.3 (5)O9—O10—O4130.9 (5)
Bi4xi—O2—O4vii64.7 (3)O3—O10—O4142.7 (5)
Fe1—O2—O4vii66.1 (4)Bi2vi—O10—O452.9 (3)
O1xii—O2—O4vii91.1 (4)P1—O10—O8100.1 (5)
P2—O2—Bi3iv92.6 (5)Bi1—O10—O848.6 (2)
Fe1xi—O2—Bi3iv118.4 (4)O1—O10—O8135.5 (4)
Bi1vii—O2—Bi3iv117.2 (4)O9—O10—O883.1 (4)
Bi4—O2—Bi3iv119.9 (4)O3—O10—O879.7 (4)
O6—O2—Bi3iv111.2 (4)Bi2vi—O10—O887.0 (3)
O5—O2—Bi3iv105.7 (4)O4—O10—O867.7 (3)
O8—O2—Bi3iv57.0 (3)P1—O10—O6109.4 (5)
Bi4xi—O2—Bi3iv114.4 (4)Bi1—O10—O687.1 (3)
Fe1—O2—Bi3iv115.6 (4)O1—O10—O6125.9 (4)
O1xii—O2—Bi3iv67.2 (3)O9—O10—O6118.1 (4)
O4vii—O2—Bi3iv134.9 (4)O3—O10—O675.4 (4)
P1—O3—Bi3110.4 (5)Bi2vi—O10—O648.0 (3)
P1—O3—O937.3 (3)O4—O10—O669.5 (3)
Bi3—O3—O975.6 (3)O8—O10—O647.9 (3)
P1—O3—O136.0 (3)P1—O10—O1xiv137.7 (5)
Bi3—O3—O1136.2 (4)Bi1—O10—O1xiv97.2 (3)
O9—O3—O162.6 (4)O1—O10—O1xiv102.2 (4)
P1—O3—O1034.3 (3)O9—O10—O1xiv147.0 (4)
Bi3—O3—O10110.6 (4)O3—O10—O1xiv141.1 (4)
O9—O3—O1060.4 (4)Bi2vi—O10—O1xiv47.2 (2)
O1—O3—O1059.9 (3)O4—O10—O1xiv56.2 (3)
P1—O3—Bi2145.4 (5)O8—O10—O1xiv121.5 (4)
Bi3—O3—Bi296.0 (3)O6—O10—O1xiv94.8 (4)
O9—O3—Bi2167.6 (4)P1—O10—O5i77.9 (4)
O1—O3—Bi2127.3 (4)Bi1—O10—O5i76.8 (3)
O10—O3—Bi2116.0 (4)O1—O10—O5i68.4 (3)
P1—O3—O7v156.0 (6)O9—O10—O5i59.5 (3)
Bi3—O3—O7v49.6 (2)O3—O10—O5i111.6 (4)
O9—O3—O7v118.9 (4)Bi2vi—O10—O5i134.7 (4)
O1—O3—O7v146.3 (4)O4—O10—O5i99.6 (4)
O10—O3—O7v153.2 (5)O8—O10—O5i117.6 (4)
Bi2—O3—O7v58.2 (3)O6—O10—O5i163.9 (4)
P1—O3—O6vi94.7 (5)O1xiv—O10—O5i88.2 (3)
Bi3—O3—O6vi147.1 (4)P1—O10—O6vi73.3 (4)
O9—O3—O6vi131.9 (5)Bi1—O10—O6vi151.3 (4)
O1—O3—O6vi76.2 (4)O1—O10—O6vi65.5 (3)
O10—O3—O6vi78.4 (4)O9—O10—O6vi107.7 (4)
Bi2—O3—O6vi53.5 (3)O3—O10—O6vi53.6 (3)
O7v—O3—O6vi109.0 (4)Bi2vi—O10—O6vi64.9 (3)
P1—O3—Fe1vi88.0 (4)O4—O10—O6vi117.3 (4)
Bi3—O3—Fe1vi146.4 (4)O8—O10—O6vi105.0 (4)
O9—O3—Fe1vi110.8 (4)O6—O10—O6vi64.2 (4)
O1—O3—Fe1vi52.4 (3)O1xiv—O10—O6vi88.0 (3)
O10—O3—Fe1vi100.4 (4)O5i—O10—O6vi131.8 (4)
Bi2—O3—Fe1vi81.3 (3)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y+1, z+2; (iii) x, y1, z; (iv) x+1, y+1, z+1; (v) x, y+1, z; (vi) x, y+1, z+1; (vii) x, y, z1; (viii) x, y+1, z+1; (ix) x+1, y+2, z+2; (x) x+1, y+2, z+1; (xi) x, y, z; (xii) x, y1, z1; (xiii) x, y, z+1; (xiv) x, y+1, z+2; (xv) x+1, y, z+1.

Experimental details

Crystal data
Chemical formulaBi6(Bi0.32Fe0.68)(PO4)4O4
Mr1801.1
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.2097 (18), 7.5214 (15), 6.9033 (14)
α, β, γ (°)112.48 (3), 93.71 (3), 106.95 (3)
V3)414.2 (2)
Z1
Radiation typeMo Kα
µ (mm1)67.86
Crystal size (mm)0.03 × 0.01 × 0.01
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionNumerical
(EUHEDRAL; Spek, 2006; de Meulenaer & Tompa, 1965)
Tmin, Tmax0.053, 0.403
No. of measured, independent and
observed [I > 2σ(I)] reflections
6043, 1855, 1600
Rint0.081
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.097, 1.11
No. of reflections1600
No. of parameters96
No. of restraints1
Δρmax, Δρmin (e Å3)4.10, 2.90

Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO-SMN (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2005).

Selected bond lengths (Å) top
Bi1—O42.083 (9)Bi3—O2iii3.067 (10)
Bi1—O9i2.965 (9)Bi4—O1iv2.291 (11)
Bi2—O4ii2.227 (9)Bi4—O4v2.999 (11)
Bi2—O52.760 (9)Fe1—O2vi2.332 (16)
Bi3—O7ii2.177 (8)Fe1—O3iv2.779 (15)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z; (iii) x+1, y+1, z+1; (iv) x, y+1, z+1; (v) x, y, z+1; (vi) x, y, z.
 

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