Pb₆Co₉(TeO₆)₅

Pb₆Co₉(TeO₆)₅, hexa­lead(II) nona­cobalt(II) penta­tellur­ate(VI), is isotypic with its nickel(II) analogue. The asymmetric unit contains two Pb atoms (site symmetries .2., ..2), four Co atoms (..2, ..2, 3.., 3.2) two Te atoms (..2, 3..) and six O atoms (all in general positions), with the Te and Co sites in octa­hedral coordination environments. The crystal structure can be subdivided into two types of layers parallel to (001). The first layer at z ≃ 0.25 is made up of edge-sharing [CoO₆] and [TeO₆] octa­hedra, with 1/6 of the octa­hedral holes not occupied. The second layer, situated at z ≃ 0, consist of an alternating arrangement of Pb^II atoms and of double octa­hedra that are made up from face-sharing [CoO₆] and [TeO₆] octa­hedra. The two types of layers are linked together through corner-sharing of [CoO₆] and [TeO₆] octa­hedra. The Pb^II atoms are situated in the cavities of the framework and are stereochemically active with one-sided [4]- and [6]-coordinations, respectively.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](Co-O) = 0.007 Å
• R factor = 0.025
• wR factor = 0.056
• Data-to-parameter ratio = 27.9

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT971_ALERT_2_A Large Calcd. Non-Metal Positive Residual Density       3.52 eA-3

Author Response: From the SHELX output ALL relevant remaining electron density is found NEAR the Pb atoms (as expected, see CIF). Probably another problem with respect to differences between PLATON and SHELXL.

Alert level C
PLAT774_ALERT_1_C Suspect X-Y Bond in CIF:   PB1    --  PB2     ..       3.58 Ang.
PLAT774_ALERT_1_C Suspect X-Y Bond in CIF:   PB1    --  PB2     ..       3.58 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              Co9 O30 Pb6 Te5
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          6
PLAT924_ALERT_1_C The Reported and Calculated Rho(min) Differ by .       1.04 eA-3
PLAT972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density      -2.50 eA-3
PLAT972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density      -2.04 eA-3
PLAT972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density      -1.74 eA-3
PLAT972_ALERT_2_C Large Calcd. Non-Metal Negative Residual Density      -1.54 eA-3
PLAT975_ALERT_2_C Positive Residual Density at 0.73A from O1     .       1.08 eA-3
PLAT976_ALERT_2_C Negative Residual Density at 0.81A from O6     .      -1.33 eA-3

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           37.57
           From the CIF: _reflns_number_total               2262
           Count of symmetry unique reflns         1386
           Completeness (_total/calc)            163.20%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       876
           Fraction of Friedel pairs measured     0.632
           Are heavy atom types Z>Si present        yes
PLAT004_ALERT_5_G Info: Polymeric Structure Found with Dimension .          3
PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF ....          ?
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported   _diffrn_ambient_temperature        293 K
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Pb1    --  Te2     ..       38.4 su
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Pb2    --  Te1     ..       36.5 su
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Te1    --  Co1     ..        6.8 su

   1 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
  11 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   8 ALERT level G = General information/check it is not something unexpected

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  10 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

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S1. Comment

Single crystals of the title compound, Pb₆Co₉(TeO₆)₅, were serendipitously obtained as a minority phase during phase formation studies in the system Pb^II/Co^II/Te^VI/O intended on crystal growth of cubic Pb₂CoTeO₆.

The crystal structure of Pb₆Co₉(TeO₆)₅ is isotypic with its nickel analogue (Wedel et al., 1998). The two Te(VI) and the four Co(II) atoms are in slightly distorted octahedral coordination environments with mean bond lengths of ¯d(Te—O) = 1.940 Å and ¯d(Co—O) = 2.105 Å, both in good agreement with literature data for oxotellurates (Levason, 1997) and for [CoO₆] octahedra (Wildner, 1992). The two lead(II) atoms exhibit coordination numbers of four and six. The crresponding Pb—O, Te—O and M—O (M = Co, Ni) bond lengths are very similar in the two isotypic structures.

The crystal structure of Pb₆Co₉(TeO₆)₅ can be described in terms of (001) layers A at z ≈ 0.25 and B at z ≈ 0 that stack alternately along [100] (Fig. 1). In layer A [TeO₆] and [CoO₆] octahedra share edges with 1/6 of the octahedral holes at the 2c and 2d positions, both with site symmetry 3.2, not occupied. The corresponding vacancies, denominated as X1 at the 2d position and as X2 at the 2c position, have different sizes. X1 has a diagonal diameter of 4.1076 (8) Å whereas X2 is somewhat larger with a diagonal diameter of 4.3258 (8) Å. This difference might be correlated with the size of the surrounding octahedra. Whereas the smaller X1 vacancy is encircled by a ring of six [CoO₆] octahedra, the larger X2 is encircled by a ring of three [CoO₆] and three slightly smaller [TeO₆] octahedra (Fig. 2). Layer B consists of double octahedra that are made up from face-sharing [CoO₆] and [TeO₆] octahedra, and by surrounding lead(II) atoms (Fig. 3). Adjacent A and B layers are linked together above and below the X1 and X2 vacancies through corner-sharing of [CoO₆] and [TeO₆] octahedra.

The resulting [Co₉Te₅O₃₀]^12- framework anion leaves space for the stereochemically active lead(II) cations. The oxygen coordination of the two Pb²⁺ cations is one-sided, with a [4]-coordination for Pb1 and a [6]-coordination for Pb2, if only Pb—O distances less than 2.75 Å are taken into account. The two cations share a common edge (O6—O6') with the lone pair electrons E pointing towards opposite directions. However, a bond valence calculation (Brown, 2002) shows a significant contribution of the four additional Pb—O distances for each of the two Pb atoms if interactions up to 3.5 Å are considered. Inclusion of these bonds increases the bond valence sum at Pb1 from 1.61 valence units (vu) to 1.83 vu and at Pb2 from 1.64 to 1.96 vu. The bond valence sum at O3 is also raised from 1.60 to 1.80 vu. Therefore the overall coordination of Pb1 might be described as [4 + 4] and that of Pb2 as [6 + 4] (Fig. 4).

Related literature

For the isotypic nickel analogue, see: Wedel et al. (1998). Reviews on the crystal chemistry of oxotellurates(VI) and of the geometry of [Co^IIO₆] polyhedra are given by Levason (1997) and Wildner (1992), respectively. For Pb₅TeO₈, see: Artner & Weil (2012). For the bond-valence method, see: Brown (2002).

S2. Experimental

1.281 (5.7 mmol) PbO, 0.216 g (2.9 mmol) CoO and 0.914 g (5.7 mmol) TeO₂ were mixed and thoroughly ground and heated in an alumina crucible under atmospheric conditions during 6 h to 1023 K and held at that temperature for 48 h. Then the furnace was shut-off. Several crystal phases could be identified from the cooled reaction mixture by single-crystal diffraction: Dark blue isometric crystals of Pb₂CoTeO₆, dark-red (nearly black) block-like crystals of Pb₅TeO₈ (Artner & Weil, 2012), colourless crystals of α-Al₂O₃ and dark red crystals of Pb₆Co₉(TeO₆)₅ with a block-like shape.

S3. Refinement

The highest remaining electron density was found 1.49 Å from atom Pb1 and the lowest remaining electron density 0.52 Å from atom Pb2. The refined Flack parameter indicates racemic twinning with an approximate ratio of 1:6 for the twin components.

Computing details

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ATOMS for Windows (Dowty, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures

	Fig. 1. The crystal structure of Pb6Co9(TeO6)5 in a projection along [010]. Displacement ellipsoids are drawn at the 90% probability level. Letters A and B indicate the two types of layers present in the structure.
	Fig. 2. Layer A (situated approximately at z ≈ 1/4) in the crystal structure of Pb6Co9(TeO6)5. Colour code and probability of the displacement parameters as in Fig. 1.
	Fig. 3. Layer B (situated approximately at z ≈ 0) in the crystal structure of Pb6Co9(TeO6)5. Colour code and probability of the displacement parameters as in Fig. 1.
	Fig. 4. The coordination spheres around the two lead atoms, considering bond lengths up to 3.5 Å; short Pb—O distances < 2.75 Å are given in black, emphasizing the one-sided [4]-coordination for Pb1 and [6]-coordination for Pb2. Longer bonds augmenting the coordination spheres are given in yellow. Probability of the displacement parameters as in Fig. 1.

hexalead(II) nonacobalt(II) pentatellurate(VI)

Crystal data

Pb6Co9(TeO6)5	Dx = 7.535 Mg m^−3
Mr = 2891.51	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6322	Cell parameters from 6739 reflections
Hall symbol: P 6c 2c	θ = 2.8–36.8°
a = 10.3915 (1) Å	µ = 50.89 mm^−1
c = 13.6273 (2) Å	T = 293 K
V = 1274.37 (3) Å^3	Parallelepiped, dark red
Z = 2	0.07 × 0.06 × 0.05 mm
F(000) = 2470

Data collection

Bruker APEXII CCD diffractometer	2262 independent reflections
Radiation source: fine-focus sealed tube	1908 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.068
ω and ϕ scans	θmax = 37.6°, θmin = 2.3°
Absorption correction: numerical (HABITUS; Herrendorf, 1997)	h = −16→17
Tmin = 0.123, Tmax = 0.200	k = −17→17
45686 measured reflections	l = −22→23

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0244P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.025	(Δ/σ)max < 0.001
wR(F^2) = 0.056	Δρmax = 2.96 e Å^−3
S = 1.09	Δρmin = −2.59 e Å^−3
2262 reflections	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
81 parameters	Extinction coefficient: 0.00019 (3)
0 restraints	Absolute structure: Flack (1983), 882 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.134 (10)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.26736 (3)	0.26736 (3)	0.0000	0.01216 (6)
Pb2	0.38848 (3)	1.0000	0.0000	0.01881 (8)
Te1	0.3333	0.6667	−0.09611 (4)	0.00407 (10)
Te2	0.16730 (4)	0.33460 (9)	0.2500	0.00433 (8)
Co1	0.3333	0.6667	0.11832 (9)	0.0066 (2)
Co2	0.16885 (10)	0.3377 (2)	−0.2500	0.00664 (18)
Co3	0.0000	0.0000	0.2500	0.0087 (3)
Co4	0.00992 (19)	0.50496 (10)	−0.2500	0.00566 (18)
O1	0.3366 (5)	0.3241 (5)	−0.1717 (3)	0.0077 (8)
O2	0.1726 (7)	0.5050 (6)	−0.1628 (3)	0.0083 (10)
O3	0.1702 (7)	0.1801 (6)	0.3277 (3)	0.0105 (9)
O5	0.3239 (8)	0.4818 (6)	0.3295 (3)	0.0076 (10)
O6	0.3481 (4)	0.5265 (4)	−0.0034 (4)	0.0069 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.01117 (9)	0.01117 (9)	0.01243 (12)	0.00429 (9)	0.00014 (9)	−0.00014 (9)
Pb2	0.01104 (9)	0.01201 (13)	0.03372 (18)	0.00601 (7)	−0.00268 (13)	−0.0054 (3)
Te1	0.00414 (14)	0.00414 (14)	0.0039 (2)	0.00207 (7)	0.000	0.000
Te2	0.00362 (13)	0.00380 (19)	0.00564 (18)	0.00190 (10)	0.0002 (4)	0.000
Co1	0.0066 (3)	0.0066 (3)	0.0066 (5)	0.00332 (16)	0.000	0.000
Co2	0.0057 (3)	0.0069 (5)	0.0077 (4)	0.0035 (2)	0.0006 (10)	0.000
Co3	0.0061 (4)	0.0061 (4)	0.0140 (7)	0.00305 (19)	0.000	0.000
Co4	0.0031 (5)	0.0045 (3)	0.0089 (4)	0.0015 (2)	0.000	−0.0002 (3)
O1	0.011 (2)	0.008 (2)	0.0048 (15)	0.0055 (14)	0.0003 (13)	−0.0022 (13)
O2	0.007 (2)	0.006 (2)	0.012 (2)	0.0022 (17)	−0.0001 (16)	−0.0034 (15)
O3	0.011 (2)	0.012 (2)	0.0077 (16)	0.0059 (15)	0.0000 (15)	0.0011 (15)
O5	0.004 (2)	0.006 (2)	0.0072 (18)	−0.0011 (18)	−0.0005 (18)	0.0009 (15)
O6	0.0058 (14)	0.0070 (14)	0.0075 (15)	0.0029 (11)	−0.001 (2)	0.002 (2)

Geometric parameters (Å, º)

Pb1—O6^i	2.387 (4)	Te2—O3^iii	1.937 (7)
Pb1—O6	2.387 (4)	Te2—O3	1.937 (7)
Pb1—O1^i	2.432 (4)	Te2—O1^xii	1.939 (5)
Pb1—O1	2.432 (4)	Te2—O1^i	1.939 (5)
Pb1—O3^ii	3.327 (7)	Co1—O5^x	2.004 (6)
Pb1—O3^iii	3.327 (7)	Co1—O5^iii	2.004 (6)
Pb1—O3^iv	3.453 (7)	Co1—O5^xiii	2.004 (6)
Pb1—O3^v	3.453 (7)	Co1—O6^vi	2.262 (5)
Pb1—Pb2^vi	3.5764 (4)	Co1—O6^vii	2.262 (5)
Pb1—Pb2^vii	3.5777 (2)	Co1—O6	2.262 (5)
Pb2—O6^viii	2.420 (3)	Co2—O2^xiv	2.090 (6)
Pb2—O6^vii	2.420 (3)	Co2—O2	2.090 (6)
Pb2—O2^ix	2.726 (5)	Co2—O3^i	2.090 (8)
Pb2—O2^vi	2.726 (5)	Co2—O3^iv	2.090 (8)
Pb2—O5^x	2.727 (5)	Co2—O1	2.108 (6)
Pb2—O5^xi	2.727 (5)	Co2—O1^xiv	2.108 (6)
Pb2—O6^vi	3.155 (3)	Co3—O3^xv	2.107 (4)
Pb2—O6^ix	3.155 (3)	Co3—O3	2.107 (4)
Pb2—O3^xi	3.230 (4)	Co3—O3^xvi	2.107 (4)
Pb2—O3^x	3.230 (4)	Co3—O3^xvii	2.107 (4)
Te1—O2^vi	1.906 (5)	Co3—O3^iii	2.107 (4)
Te1—O2	1.906 (5)	Co3—O3^v	2.107 (4)
Te1—O2^vii	1.906 (5)	Co4—O2	2.067 (7)
Te1—O6^vi	1.991 (4)	Co4—O2^xviii	2.067 (7)
Te1—O6^vii	1.991 (4)	Co4—O1^vi	2.071 (4)
Te1—O6	1.991 (4)	Co4—O1^xiv	2.071 (4)
Te2—O5	1.917 (6)	Co4—O5^xix	2.116 (7)
Te2—O5^iii	1.917 (6)	Co4—O5^iv	2.116 (7)
O6^i—Pb1—O6	84.58 (16)	O5^iii—Te2—O1^xii	85.9 (2)
O6^i—Pb1—O1^i	79.26 (18)	O3^iii—Te2—O1^xii	87.0 (2)
O6—Pb1—O1^i	77.79 (18)	O3—Te2—O1^xii	93.7 (2)
O6^i—Pb1—O1	77.79 (18)	O5—Te2—O1^i	85.9 (2)
O6—Pb1—O1	79.26 (18)	O5^iii—Te2—O1^i	93.3 (2)
O1^i—Pb1—O1	148.79 (19)	O3^iii—Te2—O1^i	93.7 (2)
O6^i—Pb1—O3^ii	95.87 (13)	O3—Te2—O1^i	87.0 (2)
O6—Pb1—O3^ii	133.98 (17)	O1^xii—Te2—O1^i	179.0 (3)
O1^i—Pb1—O3^ii	147.68 (15)	O5^x—Co1—O5^iii	108.14 (14)
O1—Pb1—O3^ii	56.26 (15)	O5^x—Co1—O5^xiii	108.14 (14)
O6^i—Pb1—O3^iii	133.98 (17)	O5^iii—Co1—O5^xiii	108.14 (14)
O6—Pb1—O3^iii	95.87 (13)	O5^x—Co1—O6^vi	87.99 (18)
O1^i—Pb1—O3^iii	56.26 (15)	O5^iii—Co1—O6^vi	85.39 (19)
O1—Pb1—O3^iii	147.68 (15)	O5^xiii—Co1—O6^vi	153.55 (18)
O3^ii—Pb1—O3^iii	114.8 (2)	O5^x—Co1—O6^vii	85.39 (19)
O6^i—Pb1—O3^iv	138.20 (17)	O5^iii—Co1—O6^vii	153.55 (18)
O6—Pb1—O3^iv	95.05 (13)	O5^xiii—Co1—O6^vii	87.99 (18)
O1^i—Pb1—O3^iv	141.63 (15)	O6^vi—Co1—O6^vii	72.17 (17)
O1—Pb1—O3^iv	61.26 (14)	O5^x—Co1—O6	153.55 (18)
O3^ii—Pb1—O3^iv	55.44 (13)	O5^iii—Co1—O6	87.99 (18)
O3^iii—Pb1—O3^iv	87.73 (10)	O5^xiii—Co1—O6	85.39 (18)
O6^i—Pb1—O3^v	95.05 (13)	O6^vi—Co1—O6	72.17 (17)
O6—Pb1—O3^v	138.20 (17)	O6^vii—Co1—O6	72.17 (17)
O1^i—Pb1—O3^v	61.26 (14)	O2^xiv—Co2—O2	87.8 (3)
O1—Pb1—O3^v	141.63 (15)	O2^xiv—Co2—O3^i	92.52 (17)
O3^ii—Pb1—O3^v	87.73 (10)	O2—Co2—O3^i	174.4 (3)
O3^iii—Pb1—O3^v	55.44 (13)	O2^xiv—Co2—O3^iv	174.4 (3)
O3^iv—Pb1—O3^v	111.4 (2)	O2—Co2—O3^iv	92.52 (17)
O6^viii—Pb2—O6^vii	83.17 (17)	O3^i—Co2—O3^iv	87.7 (2)
O6^viii—Pb2—O2^ix	61.34 (16)	O2^xiv—Co2—O1	89.3 (2)
O6^vii—Pb2—O2^ix	107.91 (19)	O2—Co2—O1	95.5 (2)
O6^viii—Pb2—O2^vi	107.91 (19)	O3^i—Co2—O1	78.9 (2)
O6^vii—Pb2—O2^vi	61.34 (16)	O3^iv—Co2—O1	96.2 (2)
O2^ix—Pb2—O2^vi	166.8 (3)	O2^xiv—Co2—O1^xiv	95.5 (2)
O6^viii—Pb2—O5^x	106.77 (19)	O2—Co2—O1^xiv	89.3 (2)
O6^vii—Pb2—O5^x	68.25 (16)	O3^i—Co2—O1^xiv	96.2 (2)
O2^ix—Pb2—O5^x	66.27 (12)	O3^iv—Co2—O1^xiv	78.9 (2)
O2^vi—Pb2—O5^x	112.94 (13)	O1—Co2—O1^xiv	173.3 (3)
O6^viii—Pb2—O5^xi	68.25 (16)	O3^xv—Co3—O3	175.2 (5)
O6^vii—Pb2—O5^xi	106.77 (19)	O3^xv—Co3—O3^xvi	79.5 (4)
O2^ix—Pb2—O5^xi	112.94 (13)	O3—Co3—O3^xvi	96.96 (14)
O2^vi—Pb2—O5^xi	66.27 (12)	O3^xv—Co3—O3^xvii	86.8 (4)
O5^x—Pb2—O5^xi	173.7 (3)	O3—Co3—O3^xvii	96.96 (14)
O6^viii—Pb2—O6^vi	138.39 (2)	O3^xvi—Co3—O3^xvii	96.96 (14)
O6^vii—Pb2—O6^vi	55.23 (15)	O3^xv—Co3—O3^iii	96.96 (14)
O2^ix—Pb2—O6^vi	126.25 (15)	O3—Co3—O3^iii	79.5 (4)
O2^vi—Pb2—O6^vi	55.67 (17)	O3^xvi—Co3—O3^iii	86.8 (4)
O5^x—Pb2—O6^vi	60.10 (16)	O3^xvii—Co3—O3^iii	175.2 (5)
O5^xi—Pb2—O6^vi	120.76 (15)	O3^xv—Co3—O3^v	96.96 (14)
O6^viii—Pb2—O6^ix	55.23 (15)	O3—Co3—O3^v	86.8 (4)
O6^vii—Pb2—O6^ix	138.39 (2)	O3^xvi—Co3—O3^v	175.2 (5)
O2^ix—Pb2—O6^ix	55.67 (17)	O3^xvii—Co3—O3^v	79.5 (4)
O2^vi—Pb2—O6^ix	126.25 (15)	O3^iii—Co3—O3^v	96.96 (14)
O5^x—Pb2—O6^ix	120.76 (15)	O2—Co4—O2^xviii	89.8 (3)
O5^xi—Pb2—O6^ix	60.10 (16)	O2—Co4—O1^vi	96.9 (2)
O6^vi—Pb2—O6^ix	166.38 (13)	O2^xviii—Co4—O1^vi	91.0 (2)
O6^viii—Pb2—O3^xi	120.59 (18)	O2—Co4—O1^xiv	91.0 (2)
O6^vii—Pb2—O3^xi	121.18 (18)	O2^xviii—Co4—O1^xiv	96.9 (2)
O2^ix—Pb2—O3^xi	130.9 (2)	O1^vi—Co4—O1^xiv	168.8 (4)
O2^vi—Pb2—O3^xi	60.21 (13)	O2—Co4—O5^xix	174.7 (3)
O5^x—Pb2—O3^xi	132.1 (2)	O2^xviii—Co4—O5^xix	90.92 (16)
O5^xi—Pb2—O3^xi	53.44 (14)	O1^vi—Co4—O5^xix	77.8 (2)
O6^vi—Pb2—O3^xi	86.29 (19)	O1^xiv—Co4—O5^xix	94.2 (2)
O6^ix—Pb2—O3^xi	84.37 (18)	O2—Co4—O5^iv	90.92 (16)
O6^viii—Pb2—O3^x	121.18 (18)	O2^xviii—Co4—O5^iv	174.7 (3)
O6^vii—Pb2—O3^x	120.59 (18)	O1^vi—Co4—O5^iv	94.2 (2)
O2^ix—Pb2—O3^x	60.21 (13)	O1^xiv—Co4—O5^iv	77.8 (2)
O2^vi—Pb2—O3^x	130.9 (2)	O5^xix—Co4—O5^iv	88.9 (3)
O5^x—Pb2—O3^x	53.44 (14)	Te2^ii—O1—Co4^vii	98.54 (19)
O5^xi—Pb2—O3^x	132.1 (2)	Te2^ii—O1—Co2	96.67 (17)
O6^vi—Pb2—O3^x	84.37 (18)	Co4^vii—O1—Co2	89.3 (2)
O6^ix—Pb2—O3^x	86.29 (19)	Te2^ii—O1—Pb1	116.6 (2)
O3^xi—Pb2—O3^x	93.32 (14)	Co4^vii—O1—Pb1	136.07 (18)
O2^vi—Te1—O2	99.15 (18)	Co2—O1—Pb1	110.4 (2)
O2^vi—Te1—O2^vii	99.15 (18)	Te1—O2—Co4	129.1 (3)
O2—Te1—O2^vii	99.15 (18)	Te1—O2—Co2	130.4 (4)
O2^vi—Te1—O6^vi	90.7 (2)	Co4—O2—Co2	89.87 (19)
O2—Te1—O6^vi	85.2 (2)	Te1—O2—Pb2^vii	95.48 (17)
O2^vii—Te1—O6^vi	168.4 (2)	Co4—O2—Pb2^vii	96.4 (2)
O2^vi—Te1—O6^vii	85.2 (2)	Co2—O2—Pb2^vii	111.0 (2)
O2—Te1—O6^vii	168.4 (2)	Te2—O3—Co2^xx	97.34 (17)
O2^vii—Te1—O6^vii	90.7 (2)	Te2—O3—Co3	96.2 (2)
O6^vi—Te1—O6^vii	84.0 (2)	Co2^xx—O3—Co3	92.8 (3)
O2^vi—Te1—O6	168.4 (2)	Te2—O5—Co1^xiii	125.5 (4)
O2—Te1—O6	90.7 (2)	Te2—O5—Co4^xx	97.7 (2)
O2^vii—Te1—O6	85.2 (2)	Co1^xiii—O5—Co4^xx	120.3 (3)
O6^vi—Te1—O6	84.0 (2)	Te2—O5—Pb2^xxi	117.3 (2)
O6^vii—Te1—O6	84.0 (2)	Co1^xiii—O5—Pb2^xxi	97.82 (18)
O5—Te2—O5^iii	92.5 (3)	Co4^xx—O5—Pb2^xxi	95.2 (2)
O5—Te2—O3^iii	177.8 (2)	Te1—O6—Co1	86.54 (14)
O5^iii—Te2—O3^iii	89.6 (2)	Te1—O6—Pb1	136.5 (2)
O5—Te2—O3	89.6 (2)	Co1—O6—Pb1	127.8 (2)
O5^iii—Te2—O3	177.8 (2)	Te1—O6—Pb2^vi	103.41 (16)
O3^iii—Te2—O3	88.2 (2)	Co1—O6—Pb2^vi	100.34 (16)
O5—Te2—O1^xii	93.3 (2)	Pb1—O6—Pb2^vi	96.12 (13)

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