Role of lone-pair electron localization in temperature-induced phase transitions in mimetite

The crystal structure of mimetite Pb₅(AsO₄)₃Cl, a phosphate with apatite structure-type has been investigated in situ at 123, 173, 273, 288, 353 and 393 K. A careful inspection of the diffraction pattern and subsequent structure refinements indicated that mimetite transforms from the monoclinic to the hexagonal polymorph with increasing temperature. At 123 K, a monoclinic superstructure, mimetite-2M, with cell parameters a = 20.4487 (9),  b = 7.4362 (2), c = 20.4513 (9) Å, β = 119.953 (6)°, V = 2694.5 (2) ų and space group P2₁ was observed. From 173 to 353 K, the reflections of the supercell were evident only along one direction of the corresponding hexagonal apatite-cell and the structure transforms to the polymorph mimetite-M with space group P2₁/b and unit-cell parameters a = 10.2378 (3), b = 20.4573 (7), c = 7.4457 (2) Å, β = 120.039 (5)°, V = 1349.96 (9) ų. Only at higher temperature, i.e. 393 K, does mimetite adopt the hexagonal space group P6₃/m characteristic of apatite structure-types. The role of the electron lone pairs of Pb atoms in the phase transition was investigated through the analysis of the electron localization function (ELF) calculated based on the DFT-geometry optimized structures of the three polymorphs. The changes in spatial distribution of the 6s² electron density during the phase transitions were explored by means of the Wannier Function Centres (WFCs) derived from ab initio molecular dynamics trajectories. In the high-temperature hexagonal structure the 6s² electrons are spherically symmetric relative to the position of Pb atoms. At low temperature the maximum of 6s² electron density is displaced relative to the position of Pb atom contributing to the polar interaction in the monoclinic polymorphs.

1. Introduction

Minerals of apatite group are the most abundant rock-forming phosphates and the main host of phospho­rus in crustal rocks. Besides, materials with apatite structure-type are used in water purification, bone replacement, ceramic membranes, catalysis, photoluminescence, biomedical applications and many others (Kohn et al., 2002). The chemical formula of apatite group minerals can be generalized as A₅(TO₄)₃X, where A = large cations, T = metals or metalloids, and X = anions. The structure can be thought in terms of a zeolite-like topology where one-dimensional tunnels are created by the framework A₂(TO₄)₃ polyhedra and A₃X represents the extra-framework component. The majority of apatite structural-types crystallize in the hexagonal space group P6₃/m (No. 176), where two A sites are distinguished: A1, which forms the framework network A₂(TO₄)₃, and A2 that is part of the extraframework unit A₃X. Apatite sensu stricto refers to three distinct minerals fluorapatite Ca₅(PO₄)₃F, chlorapatite Ca₅(PO₄)₃Cl and hy­droxy­lapatite Ca₅(PO₄)₃OH, described in the space group P6₃/m (Hughes et al., 1989; Hughes & Rakovan, 2002). Chemical substitutions on cation and/or anion sites can originate several structures, which mostly show sub-symmetries of the hexagonal one.

The presence of Pb²⁺ in the A site is of interest for both catalytic and environmental applications. Among them, Pb apatites are used as metal scavengers in treatment of water and contaminated soils, and for the immobilization of radioactive iodine (Wang, 2015; Cao et al., 2017). The stereochemical activity of the 6s² lone-pair electrons of Pb plays a crucial role in the structural and electronic properties of Pb apatites (Matar & Galy, 2015). It is generally accepted that the lone pair cations prefer the A2 site in order to reach a more stereochemically flexible environment (Peet et al., 2017).

Four minerals constitute the isotypic series of Pb apatites: vanadinite, mimetite, pyromorphite, and finnemanite. They all crystallize in the hexagonal space group P6₃/m characteristic of apatite (Gabrielson, 1955; Dai & Hughes, 1989; Dai et al., 1991). Interestingly, mimetite Pb₅(AsO₄)₃Cl was also reported to adopt a monoclinic structure, where the a_hex and b_hex axes are doubled and the monoclinic angle is close to 120°. The monoclinic polymorph has been solved in different space groups. At first, the polymorph mimetite-M, was described in space group P112₁/b (non-standard setting of space group P2₁/c, No. 14). The cell parameters imply the doubling of one axis of the hexagonal cell, resulting in: a = 10.189 (3), b = 20.372 (8), c = 7.46 (1) Å, γ = 119.88 (3)° (Dai et al., 1991). Subsequently, Yang et al. (2013) reported a monoclinic mimetite, mimetite-2M, with a superstructure characterized by the doubling of both a- and b-axes with respect to hexagonal mimetite (mimetite-H). The symmetry further reduced and the structure was refined in space group P2₁ (No. 4). Similarly, synchrotron single-crystal X-ray diffraction data collected on a natural mimetite, were indexed with a monoclinic superstructure with cell parameters: a = 20.44 (1), b = 7.437 (1), c = 20.44 (1) Å, β = 120° (Baikie et al., 2014). However, based on the analysis of the systematic absences, the authors opted for the higher-symmetry space group P2₁/a (Baikie et al., 2014). The monoclinic polymorph was observed in both synthetic and natural samples. Studies on mimetite minerals from different localities demonstrated that mimetite-M and -2M are much rarer compared to the hexagonal one. The occurrence of the monoclinic distortion was initially ascribed to changes in temperature: Keppler (1968, 1969) reported the phase transition from the monoclinic to the hexagonal polymorphs between 98 and 120°C, depending on the samples. However, these results were not supported by a powder neutron diffraction study of synthetic mimetite that showed no evidence of phase transformation between 293 and 473 K (Baikie et al., 2008). Later, a transition from monoclinic to hexagonal mimetite was suggested to be both temperature and composition dependent, with minor Ca and P substitutions that would stabilize the hexagonal structure (Baikie et al., 2014). This conclusion was drawn based on the re-interpretation and re-analysis of previous data (Flis et al., 2010) on the synthetic solid solution Pb₁₀(P_1–xAs_xO₄)₆Cl₂. Nevertheless, most mimetite structures (synthetic and natural) were found to be hexagonal at ambient temperature. Thus, it remains unclear what effect the temperature and the chemical composition have on the formation of the monoclinic polymorph.

In this study, we aimed at clarifying different open questions on mimetite. In particular we want to determine: (i) whether the transformation from hexagonal to monoclinic is temperature driven, and (ii) what is the difference between the electronic structure in terms of lone-pair electrons in the two modifications of mimetite and (iii) whether the lone-pairs distribution has an effect on the phase transition. Temperature-dependent X-ray diffraction data were collected in situ on a natural sample of mimetite by using a single-crystal X-ray diffractometer to ensure high precision of the structural analysis. To assess the role of chemical bonding and electron localization on the structural transformation in mimetite the maximal localized Wannier centres and electron localization function (ELF) were analysed from atomic trajectories of corresponding polymorphs obtained by ab initio molecular dynamic simulations and geometry optimization at DFT level of theory, respectively.

2. Methods

2.1. Sample description and chemical composition

The sample was a natural mimetite originating from Tsumeb-Otjikoto, Namibia.

The chemical composition was quantitatively determined by electron microprobe analyser (EMPA, Jeol JXA-8230) installed at Yamaguchi University, Japan. The elements, As, P, V, S, Si, Ti, Al, Cr, Fe, Mn, Mg, Ni, Cu, Pb, Ca, Na, K, Sn, F and Cl were measured using an accelerating voltage 15 kV and a beam current of 20 nA with a beam diameter of 1–10 µm. The following probe standards were used: synthetic GaAs (As), synthetic KTiPO₄ (P), synthetic PbVGe-oxide (V, Pb), natural barite (S), natural wollastonite (Si, Ca), synthetic rutile (Ti), synthetic corundum (Al), synthetic eskolaite (Cr), synthetic hematite (Fe), synthetic manganosite (Mn), synthetic periclase (Mg), synthetic bunsenite (Ni), metallic copper (Cu), natural albite (Na), natural orthoclase (K), natural cassiterite (Sn), synthetic fluorite (F) and synthetic halite (Cl). Wavelength-dispersion spectra were collected using LiF, PET, and TAP monochromator crystals to identify interfering elements and locate the best wavelengths for background measurements. The ZAF correction method was used for all elements. The chemical composition was determined from the average of 31 analytical points and calculated based on 12 oxygen atoms.

2.2. Temperature-dependent single-crystal X-ray diffraction

Diffraction data were collected on a Rigaku Synergy-S diffractometer equipped with a double microfocus sources and an Oxford Cryostream-700+ open-flow cryostat. A single fragment of mimetite with dimension 0.100 × 0.06 × 0.04 mm was selected and mounted on the tip of a glass fibre, fixed onto a goniometer head. At first, data were collected at ambient temperature (288 K) by using the Ag Kα (λ = 0.56087 Å) radiation. Preliminary screening of the crystal indicated a hexagonal unit cell with dimensions a = 10.228 (14) Å, c = 7.463 (14) Å, V = 676 (2) ų. Thus, a data set was collected based on a primitive lattice in the hexagonal Laue class 6/m. However, indexing and subsequent data analysis of this data set indicated a monoclinic unit cell with unit-cell parameters: a = 10.2354 (13), b = 17.7370 (18), c = 7.4591 (10) Å, β = 90.099 (13)°, V = 1354.2 (3) ų. A new data set was collected based on this monoclinic unit cell, ensuring high redundancy (> 5) and average total I/σ(I) > 25.

After the data collection at 288 K, the T-dependent measurements were performed in situ on the same crystal at the following temperatures: on heating at 123, 173, 273, 393 K, and on cooling at 353 K. Between each step, the crystal was equilibrated at the next temperature for at least 30 min. Data collection strategy for each data set was computed based on a monoclinic unit-cell, ensuring high redundancy (ca 4) and I/σ(I) > 20. Data were reduced by using the software package CrysAlisPro (Matsumoto et al., 2021), applying an empirical absorption correction. The structures were solved by direct methods with the software SHELXS (Sheldrick, 2008) and refined by SHELXL (Sheldrick, 2015) using neutral atomic scattering factors.

Data collection and refinement parameters of mimetite at 288 K, 123 and 393 K are summarized in Table 1. Corresponding experimental parameters of mimetite at 173, 273, and 353 K are reported in Table S1 in supporting information. All structure drawings have been produced by using the software VESTA (Momma & Izumi, 2011).

Table 1
Experimental details for mimetite at 288, 123 and 393 K

	Mimetite-M (288 K)	Mimetite-2M (123 K)	Mimetite-H (393 K)
Crystal data
Chemical formula	As2Cl0.67O8Pb3.33	As3ClO12Pb5	As3ClO12Pb5
Crystal system, space group	Monoclinic, P1121/b	Monoclinic, P21	Hexagonal, P63/m
a, b, c (Å)	10.2552 (3), 20.4913 (6), 7.4576 (2)	20.4487 (9), 7.4362 (2), 20.4513 (9)	10.2722 (3), 7.4537 (3)
β (°)	90	119.953 (6)	90
γ (°)	119.993 (2)	90	120
V (Å^3)	1357.29 (7)	2694.5 (2)	681.14 (5)
Z	6	6	2
Radiation type, λ (Å)	Ag Kα, 0.56087	Ag Kα, 0.56087	Ag Kα, 0.56087
μ (mm^−1)	37.74	37.49	37.60
Crystal size (mm)	0.10 × 0.06 × 0.04	0.10 × 0.06 × 0.04	0.10 × 0.06 × 0.04
Data collection
Diffractometer	XtaLAB Synergy, Dualflex, Hypix	XtalLAB, Synergy, Dualflex, Hypix	XtalLAB, Synergy, Dualflex, Hypix
No. of measured, independent and observed [I > 2σ(I)] reflections	27930, 5638, 4670	50947, 19430, 15378	11659, 1202, 1060
Rint	0.048	0.056	0.038
(sin θ/λ)max (Å^−1)	0.794	0.769	0.870
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.033, 0.078, 1.06	0.055, 0.129, 1.08	0.027, 0.059, 1.14
No. of reflections	5638	19430	1202
No. of parameters	190	387	39
No. of restraints		1
	w = 1/[σ^2(Fo^2) + (0.0292P)^2 + 12.8986P] where P = (Fo^2 + 2Fc^2)/3	w = 1/[σ^2(Fo^2) + 226.143P] where P = (Fo^2 + 2Fc^2)/3	w = 1/[σ^2(Fo^2) + (0.0248P)^2 + 4.3504P] where P = (Fo^2 + 2Fc^2)/3
Δρmax, Δρmin (e Å^−3)	4.21, −4.54	6.42, −11.99 (see comment in §3.1)	2.35, −3.92
Absolute structure	–	Refined as an inversion twin	–
Absolute structure parameter	–	0.51 (5)	–

2.3. DFT-based geometry optimization and molecular dynamics simulations

The optimized structures of the three polymorphs (mimetite-H, mimetite-2M, and mimetite-M) were obtained by density functional theory (DFT)-based calculations using the Gaussian and Plane Waves method (GPW) as implemented in the CP2K simulation package (http://www.cp2k.org; Kühne et al., 2020). The electron exchange and correlations were described by PBE functional (Perdew et al., 1996). The Kohn–Sham orbitals were expanded using a linear combination of atom-centred Gaussian type orbital functions. In this study, a short-range double-ξ valence polarized basis set for each atom type was used (VandeVondele & Hutter, 2007). Dispersion correction was taken into account using the DFT+D3 method (Grimme, 2006).

The initial atomic configuration was taken from the refined structure obtained from XRD experiments. A supercell 2 × 2 × 2 was used for mimetite-H, 2 × 1 × 2 for mimetite-M, and 1 × 1 × 2 for mimetite-2M. The supercell contained 80 Pb, 16 Cl, 192 O and 48 As. The analysis of the lone pair electrons of Pb atoms was performed based on the Electron Localization Function (ELF) (Becke & Edgecombe, 1990). The ELF values were calculated for the optimized structure of each polymorph based on the definition of Savin et al. (1997), where 0 < ELF < 1 is a normalized function between 0 (zero localization) and 1 (strong localization) with the value ½ corresponding to a free-electron gas behaviour.

To obtain atomic trajectories of the experimentally observed structural polymorphs at different temperatures, a series of MD simulations were performed using the following modelling strategy: The atomic coordinates of mimetite-2M (supercell 2 × 2 × 3, to account accurately for dynamic disorder) as obtained by XRD were used as input to run MD simulations at 123 K. After the thermal equilibration for at least 5 ps, atomic trajectories were collected in NPT ensemble at 123 K for 20 ps. The last atomic configuration of the run was used as the input structure to run a second set of NPT MD simulations at 173 K. The same approach was used to subsequently collect the MD trajectories at 293 and 393 K.

For each MD trajectory at 123, 173, 293 and 393 K, the maximally localized Wannier Functions Centres (WFCs) were calculated in step of 100 fs. Structural data analysis was performed by means of MDAnalysis software (Michaud-Agrawal et al., 2011; Gowers et al., 2016).

3. Results and discussion

The chemical composition obtained from EMPA is reported in Table 2. The analysed crystals were chemically homogeneous and no significant trace of Ca (wt% < 0.01) or P (wt% = 0.15) were detected. This is consistent with the refined chemical formula (Table 1).

Table 2
Average composition of mimetite obtained from EMPA

apfu is atoms per formula unit.

	wt%	Std. Dev.			apfu	Std. Dev.
As2O5	22.64	0.24		As^5+	2.72	0.02
P2O5	0.15	0.12		P^5+	0.03	0.02
V2O5	0.01	0.02		V^5+	0.00	0.00
SO3	0.01	0.02		S^6+	0.00	0.00
SiO2	0.01	0.01		Si	0.00	0.00
TiO2	0.02	0.02		Ti	0.00	0.00
Al2O3	0.01	0.01		Al	0.00	0.00
Cr2O3	0.01	0.02		Cr^3+	0.00	0.00
Fe2O3	0.01	0.02		Fe^3+	0.00	0.00
MnO	0.00	0.01		Mn^2+	0.00	0.00
MgO	0.02	0.01		Mg	0.01	0.00
NiO	0.02	0.03		Ni	0.00	0.00
CuO	0.00	0.01		Cu^2+	0.00	0.00
PbO	73.84	0.62		Pb^2+	4.58	0.02
CaO	0.01	0.01		Ca	0.00	0.00
Na2O	0.01	0.02		Na	0.00	0.01
K2O	0.00	0.00		K	0.00	0.00
SnO2	0.02	0.02		Sn^4+	0.00	0.00
F	0.02	0.03		F^−	0.01	0.02
Cl	2.47	0.08		Cl^−	0.96	0.03
Total	99.28
Ex. O†	0.57
Total − Ex. O	98.71

†Excluded oxygen content corrected for Cl and F substitution.

3.1. Structural transformations

The diffraction pattern of mimetite obtained at ambient temperature and pressure unequivocally indicated the presence of reflections which cannot be indexed by the apatite-type hexagonal unit cell [Fig. 1(a)]. Our analysis pointed to a monoclinic unit-cell, with c_m = 2b_hex. The doubling of only one unit-cell parameter with respect to the hexagonal cell of mimetite-H corresponds to the mimetite-M polymorph reported by Dai et al. (1991) and reflects the fact that the satellite reflections are mainly located along ½b_hex axis [Fig. 1(a)]. The monoclinic unit cell, a = 10.2552 (3), b = 7.45761 (19), c = 17.7473 (5) Å, β = 90.038 (3)°, V = 1357.30 (7) ų, was used to index the diffraction pattern and to perform the subsequent data reduction [Fig. 1(b)]. Structure solution indicated the space group P2₁/c (No. 14), subsequently transformed to the non-standard setting P112₁/b, with unit-cell parameters a = 10.2552 (3), b = 20.4913 (6), c = 7.4576 (2) Å, γ = 119.993 (2)°, V = 1357.29 (7) ų, for a better comparison with literature data (Dai et al., 1991). The structure did not show significant differences from mimetite-M previously reported by Dai et al. (1991). Nine oxygen atoms coordinate Pb at the A1 sites (Pb1), six are found at distances smaller than 2.8 Å and three at longer distances. Pb atoms at A2 sites (Pb2) are on average coordinated by six oxygen and two chlorine atoms. Table 3 reports the selected bond distances for mimetite-M as calculated form our data and those of mimetite-M taken from Dai et al. (1991).

Table 3
Selected geometric parameters of mimetite-M at 288 K (Å)

The second line show the corresponding distances reported by Dai et al. (1991).

Pb1A—O1B^i	2.476 (5)	Pb1B—O3D	2.706 (6)	Pb2C—O2B^i	2.364 (7)
	2.40 (4)		2.69 (3)		2.38 (3)
Pb1A—O1C	2.518 (5)	Pb1B—O2B^i	2.829 (8)	Pb2C—O3B^vii	2.443 (7)
	2.54 (3)		2.71 (4)		2.41 (3)
Pb1A—O1A	2.565 (5)	Pb1B—O2A	2.853 (6)	Pb2C—O3F	2.445 (6)
	2.53 (4)		2.81 (3)		2.47 (2)
Pb1A—O2A^ii	2.713 (6)	Pb1B—O3E	2.952 (9)	Pb2C—O1A^viii	3.077 (6)
	2.73 (2)		3.00 (2)		3.03 (2)
Pb1A—O3C^ii	2.715 (6)	Pb1B—O3F	3.208 (7)	Pb2C—O3C	3.078 (7)
	2.68 (3)		3.18 (3)		3.12 (3)
Pb1A—O2B^iii	2.725 (7)	Pb1B—Pb1A^i	3.6289 (3)	Pb2C—Cl^viii	3.1548 (19)
	2.72 (4)				3.14 (2)
Pb1A—O3B^ii	2.929 (10)	Pb1B—O1A^i	2.495 (6)	Pb2C—O3E^viii	2.834 (6)
	2.79 (2)		2.46 (4)		2.85 (2)
Pb1A—O2C^ii	2.931 (6)	Pb1B—O1C^i	2.515 (5)	AsA—O1A	1.672 (6)
	2.94 (2)		2.54 (3)		1.72 (2)
Pb1A—O3A^ii	3.156 (7)	Pb1B—O1B	2.591 (5)	AsA—O3A	1.683 (6)
	3.12 (3)		2.61 (4)		1.67 (3)
		Pb1B—O2C	2.659 (6)	AsA—O3D	1.689 (6)
			2.66 (2)		1.69 (3)
				AsA—O2A	1.691 (5)
					1.67 (2)
Pb2A—O2C	2.362 (5)	Pb2B—O2A^i	2.356 (6)	AsB—O3B^i	1.663 (7)
	2.33 (2)		2.33 (1)		1.63 (3)
Pb2A—O3C^iv	2.458 (5)	Pb2B—O3D	2.497 (6)	AsB—O3E^i	1.675 (6)
	2.48 (3)		2.48 (3)		1.67 (2)
Pb2A—O3A	2.468 (7)	Pb2B—O3E^i	2.596 (9)	AsB—O1B^ix	1.677 (5)
	2.51 (2)		2.52 (2)		1.71 (2)
Pb2A—O3F^v	2.805 (6)	Pb2B—O3A^vi	2.795 (6)	AsB—O2B	1.682 (7)
	2.81 (3)		2.79 (3)		1.70 (2)
Pb2A—O3D	3.016 (8)	Pb2B—O3B^i	2.828 (11)	AsC—O3F	1.682 (5)
	2.97 (3)		3.04 (4)		1.67 (2)
Pb2A—O1B^v	3.077 (7)	Pb2B—O1C^i	3.082 (6)	AsC—O1C^x	1.688 (5)
	3.08 (2)		3.08 (2)		1.65 (1)
Pb2A—Cl	3.2004 (17)	Pb2B—Cl	3.1370 (18)	As3—O2C	1.691 (6)
	3.19 (2)		3.11 (1)		1.69 (2)
				As3—O3C	1.692 (5)
					1.63 (3)
Symmetry code(s): (i) −x + 1, −y + 1, −z + 1; (ii) −x + 1, −y + 1, −z; (iii) x, y, z − 1; (iv) −x, −y + 1, −z; (v) −x, −y + 1, −z + 1; (vi) x, y, z + 1; (vii) −x + 1, −y + , z + ; (viii) x, y + , −z + ; (ix) x, y − , −z + ; (x) x−1, y, z; (xi) x, y + , −z + ; (xii) x + 1, y, z; (xiii) −x + 1, −y + , z − .

Figure 1 Reciprocal lattice view of mimetite diffraction data collected at 288 K. The distribution histograms of the reflections in the hexagonal (a) and monoclinic (b) unit cells are shown. The size of the reflection spots is proportional to the intensity of the reflections.

The analysis of the data set measured at 123 K pointed to a monoclinic superstructure with unit-cell parameters: a = 20.4487 (9), b = 7.4362 (2), c = 20.4513 (9) Å, β = 119.953 (6)°, V = 2694.5 (2) ų. In this case, the superstructure reflections were clearly distributed along both a and b axes of the corresponding hexagonal cell [Fig. 2(a)]. The data reduction suggested the monoclinic space group P2₁/c. However, due to unsatisfactory structure refinement (negative atomic displacement parameters for oxygen atoms and high residuals close to non-Pb atoms) and the presence of forbidden reflections, an alternative structure refinement was performed in space group P2₁. This structural modification is equivalent to mimetite-2M polymorph described by Yang et al. (2013). Despite the otherwise acceptable agreement criteria, the final refinement was characterized by high difference electron density peaks and an unusually high value for the weighting scheme parameter (Table 1). This can be explained by the pseudo-symmetry of the structure, i.e. the pseudo-centric character as indicated by the refined absolute structure parameter. Baikie et al. (2014) also noticed similar issues in the structure refinement of mimetite at low temperatures. Selected bond distances of mimetite-2M are reported in Table S2. Although small variations in the Pb—O bond distances, the coordination environment of Pb does not change with respect to that of mimetite-M.

Figure 2 Reciprocal lattice view of mimetite at (a) 123, (b) 173, (c) 393 and (d) 353 K. The distribution histograms of the reflections in the hexagonal unit cell are reported at each temperature.

At 173 K most of the satellite reflections were evident only along one axis of the corresponding hexagonal-type cell, indicating a gradual change from the 2M to M polymorph [Fig. 2(b)]. Similarly to the data set collected at 288 K, the monoclinic unit-cell a = 10.2378 (3), b = 7.4457 (2), c = 17.7096 (5) Å, β = 89.990 (3)° was refined and subsequently transformed to a = 10.2378 (3), b = 20.4573 (7), c = 7.4457 (2) Å, β = 120.039 (5)°. The structural refinement was performed in space group P112₁/b (Table S1). At 273 K, the analysis of the reflections clearly pointed to a monoclinic supercell, with doubling of one hexagonal axis, similar to that found at 173 K and at 288 K. At this temperature, the monoclinic space group P112₁/b and the structure of mimetite-M was maintained (Table S1).

After increasing the temperature to 393 K, the structure transformed to the hexagonal polymorph-H, with apatite-structure type (Table 1). Differently from the data collected at low temperature, no additional reflections, in disagreement with the hexagonal primitive unit cell, were detected in the diffraction pattern [Fig. 2(c)]. It is worth noting that, also in this case the high I/σ(I) of the collected data ensured the detection of eventual low-intensities reflections belonging to the monoclinic polymorph. When the temperature diminished to 353 K, the satellite reflections became again visible [Fig. 2(d)] and mimetite transforms to the monoclinic structure equivalent to that observed at 173 and 273 K (Table S1).

3.2. The role of temperature

Performed analysis indicated that in stoichiometric mimetite, the phase transition from the monoclinic to the hexagonal polymorph is temperature driven. This transition becomes evident with the appearance of satellite reflections, which cannot be indexed by the aristotypic hexagonal unit cell of apatite. The structural changes include two transformations: (i) from mimetite-2M (space group P2₁) to mimetite-M (space group P112₁/b) between 123 and 173 K; and (ii) from mimetite-M to mimetite-H (space group P6₃/m) between 353 and 393 K. No significant differences were noticed between the mimetite-M polymorphs collected at different temperatures, i.e. at 173, 273, 288 and 353 K, as indicated by a unit-cell volume variation smaller than 1%.

In literature, the occurrence of the monoclinic polymorph (both M and 2M) at room temperature was rarely reported. However, structural refinements of mimetite-H at ambient temperature were often associated with high residuals peaks in the difference Fourier maps, large ADPs, and presence of unindexed reflections (Calos ey al., 1990; Flis et al., 2010; Baikie et al., 2014). For instance, in their study on lead-apatite structure types, Baikie et al. (2014) obtained an unsatisfactory structural refinement in P6₃/m for a mimetite sample at ambient temperature and brought evidence of a superior fitting performed in the monoclinic space group P2₁/a. Based on these observations, it could be suggested that mimetite, at room temperature, always occurs as monoclinic, and the presence of the satellite reflections, due to their lower intensities, was easily overseen. Indeed, data reduction in the hexagonal system (especially if performed rejecting the outlier reflections) and subsequent structural refinement in space group P6₃/m may lead to apparently satisfactory results.

Baikie et al. (2014) further demonstrated the effect of the temperature on the monoclinic distortion. The authors reported that the magnitude of the residual peaks in difference Fourier maps and poor refinement indices increased at 100 K with respect the structure measured at ambient temperature.

On the other hand, the influence of the chemical composition must be taken into account as well. The re-analysis of the diffraction data reported by Flis et al. (2010) (Baikie et al., 2014) demonstrated that the supercell reflections disappear with increasing values of x in the Pb₁₀(As_1–xP_xO₄)₆Cl₂ solid solution. The effect of the chemical composition is also seen, to a certain extent, in the structural analysis reported by Dai et al. (1991). The authors investigated samples of mimetite from two different localities. The data were collected at ambient temperature by using a comparable exposure time. One sample, with chemical composition (Pb_9.99)(As_5.74Si_0.07S_0.06P_0.14)O₂₄Cl₂, was found to show the typical supercell reflections of mimetite-M polymorph with unit-cell parameters a = 10.189 (3), b = 20.372 (8), c = 7.46 (1) Å, γ = 119.88 (3)°. The second sample, identified as hexagonal mimetite-H, had chemical composition (Pb_9.75Ca_0.32)(As_5.71Si_0.13S_0.13P_0.01)O₂₄Cl₂. Thus, small substitutions at Pb sites may also induce the phase transition. Alternatively, it may cause the shift of the transition temperatures toward lower values. The sample used in this study did not contain significant amount of Ca and P impurities, in agreement with the above observations.

3.3. The role of the Pb²⁺ 6s² lone pair electrons

The distribution of 6s² electrons of lead atoms in mimetite was investigated by means of the electron localization function calculated from the cell- and geometry-optimized structures of mimetite-M, mimetite-2M and mimetite-H. The unit-cell parameters of the optimized structures, together with the deviation from the experimental XRD data, are reported in Table 4.

Table 4
Unit-cell parameters of the DFT-optimized structures of mimetite-2M, -M and -H polymorphs

The deviation from the experimental values (single-crystal X-ray diffraction) is reported.

	GEO_OPT	XRD	Deviation (%)
Mimetite-2M
a (Å)	20.764	20.4487 (9)	1.5
b (Å)	7.488	7.4362 (2)	0.7
c (Å)	20.812	20.4513 (9)	1.8
α (°)	90.0	90	0.0
β (°)	119.975	119.953 (6)	0.02
γ (°)	90.0	90	0.0
V (Å^3)	2802.86	2694.5 (2)	4.0
Mimetite-M
a (Å)	10.419	10.2552 (3)	1.6
b (Å)	20.829	20.4913 (6)	1.6
c (Å)	7.536	7.4576 (2)	1.0
α (°)	90.0	90	0.0
β (°)	90.0	90	0.0
γ (°)	119.74	119.993 (2)	0.2
V (Å^3)	1420.08	1357.29 (7)	4.6
Mimetite-H
a (Å)	10.388	10.2722 (3)	1.1
b (Å)	10.388	10.2722 (3)	1.1
c (Å)	7.4434	7.4537 (3)	0.1
α (°)	90.0	90	0.0
β (°)	90.0	90	0.0
γ (°)	120.02	120.0	0.0
V (Å^3)	695.50	681.14	2.1

Fig. 3 shows the isosurfaces of the ELF in the three polymorphs. Similar to the data reported by Peet et al. (2017), our calculations indicated that, in mimetite-H, the lone-pair electrons of Pb2 sites [Fig. 3(a)] are more localized than those at Pb1. The localization of the electron pairs at Pb2 remains overall unaltered among the different polymorphs, suggesting that the temperature has no influence on the Pb2 lone pairs. In contrast, differences in the ELF close to Pb1 sites were observed among mimetite-M, -2M and -H.

Figure 3 Fragment of the DFT-optimized structures of mimetite-2M, -M and -H (projection along the [110]hex, chex-axis vertical). ELF isosurfaces are reported in yellow and light blue for ELF = 0.96 and ELF = 0.90, respectively. As tetrahedra are shown in light green, Cl atoms in green. Dark-grey and purple spheres represent Pb atoms residing at Pb2 and Pb1 crystallographic sites, respectively.

In mimetite-H, the 6s² electrons of Pb1 site are more delocalized with respect to those in mimetite-M and -2M [Figs. 3(b) and 3(c)]. A general gradual localization of the lone pair electrons at Pb1 is observed from the higher (i.e. mimetite-H) to the lower (i.e. mimetite-2M) symmetry phase. Mimetite-M is characterized by an increased localization of 6s² at each Pb1 site with respect mimetite-H [Fig. 3(b)]. In mimetite-2M [Fig. 3(c)], 6s² electron pairs further localize at Pb1 sites corresponding to Pb11, Pb14, P15 and Pb17 sites of the refined structure (cif provided in supporting information). Thus, the increased localization does not affect equally all Pb1 sites and this might explain the monoclinic distortion at low temperatures.

This observation was further confirmed by the analysis of the WFCs computed from MD trajectories at different temperatures. To get an insight on the dynamic of the lone-pair electrons, the relative positions of the Wannier centres, representing 6s² states with respect to corresponding Pb core position, have been sampled from MD trajectory with a 100 fs interval for each data set (i.e. 123, 273, 293, 393 K). The analysis was focused on the Pb atoms residing at Pb1 crystallographic sites that are suggested to have distinct localization in different polymorphs according to ELF. The x versus z coordinates (in the simulated cell the a,b axes of the hexagonal cell correspond to a,c directions) of the extracted WFCs, at different time steps, for the selected Pb atoms were plotted to visualize the distribution of the lone-pair electrons in the (010) plane. In this way, we can observe the relative distribution of the WFCs centres with respect to reference Pb core and their spread. As an example, in Fig. 4 the density plot, for representative Pb1 atoms, is reported for the simulated structures at 123, 273, 293 and 393 K. In agreement with the prediction of ELF for the optimized structures, the electron pairs show a spherical and broader distribution around the Pb at higher temperatures. In contrast, the plot of the data set calculated at 123 K shows that the centre of WFCs density distribution is clearly displaced off from the location of Pb core.

Figure 4 Density plots of the WFCs for selected Pb atoms corresponding to six equivalent Pb1 sites in the supercell of the MD trajectories calculated at 123, 273, 293 and 393 K. The plots show the density distribution (x versus z coordinates) of the WFCs extracted from MD trajectories in steps of 100 fs. The WFCs coordinates are expressed as a difference with respect the reference Pb coordinates.

Dai et al. (1991) already suggested, based on the geometric parameters, that `a redistribution of the lone-pair electrons associated with Pb1' occurred as a result of the phase transformation from the hexagonal to the monoclinic structure. In particular, the authors stated that the lone-pair electrons of Pb²⁺ located at Pb1 sites (Pb1A and Pb1B symmetry-independent in the monoclinic structure) shifted toward O3A (for Pb1A) and O3F (for Pb1B) in mimetite-M. Our analysis partially agreed with this description. The isosurfaces of the ELF at Pb1B showed that the 6s² electrons are mostly shifted toward O2B instead of O3F [Fig. 5(a)], whereas those of Pb1A are mostly localized between O3A and O2A [Fig. 5(b)].

Figure 5 Detail of the DFT-optimized structure of mimetite-M showing the position of the ELF isosurfaces for Pb1B (a) and Pb1A sites (b). Colour code as in Fig. 3.

The phase transitions in mimetite can be related to the change of the stereochemical activity of the lone pair electrons of the Pb1 site. The same phenomenon was observed in other Pb-containing crystalline compounds. The perovskite-like structure of Pb₂MgWO₆ undergoes an antiferroelectric phase transition below 310 K from cubic to orthorhombic. Such transition is accompanied by a relocation of the lone pairs of lead atoms, `which are smeared out by the near –octahedral symmetry of the lead sites in the high-temperature phase whereas in the low temperature phase they are localized into the traditional lobes' (Seshadri et al., 1999). The authors associated the phase transition with a tendency of the lone pair electrons to localize close to the average position of Pb core. Similarly, the transitions and related structural changes in BiFeO₃ and PbTiO₃ are mainly provoked by the stereochemical activity of the lone-pair two valence s-electrons of Bi³⁺ and Pb²⁺ (Volkova & Marinin, 2011a,b). The same authors demonstrated that the increase in temperature (or pressure) diminishes the stereochemical activity of the lone-pair electrons, resulting in a decreased distortion of the cations coordination surroundings (Volkova & Udovenko, 1988; Volkova & Marinin, 2011a,b).

If the localization of the semi-local states of Pb controls the phase transition, this would also explain the absence of the supercell reflections in Ca-rich mimetite samples.

4. Conclusions

The in situ measurements brought evidence that the transformation in the sample of stoichiometric mimetite from monoclinic to hexagonal and vice versa are definitively temperature dependent. The polymorph mimetite-2M is observed only at low temperatures (below 173 K). From 173 to 353 K mimetite transforms to mimetite-M, and only at temperatures above 373 K the supercell reflections disappeared leading to the hexagonal structure, mimetite-H. Based on our results, we speculate that the majority of mimetite samples are monoclinic at ambient temperature. The presence of the additional reflections of the monoclinic supercell can be easily overlooked without a careful inspection of the reciprocal lattice.

The observed structural changes are related to the stereochemical activity of the lone pair electrons of the Pb at Pb1 site. The computed ELF for the three polymorphs unambiguously showed that the 6s² lone pair progressively localizes close to the Pb core as the temperature decreases, influencing the distortion of the coordination geometry of the Pb atoms. As previously reported for other other compounds showing similar stereochemical activity of lone pair, the charge localization acts as a stabilizing factor at lower temperatures.

These results clarify the role of temperature on the crystal symmetry of natural mimetite. Concerning the effect of the chemical compositions (presence of Ca and P impurities), we can draw some conclusions based on data published in literature. It was shown that the higher the deviation from a chemically pure mimetite composition, the less evident are the supercell reflections indicative for the monoclinic space group. Hence, we can hypothesize that the transition from the hexagonal to the monoclinic phases is progressively shifted toward lower temperatures with increasing P and Ca content in mimetite crystals.

Supporting information

Computing details

Data collection: CrysAlis PRO 1.171.41.104a (Rigaku Oxford Diffraction, 2021) for Mim123K, Mim353K; CrysAlis PRO 1.171.41.104a for Mim173K, Mim273K, Mim288K, Mim393K. Cell refinement: CrysAlis PRO 1.171.41.104a (Rigaku Oxford Diffraction, 2021) for Mim123K, Mim353K; CrysAlis PRO 1.171.41.104a for Mim173K, Mim273K, Mim288K, Mim393K. Data reduction: CrysAlis PRO 1.171.41.104a (Rigaku Oxford Diffraction, 2021) for Mim123K, Mim353K; CrysAlis PRO 1.171.41.104a for Mim173K, Mim273K, Mim288K, Mim393K. Program(s) used to solve structure: SHELXS2013 (Scheldrick, 2008) for Mim173K, Mim273K, Mim288K, Mim393K. For all structures, program(s) used to refine structure: SHELXL2014 (Sheldrick, 2014).

(Mim123K)

Crystal data

As4Cl1.33O16Pb6.67	F(000) = 4976
Mr = 1984.21	Dx = 7.337 Mg m^−3
Monoclinic, P21	Ag Kα radiation, λ = 0.56087 Å
a = 20.4487 (9) Å	Cell parameters from 23365 reflections
b = 7.4362 (2) Å	θ = 2.8–29.4°
c = 20.4513 (9) Å	µ = 37.49 mm^−1
β = 119.953 (6)°	T = 123 K
V = 2694.5 (2) Å^3	Fragment, pale orange
Z = 6	0.10 × 0.06 × 0.04 mm

Data collection

XtalLAB, Synergy, Dualflex, Hypix diffractometer	15378 reflections with I > 2σ(I)
Radiation source: micro-focus sealed X-ray tube	Rint = 0.056
o scan	θmax = 25.6°, θmin = 1.8°
Absorption correction: multi-scan	h = −31→31
Tmin = 0.304, Tmax = 1.000	k = −10→11
50947 measured reflections	l = −31→31
19430 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: Difmap
R[F^2 > 2σ(F^2)] = 0.055	w = 1/[σ^2(Fo^2) + 226.143P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.129	(Δ/σ)max < 0.001
S = 1.08	Δρmax = 6.42 e Å^−3
19430 reflections	Δρmin = −11.99 e Å^−3
387 parameters	Absolute structure: Refined as an inversion twin.
1 restraint	Absolute structure parameter: 0.51 (5)

Special details

Experimental. CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 2-component inversion twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb11	0.67158 (7)	0.67246 (18)	0.34060 (7)	0.00643 (6)
Pb12	0.65922 (7)	0.67465 (18)	0.83093 (7)	0.00643 (6)
Pb13	0.66211 (7)	0.18562 (18)	0.32800 (7)	0.00643 (6)
Pb14	0.67393 (7)	0.18808 (18)	0.83747 (7)	0.00643 (6)
Pb15	0.16622 (7)	0.19052 (18)	0.82798 (7)	0.00643 (6)
Pb16	0.83427 (7)	0.6856 (2)	0.66017 (7)	0.00643 (6)
Pb17	0.83212 (7)	0.17129 (19)	0.67397 (7)	0.00643 (6)
Pb18	0.16661 (7)	0.67599 (19)	0.83806 (7)	0.00643 (6)
Pb21	0.00278 (9)	0.9229 (2)	0.87644 (9)	0.0137 (3)
Pb22	0.62372 (8)	0.94856 (19)	0.62674 (8)	0.0045 (2)
Pb23	0.87531 (7)	0.92029 (19)	−0.00039 (8)	0.0051 (2)
Pb24	0.37581 (8)	0.4192 (2)	0.87265 (8)	0.0079 (3)
Pb25	−0.00268 (7)	0.41789 (17)	0.62334 (7)	0.00270 (19)*
Pb26	0.87589 (9)	0.9330 (2)	0.49943 (9)	0.0145 (3)
Pb27	0.87685 (8)	0.4587 (2)	0.87806 (8)	0.0056 (2)
Pb28	0.62367 (8)	0.45183 (17)	0.50066 (8)	0.0044 (2)
Pb29	0.49970 (8)	0.4576 (2)	0.62329 (8)	0.0059 (2)*
P210	0.62524 (8)	0.4179 (2)	0.00207 (8)	0.0081 (2)
P211	0.50022 (8)	0.4205 (2)	0.12313 (8)	0.0084 (2)
P212	0.87712 (8)	0.3999 (2)	0.37818 (8)	0.0087 (3)
As1	0.4879 (2)	0.4280 (6)	0.2944 (2)	0.0048 (3)
As11	0.4860 (2)	0.4292 (6)	0.7945 (2)	0.0048 (3)
As2	0.7059 (2)	0.4383 (6)	0.1954 (2)	0.0045 (5)
As21	0.2027 (2)	0.4312 (6)	0.6906 (2)	0.0045 (5)
As3	0.7057 (2)	0.4225 (6)	0.6954 (2)	0.0058 (6)
As31	0.7958 (2)	0.9329 (6)	0.8091 (2)	0.0045 (6)
As4	0.8062 (2)	0.4314 (6)	1.0121 (2)	0.0051 (5)
As41	0.6929 (2)	0.9320 (6)	−0.0112 (2)	0.0051 (5)
As5	0.8073 (2)	0.4318 (6)	0.5137 (2)	0.0046 (4)
As51	0.6925 (2)	0.9245 (6)	0.4895 (2)	0.0046 (4)
As6	1.0096 (2)	0.9389 (5)	0.7031 (2)	0.0038 (6)
As61	−0.0105 (2)	0.4240 (6)	0.7979 (2)	0.0051 (6)
Cl1	0.9919 (4)	0.6691 (12)	0.4902 (4)	0.0066 (12)*
Cl2	0.5013 (5)	0.6958 (13)	0.4944 (5)	0.0119 (14)*
Cl3	0.5008 (4)	0.6711 (10)	0.9981 (4)	0.0025 (10)*
Cl4	0.0087 (5)	0.6782 (13)	0.0099 (4)	0.0091 (13)*
O11	0.0828 (15)	0.431 (4)	0.8397 (15)	0.0066 (8)
O12	0.1571 (14)	0.423 (3)	0.7435 (15)	0.0066 (8)
O13	0.7423 (14)	0.930 (3)	0.0830 (16)	0.0066 (8)
O14	0.9138 (15)	0.936 (3)	0.6655 (15)	0.0066 (8)
O15	0.8360 (14)	0.923 (3)	0.7554 (15)	0.0066 (8)
O16	0.7499 (14)	0.935 (3)	0.5848 (16)	0.0066 (8)
O17	0.7578 (14)	0.428 (3)	0.4183 (15)	0.0066 (8)
O18	0.6658 (15)	0.427 (3)	0.2516 (15)	0.0066 (8)
O19	0.5869 (14)	0.438 (3)	0.3411 (14)	0.0066 (8)
O110	0.7483 (14)	0.435 (3)	0.9173 (15)	0.0066 (8)
O111	0.6648 (15)	0.426 (4)	0.7468 (15)	0.0066 (8)
O112	0.5784 (14)	0.429 (4)	0.8338 (14)	0.0066 (8)
O21	0.8037 (14)	0.415 (3)	0.2461 (13)	0.0083 (9)
O22	0.7533 (14)	0.453 (3)	1.0588 (15)	0.0083 (9)
O23	1.0512 (14)	0.882 (3)	0.7957 (15)	0.0083 (9)
O24	−0.0548 (14)	0.468 (4)	0.7045 (15)	0.0083 (9)
O25	0.7573 (14)	0.394 (3)	0.5543 (14)	0.0083 (9)
O26	0.7978 (13)	0.478 (3)	0.7465 (13)	0.0083 (9)
O27	0.2942 (14)	0.484 (4)	0.7442 (13)	0.0083 (9)
O28	0.7469 (12)	0.980 (3)	0.4464 (13)	0.0083 (9)
O29	0.4427 (15)	0.399 (4)	0.7002 (16)	0.0083 (9)
O210	0.4466 (15)	0.450 (3)	0.1995 (16)	0.0083 (9)
O211	0.7424 (14)	0.922 (3)	−0.0530 (14)	0.0083 (9)
O212	0.7008 (14)	0.890 (4)	0.7581 (13)	0.0083 (9)
O31	0.6221 (16)	1.087 (4)	0.4554 (17)	0.0115 (7)*
O32	0.6517 (15)	0.726 (4)	0.4562 (15)	0.0115 (7)*
O33	0.8481 (14)	0.638 (4)	0.5449 (15)	0.0115 (7)*
O34	0.6644 (16)	0.570 (4)	0.6226 (15)	0.0115 (7)*
O35	0.6997 (15)	0.216 (4)	0.6601 (15)	0.0115 (7)*
O36	0.8390 (14)	0.777 (3)	0.8785 (14)	0.0115 (7)*
O37	−0.0429 (15)	0.214 (4)	0.8069 (15)	0.0115 (7)*
O38	0.4511 (15)	0.586 (4)	0.3254 (15)	0.0115 (7)*
O39	−0.0409 (16)	0.579 (4)	0.8375 (16)	0.0115 (7)*
O310	1.0407 (15)	1.141 (4)	0.6957 (15)	0.0115 (7)*
O311	1.0371 (15)	0.791 (4)	0.6583 (15)	0.0115 (7)*
O312	0.8046 (14)	1.134 (3)	0.8515 (13)	0.0115 (7)*
O313	0.4542 (15)	0.268 (4)	0.8302 (15)	0.0115 (7)*
O314	0.8762 (15)	0.282 (3)	0.5419 (15)	0.0115 (7)*
O315	0.8712 (15)	0.603 (3)	1.0450 (15)	0.0115 (7)*
O316	0.4580 (14)	0.219 (3)	0.3036 (14)	0.0115 (7)*
O317	0.4547 (14)	0.616 (3)	0.8130 (14)	0.0115 (7)*
O318	0.6249 (16)	0.788 (4)	−0.0432 (16)	0.0115 (7)*
O319	0.6696 (15)	0.281 (4)	0.1269 (15)	0.0115 (7)*
O320	0.1887 (14)	0.249 (3)	0.6372 (13)	0.0115 (7)*
O321	0.1715 (14)	0.601 (4)	0.6271 (14)	0.0115 (7)*
O322	0.6545 (15)	1.146 (4)	−0.0390 (15)	0.0115 (7)*
O323	0.6952 (15)	0.640 (4)	0.1561 (15)	0.0115 (7)*
O324	0.8570 (14)	0.243 (3)	1.0470 (15)	0.0115 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb11	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb12	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb13	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb14	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb15	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb16	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb17	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb18	0.00727 (11)	0.00460 (11)	0.00703 (10)	0.00011 (10)	0.00327 (9)	0.00000 (10)
Pb21	0.0115 (5)	0.0218 (7)	0.0087 (5)	0.0017 (4)	0.0057 (4)	−0.0012 (4)
Pb22	0.0059 (5)	0.0018 (5)	0.0051 (5)	−0.0013 (4)	0.0021 (5)	−0.0019 (4)
Pb23	0.0049 (5)	0.0024 (4)	0.0080 (5)	−0.0014 (4)	0.0034 (5)	−0.0021 (4)
Pb24	0.0054 (5)	0.0110 (7)	0.0062 (5)	0.0002 (5)	0.0021 (5)	0.0005 (4)
Pb26	0.0061 (6)	0.0289 (10)	0.0084 (6)	0.0011 (6)	0.0037 (5)	0.0036 (6)
Pb27	0.0051 (5)	0.0042 (5)	0.0054 (5)	0.0011 (4)	0.0011 (5)	0.0013 (4)
Pb28	0.0065 (5)	0.0012 (5)	0.0061 (5)	−0.0003 (4)	0.0036 (5)	0.0000 (4)
P210	0.0042 (5)	0.0123 (6)	0.0070 (5)	0.0016 (5)	0.0021 (5)	0.0010 (5)
P211	0.0070 (5)	0.0116 (5)	0.0051 (4)	0.0001 (3)	0.0019 (4)	0.0012 (3)
P212	0.0055 (5)	0.0144 (6)	0.0057 (5)	−0.0002 (5)	0.0025 (5)	−0.0006 (5)
As1	0.0041 (6)	0.0047 (7)	0.0051 (6)	−0.0003 (12)	0.0019 (5)	0.0010 (12)
As11	0.0041 (6)	0.0047 (7)	0.0051 (6)	−0.0003 (12)	0.0019 (5)	0.0010 (12)
As2	0.0023 (10)	0.0056 (10)	0.0048 (12)	0.0005 (12)	0.0011 (10)	0.0000 (11)
As21	0.0023 (10)	0.0056 (10)	0.0048 (12)	0.0005 (12)	0.0011 (10)	0.0000 (11)
As3	0.0079 (14)	0.0050 (13)	0.0025 (14)	−0.0011 (14)	0.0012 (13)	−0.0020 (13)
As31	0.0067 (14)	0.0044 (14)	0.0035 (14)	−0.0006 (13)	0.0034 (13)	−0.0006 (12)
As4	0.0034 (10)	0.0063 (12)	0.0045 (8)	0.0003 (5)	0.0011 (9)	−0.0018 (5)
As41	0.0034 (10)	0.0063 (12)	0.0045 (8)	0.0003 (5)	0.0011 (9)	−0.0018 (5)
As5	0.0043 (10)	0.0042 (11)	0.0041 (8)	−0.0005 (5)	0.0012 (9)	−0.0004 (5)
As51	0.0043 (10)	0.0042 (11)	0.0041 (8)	−0.0005 (5)	0.0012 (9)	−0.0004 (5)
As6	0.0018 (14)	0.0032 (16)	0.0075 (14)	0.0011 (12)	0.0031 (13)	0.0007 (13)
As61	0.0059 (15)	0.0055 (16)	0.0031 (13)	−0.0020 (14)	0.0016 (13)	−0.0017 (13)
O11	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O12	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O13	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O14	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O15	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O16	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O17	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O18	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O19	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O110	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O111	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O112	0.004 (2)	0.0077 (19)	0.0080 (19)	0.0001 (18)	0.0032 (17)	0.0019 (19)
O21	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O22	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O23	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O24	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O25	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O26	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O27	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O28	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O29	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O210	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O211	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)
O212	0.007 (2)	0.012 (3)	0.0078 (18)	−0.001 (2)	0.0052 (17)	0.000 (2)

Geometric parameters (Å, º)

Pb11—O19	2.46 (2)	As21—O12	1.75 (2)
Pb11—O17	2.48 (3)	As21—Pb26^iii	3.384 (4)
Pb11—O18	2.54 (3)	As21—Pb11^iii	3.515 (4)
Pb11—O32	2.62 (2)	As21—Pb13^i	3.524 (4)
Pb11—O29^i	2.66 (2)	As21—P212^i	3.808 (5)
Pb11—O320^i	2.72 (2)	As3—O111	1.64 (2)
Pb11—O28	3.00 (2)	As3—O35	1.68 (3)
Pb11—O27^i	3.17 (2)	As3—O26	1.69 (2)
Pb11—O313^i	3.22 (3)	As3—O34	1.70 (3)
Pb12—O112	2.48 (3)	As3—Pb22^iv	3.854 (5)
Pb12—O110	2.53 (3)	As31—O15	1.67 (2)
Pb12—O111	2.57 (3)	As31—O312	1.69 (3)
Pb12—O212	2.60 (2)	As31—O36	1.70 (3)
Pb12—O316^i	2.62 (3)	As31—O212	1.71 (3)
Pb12—O211^ii	2.81 (2)	As31—Pb23^ii	3.392 (4)
Pb12—O210^i	2.82 (2)	As31—Pb14^xi	3.405 (4)
Pb12—O318^ii	3.10 (3)	As31—Pb17^xi	3.657 (4)
Pb12—As1^i	3.386 (4)	As31—Pb21^viii	3.741 (4)
Pb13—O18	2.40 (2)	As4—O324	1.68 (3)
Pb13—O19	2.52 (3)	As4—O110	1.69 (3)
Pb13—O27^iii	2.56 (2)	As4—O315	1.72 (3)
Pb13—O17	2.62 (3)	As4—O22	1.77 (2)
Pb13—O28^iv	2.65 (2)	As4—Pb21^vii	3.401 (4)
Pb13—O317^iii	2.72 (3)	As4—Pb18^vii	3.408 (4)
Pb13—O29^iii	2.87 (3)	As4—Pb15^x	3.590 (4)
Pb13—O321^iii	3.11 (2)	As4—P210^ii	3.604 (4)
Pb13—O31^iv	3.18 (3)	As4—Pb23^ii	3.954 (5)
Pb14—O110	2.42 (3)	As41—O318	1.61 (3)
Pb14—O111	2.50 (3)	As41—O211	1.62 (2)
Pb14—O312^iv	2.57 (2)	As41—O13	1.67 (3)
Pb14—O112	2.62 (2)	As41—O322	1.74 (3)
Pb14—O322^v	2.76 (2)	As41—P211^xv	3.437 (4)
Pb14—O211^v	2.79 (2)	As41—Pb14^xiv	3.487 (4)
Pb14—O210^iii	2.81 (2)	As41—Pb12^xiii	3.514 (4)
Pb14—O212^iv	2.96 (2)	As41—Pb18^i	3.731 (4)
Pb14—O38^iii	3.12 (3)	As41—Pb24^i	3.740 (4)
Pb15—O12	2.38 (2)	As41—Pb15^i	3.845 (4)
Pb15—O11	2.56 (2)	As41—P210^xi	3.926 (5)
Pb15—O13^iii	2.57 (3)	As5—O25	1.63 (2)
Pb15—O310^vi	2.67 (3)	As5—O314	1.66 (3)
Pb15—O323^iii	2.71 (3)	As5—O17	1.69 (3)
Pb15—O22^vii	2.72 (3)	As5—O33	1.71 (3)
Pb15—O21^iii	2.79 (2)	As5—Pb25^viii	3.382 (4)
Pb15—O23^vi	3.11 (2)	As5—Pb26^iv	4.027 (4)
Pb15—O315^vii	3.12 (2)	As51—O32	1.66 (3)
Pb16—O14	2.44 (3)	As51—O16	1.70 (3)
Pb16—O16	2.47 (3)	As51—O31	1.74 (3)
Pb16—O33	2.53 (2)	As51—O28	1.78 (2)
Pb16—O24^viii	2.56 (3)	As51—Pb29^i	3.432 (4)
Pb16—O15	2.62 (3)	As51—Pb13^xi	3.608 (4)
Pb16—O26	2.71 (2)	As51—Pb17^xi	3.872 (4)
Pb16—O25	2.91 (3)	As6—O310	1.67 (3)
Pb16—O34	3.28 (3)	As6—O311	1.70 (3)
Pb16—O39^viii	3.33 (3)	As6—O23	1.70 (3)
Pb17—O15^iv	2.46 (2)	As6—O14	1.71 (3)
Pb17—O14^iv	2.48 (2)	As6—P212^xvi	3.472 (3)
Pb17—O16^iv	2.49 (3)	As6—Pb15^xx	3.480 (4)
Pb17—O35	2.60 (2)	As6—Pb18^viii	3.591 (4)
Pb17—O37^viii	2.66 (3)	As6—Pb21^viii	3.618 (4)
Pb17—O25	2.71 (3)	As6—Pb17^xi	3.789 (4)
Pb17—O26	2.99 (2)	As6—Pb25^xx	3.873 (4)
Pb17—O24^viii	3.03 (3)	As61—O11	1.66 (3)
Pb17—O314	3.35 (2)	As61—O24	1.69 (3)
Pb18—O11	2.51 (3)	As61—O39	1.69 (3)
Pb18—O13^iii	2.53 (3)	As61—O37	1.74 (3)
Pb18—O23^ix	2.57 (3)	As61—Pb27^ix	3.440 (4)
Pb18—O12	2.63 (3)	As61—Pb17^ix	3.488 (4)
Pb18—O324^x	2.67 (2)	As61—Pb16^ix	3.587 (5)
Pb18—O21^i	2.75 (2)	As61—Pb23^iii	3.655 (4)
Pb18—O22^x	2.82 (3)	Cl1—Pb25^i	3.062 (8)
Pb18—O319^i	3.15 (3)	Cl1—Pb26^xix	3.141 (8)
Pb18—O311^ix	3.40 (3)	Cl1—P212^xvi	3.189 (8)
Pb21—O23^ix	2.33 (2)	Cl1—Pb25^viii	3.258 (8)
Pb21—O37^xi	2.50 (3)	Cl2—Pb29^i	3.087 (8)
Pb21—O315^x	2.63 (3)	Cl2—Pb22^iii	3.120 (9)
Pb21—O39	2.70 (3)	Cl2—Pb28^i	3.229 (9)
Pb21—O324^x	2.82 (2)	Cl3—P211^i	3.088 (7)
Pb21—O15^ix	3.05 (3)	Cl3—P210^ii	3.134 (7)
Pb21—Cl4^xii	3.100 (8)	Cl3—P210^i	3.162 (7)
Pb21—Cl4^ii	3.232 (8)	Cl3—P211^ii	3.169 (7)
Pb21—As4^x	3.401 (4)	Cl3—Pb24^x	3.177 (7)
Pb22—O212	2.38 (2)	Cl4—Pb21^xxi	3.100 (8)
Pb22—O35^xi	2.40 (3)	Cl4—Pb27^i	3.118 (9)
Pb22—O38^i	2.42 (3)	Cl4—Pb23^xviii	3.130 (8)
Pb22—O34	2.95 (3)	Cl4—Pb27^xxii	3.154 (9)
Pb22—O16	3.10 (2)	Cl4—Pb23^ix	3.187 (9)
Pb22—Cl2^i	3.120 (9)	Cl4—Pb21^xiii	3.232 (8)
Pb22—O316^i	3.18 (2)	O11—Pb23^iii	2.95 (3)
Pb22—Cl2	3.218 (9)	O11—Pb21^iv	4.33 (3)
Pb22—As1^i	3.392 (4)	O12—P212^i	4.19 (3)
Pb23—O211	2.37 (2)	O13—Pb18^i	2.53 (3)
Pb23—O36^xiii	2.45 (2)	O13—Pb15^i	2.57 (3)
Pb23—O315^xiii	2.55 (3)	O13—Pb24^i	2.97 (2)
Pb23—O324^xiv	2.68 (3)	O13—P210^xi	4.20 (3)
Pb23—O11^i	2.95 (3)	O14—Pb17^xi	2.48 (2)
Pb23—O312^xiii	3.07 (2)	O14—Pb21^viii	3.75 (3)
Pb23—Cl4^xv	3.130 (9)	O14—Pb25^xx	4.24 (3)
Pb23—Cl4^viii	3.187 (9)	O15—Pb17^xi	2.46 (2)
Pb23—As31^xiii	3.392 (4)	O15—Pb21^viii	3.05 (3)
Pb24—O27	2.35 (2)	O16—Pb17^xi	2.49 (3)
Pb24—O323^iii	2.43 (3)	O17—Pb26^iv	4.26 (3)
Pb24—O313	2.44 (3)	O18—Pb24^i	4.29 (2)
Pb24—O319^i	2.85 (3)	O19—Pb29^iii	4.21 (2)
Pb24—O317	2.86 (2)	O110—P210^ii	3.70 (2)
Pb24—O13^iii	2.97 (2)	O110—Pb23^ii	4.27 (3)
Pb24—Cl3	3.175 (8)	O111—Pb22^iv	4.16 (3)
Pb24—Cl3^vii	3.177 (7)	O112—P210^ii	3.08 (3)
Pb24—As11	3.352 (4)	O112—P211^i	4.26 (3)
Pb25—O24	2.41 (2)	O21—Pb18^iii	2.75 (2)
Pb25—O314^ix	2.41 (3)	O21—Pb15^i	2.79 (2)
Pb25—O310^vi	2.43 (3)	O22—P210^ii	2.29 (3)
Pb25—O311^ix	2.88 (3)	O22—Pb15^x	2.72 (3)
Pb25—O12	2.95 (3)	O22—Pb18^vii	2.82 (2)
Pb25—Cl1^iii	3.062 (8)	O23—Pb21^viii	2.33 (2)
Pb25—O33^ix	3.11 (2)	O23—Pb18^viii	2.57 (3)
Pb25—Cl1^ix	3.258 (8)	O23—Pb15^xx	3.11 (2)
Pb25—As5^ix	3.382 (4)	O24—Pb16^ix	2.56 (3)
Pb26—O28	2.32 (2)	O24—Pb17^ix	3.03 (2)
Pb26—O33	2.55 (3)	O27—Pb13^i	2.56 (2)
Pb26—O321^i	2.59 (2)	O27—Pb11^iii	3.17 (2)
Pb26—O314^xi	2.73 (3)	O28—Pb13^xi	2.65 (2)
Pb26—O320^i	2.78 (2)	O28—Pb17^xi	4.31 (2)
Pb26—O14	3.08 (3)	O29—Pb11^iii	2.66 (2)
Pb26—Cl1^xvi	3.141 (8)	O29—Pb13^i	2.87 (3)
Pb26—Cl1	3.156 (8)	O210—Pb14^i	2.81 (2)
Pb26—As21^i	3.384 (4)	O210—Pb12^iii	2.82 (2)
Pb27—O26	2.35 (2)	O211—Pb14^xiv	2.79 (2)
Pb27—O39^viii	2.39 (3)	O211—Pb12^xiii	2.81 (2)
Pb27—O36	2.49 (3)	O211—Pb18^i	4.27 (2)
Pb27—O312^iv	2.74 (3)	O212—Pb14^xi	2.96 (2)
Pb27—O110	3.11 (2)	O31—Pb29^i	2.39 (3)
Pb27—Cl4^iii	3.118 (9)	O31—Pb28^xi	2.86 (3)
Pb27—Cl4^xvii	3.154 (9)	O31—Pb13^xi	3.18 (3)
Pb27—O37^viii	3.24 (2)	O32—Pb29^i	3.19 (3)
Pb27—As61^viii	3.440 (4)	O33—Pb25^viii	3.11 (2)
Pb28—O34	2.37 (3)	O35—Pb22^iv	2.40 (3)
Pb28—O32	2.41 (3)	O36—Pb23^ii	2.45 (2)
Pb28—O25	2.42 (2)	O36—Pb21^viii	3.54 (2)
Pb28—O31^iv	2.86 (3)	O36—Pb14^xi	4.32 (3)
Pb28—O19	2.96 (2)	O37—Pb21^iv	2.50 (3)
Pb28—Cl2	3.040 (9)	O37—Pb17^ix	2.66 (3)
Pb28—Cl2^iii	3.229 (9)	O37—Pb27^ix	3.24 (2)
Pb28—O35	3.33 (3)	O37—Pb23^iii	4.03 (3)
Pb28—As3	3.471 (4)	O38—Pb22^iii	2.42 (3)
Pb29—O316^i	2.34 (3)	O38—Pb29^i	2.95 (3)
Pb29—O31^iii	2.39 (3)	O38—Pb14^i	3.12 (3)
Pb29—O29	2.42 (2)	O38—Pb12^iii	4.18 (3)
Pb29—O38^iii	2.95 (3)	O39—Pb27^ix	2.39 (3)
Pb29—O111	3.05 (3)	O39—Pb16^ix	3.33 (3)
Pb29—Cl2^iii	3.087 (8)	O39—Pb23^iii	3.56 (3)
Pb29—O32^iii	3.19 (3)	O39—Pb17^ix	4.29 (3)
Pb29—Cl2	3.190 (8)	O310—Pb25^xx	2.43 (3)
Pb29—As51^iii	3.432 (4)	O310—Pb15^xx	2.67 (3)
P210—O22^xiii	2.29 (3)	O310—P212^xvi	3.29 (2)
P210—O322^iv	2.38 (3)	O310—Pb17^xi	4.07 (2)
P210—O319	2.46 (3)	O311—P212^xvi	2.36 (2)
P210—O318	2.90 (3)	O311—Pb25^viii	2.88 (3)
P210—O112^xiii	3.08 (3)	O311—Pb18^viii	3.40 (3)
P210—Cl3^xiii	3.134 (7)	O311—Pb15^xx	4.32 (3)
P210—Cl3^iii	3.162 (7)	O312—Pb14^xi	2.57 (2)
P210—O323	3.19 (3)	O312—Pb27^xi	2.74 (3)
P210—As2	3.444 (4)	O312—Pb23^ii	3.07 (2)
P211—O210	2.32 (2)	O312—Pb17^xi	3.95 (2)
P211—O318^xviii	2.45 (3)	O312—Pb21^viii	4.13 (2)
P211—O317^iii	2.54 (2)	O313—P211^iii	2.75 (3)
P211—O313^i	2.75 (3)	O313—Pb11^iii	3.22 (3)
P211—O18	3.08 (3)	O313—P210^ii	3.68 (3)
P211—Cl3^iii	3.088 (7)	O313—Pb13^i	4.25 (3)
P211—Cl3^xiii	3.168 (7)	O314—Pb25^viii	2.41 (3)
P211—O322^xviii	3.22 (3)	O314—Pb26^iv	2.73 (3)
P211—As41^xviii	3.437 (4)	O315—Pb23^ii	2.55 (3)
P212—O21	2.35 (2)	O315—Pb21^vii	2.62 (3)
P212—O311^xix	2.36 (2)	O315—Pb15^x	3.12 (2)
P212—O321^iii	2.42 (3)	O315—Pb18^vii	4.27 (3)
P212—O320^i	2.87 (3)	O316—Pb29^iii	2.34 (2)
P212—O17	2.94 (2)	O316—Pb12^iii	2.62 (3)
P212—Cl1	3.065 (9)	O316—Pb22^iii	3.18 (2)
P212—Cl1^xix	3.189 (8)	O317—P211^i	2.54 (2)
P212—O310^xix	3.29 (2)	O317—Pb13^i	2.72 (2)
P212—O314	3.47 (2)	O317—P210^ii	3.98 (2)
As1—O38	1.68 (3)	O318—P211^xv	2.45 (3)
As1—O210	1.69 (3)	O318—Pb12^xiii	3.10 (3)
As1—O316	1.71 (2)	O318—Pb24^i	3.63 (3)
As1—O19	1.76 (2)	O318—Pb14^xiv	4.27 (3)
As1—Pb12^iii	3.386 (4)	O319—Pb24^iii	2.85 (3)
As1—Pb22^iii	3.392 (4)	O319—Pb18^iii	3.15 (3)
As1—Pb14^i	3.612 (4)	O319—Pb15^i	4.28 (3)
As1—Pb29^iii	3.835 (5)	O320—Pb11^iii	2.72 (2)
As11—O112	1.64 (2)	O320—Pb26^iii	2.78 (2)
As11—O317	1.65 (2)	O320—P212^iii	2.87 (3)
As11—O29	1.69 (3)	O320—Pb13^i	4.26 (3)
As11—O313	1.69 (3)	O321—P212^i	2.42 (3)
As11—Pb13^i	3.392 (4)	O321—Pb26^iii	2.59 (2)
As11—Pb11^iii	3.574 (4)	O321—Pb13^i	3.11 (2)
As11—P210^ii	3.750 (4)	O321—Pb11^iii	4.33 (3)
As11—P211^i	3.973 (5)	O322—P210^xi	2.38 (3)
As2—O323	1.66 (3)	O322—Pb14^xiv	2.76 (2)
As2—O319	1.68 (3)	O322—P211^xv	3.22 (3)
As2—O18	1.72 (2)	O322—Pb18^i	3.91 (3)
As2—O21	1.74 (2)	O322—Pb24^i	4.11 (2)
As2—Pb15^i	3.439 (4)	O323—Pb24^i	2.43 (3)
As2—Pb18^iii	3.584 (4)	O323—Pb15^i	2.71 (2)
As2—Pb24^i	3.898 (5)	O324—Pb18^vii	2.67 (2)
As21—O320	1.67 (3)	O324—Pb23^v	2.68 (3)
As21—O27	1.68 (3)	O324—Pb21^vii	2.82 (2)
As21—O321	1.69 (3)
O19—Pb11—O17	75.8 (8)	O315—As4—Pb15^x	60.3 (8)
O19—Pb11—O18	73.3 (8)	O22—As4—Pb15^x	47.2 (8)
O17—Pb11—O18	72.3 (8)	Pb21^vii—As4—Pb15^x	78.10 (9)
O19—Pb11—O32	71.2 (8)	Pb18^vii—As4—Pb15^x	66.33 (7)
O17—Pb11—O32	85.1 (8)	O324—As4—P210^ii	113.6 (8)
O18—Pb11—O32	141.5 (8)	O110—As4—P210^ii	79.9 (8)
O19—Pb11—O29^i	86.7 (8)	O315—As4—P210^ii	127.8 (8)
O17—Pb11—O29^i	154.2 (7)	O22—As4—P210^ii	31.5 (9)
O18—Pb11—O29^i	120.9 (9)	Pb21^vii—As4—P210^ii	147.18 (12)
O32—Pb11—O29^i	71.3 (8)	Pb18^vii—As4—P210^ii	74.76 (8)
O19—Pb11—O320^i	146.2 (8)	Pb15^x—As4—P210^ii	75.90 (7)
O17—Pb11—O320^i	72.3 (8)	O324—As4—Pb27	88.5 (8)
O18—Pb11—O320^i	86.6 (7)	O110—As4—Pb27	57.2 (8)
O32—Pb11—O320^i	116.1 (8)	O315—As4—Pb27	74.8 (8)
O29^i—Pb11—O320^i	127.2 (8)	O22—As4—Pb27	165.2 (9)
O19—Pb11—O28	130.4 (7)	Pb21^vii—As4—Pb27	75.79 (8)
O17—Pb11—O28	98.8 (8)	Pb18^vii—As4—Pb27	138.67 (13)
O18—Pb11—O28	153.0 (7)	Pb15^x—As4—Pb27	134.93 (13)
O32—Pb11—O28	59.2 (7)	P210^ii—As4—Pb27	137.03 (12)
O29^i—Pb11—O28	78.2 (7)	O324—As4—Pb14	90.1 (9)
O320^i—Pb11—O28	66.5 (6)	O110—As4—Pb14	31.4 (8)
O19—Pb11—O27^i	150.1 (8)	O315—As4—Pb14	142.3 (9)
O17—Pb11—O27^i	127.2 (7)	O22—As4—Pb14	102.5 (9)
O18—Pb11—O27^i	94.4 (7)	Pb21^vii—As4—Pb14	132.79 (12)
O32—Pb11—O27^i	123.9 (8)	Pb18^vii—As4—Pb14	107.92 (12)
O29^i—Pb11—O27^i	76.3 (7)	Pb15^x—As4—Pb14	148.01 (11)
O320^i—Pb11—O27^i	55.8 (7)	P210^ii—As4—Pb14	72.33 (8)
O28—Pb11—O27^i	70.3 (6)	Pb27—As4—Pb14	71.25 (7)
O19—Pb11—O313^i	88.8 (8)	O324—As4—Pb12	145.1 (9)
O17—Pb11—O313^i	141.8 (8)	O110—As4—Pb12	29.6 (8)
O18—Pb11—O313^i	69.8 (8)	O315—As4—Pb12	96.1 (9)
O32—Pb11—O313^i	123.1 (7)	O22—As4—Pb12	94.7 (9)
O29^i—Pb11—O313^i	54.4 (7)	Pb21^vii—As4—Pb12	137.34 (12)
O320^i—Pb11—O313^i	109.8 (7)	Pb18^vii—As4—Pb12	145.42 (11)
O28—Pb11—O313^i	117.3 (7)	Pb15^x—As4—Pb12	108.40 (11)
O27^i—Pb11—O313^i	61.3 (7)	P210^ii—As4—Pb12	70.93 (8)
O112—Pb12—O110	73.8 (8)	Pb27—As4—Pb12	70.57 (7)
O112—Pb12—O111	74.9 (8)	Pb14—As4—Pb12	57.29 (6)
O110—Pb12—O111	72.7 (9)	O324—As4—Pb23^ii	129.1 (8)
O112—Pb12—O212	151.4 (8)	O110—As4—Pb23^ii	88.9 (9)
O110—Pb12—O212	120.4 (7)	O315—As4—Pb23^ii	27.3 (9)
O111—Pb12—O212	85.6 (8)	O22—As4—Pb23^ii	106.6 (8)
O112—Pb12—O316^i	81.2 (8)	Pb21^vii—As4—Pb23^ii	74.50 (9)
O110—Pb12—O316^i	141.8 (8)	Pb18^vii—As4—Pb23^ii	131.86 (12)
O111—Pb12—O316^i	73.1 (8)	Pb15^x—As4—Pb23^ii	70.53 (8)
O212—Pb12—O316^i	73.1 (7)	P210^ii—As4—Pb23^ii	114.32 (11)
O112—Pb12—O211^ii	126.3 (7)	Pb27—As4—Pb23^ii	67.44 (7)
O110—Pb12—O211^ii	87.2 (8)	Pb14—As4—Pb23^ii	120.00 (11)
O111—Pb12—O211^ii	145.9 (7)	Pb12—As4—Pb23^ii	68.88 (8)
O212—Pb12—O211^ii	81.2 (7)	O318—As41—O211	113.2 (12)
O316^i—Pb12—O211^ii	131.1 (7)	O318—As41—O13	111.4 (13)
O112—Pb12—O210^i	95.3 (7)	O211—As41—O13	115.6 (12)
O110—Pb12—O210^i	150.8 (7)	O318—As41—O322	108.5 (13)
O111—Pb12—O210^i	131.5 (9)	O211—As41—O322	99.7 (11)
O212—Pb12—O210^i	82.0 (7)	O13—As41—O322	107.5 (12)
O316^i—Pb12—O210^i	58.4 (8)	O318—As41—P211^xv	40.7 (10)
O211^ii—Pb12—O210^i	77.6 (7)	O211—As41—P211^xv	117.4 (9)
O112—Pb12—O318^ii	75.6 (8)	O13—As41—P211^xv	126.9 (8)
O110—Pb12—O318^ii	89.7 (8)	O322—As41—P211^xv	67.9 (9)
O111—Pb12—O318^ii	148.8 (8)	O318—As41—Pb14^xiv	108.1 (10)
O212—Pb12—O318^ii	125.6 (7)	O211—As41—Pb14^xiv	51.6 (8)
O316^i—Pb12—O318^ii	111.7 (7)	O13—As41—Pb14^xiv	139.8 (9)
O211^ii—Pb12—O318^ii	54.1 (7)	O322—As41—Pb14^xiv	51.6 (8)
O210^i—Pb12—O318^ii	61.2 (8)	P211^xv—As41—Pb14^xiv	80.84 (9)
O112—Pb12—As1^i	94.4 (6)	O318—As41—Pb12^xiii	62.1 (9)
O110—Pb12—As1^i	168.0 (6)	O211—As41—Pb12^xiii	51.5 (8)
O111—Pb12—As1^i	102.3 (6)	O13—As41—Pb12^xiii	141.6 (9)
O212—Pb12—As1^i	69.2 (5)	O322—As41—Pb12^xiii	110.4 (9)
O316^i—Pb12—As1^i	29.8 (5)	P211^xv—As41—Pb12^xiii	75.01 (9)
O211^ii—Pb12—As1^i	102.1 (5)	Pb14^xiv—As41—Pb12^xiii	66.28 (7)
O210^i—Pb12—As1^i	30.0 (6)	O318—As41—Pb23	131.4 (9)
O318^ii—Pb12—As1^i	89.6 (5)	O211—As41—Pb23	30.3 (9)
O18—Pb13—O19	74.6 (8)	O13—As41—Pb23	85.3 (8)
O18—Pb13—O27^iii	85.9 (8)	O322—As41—Pb23	109.0 (8)
O19—Pb13—O27^iii	154.7 (8)	P211^xv—As41—Pb23	147.64 (12)
O18—Pb13—O17	71.9 (9)	Pb14^xiv—As41—Pb23	73.87 (7)
O19—Pb13—O17	72.2 (8)	Pb12^xiii—As41—Pb23	76.49 (7)
O27^iii—Pb13—O17	117.2 (7)	O318—As41—Pb18^i	143.8 (10)
O18—Pb13—O28^iv	143.7 (8)	O211—As41—Pb18^i	97.8 (9)
O19—Pb13—O28^iv	119.1 (7)	O13—As41—Pb18^i	34.3 (9)
O27^iii—Pb13—O28^iv	86.1 (7)	O322—As41—Pb18^i	82.8 (9)
O17—Pb13—O28^iv	80.5 (8)	P211^xv—As41—Pb18^i	136.75 (12)
O18—Pb13—O317^iii	75.4 (8)	Pb14^xiv—As41—Pb18^i	105.58 (11)
O19—Pb13—O317^iii	89.7 (7)	Pb12^xiii—As41—Pb18^i	147.32 (11)
O27^iii—Pb13—O317^iii	69.6 (7)	Pb23—As41—Pb18^i	70.90 (8)
O17—Pb13—O317^iii	145.8 (8)	O318—As41—Pb24^i	73.5 (9)
O28^iv—Pb13—O317^iii	133.5 (7)	O211—As41—Pb24^i	165.6 (9)
O18—Pb13—O29^iii	133.3 (9)	O13—As41—Pb24^i	50.6 (8)
O19—Pb13—O29^iii	98.0 (7)	O322—As41—Pb24^i	89.5 (8)
O27^iii—Pb13—O29^iii	83.7 (7)	P211^xv—As41—Pb24^i	76.28 (8)
O17—Pb13—O29^iii	150.7 (7)	Pb14^xiv—As41—Pb24^i	140.28 (13)
O28^iv—Pb13—O29^iii	80.7 (7)	Pb12^xiii—As41—Pb24^i	134.99 (13)
O317^iii—Pb13—O29^iii	58.3 (8)	Pb23—As41—Pb24^i	135.85 (12)
O18—Pb13—O321^iii	87.6 (8)	Pb18^i—As41—Pb24^i	72.31 (7)
O19—Pb13—O321^iii	138.9 (8)	O318—As41—Pb15^i	99.2 (11)
O27^iii—Pb13—O321^iii	53.6 (7)	O211—As41—Pb15^i	97.5 (9)
O17—Pb13—O321^iii	67.1 (7)	O13—As41—Pb15^i	31.2 (9)
O28^iv—Pb13—O321^iii	59.6 (6)	O322—As41—Pb15^i	137.9 (9)
O317^iii—Pb13—O321^iii	121.7 (7)	P211^xv—As41—Pb15^i	133.63 (12)
O29^iii—Pb13—O321^iii	120.4 (7)	Pb14^xiv—As41—Pb15^i	144.81 (11)
O18—Pb13—O31^iv	144.0 (8)	Pb12^xiii—As41—Pb15^i	110.42 (11)
O19—Pb13—O31^iv	70.4 (7)	Pb23—As41—Pb15^i	71.46 (8)
O27^iii—Pb13—O31^iv	130.1 (7)	Pb18^i—As41—Pb15^i	56.99 (7)
O17—Pb13—O31^iv	89.4 (7)	Pb24^i—As41—Pb15^i	68.41 (7)
O28^iv—Pb13—O31^iv	55.7 (7)	O318—As41—P210^xi	112.2 (10)
O317^iii—Pb13—O31^iv	112.1 (7)	O211—As41—P210^xi	114.4 (8)
O29^iii—Pb13—O31^iv	61.4 (7)	O13—As41—P210^xi	87.7 (9)
O321^iii—Pb13—O31^iv	113.7 (7)	O322—As41—P210^xi	20.6 (8)
O110—Pb14—O111	75.7 (9)	P211^xv—As41—P210^xi	75.03 (8)
O110—Pb14—O312^iv	77.0 (8)	Pb14^xiv—As41—P210^xi	70.85 (8)
O111—Pb14—O312^iv	83.2 (8)	Pb12^xiii—As41—P210^xi	130.58 (12)
O110—Pb14—O112	73.2 (8)	Pb23—As41—P210^xi	113.90 (11)
O111—Pb14—O112	73.5 (8)	Pb18^i—As41—P210^xi	67.54 (8)
O312^iv—Pb14—O112	145.7 (8)	Pb24^i—As41—P210^xi	72.10 (7)
O110—Pb14—O322^v	78.4 (8)	Pb15^i—As41—P210^xi	118.75 (10)
O111—Pb14—O322^v	140.0 (8)	O25—As5—O314	110.2 (12)
O312^iv—Pb14—O322^v	119.7 (8)	O25—As5—O17	114.7 (12)
O112—Pb14—O322^v	70.1 (8)	O314—As5—O17	107.8 (13)
O110—Pb14—O211^v	95.8 (8)	O25—As5—O33	106.2 (12)
O111—Pb14—O211^v	156.9 (8)	O314—As5—O33	107.6 (12)
O312^iv—Pb14—O211^v	73.9 (7)	O17—As5—O33	110.1 (12)
O112—Pb14—O211^v	125.2 (7)	O25—As5—Pb16	60.5 (9)
O322^v—Pb14—O211^v	55.1 (7)	O314—As5—Pb16	109.7 (10)
O110—Pb14—O210^iii	145.9 (7)	O17—As5—Pb16	141.1 (9)
O111—Pb14—O210^iii	121.0 (8)	O33—As5—Pb16	47.8 (8)
O312^iv—Pb14—O210^iii	130.9 (8)	O25—As5—Pb25^viii	117.5 (9)
O112—Pb14—O210^iii	83.2 (7)	O314—As5—Pb25^viii	41.7 (9)
O322^v—Pb14—O210^iii	70.6 (8)	O17—As5—Pb25^viii	126.3 (8)
O211^v—Pb14—O210^iii	77.9 (7)	O33—As5—Pb25^viii	66.1 (8)
O110—Pb14—O212^iv	135.4 (7)	Pb16—As5—Pb25^viii	78.60 (9)
O111—Pb14—O212^iv	95.1 (7)	O25—As5—Pb17	44.4 (9)
O312^iv—Pb14—O212^iv	58.5 (8)	O314—As5—Pb17	67.4 (8)
O112—Pb14—O212^iv	146.7 (8)	O17—As5—Pb17	140.3 (9)
O322^v—Pb14—O212^iv	124.5 (8)	O33—As5—Pb17	108.7 (9)
O211^v—Pb14—O212^iv	75.6 (7)	Pb16—As5—Pb17	66.74 (7)
O210^iii—Pb14—O212^iv	76.1 (7)	Pb25^viii—As5—Pb17	77.76 (9)
O110—Pb14—O38^iii	144.1 (8)	O25—As5—Pb28	32.6 (9)
O111—Pb14—O38^iii	70.3 (8)	O314—As5—Pb28	136.2 (8)
O312^iv—Pb14—O38^iii	109.5 (7)	O17—As5—Pb28	85.1 (8)
O112—Pb14—O38^iii	86.2 (8)	O33—As5—Pb28	106.5 (8)
O322^v—Pb14—O38^iii	122.2 (7)	Pb16—As5—Pb28	75.22 (8)
O211^v—Pb14—O38^iii	120.1 (7)	Pb25^viii—As5—Pb28	148.59 (12)
O210^iii—Pb14—O38^iii	54.4 (7)	Pb17—As5—Pb28	76.17 (7)
O212^iv—Pb14—O38^iii	60.6 (7)	O25—As5—Pb11	102.1 (9)
O12—Pb15—O11	75.3 (8)	O314—As5—Pb11	139.5 (9)
O12—Pb15—O13^iii	77.0 (9)	O17—As5—Pb11	34.0 (9)
O11—Pb15—O13^iii	74.5 (8)	O33—As5—Pb11	85.2 (9)
O12—Pb15—O310^vi	71.2 (8)	Pb16—As5—Pb11	107.10 (11)
O11—Pb15—O310^vi	81.0 (8)	Pb25^viii—As5—Pb11	135.67 (12)
O13^iii—Pb15—O310^vi	143.8 (9)	Pb17—As5—Pb11	145.75 (11)
O12—Pb15—O323^iii	83.5 (8)	Pb28—As5—Pb11	69.82 (8)
O11—Pb15—O323^iii	142.2 (9)	O25—As5—P212	160.5 (9)
O13^iii—Pb15—O323^iii	70.3 (8)	O314—As5—P212	68.8 (8)
O310^vi—Pb15—O323^iii	121.4 (7)	O17—As5—P212	50.8 (8)
O12—Pb15—O22^vii	152.1 (8)	O33—As5—P212	92.2 (8)
O11—Pb15—O22^vii	121.4 (7)	Pb16—As5—P212	138.85 (13)
O13^iii—Pb15—O22^vii	86.0 (8)	Pb25^viii—As5—P212	75.50 (8)
O310^vi—Pb15—O22^vii	129.9 (8)	Pb17—As5—P212	135.34 (12)
O323^iii—Pb15—O22^vii	69.8 (7)	Pb28—As5—P212	135.89 (12)
O12—Pb15—O21^iii	95.6 (8)	Pb11—As5—P212	72.51 (7)
O11—Pb15—O21^iii	154.1 (8)	O25—As5—Pb13	92.7 (9)
O13^iii—Pb15—O21^iii	127.9 (7)	O314—As5—Pb13	97.1 (10)
O310^vi—Pb15—O21^iii	73.1 (8)	O17—As5—Pb13	31.4 (8)
O323^iii—Pb15—O21^iii	57.5 (8)	O33—As5—Pb13	140.7 (9)
O22^vii—Pb15—O21^iii	77.4 (7)	Pb16—As5—Pb13	147.00 (11)
O12—Pb15—O23^vi	127.1 (8)	Pb25^viii—As5—Pb13	133.83 (11)
O11—Pb15—O23^vi	93.8 (7)	Pb17—As5—Pb13	108.90 (11)
O13^iii—Pb15—O23^vi	150.3 (7)	Pb28—As5—Pb13	72.09 (8)
O310^vi—Pb15—O23^vi	56.0 (8)	Pb11—As5—Pb13	56.87 (6)
O323^iii—Pb15—O23^vi	123.8 (7)	P212—As5—Pb13	68.48 (7)
O22^vii—Pb15—O23^vi	76.9 (7)	O25—As5—Pb26^iv	101.9 (9)
O21^iii—Pb15—O23^vi	72.1 (7)	O314—As5—Pb26^iv	30.7 (9)
O12—Pb15—O315^vii	142.2 (8)	O17—As5—Pb26^iv	86.1 (9)
O11—Pb15—O315^vii	67.4 (7)	O33—As5—Pb26^iv	136.9 (8)
O13^iii—Pb15—O315^vii	87.1 (7)	Pb16—As5—Pb26^iv	132.61 (12)
O310^vi—Pb15—O315^vii	107.7 (7)	Pb25^viii—As5—Pb26^iv	72.15 (8)
O323^iii—Pb15—O315^vii	123.1 (7)	Pb17—As5—Pb26^iv	71.11 (8)
O22^vii—Pb15—O315^vii	56.7 (7)	Pb28—As5—Pb26^iv	114.66 (11)
O21^iii—Pb15—O315^vii	120.7 (7)	Pb11—As5—Pb26^iv	119.95 (10)
O23^vi—Pb15—O315^vii	63.2 (7)	P212—As5—Pb26^iv	66.96 (7)
O14—Pb16—O16	72.5 (9)	Pb13—As5—Pb26^iv	67.79 (7)
O14—Pb16—O33	76.4 (8)	O32—As51—O16	115.2 (13)
O16—Pb16—O33	83.8 (8)	O32—As51—O31	107.8 (14)
O14—Pb16—O24^viii	90.8 (8)	O16—As51—O31	112.8 (13)
O16—Pb16—O24^viii	156.1 (8)	O32—As51—O28	108.4 (11)
O33—Pb16—O24^viii	75.6 (8)	O16—As51—O28	108.3 (11)
O14—Pb16—O15	72.0 (7)	O31—As51—O28	103.7 (12)
O16—Pb16—O15	72.8 (9)	O32—As51—Pb11	48.3 (8)
O33—Pb16—O15	145.0 (8)	O16—As51—Pb11	138.9 (9)
O24^viii—Pb16—O15	119.0 (8)	O31—As51—Pb11	108.3 (10)
O14—Pb16—O26	143.0 (8)	O28—As51—Pb11	61.2 (8)
O16—Pb16—O26	119.8 (7)	O32—As51—Pb29^i	67.4 (9)
O33—Pb16—O26	136.1 (8)	O16—As51—Pb29^i	132.0 (8)
O24^viii—Pb16—O26	83.8 (7)	O31—As51—Pb29^i	40.4 (10)
O15—Pb16—O26	78.8 (7)	O28—As51—Pb29^i	116.1 (8)
O14—Pb16—O25	134.7 (7)	Pb11—As51—Pb29^i	81.27 (9)
O16—Pb16—O25	98.3 (8)	O32—As51—Pb13^xi	106.3 (9)
O33—Pb16—O25	58.3 (7)	O16—As51—Pb13^xi	136.9 (9)
O24^viii—Pb16—O25	81.1 (8)	O31—As51—Pb13^xi	61.9 (9)
O15—Pb16—O25	149.1 (7)	O28—As51—Pb13^xi	44.4 (8)
O26—Pb16—O25	80.6 (7)	Pb11—As51—Pb13^xi	65.89 (7)
O14—Pb16—O34	144.7 (8)	Pb29^i—As51—Pb13^xi	74.33 (8)
O16—Pb16—O34	73.9 (8)	O32—As51—Pb26	109.3 (9)
O33—Pb16—O34	110.1 (8)	O16—As51—Pb26	80.5 (8)
O24^viii—Pb16—O34	124.5 (8)	O31—As51—Pb26	129.3 (9)
O15—Pb16—O34	88.3 (7)	O28—As51—Pb26	31.3 (8)
O26—Pb16—O34	53.1 (7)	Pb11—As51—Pb26	74.18 (8)
O25—Pb16—O34	60.9 (6)	Pb29^i—As51—Pb26	146.66 (11)
O14—Pb16—O39^viii	90.2 (8)	Pb13^xi—As51—Pb26	75.19 (7)
O16—Pb16—O39^viii	140.8 (8)	O32—As51—Pb16	87.5 (10)
O33—Pb16—O39^viii	126.9 (7)	O16—As51—Pb16	34.1 (9)
O24^viii—Pb16—O39^viii	53.1 (7)	O31—As51—Pb16	144.7 (9)
O15—Pb16—O39^viii	68.4 (8)	O28—As51—Pb16	101.0 (8)
O26—Pb16—O39^viii	57.6 (7)	Pb11—As51—Pb16	105.59 (12)
O25—Pb16—O39^viii	117.9 (7)	Pb29^i—As51—Pb16	139.90 (12)
O34—Pb16—O39^viii	109.8 (7)	Pb13^xi—As51—Pb16	145.03 (11)
O15^iv—Pb17—O14^iv	74.0 (8)	Pb26—As51—Pb16	69.91 (8)
O15^iv—Pb17—O16^iv	75.4 (9)	O32—As51—Pb22	92.8 (8)
O14^iv—Pb17—O16^iv	71.5 (9)	O16—As51—Pb22	55.8 (8)
O15^iv—Pb17—O35	81.3 (8)	O31—As51—Pb22	73.7 (9)
O14^iv—Pb17—O35	141.5 (9)	O28—As51—Pb22	158.1 (8)
O16^iv—Pb17—O35	74.0 (8)	Pb11—As51—Pb22	140.62 (13)
O15^iv—Pb17—O37^viii	73.0 (8)	Pb29^i—As51—Pb22	76.46 (8)
O14^iv—Pb17—O37^viii	79.6 (8)	Pb13^xi—As51—Pb22	135.04 (13)
O16^iv—Pb17—O37^viii	141.8 (9)	Pb26—As51—Pb22	136.21 (12)
O35—Pb17—O37^viii	120.9 (8)	Pb16—As51—Pb22	73.98 (7)
O15^iv—Pb17—O25	152.0 (8)	O32—As51—Pb28	24.2 (9)
O14^iv—Pb17—O25	117.6 (7)	O16—As51—Pb28	92.0 (9)
O16^iv—Pb17—O25	84.2 (8)	O31—As51—Pb28	113.9 (9)
O35—Pb17—O25	74.6 (7)	O28—As51—Pb28	125.7 (8)
O37^viii—Pb17—O25	132.2 (8)	Pb11—As51—Pb28	70.36 (8)
O15^iv—Pb17—O26	99.9 (7)	Pb29^i—As51—Pb28	76.96 (9)
O14^iv—Pb17—O26	154.8 (8)	Pb13^xi—As51—Pb28	130.32 (12)
O16^iv—Pb17—O26	131.6 (7)	Pb26—As51—Pb28	114.20 (12)
O35—Pb17—O26	57.8 (8)	Pb16—As51—Pb28	68.98 (8)
O37^viii—Pb17—O26	75.3 (7)	Pb22—As51—Pb28	73.19 (7)
O25—Pb17—O26	79.4 (7)	O32—As51—Pb17^xi	142.6 (9)
O15^iv—Pb17—O24^viii	130.1 (8)	O16—As51—Pb17^xi	27.4 (9)
O14^iv—Pb17—O24^viii	93.2 (8)	O31—As51—Pb17^xi	97.0 (10)
O16^iv—Pb17—O24^viii	146.5 (7)	O28—As51—Pb17^xi	91.9 (8)
O35—Pb17—O24^viii	125.2 (8)	Pb11—As51—Pb17^xi	146.30 (11)
O37^viii—Pb17—O24^viii	57.1 (8)	Pb29^i—As51—Pb17^xi	131.35 (12)
O25—Pb17—O24^viii	76.7 (8)	Pb13^xi—As51—Pb17^xi	110.06 (11)
O26—Pb17—O24^viii	71.7 (6)	Pb26—As51—Pb17^xi	72.59 (8)
O15^iv—Pb17—O314	143.1 (7)	Pb16—As51—Pb17^xi	57.20 (6)
O14^iv—Pb17—O314	69.9 (7)	Pb22—As51—Pb17^xi	67.33 (7)
O16^iv—Pb17—O314	86.5 (7)	Pb28—As51—Pb17^xi	119.37 (10)
O35—Pb17—O314	124.4 (7)	O310—As6—O311	106.8 (12)
O37^viii—Pb17—O314	106.6 (7)	O310—As6—O23	109.0 (13)
O25—Pb17—O314	51.6 (6)	O311—As6—O23	109.0 (12)
O26—Pb17—O314	115.9 (6)	O310—As6—O14	112.0 (13)
O24^viii—Pb17—O314	60.1 (7)	O311—As6—O14	111.2 (13)
O11—Pb18—O13^iii	76.0 (8)	O23—As6—O14	108.8 (11)
O11—Pb18—O23^ix	85.3 (8)	O310—As6—P212^xvi	69.9 (8)
O13^iii—Pb18—O23^ix	154.6 (7)	O311—As6—P212^xvi	37.5 (9)
O11—Pb18—O12	72.0 (7)	O23—As6—P212^xvi	115.5 (8)
O13^iii—Pb18—O12	73.3 (9)	O14—As6—P212^xvi	132.2 (8)
O23^ix—Pb18—O12	117.3 (8)	O310—As6—Pb15^xx	47.9 (10)
O11—Pb18—O324^x	72.5 (8)	O311—As6—Pb15^xx	108.2 (10)
O13^iii—Pb18—O324^x	88.5 (8)	O23—As6—Pb15^xx	63.3 (8)
O23^ix—Pb18—O324^x	69.3 (8)	O14—As6—Pb15^xx	139.9 (9)
O12—Pb18—O324^x	143.1 (8)	P212^xvi—As6—Pb15^xx	78.87 (8)
O11—Pb18—O21^i	147.5 (8)	O310—As6—Pb18^viii	109.0 (10)
O13^iii—Pb18—O21^i	123.0 (7)	O311—As6—Pb18^viii	69.7 (9)
O23^ix—Pb18—O21^i	81.8 (7)	O23—As6—Pb18^viii	41.3 (8)
O12—Pb18—O21^i	87.7 (7)	O14—As6—Pb18^viii	136.2 (9)
O324^x—Pb18—O21^i	128.6 (7)	P212^xvi—As6—Pb18^viii	76.62 (8)
O11—Pb18—O22^x	131.7 (7)	Pb15^xx—As6—Pb18^viii	65.60 (8)
O13^iii—Pb18—O22^x	94.8 (8)	O310—As6—Pb21^viii	108.8 (9)
O23^ix—Pb18—O22^x	84.8 (8)	O311—As6—Pb21^viii	134.0 (9)
O12—Pb18—O22^x	151.0 (7)	O23—As6—Pb21^viii	30.9 (8)
O324^x—Pb18—O22^x	59.8 (7)	O14—As6—Pb21^viii	81.1 (8)
O21^i—Pb18—O22^x	76.6 (7)	P212^xvi—As6—Pb21^viii	145.86 (13)
O11—Pb18—O319^i	146.2 (8)	Pb15^xx—As6—Pb21^viii	76.73 (9)
O13^iii—Pb18—O319^i	71.0 (8)	Pb18^viii—As6—Pb21^viii	71.71 (8)
O23^ix—Pb18—O319^i	128.3 (7)	O310—As6—Pb26	90.5 (10)
O12—Pb18—O319^i	91.4 (7)	O311—As6—Pb26	68.8 (9)
O324^x—Pb18—O319^i	113.1 (8)	O23—As6—Pb26	159.7 (8)
O21^i—Pb18—O319^i	55.9 (7)	O14—As6—Pb26	56.8 (8)
O22^x—Pb18—O319^i	59.6 (7)	P212^xvi—As6—Pb26	75.67 (8)
O11—Pb18—O311^ix	91.7 (8)	Pb15^xx—As6—Pb26	136.96 (12)
O13^iii—Pb18—O311^ix	143.1 (8)	Pb18^viii—As6—Pb26	137.70 (12)
O23^ix—Pb18—O311^ix	52.9 (7)	Pb21^viii—As6—Pb26	137.76 (11)
O12—Pb18—O311^ix	69.8 (7)	O310—As6—Pb16	142.7 (10)
O324^x—Pb18—O311^ix	121.3 (7)	O311—As6—Pb16	94.8 (9)
O21^i—Pb18—O311^ix	57.0 (7)	O23—As6—Pb16	91.3 (8)
O22^x—Pb18—O311^ix	118.3 (7)	O14—As6—Pb16	30.7 (9)
O319^i—Pb18—O311^ix	110.4 (7)	P212^xvi—As6—Pb16	129.41 (12)
O23^ix—Pb21—O37^xi	83.1 (8)	Pb15^xx—As6—Pb16	149.86 (11)
O23^ix—Pb21—O315^x	82.3 (8)	Pb18^viii—As6—Pb16	106.86 (11)
O37^xi—Pb21—O315^x	83.1 (8)	Pb21^viii—As6—Pb16	73.29 (7)
O23^ix—Pb21—O39	82.1 (8)	Pb26—As6—Pb16	69.15 (8)
O37^xi—Pb21—O39	132.8 (9)	O310—As6—Pb17^xi	87.3 (9)
O315^x—Pb21—O39	138.2 (8)	O311—As6—Pb17^xi	139.4 (10)
O23^ix—Pb21—O324^x	70.0 (8)	O23—As6—Pb17^xi	101.3 (8)
O37^xi—Pb21—O324^x	135.4 (8)	O14—As6—Pb17^xi	31.0 (9)
O315^x—Pb21—O324^x	59.2 (8)	P212^xvi—As6—Pb17^xi	141.11 (13)
O39—Pb21—O324^x	79.0 (8)	Pb15^xx—As6—Pb17^xi	109.18 (11)
O23^ix—Pb21—O15^ix	97.1 (8)	Pb18^viii—As6—Pb17^xi	141.98 (11)
O37^xi—Pb21—O15^ix	65.7 (8)	Pb21^viii—As6—Pb17^xi	70.52 (7)
O315^x—Pb21—O15^ix	148.5 (7)	Pb26—As6—Pb17^xi	73.40 (8)
O39—Pb21—O15^ix	72.0 (8)	Pb16—As6—Pb17^xi	57.50 (6)
O324^x—Pb21—O15^ix	149.7 (7)	O310—As6—Pb25^xx	23.2 (10)
O23^ix—Pb21—Cl4^xii	146.1 (7)	O311—As6—Pb25^xx	109.7 (9)
O37^xi—Pb21—Cl4^xii	75.5 (6)	O23—As6—Pb25^xx	126.2 (9)
O315^x—Pb21—Cl4^xii	69.3 (6)	O14—As6—Pb25^xx	90.2 (9)
O39—Pb21—Cl4^xii	131.6 (5)	P212^xvi—As6—Pb25^xx	78.10 (8)
O324^x—Pb21—Cl4^xii	108.1 (5)	Pb15^xx—As6—Pb25^xx	69.95 (8)
O15^ix—Pb21—Cl4^xii	97.7 (5)	Pb18^viii—As6—Pb25^xx	132.04 (11)
O23^ix—Pb21—Cl4^ii	132.4 (7)	Pb21^viii—As6—Pb25^xx	114.64 (11)
O37^xi—Pb21—Cl4^ii	144.5 (6)	Pb26—As6—Pb25^xx	71.20 (8)
O315^x—Pb21—Cl4^ii	99.2 (6)	Pb16—As6—Pb25^xx	120.68 (11)
O39—Pb21—Cl4^ii	65.3 (6)	Pb17^xi—As6—Pb25^xx	70.04 (7)
O324^x—Pb21—Cl4^ii	70.5 (5)	O11—As61—O24	114.1 (11)
O15^ix—Pb21—Cl4^ii	104.0 (5)	O11—As61—O39	109.6 (13)
Cl4^xii—Pb21—Cl4^ii	72.33 (4)	O24—As61—O39	107.1 (13)
O23^ix—Pb21—As4^x	74.1 (7)	O11—As61—O37	112.0 (13)
O37^xi—Pb21—As4^x	110.1 (6)	O24—As61—O37	105.9 (13)
O315^x—Pb21—As4^x	29.8 (6)	O39—As61—O37	108.0 (12)
O39—Pb21—As4^x	108.4 (6)	O11—As61—Pb27^ix	128.6 (9)
O324^x—Pb21—As4^x	29.4 (6)	O24—As61—Pb27^ix	114.6 (8)
O15^ix—Pb21—As4^x	170.9 (4)	O39—As61—Pb27^ix	39.4 (9)
Cl4^xii—Pb21—As4^x	88.71 (17)	O37—As61—Pb27^ix	68.7 (8)
Cl4^ii—Pb21—As4^x	84.14 (16)	O11—As61—Pb17^ix	143.0 (9)
O212—Pb22—O35^xi	82.1 (9)	O24—As61—Pb17^ix	60.1 (9)
O212—Pb22—O38^i	79.5 (8)	O39—As61—Pb17^ix	106.7 (10)
O35^xi—Pb22—O38^i	89.2 (9)	O37—As61—Pb17^ix	48.1 (9)
O212—Pb22—O34	79.6 (8)	Pb27^ix—As61—Pb17^ix	78.00 (8)
O35^xi—Pb22—O34	130.3 (8)	O11—As61—Pb16^ix	136.7 (9)
O38^i—Pb22—O34	131.3 (8)	O24—As61—Pb16^ix	40.7 (9)
O212—Pb22—O16	97.6 (7)	O39—As61—Pb16^ix	67.4 (10)
O35^xi—Pb22—O16	66.2 (8)	O37—As61—Pb16^ix	109.6 (9)
O38^i—Pb22—O16	155.4 (8)	Pb27^ix—As61—Pb16^ix	78.05 (9)
O34—Pb22—O16	71.0 (7)	Pb17^ix—As61—Pb16^ix	65.66 (8)
O212—Pb22—Cl2^i	145.4 (6)	O11—As61—Pb25	84.5 (8)
O35^xi—Pb22—Cl2^i	84.0 (7)	O24—As61—Pb25	32.5 (8)
O38^i—Pb22—Cl2^i	68.8 (7)	O39—As61—Pb25	133.0 (9)
O34—Pb22—Cl2^i	132.1 (6)	O37—As61—Pb25	107.2 (8)
O16—Pb22—Cl2^i	105.4 (5)	Pb27^ix—As61—Pb25	146.43 (13)
O212—Pb22—O316^i	66.2 (8)	Pb17^ix—As61—Pb25	75.99 (8)
O35^xi—Pb22—O316^i	136.6 (7)	Pb16^ix—As61—Pb25	72.10 (8)
O38^i—Pb22—O316^i	57.6 (8)	O11—As61—Pb23^iii	52.5 (8)
O34—Pb22—O316^i	73.7 (7)	O24—As61—Pb23^iii	163.5 (9)
O16—Pb22—O316^i	143.3 (6)	O39—As61—Pb23^iii	73.4 (10)
Cl2^i—Pb22—O316^i	105.4 (5)	O37—As61—Pb23^iii	89.2 (9)
O212—Pb22—Cl2	129.8 (7)	Pb27^ix—As61—Pb23^iii	76.60 (8)
O35^xi—Pb22—Cl2	147.5 (6)	Pb17^ix—As61—Pb23^iii	136.10 (12)
O38^i—Pb22—Cl2	101.8 (7)	Pb16^ix—As61—Pb23^iii	139.99 (13)
O34—Pb22—Cl2	62.0 (6)	Pb25—As61—Pb23^iii	136.88 (11)
O16—Pb22—Cl2	98.8 (5)	O11—As61—Pb15	33.7 (9)
Cl2^i—Pb22—Cl2	72.03 (3)	O24—As61—Pb15	101.7 (8)
O316^i—Pb22—Cl2	72.6 (5)	O39—As61—Pb15	141.7 (10)
O212—Pb22—As1^i	71.3 (5)	O37—As61—Pb15	87.3 (9)
O35^xi—Pb22—As1^i	113.3 (6)	Pb27^ix—As61—Pb15	140.50 (13)
O38^i—Pb22—As1^i	27.6 (6)	Pb17^ix—As61—Pb15	109.37 (12)
O34—Pb22—As1^i	103.7 (5)	Pb16^ix—As61—Pb15	141.06 (10)
O16—Pb22—As1^i	168.6 (5)	Pb25—As61—Pb15	69.38 (7)
Cl2^i—Pb22—As1^i	85.68 (16)	Pb23^iii—As61—Pb15	71.99 (8)
O316^i—Pb22—As1^i	30.0 (4)	O11—As61—Pb18	30.9 (9)
Cl2—Pb22—As1^i	87.04 (15)	O24—As61—Pb18	93.7 (8)
O211—Pb23—O36^xiii	81.0 (8)	O39—As61—Pb18	95.8 (10)
O211—Pb23—O315^xiii	86.1 (8)	O37—As61—Pb18	142.5 (9)
O36^xiii—Pb23—O315^xiii	85.2 (8)	Pb27^ix—As61—Pb18	130.94 (12)
O211—Pb23—O324^xiv	79.9 (7)	Pb17^ix—As61—Pb18	149.31 (11)
O36^xiii—Pb23—O324^xiv	136.9 (8)	Pb16^ix—As61—Pb18	106.12 (11)
O315^xiii—Pb23—O324^xiv	131.2 (7)	Pb25—As61—Pb18	73.40 (7)
O211—Pb23—O11^i	97.7 (7)	Pb23^iii—As61—Pb18	69.97 (8)
O36^xiii—Pb23—O11^i	155.5 (8)	Pb15—As61—Pb18	57.16 (6)
O315^xiii—Pb23—O11^i	70.3 (8)	O11—As61—Pb21	86.2 (9)
O324^xiv—Pb23—O11^i	65.8 (8)	O24—As61—Pb21	99.6 (10)
O211—Pb23—O312^xiii	71.4 (7)	O39—As61—Pb21	31.3 (9)
O36^xiii—Pb23—O312^xiii	58.2 (8)	O37—As61—Pb21	138.0 (8)
O315^xiii—Pb23—O312^xiii	138.9 (8)	Pb27^ix—As61—Pb21	70.50 (8)
O324^xiv—Pb23—O312^xiii	79.1 (7)	Pb17^ix—As61—Pb21	130.16 (12)
O11^i—Pb23—O312^xiii	144.7 (7)	Pb16^ix—As61—Pb21	70.62 (9)
O211—Pb23—Cl4^xv	134.5 (5)	Pb25—As61—Pb21	112.15 (11)
O36^xiii—Pb23—Cl4^xv	93.5 (6)	Pb23^iii—As61—Pb21	71.98 (8)
O315^xiii—Pb23—Cl4^xv	138.8 (6)	Pb15—As61—Pb21	119.62 (11)
O324^xiv—Pb23—Cl4^xv	73.8 (5)	Pb18—As61—Pb21	65.66 (8)
O11^i—Pb23—Cl4^xv	104.2 (5)	Pb25^i—Cl1—P212	98.4 (2)
O312^xiii—Pb23—Cl4^xv	67.6 (5)	Pb25^i—Cl1—Pb26^xix	90.18 (18)
O211—Pb23—Cl4^viii	141.5 (5)	P212—Cl1—Pb26^xix	89.9 (2)
O36^xiii—Pb23—Cl4^viii	68.7 (6)	Pb25^i—Cl1—Pb26	90.6 (2)
O315^xiii—Pb23—Cl4^viii	68.7 (5)	P212—Cl1—Pb26	97.6 (2)
O324^xiv—Pb23—Cl4^viii	138.6 (5)	Pb26^xix—Cl1—Pb26	172.3 (3)
O11^i—Pb23—Cl4^viii	100.3 (5)	Pb25^i—Cl1—P212^xvi	88.1 (2)
O312^xiii—Pb23—Cl4^viii	108.9 (5)	P212—Cl1—P212^xvi	171.7 (3)
Cl4^xv—Pb23—Cl4^viii	72.55 (4)	Pb26^xix—Cl1—P212^xvi	84.94 (19)
O211—Pb23—As31^xiii	72.3 (5)	Pb26—Cl1—P212^xvi	87.4 (2)
O36^xiii—Pb23—As31^xiii	28.4 (6)	Pb25^i—Cl1—Pb25^viii	174.3 (3)
O315^xiii—Pb23—As31^xiii	111.1 (6)	P212—Cl1—Pb25^viii	86.8 (2)
O324^xiv—Pb23—As31^xiii	108.5 (6)	Pb26^xix—Cl1—Pb25^viii	87.4 (2)
O11^i—Pb23—As31^xiii	169.5 (5)	Pb26—Cl1—Pb25^viii	91.13 (17)
O312^xiii—Pb23—As31^xiii	29.9 (5)	P212^xvi—Cl1—Pb25^viii	86.53 (18)
Cl4^xv—Pb23—As31^xiii	81.67 (16)	Pb28—Cl2—Pb29^i	95.4 (2)
Cl4^viii—Pb23—As31^xiii	89.71 (15)	Pb28—Cl2—Pb22^iii	90.7 (2)
O27—Pb24—O323^iii	84.3 (9)	Pb29^i—Cl2—Pb22^iii	93.9 (2)
O27—Pb24—O313	85.6 (8)	Pb28—Cl2—Pb29	89.0 (2)
O323^iii—Pb24—O313	86.6 (9)	Pb29^i—Cl2—Pb29	174.6 (3)
O27—Pb24—O319^i	76.1 (8)	Pb22^iii—Cl2—Pb29	89.2 (2)
O323^iii—Pb24—O319^i	130.7 (8)	Pb28—Cl2—Pb22	92.0 (2)
O313—Pb24—O319^i	135.0 (8)	Pb29^i—Cl2—Pb22	89.3 (2)
O27—Pb24—O317	69.9 (8)	Pb22^iii—Cl2—Pb22	175.6 (3)
O323^iii—Pb24—O317	136.8 (7)	Pb29—Cl2—Pb22	87.4 (2)
O313—Pb24—O317	58.3 (9)	Pb28—Cl2—Pb28^i	176.3 (3)
O319^i—Pb24—O317	76.8 (7)	Pb29^i—Cl2—Pb28^i	87.4 (2)
O27—Pb24—O13^iii	95.9 (7)	Pb22^iii—Cl2—Pb28^i	91.4 (2)
O323^iii—Pb24—O13^iii	67.6 (8)	Pb29—Cl2—Pb28^i	88.07 (18)
O313—Pb24—O13^iii	153.8 (8)	Pb22—Cl2—Pb28^i	85.7 (2)
O319^i—Pb24—O13^iii	70.0 (7)	P211^i—Cl3—P210^ii	93.51 (16)
O317—Pb24—O13^iii	146.2 (7)	P211^i—Cl3—P210^i	88.4 (2)
O27—Pb24—Cl3	128.1 (7)	P210^ii—Cl3—P210^i	178.1 (2)
O323^iii—Pb24—Cl3	147.3 (6)	P211^i—Cl3—P211^ii	179.0 (3)
O313—Pb24—Cl3	98.7 (7)	P210^ii—Cl3—P211^ii	87.48 (19)
O319^i—Pb24—Cl3	64.7 (6)	P210^i—Cl3—P211^ii	90.63 (15)
O317—Pb24—Cl3	69.2 (5)	P211^i—Cl3—Pb24	91.44 (18)
O13^iii—Pb24—Cl3	100.7 (5)	P210^ii—Cl3—Pb24	88.96 (19)
O27—Pb24—Cl3^vii	150.8 (6)	P210^i—Cl3—Pb24	90.83 (18)
O323^iii—Pb24—Cl3^vii	80.5 (6)	P211^ii—Cl3—Pb24	88.80 (19)
O313—Pb24—Cl3^vii	68.9 (7)	P211^i—Cl3—Pb24^x	90.21 (19)
O319^i—Pb24—Cl3^vii	132.1 (6)	P210^ii—Cl3—Pb24^x	91.73 (18)
O317—Pb24—Cl3^vii	105.6 (5)	P210^i—Cl3—Pb24^x	88.43 (18)
O13^iii—Pb24—Cl3^vii	101.0 (5)	P211^ii—Cl3—Pb24^x	89.54 (17)
Cl3—Pb24—Cl3^vii	71.69 (3)	Pb24—Cl3—Pb24^x	178.2 (2)
O27—Pb24—As11	74.6 (5)	Pb21^xxi—Cl4—Pb27^i	99.7 (2)
O323^iii—Pb24—As11	111.5 (6)	Pb21^xxi—Cl4—Pb23^xviii	90.9 (3)
O313—Pb24—As11	28.9 (7)	Pb27^i—Cl4—Pb23^xviii	98.2 (2)
O319^i—Pb24—As11	106.1 (5)	Pb21^xxi—Cl4—Pb27^xxii	88.4 (2)
O317—Pb24—As11	29.5 (5)	Pb27^i—Cl4—Pb27^xxii	169.1 (3)
O13^iii—Pb24—As11	170.5 (5)	Pb23^xviii—Cl4—Pb27^xxii	88.9 (2)
Cl3—Pb24—As11	84.88 (13)	Pb21^xxi—Cl4—Pb23^ix	90.71 (18)
Cl3^vii—Pb24—As11	88.04 (13)	Pb27^i—Cl4—Pb23^ix	88.5 (2)
O24—Pb25—O314^ix	83.4 (9)	Pb23^xviii—Cl4—Pb23^ix	172.8 (3)
O24—Pb25—O310^vi	82.1 (9)	Pb27^xxii—Cl4—Pb23^ix	84.1 (2)
O314^ix—Pb25—O310^vi	90.1 (9)	Pb21^xxi—Cl4—Pb21^xiii	173.3 (3)
O24—Pb25—O311^ix	81.3 (8)	Pb27^i—Cl4—Pb21^xiii	86.7 (2)
O314^ix—Pb25—O311^ix	129.8 (8)	Pb23^xviii—Cl4—Pb21^xiii	90.16 (18)
O310^vi—Pb25—O311^ix	133.9 (9)	Pb27^xxii—Cl4—Pb21^xiii	85.06 (19)
O24—Pb25—O12	96.4 (8)	Pb23^ix—Cl4—Pb21^xiii	87.5 (2)
O314^ix—Pb25—O12	155.5 (8)	As61—O11—Pb18	129.3 (14)
O310^vi—Pb25—O12	65.7 (8)	As61—O11—Pb15	125.3 (14)
O311^ix—Pb25—O12	73.9 (7)	Pb18—O11—Pb15	90.8 (8)
O24—Pb25—Cl1^iii	147.2 (7)	As61—O11—Pb23^iii	101.1 (10)
O314^ix—Pb25—Cl1^iii	70.2 (6)	Pb18—O11—Pb23^iii	102.3 (9)
O310^vi—Pb25—Cl1^iii	78.9 (6)	Pb15—O11—Pb23^iii	104.4 (9)
O311^ix—Pb25—Cl1^iii	130.7 (5)	As61—O11—Pb25	70.2 (9)
O12—Pb25—Cl1^iii	99.8 (5)	Pb18—O11—Pb25	85.7 (6)
O24—Pb25—O33^ix	67.4 (8)	Pb15—O11—Pb25	79.4 (6)
O314^ix—Pb25—O33^ix	57.3 (8)	Pb23^iii—O11—Pb25	170.9 (9)
O310^vi—Pb25—O33^ix	136.6 (7)	As61—O11—Pb21	70.8 (8)
O311^ix—Pb25—O33^ix	72.7 (7)	Pb18—O11—Pb21	72.7 (6)
O12—Pb25—O33^ix	144.7 (7)	Pb15—O11—Pb21	162.8 (9)
Cl1^iii—Pb25—O33^ix	110.5 (5)	Pb23^iii—O11—Pb21	75.4 (5)
O24—Pb25—Cl1^ix	130.2 (7)	Pb25—O11—Pb21	103.4 (6)
O314^ix—Pb25—Cl1^ix	93.9 (6)	As61—O11—Pb21^iv	68.0 (8)
O310^vi—Pb25—Cl1^ix	147.6 (6)	Pb18—O11—Pb21^iv	162.6 (9)
O311^ix—Pb25—Cl1^ix	62.8 (5)	Pb15—O11—Pb21^iv	74.6 (6)
O12—Pb25—Cl1^ix	104.5 (5)	Pb23^iii—O11—Pb21^iv	73.0 (5)
Cl1^iii—Pb25—Cl1^ix	72.42 (3)	Pb25—O11—Pb21^iv	100.5 (6)
O33^ix—Pb25—Cl1^ix	69.6 (5)	Pb21—O11—Pb21^iv	120.7 (5)
O24—Pb25—As5^ix	72.2 (7)	As21—O12—Pb15	126.9 (14)
O314^ix—Pb25—As5^ix	27.2 (6)	As21—O12—Pb18	124.3 (11)
O310^vi—Pb25—As5^ix	112.3 (6)	Pb15—O12—Pb18	92.1 (8)
O311^ix—Pb25—As5^ix	102.9 (5)	As21—O12—Pb25	101.3 (11)
O12—Pb25—As5^ix	168.6 (5)	Pb15—O12—Pb25	104.3 (8)
Cl1^iii—Pb25—As5^ix	90.56 (16)	Pb18—O12—Pb25	105.5 (8)
O33^ix—Pb25—As5^ix	30.2 (5)	As21—O12—Pb24	68.5 (8)
Cl1^ix—Pb25—As5^ix	83.11 (15)	Pb15—O12—Pb24	81.7 (7)
O28—Pb26—O33	83.8 (8)	Pb18—O12—Pb24	82.5 (6)
O28—Pb26—O321^i	71.9 (7)	Pb25—O12—Pb24	169.7 (8)
O33—Pb26—O321^i	137.6 (9)	As21—O12—P212^i	65.5 (8)
O28—Pb26—O314^xi	80.0 (8)	Pb15—O12—P212^i	167.0 (10)
O33—Pb26—O314^xi	131.6 (7)	Pb18—O12—P212^i	76.2 (6)
O321^i—Pb26—O314^xi	78.5 (8)	Pb25—O12—P212^i	74.3 (5)
O28—Pb26—O320^i	75.3 (8)	Pb24—O12—P212^i	101.8 (5)
O33—Pb26—O320^i	82.2 (8)	As41—O13—Pb18^i	123.9 (13)
O321^i—Pb26—O320^i	58.6 (8)	As41—O13—Pb15^i	129.1 (13)
O314^xi—Pb26—O320^i	135.2 (8)	Pb18^i—O13—Pb15^i	90.3 (9)
O28—Pb26—O14	96.6 (7)	As41—O13—Pb24^i	103.7 (11)
O33—Pb26—O14	65.4 (8)	Pb18^i—O13—Pb24^i	106.0 (9)
O321^i—Pb26—O14	149.5 (7)	Pb15^i—O13—Pb24^i	100.4 (8)
O314^xi—Pb26—O14	71.6 (7)	As41—O13—Pb23	69.2 (8)
O320^i—Pb26—O14	147.4 (7)	Pb18^i—O13—Pb23	80.7 (6)
O28—Pb26—Cl1^xvi	133.2 (6)	Pb15^i—O13—Pb23	82.8 (6)
O33—Pb26—Cl1^xvi	142.7 (6)	Pb24^i—O13—Pb23	172.4 (9)
O321^i—Pb26—Cl1^xvi	71.2 (6)	As41—O13—P210^xi	68.9 (8)
O314^xi—Pb26—Cl1^xvi	65.4 (5)	Pb18^i—O13—P210^xi	73.8 (6)
O320^i—Pb26—Cl1^xvi	107.6 (5)	Pb15^i—O13—P210^xi	161.5 (10)
O14—Pb26—Cl1^xvi	100.8 (5)	Pb24^i—O13—P210^xi	75.8 (5)
O28—Pb26—Cl1	141.1 (6)	Pb23—O13—P210^xi	103.3 (6)
O33—Pb26—Cl1	78.4 (5)	As6—O14—Pb16	128.2 (14)
O321^i—Pb26—Cl1	99.1 (5)	As6—O14—Pb17^xi	128.2 (13)
O314^xi—Pb26—Cl1	136.6 (5)	Pb16—O14—Pb17^xi	94.8 (8)
O320^i—Pb26—Cl1	68.2 (5)	As6—O14—Pb26	95.6 (9)
O14—Pb26—Cl1	106.7 (5)	Pb16—O14—Pb26	98.7 (9)
Cl1^xvi—Pb26—Cl1	72.80 (4)	Pb17^xi—O14—Pb26	105.9 (9)
O28—Pb26—As21^i	71.8 (5)	As6—O14—Pb21^viii	72.2 (9)
O33—Pb26—As21^i	110.5 (6)	Pb16—O14—Pb21^viii	87.8 (7)
O321^i—Pb26—As21^i	29.2 (6)	Pb17^xi—O14—Pb21^viii	84.0 (6)
O314^xi—Pb26—As21^i	107.0 (6)	Pb26—O14—Pb21^viii	167.6 (8)
O320^i—Pb26—As21^i	29.4 (5)	As6—O14—Pb25^xx	66.0 (8)
O14—Pb26—As21^i	168.3 (5)	Pb16—O14—Pb25^xx	164.5 (10)
Cl1^xvi—Pb26—As21^i	88.79 (15)	Pb17^xi—O14—Pb25^xx	76.8 (6)
Cl1—Pb26—As21^i	82.47 (15)	Pb26—O14—Pb25^xx	71.8 (5)
O26—Pb27—O39^viii	77.3 (9)	Pb21^viii—O14—Pb25^xx	104.0 (6)
O26—Pb27—O36	84.8 (8)	As31—O15—Pb17^xi	123.7 (13)
O39^viii—Pb27—O36	85.5 (9)	As31—O15—Pb16	133.6 (13)
O26—Pb27—O312^iv	80.3 (8)	Pb17^xi—O15—Pb16	91.0 (8)
O39^viii—Pb27—O312^iv	131.6 (8)	As31—O15—Pb21^viii	100.6 (11)
O36—Pb27—O312^iv	134.4 (7)	Pb17^xi—O15—Pb21^viii	101.3 (7)
O26—Pb27—O110	96.4 (7)	Pb16—O15—Pb21^viii	101.3 (8)
O39^viii—Pb27—O110	160.5 (8)	As31—O15—Pb22	71.7 (8)
O36—Pb27—O110	75.5 (7)	Pb17^xi—O15—Pb22	81.6 (7)
O312^iv—Pb27—O110	63.9 (7)	Pb16—O15—Pb22	86.1 (7)
O26—Pb27—Cl4^iii	135.8 (6)	Pb21^viii—O15—Pb22	171.9 (8)
O39^viii—Pb27—Cl4^iii	96.0 (7)	As31—O15—Pb27	69.5 (8)
O36—Pb27—Cl4^iii	138.9 (6)	Pb17^xi—O15—Pb27	166.7 (9)
O312^iv—Pb27—Cl4^iii	71.9 (5)	Pb16—O15—Pb27	79.0 (6)
O110—Pb27—Cl4^iii	101.1 (5)	Pb21^viii—O15—Pb27	72.5 (5)
O26—Pb27—Cl4^xvii	138.8 (6)	Pb22—O15—Pb27	106.2 (5)
O39^viii—Pb27—Cl4^xvii	69.7 (7)	As51—O16—Pb16	123.2 (13)
O36—Pb27—Cl4^xvii	68.9 (6)	As51—O16—Pb17^xi	134.2 (13)
O312^iv—Pb27—Cl4^xvii	140.5 (5)	Pb16—O16—Pb17^xi	93.8 (9)
O110—Pb27—Cl4^xvii	106.3 (5)	As51—O16—Pb22	97.2 (10)
Cl4^iii—Pb27—Cl4^xvii	73.16 (4)	Pb16—O16—Pb22	105.7 (8)
O26—Pb27—O37^viii	74.5 (7)	Pb17^xi—O16—Pb22	97.2 (8)
O39^viii—Pb27—O37^viii	56.7 (8)	As51—O16—Pb26	73.0 (8)
O36—Pb27—O37^viii	139.7 (7)	Pb16—O16—Pb26	82.0 (6)
O312^iv—Pb27—O37^viii	76.1 (7)	Pb17^xi—O16—Pb26	88.5 (6)
O110—Pb27—O37^viii	139.9 (7)	Pb22—O16—Pb26	170.0 (9)
Cl4^iii—Pb27—O37^viii	65.9 (5)	As51—O16—Pb28	64.4 (8)
Cl4^xvii—Pb27—O37^viii	105.4 (5)	Pb16—O16—Pb28	73.4 (6)
O26—Pb27—As61^viii	72.6 (5)	Pb17^xi—O16—Pb28	161.1 (9)
O39^viii—Pb27—As61^viii	26.8 (7)	Pb22—O16—Pb28	73.7 (5)
O36—Pb27—As61^viii	110.9 (5)	Pb26—O16—Pb28	103.1 (6)
O312^iv—Pb27—As61^viii	105.2 (5)	As5—O17—Pb11	123.6 (13)
O110—Pb27—As61^viii	166.2 (5)	As5—O17—Pb13	129.0 (12)
Cl4^iii—Pb27—As61^viii	82.23 (15)	Pb11—O17—Pb13	90.6 (8)
Cl4^xvii—Pb27—As61^viii	87.47 (15)	As5—O17—P212	102.8 (10)
O37^viii—Pb27—As61^viii	30.1 (5)	Pb11—O17—P212	107.3 (8)
O34—Pb28—O32	93.3 (9)	Pb13—O17—P212	100.7 (8)
O34—Pb28—O25	82.3 (9)	As5—O17—Pb28	69.1 (7)
O32—Pb28—O25	84.0 (9)	Pb11—O17—Pb28	79.3 (6)
O34—Pb28—O31^iv	129.3 (9)	Pb13—O17—Pb28	84.0 (6)
O32—Pb28—O31^iv	130.2 (8)	P212—O17—Pb28	171.7 (9)
O25—Pb28—O31^iv	78.7 (8)	As5—O17—Pb26^iv	70.6 (8)
O34—Pb28—O19	159.3 (8)	Pb11—O17—Pb26^iv	165.3 (10)
O32—Pb28—O19	66.0 (8)	Pb13—O17—Pb26^iv	76.0 (6)
O25—Pb28—O19	95.8 (7)	P212—O17—Pb26^iv	70.1 (5)
O31^iv—Pb28—O19	69.8 (7)	Pb28—O17—Pb26^iv	104.9 (5)
O34—Pb28—Cl2	70.9 (7)	As5—O17—Pb26	69.2 (8)
O32—Pb28—Cl2	79.9 (6)	Pb11—O17—Pb26	72.0 (6)
O25—Pb28—Cl2	147.6 (6)	Pb13—O17—Pb26	160.9 (9)
O31^iv—Pb28—Cl2	132.5 (6)	P212—O17—Pb26	77.7 (5)
O19—Pb28—Cl2	102.9 (5)	Pb28—O17—Pb26	100.1 (5)
O34—Pb28—Cl2^iii	93.1 (6)	Pb26^iv—O17—Pb26	120.1 (6)
O32—Pb28—Cl2^iii	148.2 (7)	As2—O18—Pb13	130.8 (13)
O25—Pb28—Cl2^iii	127.7 (6)	As2—O18—Pb11	125.3 (13)
O31^iv—Pb28—Cl2^iii	64.5 (5)	Pb13—O18—Pb11	94.4 (8)
O19—Pb28—Cl2^iii	104.1 (5)	As2—O18—P211	96.8 (11)
Cl2—Pb28—Cl2^iii	72.88 (3)	Pb13—O18—P211	99.5 (8)
O34—Pb28—O35	54.4 (8)	Pb11—O18—P211	105.1 (8)
O32—Pb28—O35	137.0 (8)	As2—O18—P212	72.3 (9)
O25—Pb28—O35	65.9 (7)	Pb13—O18—P212	84.9 (7)
O31^iv—Pb28—O35	75.0 (7)	Pb11—O18—P212	85.4 (7)
O19—Pb28—O35	143.0 (7)	P211—O18—P212	168.2 (8)
Cl2—Pb28—O35	109.2 (5)	As2—O18—Pb24^i	65.2 (8)
Cl2^iii—Pb28—O35	69.4 (5)	Pb13—O18—Pb24^i	163.7 (9)
O34—Pb28—As3	26.0 (7)	Pb11—O18—Pb24^i	74.6 (6)
O32—Pb28—As3	114.5 (7)	P211—O18—Pb24^i	72.5 (5)
O25—Pb28—As3	71.3 (5)	P212—O18—Pb24^i	105.8 (6)
O31^iv—Pb28—As3	103.4 (6)	As1—O19—Pb11	130.4 (13)
O19—Pb28—As3	166.7 (5)	As1—O19—Pb13	120.7 (12)
Cl2—Pb28—As3	90.13 (17)	Pb11—O19—Pb13	93.3 (8)
Cl2^iii—Pb28—As3	82.18 (16)	As1—O19—Pb28	101.0 (10)
O35—Pb28—As3	28.4 (5)	Pb11—O19—Pb28	100.8 (8)
O316^i—Pb29—O31^iii	91.4 (9)	Pb13—O19—Pb28	108.1 (9)
O316^i—Pb29—O29	83.0 (8)	As1—O19—P211	68.5 (8)
O31^iii—Pb29—O29	80.3 (9)	Pb11—O19—P211	86.4 (7)
O316^i—Pb29—O38^iii	126.9 (8)	Pb13—O19—P211	78.8 (6)
O31^iii—Pb29—O38^iii	132.2 (9)	Pb28—O19—P211	169.5 (8)
O29—Pb29—O38^iii	77.9 (8)	As1—O19—Pb29^iii	65.7 (7)
O316^i—Pb29—O111	68.4 (8)	Pb11—O19—Pb29^iii	163.7 (9)
O31^iii—Pb29—O111	159.8 (8)	Pb13—O19—Pb29^iii	73.7 (6)
O29—Pb29—O111	98.1 (8)	Pb28—O19—Pb29^iii	74.8 (5)
O38^iii—Pb29—O111	66.0 (7)	P211—O19—Pb29^iii	100.4 (5)
O316^i—Pb29—Cl2^iii	151.5 (5)	As4—O110—Pb14	127.3 (13)
O31^iii—Pb29—Cl2^iii	97.4 (7)	As4—O110—Pb12	131.1 (13)
O29—Pb29—Cl2^iii	125.2 (7)	Pb14—O110—Pb12	94.1 (9)
O38^iii—Pb29—Cl2^iii	63.6 (5)	As4—O110—Pb27	95.6 (10)
O111—Pb29—Cl2^iii	99.9 (5)	Pb14—O110—Pb27	101.3 (8)
O316^i—Pb29—O32^iii	136.9 (7)	Pb12—O110—Pb27	100.7 (8)
O31^iii—Pb29—O32^iii	56.9 (8)	As4—O110—P210^ii	73.4 (8)
O29—Pb29—O32^iii	64.9 (8)	Pb14—O110—P210^ii	86.9 (6)
O38^iii—Pb29—O32^iii	75.3 (8)	Pb12—O110—P210^ii	86.0 (6)
O111—Pb29—O32^iii	140.5 (7)	Pb27—O110—P210^ii	168.9 (9)
Cl2^iii—Pb29—O32^iii	68.6 (5)	As4—O110—Pb23^ii	67.7 (8)
O316^i—Pb29—Cl2	85.0 (6)	Pb14—O110—Pb23^ii	163.6 (9)
O31^iii—Pb29—Cl2	70.0 (6)	Pb12—O110—Pb23^ii	76.3 (6)
O29—Pb29—Cl2	147.6 (7)	Pb27—O110—Pb23^ii	68.1 (4)
O38^iii—Pb29—Cl2	132.2 (5)	P210^ii—O110—Pb23^ii	105.4 (6)
O111—Pb29—Cl2	105.2 (5)	As3—O111—Pb14	126.2 (14)
Cl2^iii—Pb29—Cl2	72.83 (3)	As3—O111—Pb12	130.5 (13)
O32^iii—Pb29—Cl2	106.6 (5)	Pb14—O111—Pb12	91.4 (8)
O316^i—Pb29—As51^iii	115.0 (6)	As3—O111—Pb29	100.3 (12)
O31^iii—Pb29—As51^iii	28.0 (7)	Pb14—O111—Pb29	108.1 (8)
O29—Pb29—As51^iii	70.3 (7)	Pb12—O111—Pb29	95.7 (8)
O38^iii—Pb29—As51^iii	104.2 (5)	As3—O111—Pb27	71.7 (9)
O111—Pb29—As51^iii	166.7 (5)	Pb14—O111—Pb27	83.4 (7)
Cl2^iii—Pb29—As51^iii	82.58 (18)	Pb12—O111—Pb27	84.1 (7)
O32^iii—Pb29—As51^iii	28.8 (5)	Pb29—O111—Pb27	168.5 (8)
Cl2—Pb29—As51^iii	88.02 (18)	As3—O111—Pb22^iv	67.9 (9)
O22^xiii—P210—O322^iv	81.4 (9)	Pb14—O111—Pb22^iv	75.6 (6)
O22^xiii—P210—O319	77.7 (9)	Pb12—O111—Pb22^iv	161.4 (9)
O322^iv—P210—O319	89.3 (9)	Pb29—O111—Pb22^iv	76.3 (5)
O22^xiii—P210—O318	82.7 (8)	Pb27—O111—Pb22^iv	107.1 (6)
O322^iv—P210—O318	130.9 (8)	As11—O112—Pb12	127.2 (13)
O319—P210—O318	131.5 (9)	As11—O112—Pb14	132.2 (14)
O22^xiii—P210—O112^xiii	101.7 (7)	Pb12—O112—Pb14	90.5 (7)
O322^iv—P210—O112^xiii	67.7 (8)	As11—O112—P210^ii	100.8 (10)
O319—P210—O112^xiii	156.7 (8)	Pb12—O112—P210^ii	101.9 (9)
O318—P210—O112^xiii	70.6 (7)	Pb14—O112—P210^ii	97.9 (8)
O22^xiii—P210—Cl3^xiii	130.8 (6)	As11—O112—Pb29	73.2 (9)
O322^iv—P210—Cl3^xiii	147.8 (7)	Pb12—O112—Pb29	80.9 (6)
O319—P210—Cl3^xiii	98.5 (6)	Pb14—O112—Pb29	87.6 (7)
O318—P210—Cl3^xiii	63.2 (5)	P210^ii—O112—Pb29	173.7 (8)
O112^xiii—P210—Cl3^xiii	99.2 (5)	As11—O112—P211^i	68.9 (8)
O22^xiii—P210—Cl3^iii	142.5 (6)	Pb12—O112—P211^i	72.4 (6)
O322^iv—P210—Cl3^iii	81.6 (6)	Pb14—O112—P211^i	158.9 (9)
O319—P210—Cl3^iii	68.9 (7)	P210^ii—O112—P211^i	74.4 (5)
O318—P210—Cl3^iii	132.6 (5)	Pb29—O112—P211^i	101.4 (6)
O112^xiii—P210—Cl3^iii	102.5 (5)	As2—O21—P212	125.1 (11)
Cl3^xiii—P210—Cl3^iii	72.41 (3)	As2—O21—Pb18^iii	103.8 (10)
O22^xiii—P210—O323	66.7 (8)	P212—O21—Pb18^iii	118.4 (10)
O322^iv—P210—O323	136.1 (8)	As2—O21—Pb15^i	95.9 (10)
O319—P210—O323	55.8 (8)	P212—O21—Pb15^i	118.1 (9)
O318—P210—O323	75.7 (7)	Pb18^iii—O21—Pb15^i	87.5 (6)
O112^xiii—P210—O323	145.6 (7)	As2—O21—Pb13	58.8 (6)
Cl3^xiii—P210—O323	70.9 (5)	P212—O21—Pb13	72.8 (5)
Cl3^iii—P210—O323	105.4 (5)	Pb18^iii—O21—Pb13	112.7 (6)
O22^xiii—P210—As2	69.0 (6)	Pb15^i—O21—Pb13	149.9 (8)
O322^iv—P210—As2	112.4 (7)	As4—O22—P210^ii	124.6 (13)
O319—P210—As2	27.2 (7)	As4—O22—Pb15^x	104.2 (10)
O318—P210—As2	104.4 (6)	P210^ii—O22—Pb15^x	124.0 (9)
O112^xiii—P210—As2	170.2 (5)	As4—O22—Pb18^vii	93.1 (10)
Cl3^xiii—P210—As2	85.44 (14)	P210^ii—O22—Pb18^vii	112.7 (8)
Cl3^iii—P210—As2	87.14 (14)	Pb15^x—O22—Pb18^vii	87.6 (8)
O323—P210—As2	28.7 (5)	As6—O23—Pb21^viii	127.2 (13)
O210—P211—O318^xviii	78.5 (9)	As6—O23—Pb18^viii	112.9 (11)
O210—P211—O317^iii	84.9 (8)	Pb21^viii—O23—Pb18^viii	118.8 (11)
O318^xviii—P211—O317^iii	88.6 (8)	As6—O23—Pb15^xx	87.5 (9)
O210—P211—O313^i	82.5 (8)	Pb21^viii—O23—Pb15^xx	107.3 (9)
O318^xviii—P211—O313^i	132.0 (9)	Pb18^viii—O23—Pb15^xx	84.2 (7)
O317^iii—P211—O313^i	133.2 (8)	As6—O23—Pb16	64.5 (8)
O210—P211—O18	96.4 (8)	Pb21^viii—O23—Pb16	80.1 (6)
O318^xviii—P211—O18	155.7 (8)	Pb18^viii—O23—Pb16	120.7 (8)
O317^iii—P211—O18	67.2 (7)	Pb15^xx—O23—Pb16	147.5 (8)
O313^i—P211—O18	69.7 (8)	As61—O24—Pb25	125.4 (13)
O210—P211—Cl3^iii	141.3 (6)	As61—O24—Pb16^ix	113.8 (11)
O318^xviii—P211—Cl3^iii	68.7 (6)	Pb25—O24—Pb16^ix	118.2 (11)
O317^iii—P211—Cl3^iii	74.6 (5)	As61—O24—Pb17^ix	90.9 (10)
O313^i—P211—Cl3^iii	135.0 (5)	Pb25—O24—Pb17^ix	107.6 (9)
O18—P211—Cl3^iii	105.0 (5)	Pb16^ix—O24—Pb17^ix	86.4 (7)
O210—P211—Cl3^xiii	132.8 (6)	As61—O24—Pb18	62.9 (8)
O318^xviii—P211—Cl3^xiii	97.0 (6)	Pb25—O24—Pb18	78.6 (6)
O317^iii—P211—Cl3^xiii	142.3 (5)	Pb16^ix—O24—Pb18	118.0 (8)
O313^i—P211—Cl3^xiii	65.8 (6)	Pb17^ix—O24—Pb18	149.2 (9)
O18—P211—Cl3^xiii	103.5 (5)	As5—O25—Pb28	126.2 (14)
Cl3^iii—P211—Cl3^xiii	72.93 (3)	As5—O25—Pb17	110.6 (11)
O210—P211—O322^xviii	69.0 (8)	Pb28—O25—Pb17	121.3 (9)
O318^xviii—P211—O322^xviii	55.4 (8)	As5—O25—Pb16	90.3 (10)
O317^iii—P211—O322^xviii	138.2 (7)	Pb28—O25—Pb16	105.8 (8)
O313^i—P211—O322^xviii	76.6 (8)	Pb17—O25—Pb16	86.1 (7)
O18—P211—O322^xviii	144.8 (7)	As5—O25—Pb13	65.1 (8)
Cl3^iii—P211—O322^xviii	105.8 (5)	Pb28—O25—Pb13	77.0 (6)
Cl3^xiii—P211—O322^xviii	70.2 (4)	Pb17—O25—Pb13	120.0 (7)
O210—P211—As41^xviii	71.0 (7)	Pb16—O25—Pb13	148.4 (8)
O318^xviii—P211—As41^xviii	25.4 (6)	As5—O25—Pb11	56.3 (8)
O317^iii—P211—As41^xviii	111.5 (6)	Pb28—O25—Pb11	70.2 (6)
O313^i—P211—As41^xviii	106.5 (6)	Pb17—O25—Pb11	164.7 (7)
O18—P211—As41^xviii	167.4 (5)	Pb16—O25—Pb11	100.9 (7)
Cl3^iii—P211—As41^xviii	86.28 (15)	Pb13—O25—Pb11	49.6 (3)
Cl3^xiii—P211—As41^xviii	85.06 (14)	As3—O26—Pb27	127.7 (11)
O322^xviii—P211—As41^xviii	30.0 (5)	As3—O26—Pb16	108.7 (11)
O21—P212—O311^xix	78.6 (9)	Pb27—O26—Pb16	121.6 (10)
O21—P212—O321^iii	88.9 (8)	As3—O26—Pb17	88.4 (9)
O311^xix—P212—O321^iii	91.5 (9)	Pb27—O26—Pb17	108.9 (9)
O21—P212—O320^i	80.5 (8)	Pb16—O26—Pb17	84.4 (5)
O311^xix—P212—O320^i	130.9 (8)	As3—O26—Pb12	64.6 (6)
O321^iii—P212—O320^i	131.9 (8)	Pb27—O26—Pb12	76.9 (5)
O21—P212—O17	100.0 (8)	Pb16—O26—Pb12	121.6 (7)
O311^xix—P212—O17	163.9 (8)	Pb17—O26—Pb12	146.5 (8)
O321^iii—P212—O17	72.5 (7)	As21—O27—Pb24	128.3 (12)
O320^i—P212—O17	63.7 (7)	As21—O27—Pb13^i	110.9 (12)
O21—P212—Cl1	129.8 (6)	Pb24—O27—Pb13^i	120.5 (10)
O311^xix—P212—Cl1	92.7 (7)	As21—O27—Pb11^iii	87.2 (10)
O321^iii—P212—Cl1	141.2 (6)	Pb24—O27—Pb11^iii	103.5 (9)
O320^i—P212—Cl1	68.5 (5)	Pb13^i—O27—Pb11^iii	82.9 (5)
O17—P212—Cl1	100.2 (5)	As21—O27—Pb18	68.4 (7)
O21—P212—Cl1^xix	141.5 (6)	Pb24—O27—Pb18	79.4 (5)
O311^xix—P212—Cl1^xix	68.9 (7)	Pb13^i—O27—Pb18	122.8 (8)
O321^iii—P212—Cl1^xix	72.3 (6)	Pb11^iii—O27—Pb18	149.0 (8)
O320^i—P212—Cl1^xix	136.9 (5)	As51—O28—Pb26	125.3 (12)
O17—P212—Cl1^xix	105.5 (5)	As51—O28—Pb13^xi	107.6 (10)
Cl1—P212—Cl1^xix	73.35 (4)	Pb26—O28—Pb13^xi	125.9 (8)
O21—P212—O310^xix	68.1 (7)	As51—O28—Pb11	87.5 (8)
O311^xix—P212—O310^xix	54.0 (8)	Pb26—O28—Pb11	106.0 (8)
O321^iii—P212—O310^xix	140.6 (7)	Pb13^xi—O28—Pb11	85.1 (6)
O320^i—P212—O310^xix	77.0 (7)	As51—O28—Pb17^xi	63.8 (7)
O17—P212—O310^xix	140.6 (7)	Pb26—O28—Pb17^xi	78.1 (6)
Cl1—P212—O310^xix	67.2 (5)	Pb13^xi—O28—Pb17^xi	121.7 (7)
Cl1^xix—P212—O310^xix	105.9 (5)	Pb11—O28—Pb17^xi	144.7 (7)
O21—P212—O314	144.4 (7)	As11—O29—Pb29	124.8 (13)
O311^xix—P212—O314	125.5 (8)	As11—O29—Pb11^iii	108.7 (10)
O321^iii—P212—O314	67.1 (7)	Pb29—O29—Pb11^iii	122.9 (11)
O320^i—P212—O314	96.1 (6)	As11—O29—Pb13^i	92.6 (10)
O17—P212—O314	49.1 (7)	Pb29—O29—Pb13^i	106.9 (9)
Cl1—P212—O314	79.3 (5)	Pb11^iii—O29—Pb13^i	87.5 (7)
Cl1^xix—P212—O314	57.1 (5)	As1—O210—P211	129.0 (14)
O310^xix—P212—O314	146.1 (7)	As1—O210—Pb14^i	103.7 (10)
O38—As1—O210	107.7 (12)	P211—O210—Pb14^i	121.5 (11)
O38—As1—O316	109.9 (12)	As1—O210—Pb12^iii	94.0 (10)
O210—As1—O316	102.3 (12)	P211—O210—Pb12^iii	110.6 (9)
O38—As1—O19	112.2 (13)	Pb14^i—O210—Pb12^iii	85.7 (7)
O210—As1—O19	113.5 (11)	As1—O210—Pb13	59.0 (8)
O316—As1—O19	110.8 (12)	P211—O210—Pb13	71.7 (6)
O38—As1—Pb12^iii	106.2 (10)	Pb14^i—O210—Pb13	160.3 (9)
O210—As1—Pb12^iii	56.0 (8)	Pb12^iii—O210—Pb13	104.0 (7)
O316—As1—Pb12^iii	49.3 (8)	As1—O210—Pb11	61.4 (8)
O19—As1—Pb12^iii	141.4 (8)	P211—O210—Pb11	77.6 (6)
O38—As1—Pb22^iii	41.9 (9)	Pb14^i—O210—Pb11	115.7 (7)
O210—As1—Pb22^iii	118.2 (8)	Pb12^iii—O210—Pb11	149.8 (9)
O316—As1—Pb22^iii	68.1 (7)	Pb13—O210—Pb11	49.5 (3)
O19—As1—Pb22^iii	127.3 (8)	As41—O211—Pb23	129.6 (13)
Pb12^iii—As1—Pb22^iii	80.26 (9)	As41—O211—Pb14^xiv	101.3 (10)
O38—As1—Pb14^i	59.5 (10)	Pb23—O211—Pb14^xiv	111.8 (8)
O210—As1—Pb14^i	49.2 (8)	As41—O211—Pb12^xiii	101.7 (10)
O316—As1—Pb14^i	108.9 (9)	Pb23—O211—Pb12^xiii	117.0 (8)
O19—As1—Pb14^i	139.6 (9)	Pb14^xiv—O211—Pb12^xiii	86.4 (7)
Pb12^iii—As1—Pb14^i	66.20 (8)	As41—O211—Pb18^i	60.1 (7)
Pb22^iii—As1—Pb14^i	75.41 (8)	Pb23—O211—Pb18^i	73.9 (6)
O38—As1—P211	129.3 (9)	Pb14^xiv—O211—Pb18^i	107.4 (6)
O210—As1—P211	29.8 (8)	Pb12^xiii—O211—Pb18^i	158.5 (7)
O316—As1—P211	107.0 (7)	As31—O212—Pb22	124.2 (12)
O19—As1—P211	84.8 (8)	As31—O212—Pb12	111.2 (12)
Pb12^iii—As1—P211	74.03 (8)	Pb22—O212—Pb12	122.5 (10)
Pb22^iii—As1—P211	147.73 (13)	As31—O212—Pb14^xi	89.5 (10)
Pb14^i—As1—P211	76.54 (8)	Pb22—O212—Pb14^xi	106.4 (9)
O38—As1—Pb28	76.1 (10)	Pb12—O212—Pb14^xi	86.8 (6)
O210—As1—Pb28	163.1 (8)	As51—O31—Pb29^i	111.6 (14)
O316—As1—Pb28	91.4 (8)	As51—O31—Pb28^xi	131.0 (15)
O19—As1—Pb28	51.4 (8)	Pb29^i—O31—Pb28^xi	116.0 (10)
Pb12^iii—As1—Pb28	139.72 (12)	As51—O31—Pb13^xi	89.3 (9)
Pb22^iii—As1—Pb28	75.96 (8)	Pb29^i—O31—Pb13^xi	98.5 (9)
Pb14^i—As1—Pb28	135.08 (12)	Pb28^xi—O31—Pb13^xi	94.5 (8)
P211—As1—Pb28	136.18 (11)	As51—O31—Pb22	79.1 (9)
O38—As1—Pb13	146.4 (10)	Pb29^i—O31—Pb22	92.3 (7)
O210—As1—Pb13	98.1 (8)	Pb28^xi—O31—Pb22	87.9 (7)
O316—As1—Pb13	84.4 (8)	Pb13^xi—O31—Pb22	166.4 (10)
O19—As1—Pb13	35.5 (8)	As51—O31—Pb11	49.1 (7)
Pb12^iii—As1—Pb13	106.00 (11)	Pb29^i—O31—Pb11	78.1 (7)
Pb22^iii—As1—Pb13	137.74 (13)	Pb28^xi—O31—Pb11	152.9 (8)
Pb14^i—As1—Pb13	145.99 (11)	Pb13^xi—O31—Pb11	59.4 (4)
P211—As1—Pb13	69.59 (7)	Pb22—O31—Pb11	115.7 (7)
Pb28—As1—Pb13	73.21 (8)	As51—O32—Pb28	139.4 (14)
O38—As1—Pb29^iii	114.6 (9)	As51—O32—Pb11	103.4 (11)
O210—As1—Pb29^iii	118.5 (8)	Pb28—O32—Pb11	112.6 (11)
O316—As1—Pb29^iii	22.2 (9)	As51—O32—Pb29^i	83.8 (10)
O19—As1—Pb29^iii	89.6 (8)	Pb28—O32—Pb29^i	107.2 (9)
Pb12^iii—As1—Pb29^iii	70.36 (8)	Pb11—O32—Pb29^i	99.8 (8)
Pb22^iii—As1—Pb29^iii	75.25 (8)	As51—O32—Pb16	67.8 (9)
Pb14^i—As1—Pb29^iii	130.64 (11)	Pb28—O32—Pb16	79.4 (7)
P211—As1—Pb29^iii	112.79 (11)	Pb11—O32—Pb16	116.5 (8)
Pb28—As1—Pb29^iii	72.39 (8)	Pb29^i—O32—Pb16	137.6 (8)
Pb13—As1—Pb29^iii	68.36 (8)	As51—O32—Pb22	63.5 (8)
O38—As1—Pb11	98.2 (9)	Pb28—O32—Pb22	82.1 (6)
O210—As1—Pb11	95.8 (8)	Pb11—O32—Pb22	165.2 (10)
O316—As1—Pb11	139.5 (8)	Pb29^i—O32—Pb22	73.0 (5)
O19—As1—Pb11	29.2 (8)	Pb16—O32—Pb22	66.5 (4)
Pb12^iii—As1—Pb11	147.04 (11)	As5—O33—Pb16	102.2 (11)
Pb22^iii—As1—Pb11	131.99 (12)	As5—O33—Pb26	142.2 (14)
Pb14^i—As1—Pb11	110.42 (11)	Pb16—O33—Pb26	111.6 (10)
P211—As1—Pb11	73.41 (7)	As5—O33—Pb25^viii	83.7 (9)
Pb28—As1—Pb11	67.30 (7)	Pb16—O33—Pb25^viii	97.5 (8)
Pb13—As1—Pb11	57.16 (6)	Pb26—O33—Pb25^viii	107.5 (8)
Pb29^iii—As1—Pb11	118.76 (11)	As5—O33—Pb11	69.2 (9)
O112—As11—O317	111.8 (13)	Pb16—O33—Pb11	120.6 (8)
O112—As11—O29	112.3 (12)	Pb26—O33—Pb11	79.1 (6)
O317—As11—O29	109.3 (13)	Pb25^viii—O33—Pb11	136.4 (8)
O112—As11—O313	112.6 (13)	As5—O33—P212	63.4 (7)
O317—As11—O313	102.7 (12)	Pb16—O33—P212	162.5 (9)
O29—As11—O313	107.8 (13)	Pb26—O33—P212	85.3 (6)
O112—As11—Pb24	130.5 (9)	Pb25^viii—O33—P212	72.1 (4)
O317—As11—Pb24	58.7 (7)	Pb11—O33—P212	65.5 (4)
O29—As11—Pb24	116.6 (8)	As3—O34—Pb28	116.3 (13)
O313—As11—Pb24	44.3 (9)	As3—O34—Pb22	128.1 (13)
O112—As11—Pb13^i	138.3 (9)	Pb28—O34—Pb22	115.4 (11)
O317—As11—Pb13^i	52.5 (9)	As3—O34—Pb16	87.6 (10)
O29—As11—Pb13^i	57.6 (9)	Pb28—O34—Pb16	96.8 (8)
O313—As11—Pb13^i	108.8 (10)	Pb22—O34—Pb16	91.4 (7)
Pb24—As11—Pb13^i	78.45 (9)	As3—O34—Pb29	84.3 (9)
O112—As11—Pb11^iii	138.7 (10)	Pb28—O34—Pb29	94.8 (8)
O317—As11—Pb11^iii	108.9 (9)	Pb22—O34—Pb29	86.7 (7)
O29—As11—Pb11^iii	44.8 (8)	Pb16—O34—Pb29	168.0 (9)
O313—As11—Pb11^iii	64.1 (10)	As3—O34—Pb17	49.0 (7)
Pb24—As11—Pb11^iii	78.19 (8)	Pb28—O34—Pb17	79.5 (7)
Pb13^i—As11—Pb11^iii	66.51 (8)	Pb22—O34—Pb17	149.7 (9)
O112—As11—Pb29	81.3 (9)	Pb16—O34—Pb17	59.6 (4)
O317—As11—Pb29	113.2 (8)	Pb29—O34—Pb17	119.7 (7)
O29—As11—Pb29	32.9 (8)	As3—O35—Pb22^iv	141.1 (13)
O313—As11—Pb29	133.2 (9)	As3—O35—Pb17	102.8 (12)
Pb24—As11—Pb29	148.14 (13)	Pb22^iv—O35—Pb17	114.6 (10)
Pb13^i—As11—Pb29	74.18 (8)	As3—O35—Pb28	80.6 (9)
Pb11^iii—As11—Pb29	76.18 (8)	Pb22^iv—O35—Pb28	103.8 (9)
O112—As11—Pb12	32.2 (9)	Pb17—O35—Pb28	97.3 (7)
O317—As11—Pb12	88.9 (8)	As3—O35—Pb14	70.4 (8)
O29—As11—Pb12	101.4 (8)	Pb22^iv—O35—Pb14	81.5 (6)
O313—As11—Pb12	142.6 (10)	Pb17—O35—Pb14	120.4 (8)
Pb24—As11—Pb12	135.73 (13)	Pb28—O35—Pb14	136.2 (8)
Pb13^i—As11—Pb12	106.40 (11)	As3—O35—Pb29	62.5 (8)
Pb11^iii—As11—Pb12	144.99 (11)	Pb22^iv—O35—Pb29	82.4 (7)
Pb29—As11—Pb12	69.05 (7)	Pb17—O35—Pb29	161.4 (10)
O112—As11—P210^ii	53.7 (9)	Pb28—O35—Pb29	70.1 (5)
O317—As11—P210^ii	85.5 (9)	Pb14—O35—Pb29	67.5 (4)
O29—As11—P210^ii	163.6 (9)	As31—O36—Pb23^ii	108.3 (12)
O313—As11—P210^ii	74.5 (10)	As31—O36—Pb27	132.7 (13)
Pb24—As11—P210^ii	76.76 (8)	Pb23^ii—O36—Pb27	118.8 (11)
Pb13^i—As11—P210^ii	137.89 (13)	As31—O36—Pb12	82.9 (9)
Pb11^iii—As11—P210^ii	138.15 (12)	Pb23^ii—O36—Pb12	97.2 (7)
Pb29—As11—P210^ii	135.04 (11)	Pb27—O36—Pb12	94.7 (7)
Pb12—As11—P210^ii	71.04 (8)	As31—O36—Pb21^viii	83.1 (8)
O112—As11—Pb14	29.7 (9)	Pb23^ii—O36—Pb21^viii	93.9 (7)
O317—As11—Pb14	141.4 (9)	Pb27—O36—Pb21^viii	89.7 (7)
O29—As11—Pb14	95.3 (9)	Pb12—O36—Pb21^viii	164.3 (8)
O313—As11—Pb14	97.1 (9)	As31—O36—Pb14^xi	47.4 (7)
Pb24—As11—Pb14	134.40 (12)	Pb23^ii—O36—Pb14^xi	72.5 (6)
Pb13^i—As11—Pb14	146.73 (11)	Pb27—O36—Pb14^xi	152.5 (8)
Pb11^iii—As11—Pb14	109.47 (11)	Pb12—O36—Pb14^xi	58.1 (4)
Pb29—As11—Pb14	72.90 (7)	Pb21^viii—O36—Pb14^xi	115.6 (6)
Pb12—As11—Pb14	56.65 (6)	As61—O37—Pb21^iv	141.5 (15)
P210^ii—As11—Pb14	68.34 (7)	As61—O37—Pb17^ix	102.8 (12)
O112—As11—P211^i	88.4 (9)	Pb21^iv—O37—Pb17^ix	112.0 (10)
O317—As11—P211^i	23.4 (9)	As61—O37—Pb27^ix	81.2 (9)
O29—As11—P211^i	119.4 (9)	Pb21^iv—O37—Pb27^ix	111.1 (8)
O313—As11—P211^i	115.4 (9)	Pb17^ix—O37—Pb27^ix	94.7 (8)
Pb24—As11—P211^i	74.96 (8)	As61—O37—Pb23^iii	65.2 (8)
Pb13^i—As11—P211^i	69.18 (8)	Pb21^iv—O37—Pb23^iii	83.0 (7)
Pb11^iii—As11—P211^i	131.65 (11)	Pb17^ix—O37—Pb23^iii	163.9 (10)
Pb29—As11—P211^i	109.27 (11)	Pb27^ix—O37—Pb23^iii	73.6 (5)
Pb12—As11—P211^i	66.71 (7)	As61—O37—Pb15	67.4 (8)
P210^ii—As11—P211^i	71.80 (8)	Pb21^iv—O37—Pb15	80.2 (6)
Pb14—As11—P211^i	118.11 (10)	Pb17^ix—O37—Pb15	121.6 (7)
O323—As2—O319	109.0 (12)	Pb27^ix—O37—Pb15	135.6 (8)
O323—As2—O18	112.1 (12)	Pb23^iii—O37—Pb15	65.2 (4)
O319—As2—O18	111.2 (13)	As1—O38—Pb22^iii	110.5 (13)
O323—As2—O21	102.3 (12)	As1—O38—Pb29^i	130.7 (13)
O319—As2—O21	109.0 (12)	Pb22^iii—O38—Pb29^i	115.1 (9)
O18—As2—O21	112.7 (12)	As1—O38—Pb14^i	92.8 (11)
O323—As2—Pb15^i	50.8 (9)	Pb22^iii—O38—Pb14^i	100.8 (9)
O319—As2—Pb15^i	108.3 (9)	Pb29^i—O38—Pb14^i	96.0 (8)
O18—As2—Pb15^i	140.5 (9)	As1—O38—Pb28	77.7 (10)
O21—As2—Pb15^i	53.9 (7)	Pb22^iii—O38—Pb28	89.1 (8)
O323—As2—P210	67.2 (9)	Pb29^i—O38—Pb28	85.3 (7)
O319—As2—P210	41.9 (9)	Pb14^i—O38—Pb28	168.3 (8)
O18—As2—P210	130.7 (9)	As1—O38—Pb12^iii	51.1 (8)
O21—As2—P210	115.4 (8)	Pb22^iii—O38—Pb12^iii	77.9 (7)
Pb15^i—As2—P210	79.99 (8)	Pb29^i—O38—Pb12^iii	156.3 (9)
O323—As2—Pb18^iii	109.3 (8)	Pb14^i—O38—Pb12^iii	61.2 (5)
O319—As2—Pb18^iii	61.7 (9)	Pb28—O38—Pb12^iii	115.7 (7)
O18—As2—Pb18^iii	137.5 (9)	As61—O39—Pb27^ix	113.8 (14)
O21—As2—Pb18^iii	48.1 (8)	As61—O39—Pb21	129.6 (13)
Pb15^i—As2—Pb18^iii	66.09 (7)	Pb27^ix—O39—Pb21	116.0 (10)
P210—As2—Pb18^iii	74.58 (8)	As61—O39—Pb16^ix	84.6 (10)
O323—As2—P212	113.2 (9)	Pb27^ix—O39—Pb16^ix	100.3 (9)
O319—As2—P212	126.8 (9)	Pb21—O39—Pb16^ix	93.2 (8)
O18—As2—P212	81.0 (9)	As61—O39—Pb23^iii	79.5 (10)
O21—As2—P212	31.9 (7)	Pb27^ix—O39—Pb23^iii	93.3 (8)
Pb15^i—As2—P212	77.14 (8)	Pb21—O39—Pb23^iii	91.0 (8)
P210—As2—P212	147.09 (11)	Pb16^ix—O39—Pb23^iii	162.3 (8)
Pb18^iii—As2—P212	74.65 (8)	As61—O39—Pb17^ix	51.1 (8)
O323—As2—P211	89.4 (9)	Pb27^ix—O39—Pb17^ix	75.6 (7)
O319—As2—P211	72.6 (9)	Pb21—O39—Pb17^ix	151.8 (9)
O18—As2—P211	55.8 (9)	Pb16^ix—O39—Pb17^ix	58.9 (5)
O21—As2—P211	166.6 (7)	Pb23^iii—O39—Pb17^ix	114.7 (7)
Pb15^i—As2—P211	139.06 (13)	As61—O39—Pb18	61.1 (8)
P210—As2—P211	75.07 (8)	Pb27^ix—O39—Pb18	158.0 (10)
Pb18^iii—As2—P211	133.98 (12)	Pb21—O39—Pb18	70.0 (6)
P212—As2—P211	136.57 (10)	Pb16^ix—O39—Pb18	100.4 (6)
O323—As2—Pb13	141.1 (8)	Pb23^iii—O39—Pb18	65.0 (4)
O319—As2—Pb13	95.0 (9)	Pb17^ix—O39—Pb18	109.4 (6)
O18—As2—Pb13	29.0 (9)	As6—O310—Pb25^xx	141.2 (16)
O21—As2—Pb13	97.9 (7)	As6—O310—Pb15^xx	104.4 (13)
Pb15^i—As2—Pb13	147.66 (12)	Pb25^xx—O310—Pb15^xx	112.0 (10)
P210—As2—Pb13	131.02 (12)	As6—O310—P212^xvi	81.7 (10)
Pb18^iii—As2—Pb13	108.91 (11)	Pb25^xx—O310—P212^xvi	107.3 (8)
P212—As2—Pb13	70.92 (8)	Pb15^xx—O310—P212^xvi	95.0 (8)
P211—As2—Pb13	68.72 (7)	As6—O310—Pb26	65.1 (9)
O323—As2—Pb11	86.2 (8)	Pb25^xx—O310—Pb26	81.4 (7)
O319—As2—Pb11	142.2 (9)	Pb15^xx—O310—Pb26	164.4 (10)
O18—As2—Pb11	33.1 (9)	P212^xvi—O310—Pb26	72.5 (5)
O21—As2—Pb11	100.7 (8)	As6—O310—Pb17^xi	68.5 (8)
Pb15^i—As2—Pb11	107.98 (11)	Pb25^xx—O310—Pb17^xi	80.9 (7)
P210—As2—Pb11	138.41 (12)	Pb15^xx—O310—Pb17^xi	121.9 (7)
Pb18^iii—As2—Pb11	146.59 (12)	P212^xvi—O310—Pb17^xi	136.6 (8)
P212—As2—Pb11	72.03 (7)	Pb26—O310—Pb17^xi	66.7 (4)
P211—As2—Pb11	73.23 (7)	As6—O311—P212^xvi	116.6 (14)
Pb13—As2—Pb11	57.39 (6)	As6—O311—Pb25^viii	129.0 (12)
O323—As2—Pb24^i	21.7 (8)	P212^xvi—O311—Pb25^viii	114.4 (10)
O319—As2—Pb24^i	114.0 (9)	As6—O311—Pb18^viii	82.4 (10)
O18—As2—Pb24^i	91.2 (9)	P212^xvi—O311—Pb18^viii	97.3 (9)
O21—As2—Pb24^i	117.6 (8)	Pb25^viii—O311—Pb18^viii	89.7 (7)
Pb15^i—As2—Pb24^i	70.75 (8)	As6—O311—Pb26	83.9 (10)
P210—As2—Pb24^i	75.89 (9)	P212^xvi—O311—Pb26	96.3 (8)
Pb18^iii—As2—Pb24^i	130.85 (10)	Pb25^viii—O311—Pb26	92.4 (8)
P212—As2—Pb24^i	117.37 (11)	Pb18^viii—O311—Pb26	163.9 (8)
P211—As2—Pb24^i	71.99 (8)	As6—O311—Pb16	61.7 (8)
Pb13—As2—Pb24^i	120.14 (9)	P212^xvi—O311—Pb16	161.7 (10)
Pb11—As2—Pb24^i	69.19 (7)	Pb25^viii—O311—Pb16	70.6 (5)
O320—As21—O27	112.8 (12)	Pb18^viii—O311—Pb16	100.4 (6)
O320—As21—O321	103.1 (12)	Pb26—O311—Pb16	65.5 (4)
O27—As21—O321	101.4 (12)	As6—O311—Pb15^xx	49.9 (8)
O320—As21—O12	114.0 (12)	P212^xvi—O311—Pb15^xx	76.5 (7)
O27—As21—O12	111.7 (11)	Pb25^viii—O311—Pb15^xx	147.6 (9)
O321—As21—O12	112.8 (12)	Pb18^viii—O311—Pb15^xx	58.0 (4)
O320—As21—Pb26^iii	54.9 (8)	Pb26—O311—Pb15^xx	117.5 (7)
O27—As21—Pb26^iii	119.0 (7)	Pb16—O311—Pb15^xx	109.2 (6)
O321—As21—Pb26^iii	48.3 (9)	As31—O312—Pb14^xi	104.0 (11)
O12—As21—Pb26^iii	128.1 (9)	As31—O312—Pb27^xi	142.1 (12)
O320—As21—Pb11^iii	48.7 (9)	Pb14^xi—O312—Pb27^xi	108.2 (9)
O27—As21—Pb11^iii	64.4 (8)	As31—O312—Pb23^ii	85.6 (9)
O321—As21—Pb11^iii	107.4 (8)	Pb14^xi—O312—Pb23^ii	98.1 (7)
O12—As21—Pb11^iii	139.4 (9)	Pb27^xi—O312—Pb23^ii	108.6 (8)
Pb26^iii—As21—Pb11^iii	76.39 (8)	As31—O312—Pb17^xi	67.6 (7)
O320—As21—Pb13^i	104.6 (8)	Pb14^xi—O312—Pb17^xi	120.2 (8)
O27—As21—Pb13^i	42.7 (8)	Pb27^xi—O312—Pb17^xi	79.1 (5)
O321—As21—Pb13^i	62.1 (8)	Pb23^ii—O312—Pb17^xi	136.9 (7)
O12—As21—Pb13^i	140.9 (9)	As31—O312—Pb21^viii	64.8 (7)
Pb26^iii—As21—Pb13^i	79.75 (8)	Pb14^xi—O312—Pb21^viii	166.5 (9)
Pb11^iii—As21—Pb13^i	65.79 (7)	Pb27^xi—O312—Pb21^viii	85.0 (6)
O320—As21—Pb24	114.2 (9)	Pb23^ii—O312—Pb21^viii	74.4 (5)
O27—As21—Pb24	30.5 (8)	Pb17^xi—O312—Pb21^viii	63.9 (3)
O321—As21—Pb24	127.3 (9)	As11—O313—Pb24	106.9 (13)
O12—As21—Pb24	85.0 (9)	As11—O313—P211^iii	132.7 (13)
Pb26^iii—As21—Pb24	146.81 (11)	Pb24—O313—P211^iii	118.5 (10)
Pb11^iii—As21—Pb24	75.30 (8)	As11—O313—Pb11^iii	87.6 (10)
Pb13^i—As21—Pb24	73.07 (8)	Pb24—O313—Pb11^iii	100.2 (9)
O320—As21—Pb15	94.1 (8)	P211^iii—O313—Pb11^iii	96.7 (8)
O27—As21—Pb15	101.4 (8)	As11—O313—P210^ii	79.2 (10)
O321—As21—Pb15	143.2 (8)	Pb24—O313—P210^ii	90.1 (8)
O12—As21—Pb15	31.0 (9)	P211^iii—O313—P210^ii	87.6 (7)
Pb26^iii—As21—Pb15	135.43 (12)	Pb11^iii—O313—P210^ii	165.2 (8)
Pb11^iii—As21—Pb15	108.39 (11)	As11—O313—Pb13^i	49.0 (8)
Pb13^i—As21—Pb15	143.76 (12)	Pb24—O313—Pb13^i	73.6 (7)
Pb24—As21—Pb15	70.96 (8)	P211^iii—O313—Pb13^i	156.0 (9)
O320—As21—Pb25	86.7 (9)	Pb11^iii—O313—Pb13^i	59.7 (5)
O27—As21—Pb25	159.4 (8)	P210^ii—O313—Pb13^i	114.2 (7)
O321—As21—Pb25	79.2 (8)	As5—O314—Pb25^viii	111.1 (13)
O12—As21—Pb25	51.2 (9)	As5—O314—Pb26^iv	131.3 (14)
Pb26^iii—As21—Pb25	76.92 (9)	Pb25^viii—O314—Pb26^iv	117.1 (10)
Pb11^iii—As21—Pb25	135.48 (12)	As5—O314—Pb17	85.5 (9)
Pb13^i—As21—Pb25	141.07 (13)	Pb25^viii—O314—Pb17	98.2 (8)
Pb24—As21—Pb25	136.17 (10)	Pb26^iv—O314—Pb17	93.7 (7)
Pb15—As21—Pb25	69.47 (7)	As5—O314—P212	84.7 (9)
O320—As21—P212^i	126.7 (8)	Pb25^viii—O314—P212	93.6 (7)
O27—As21—P212^i	99.2 (9)	Pb26^iv—O314—P212	86.2 (7)
O321—As21—P212^i	26.5 (8)	Pb17—O314—P212	166.8 (9)
O12—As21—P212^i	89.8 (9)	As5—O314—Pb16	48.5 (7)
Pb26^iii—As21—P212^i	72.65 (9)	Pb25^viii—O314—Pb16	74.8 (6)
Pb11^iii—As21—P212^i	130.65 (11)	Pb26^iv—O314—Pb16	153.0 (7)
Pb13^i—As21—P212^i	71.54 (8)	Pb17—O314—Pb16	59.8 (4)
Pb24—As21—P212^i	114.78 (12)	P212—O314—Pb16	118.4 (7)
Pb15—As21—P212^i	120.70 (10)	As4—O315—Pb23^ii	134.7 (14)
Pb25—As21—P212^i	71.97 (8)	As4—O315—Pb21^vii	101.0 (11)
O320—As21—Pb18	147.9 (8)	Pb23^ii—O315—Pb21^vii	119.6 (10)
O27—As21—Pb18	88.0 (7)	As4—O315—Pb15^x	91.1 (9)
O321—As21—Pb18	95.8 (9)	Pb23^ii—O315—Pb15^x	100.2 (7)
O12—As21—Pb18	33.9 (8)	Pb21^vii—O315—Pb15^x	99.8 (8)
Pb26^iii—As21—Pb18	136.25 (12)	As4—O315—Pb27	78.0 (8)
Pb11^iii—As21—Pb18	146.59 (12)	Pb23^ii—O315—Pb27	84.8 (6)
Pb13^i—As21—Pb18	107.15 (11)	Pb21^vii—O315—Pb27	86.6 (6)
Pb24—As21—Pb18	71.51 (7)	Pb15^x—O315—Pb27	168.3 (9)
Pb15—As21—Pb18	56.73 (6)	As4—O315—Pb18^vii	49.2 (7)
Pb25—As21—Pb18	71.50 (7)	Pb23^ii—O315—Pb18^vii	159.9 (8)
P212^i—As21—Pb18	69.29 (7)	Pb21^vii—O315—Pb18^vii	71.0 (6)
O111—As3—O35	109.9 (13)	Pb15^x—O315—Pb18^vii	60.1 (4)
O111—As3—O26	111.6 (12)	Pb27—O315—Pb18^vii	113.9 (6)
O35—As3—O26	108.1 (12)	As1—O316—Pb29^iii	141.7 (14)
O111—As3—O34	111.2 (13)	As1—O316—Pb12^iii	100.9 (11)
O35—As3—O34	108.5 (13)	Pb29^iii—O316—Pb12^iii	114.8 (9)
O26—As3—O34	107.4 (12)	As1—O316—Pb22^iii	81.9 (8)
O111—As3—Pb17	139.3 (10)	Pb29^iii—O316—Pb22^iii	105.6 (7)
O35—As3—Pb17	48.4 (9)	Pb12^iii—O316—Pb22^iii	97.4 (7)
O26—As3—Pb17	61.8 (8)	As1—O316—Pb13	70.1 (7)
O34—As3—Pb17	108.8 (9)	Pb29^iii—O316—Pb13	80.6 (6)
O111—As3—Pb28	128.7 (10)	Pb12^iii—O316—Pb13	118.6 (7)
O35—As3—Pb28	71.0 (9)	Pb22^iii—O316—Pb13	137.3 (7)
O26—As3—Pb28	116.5 (7)	As1—O316—Pb28	64.1 (8)
O34—As3—Pb28	37.7 (9)	Pb29^iii—O316—Pb28	82.1 (7)
Pb17—As3—Pb28	81.35 (8)	Pb12^iii—O316—Pb28	162.5 (9)
O111—As3—Pb16	140.5 (9)	Pb22^iii—O316—Pb28	72.4 (4)
O35—As3—Pb16	108.3 (8)	Pb13—O316—Pb28	66.7 (4)
O26—As3—Pb16	45.2 (8)	As11—O317—P211^i	141.6 (13)
O34—As3—Pb16	64.5 (9)	As11—O317—Pb13^i	98.7 (11)
Pb17—As3—Pb16	66.22 (7)	P211^i—O317—Pb13^i	106.1 (8)
Pb28—As3—Pb16	73.83 (8)	As11—O317—Pb24	91.8 (9)
O111—As3—Pb27	82.9 (10)	P211^i—O317—Pb24	111.9 (8)
O35—As3—Pb27	109.7 (9)	Pb13^i—O317—Pb24	99.5 (8)
O26—As3—Pb27	30.8 (7)	As11—O317—P210^ii	70.0 (8)
O34—As3—Pb27	131.0 (9)	P211^i—O317—P210^ii	85.0 (7)
Pb17—As3—Pb27	76.64 (9)	Pb13^i—O317—P210^ii	168.4 (9)
Pb28—As3—Pb27	147.17 (12)	Pb24—O317—P210^ii	78.6 (5)
Pb16—As3—Pb27	75.11 (8)	As11—O317—Pb12	67.0 (7)
O111—As3—Pb29	54.0 (10)	P211^i—O317—Pb12	76.4 (6)
O35—As3—Pb29	93.9 (9)	Pb13^i—O317—Pb12	113.4 (6)
O26—As3—Pb29	157.4 (8)	Pb24—O317—Pb12	142.6 (8)
O34—As3—Pb29	68.7 (9)	P210^ii—O317—Pb12	65.5 (4)
Pb17—As3—Pb29	140.76 (13)	As41—O318—P211^xv	113.8 (14)
Pb28—As3—Pb29	74.77 (8)	As41—O318—P210	129.5 (15)
Pb16—As3—Pb29	132.42 (13)	P211^xv—O318—P210	115.5 (10)
Pb27—As3—Pb29	136.19 (10)	As41—O318—Pb12^xiii	90.6 (10)
O111—As3—Pb14	32.9 (9)	P211^xv—O318—Pb12^xiii	98.6 (9)
O35—As3—Pb14	84.4 (8)	P210—O318—Pb12^xiii	92.4 (7)
O26—As3—Pb14	102.0 (8)	As41—O318—Pb24^i	81.2 (10)
O34—As3—Pb14	141.7 (9)	P211^xv—O318—Pb24^i	91.7 (7)
Pb17—As3—Pb14	106.56 (12)	P210—O318—Pb24^i	87.1 (7)
Pb28—As3—Pb14	138.92 (13)	Pb12^xiii—O318—Pb24^i	168.9 (10)
Pb16—As3—Pb14	146.75 (12)	As41—O318—Pb14^xiv	50.8 (8)
Pb27—As3—Pb14	71.66 (7)	P211^xv—O318—Pb14^xiv	78.7 (7)
Pb29—As3—Pb14	74.71 (7)	P210—O318—Pb14^xiv	151.5 (8)
O111—As3—Pb12	30.5 (9)	Pb12^xiii—O318—Pb14^xiv	60.0 (4)
O35—As3—Pb12	140.1 (8)	Pb24^i—O318—Pb14^xiv	118.4 (7)
O26—As3—Pb12	92.0 (7)	As2—O319—P210	110.9 (13)
O34—As3—Pb12	97.1 (9)	As2—O319—Pb24^iii	131.5 (13)
Pb17—As3—Pb12	147.37 (12)	P210—O319—Pb24^iii	116.2 (10)
Pb28—As3—Pb12	130.20 (13)	As2—O319—Pb18^iii	90.3 (11)
Pb16—As3—Pb12	110.21 (11)	P210—O319—Pb18^iii	97.9 (8)
Pb27—As3—Pb12	71.35 (7)	Pb24^iii—O319—Pb18^iii	94.3 (7)
Pb29—As3—Pb12	67.12 (7)	As2—O319—P211	80.7 (9)
Pb14—As3—Pb12	57.38 (6)	P210—O319—P211	90.4 (8)
O111—As3—Pb22^iv	88.8 (9)	Pb24^iii—O319—P211	87.7 (7)
O35—As3—Pb22^iv	23.0 (8)	Pb18^iii—O319—P211	169.5 (9)
O26—As3—Pb22^iv	126.7 (9)	As2—O319—Pb13	61.7 (8)
O34—As3—Pb22^iv	109.6 (9)	P210—O319—Pb13	154.1 (9)
Pb17—As3—Pb22^iv	70.74 (9)	Pb24^iii—O319—Pb13	70.7 (5)
Pb28—As3—Pb22^iv	76.49 (8)	Pb18^iii—O319—Pb13	106.6 (7)
Pb16—As3—Pb22^iv	130.39 (11)	P211—O319—Pb13	64.4 (4)
Pb27—As3—Pb22^iv	117.55 (12)	As2—O319—Pb15^i	49.8 (7)
Pb29—As3—Pb22^iv	73.64 (8)	P210—O319—Pb15^i	76.9 (6)
Pb14—As3—Pb22^iv	68.98 (8)	Pb24^iii—O319—Pb15^i	153.3 (9)
Pb12—As3—Pb22^iv	119.33 (10)	Pb18^iii—O319—Pb15^i	59.8 (4)
O15—As31—O312	114.3 (12)	P211—O319—Pb15^i	116.5 (7)
O15—As31—O36	107.4 (12)	Pb13—O319—Pb15^i	108.3 (6)
O312—As31—O36	107.4 (11)	As21—O320—Pb11^iii	103.8 (11)
O15—As31—O212	111.9 (11)	As21—O320—Pb26^iii	95.7 (10)
O312—As31—O212	106.0 (12)	Pb11^iii—O320—Pb26^iii	101.7 (7)
O36—As31—O212	109.8 (12)	As21—O320—P212^iii	136.3 (11)
O15—As31—Pb23^ii	130.0 (9)	Pb11^iii—O320—P212^iii	102.9 (8)
O312—As31—Pb23^ii	64.5 (8)	Pb26^iii—O320—P212^iii	111.9 (9)
O36—As31—Pb23^ii	43.2 (8)	As21—O320—Pb25	68.5 (8)
O212—As31—Pb23^ii	116.1 (7)	Pb11^iii—O320—Pb25	172.3 (9)
O15—As31—Pb14^xi	141.1 (9)	Pb26^iii—O320—Pb25	79.5 (6)
O312—As31—Pb14^xi	47.2 (8)	P212^iii—O320—Pb25	83.5 (6)
O36—As31—Pb14^xi	111.0 (8)	As21—O320—Pb15	62.4 (7)
O212—As31—Pb14^xi	60.3 (8)	Pb11^iii—O320—Pb15	114.8 (7)
Pb23^ii—As31—Pb14^xi	77.95 (8)	Pb26^iii—O320—Pb15	140.6 (8)
O15—As31—Pb12	136.6 (9)	P212^iii—O320—Pb15	75.1 (5)
O312—As31—Pb12	107.4 (8)	Pb25—O320—Pb15	62.4 (3)
O36—As31—Pb12	69.1 (8)	As21—O320—Pb13^i	53.1 (7)
O212—As31—Pb12	42.4 (8)	Pb11^iii—O320—Pb13^i	61.8 (5)
Pb23^ii—As31—Pb12	78.40 (8)	Pb26^iii—O320—Pb13^i	74.6 (5)
Pb14^xi—As31—Pb12	66.20 (7)	P212^iii—O320—Pb13^i	164.7 (8)
O15—As31—Pb22	82.5 (9)	Pb25—O320—Pb13^i	111.6 (6)
O312—As31—Pb22	107.3 (8)	Pb15—O320—Pb13^i	109.1 (6)
O36—As31—Pb22	135.4 (9)	As21—O321—P212^i	135.3 (13)
O212—As31—Pb22	32.8 (8)	As21—O321—Pb26^iii	102.5 (12)
Pb23^ii—As31—Pb22	147.44 (11)	P212^i—O321—Pb26^iii	117.3 (10)
Pb14^xi—As31—Pb22	74.98 (8)	As21—O321—Pb13^i	89.2 (10)
Pb12—As31—Pb22	74.35 (8)	P212^i—O321—Pb13^i	101.1 (8)
O15—As31—Pb17^xi	34.0 (9)	Pb26^iii—O321—Pb13^i	101.6 (8)
O312—As31—Pb17^xi	87.0 (7)	As21—O321—Pb25	74.8 (8)
O36—As31—Pb17^xi	138.1 (8)	P212^i—O321—Pb25	88.2 (7)
O212—As31—Pb17^xi	103.1 (8)	Pb26^iii—O321—Pb25	85.8 (6)
Pb23^ii—As31—Pb17^xi	136.02 (12)	Pb13^i—O321—Pb25	163.6 (9)
Pb14^xi—As31—Pb17^xi	107.50 (11)	As21—O321—Pb11^iii	50.7 (7)
Pb12—As31—Pb17^xi	144.67 (12)	P212^i—O321—Pb11^iii	160.2 (9)
Pb22—As31—Pb17^xi	70.55 (7)	Pb26^iii—O321—Pb11^iii	71.1 (6)
O15—As31—Pb21^viii	53.4 (9)	Pb13^i—O321—Pb11^iii	59.1 (4)
O312—As31—Pb21^viii	91.0 (8)	Pb25—O321—Pb11^iii	110.9 (6)
O36—As31—Pb21^viii	70.0 (8)	As41—O322—P210^xi	144.5 (14)
O212—As31—Pb21^viii	161.8 (8)	As41—O322—Pb14^xiv	99.0 (10)
Pb23^ii—As31—Pb21^viii	76.78 (9)	P210^xi—O322—Pb14^xiv	113.7 (10)
Pb14^xi—As31—Pb21^viii	137.58 (12)	As41—O322—P211^xv	82.1 (9)
Pb12—As31—Pb21^viii	138.56 (12)	P210^xi—O322—P211^xv	106.2 (8)
Pb22—As31—Pb21^viii	135.77 (10)	Pb14^xiv—O322—P211^xv	97.0 (8)
Pb17^xi—As31—Pb21^viii	70.66 (7)	As41—O322—Pb18^i	71.1 (9)
O15—As31—Pb27	86.5 (9)	P210^xi—O322—Pb18^i	81.3 (7)
O312—As31—Pb27	134.9 (8)	Pb14^xiv—O322—Pb18^i	117.9 (8)
O36—As31—Pb27	28.3 (8)	P211^xv—O322—Pb18^i	138.3 (8)
O212—As31—Pb27	101.6 (9)	As41—O322—Pb24^i	65.4 (8)
Pb23^ii—As31—Pb27	71.47 (8)	P210^xi—O322—Pb24^i	83.6 (6)
Pb14^xi—As31—Pb27	131.71 (11)	Pb14^xiv—O322—Pb24^i	162.3 (9)
Pb12—As31—Pb27	71.60 (8)	P211^xv—O322—Pb24^i	73.4 (5)
Pb22—As31—Pb27	115.11 (11)	Pb18^i—O322—Pb24^i	66.6 (4)
Pb17^xi—As31—Pb27	120.53 (10)	As2—O323—Pb24^i	143.7 (13)
Pb21^viii—As31—Pb27	69.28 (8)	As2—O323—Pb15^i	100.9 (12)
O15—As31—Pb16	28.6 (9)	Pb24^i—O323—Pb15^i	111.8 (10)
O312—As31—Pb16	142.5 (8)	As2—O323—P210	84.1 (10)
O36—As31—Pb16	96.0 (8)	Pb24^i—O323—P210	106.5 (9)
O212—As31—Pb16	92.6 (7)	Pb15^i—O323—P210	96.7 (7)
Pb23^ii—As31—Pb16	134.87 (12)	As2—O323—P211	66.3 (8)
Pb14^xi—As31—Pb16	146.47 (12)	Pb24^i—O323—P211	83.4 (7)
Pb12—As31—Pb16	108.20 (10)	Pb15^i—O323—P211	163.9 (9)
Pb22—As31—Pb16	71.81 (7)	P210—O323—P211	73.0 (5)
Pb17^xi—As31—Pb16	56.68 (6)	As2—O323—Pb11	69.6 (8)
Pb21^viii—As31—Pb16	69.58 (7)	Pb24^i—O323—Pb11	80.7 (6)
Pb27—As31—Pb16	69.02 (7)	Pb15^i—O323—Pb11	118.9 (8)
O324—As4—O110	115.5 (12)	P210—O323—Pb11	138.4 (8)
O324—As4—O315	105.1 (12)	P211—O323—Pb11	67.2 (4)
O110—As4—O315	113.6 (12)	As4—O324—Pb18^vii	100.7 (10)
O324—As4—O22	105.1 (11)	As4—O324—Pb23^v	139.6 (14)
O110—As4—O22	110.5 (12)	Pb18^vii—O324—Pb23^v	105.6 (9)
O315—As4—O22	106.3 (11)	As4—O324—Pb21^vii	94.7 (10)
O324—As4—Pb21^vii	55.8 (8)	Pb18^vii—O324—Pb21^vii	100.4 (8)
O110—As4—Pb21^vii	132.9 (8)	Pb23^v—O324—Pb21^vii	109.7 (8)
O315—As4—Pb21^vii	49.3 (9)	As4—O324—Pb27	66.8 (8)
O22—As4—Pb21^vii	116.5 (9)	Pb18^vii—O324—Pb27	166.7 (9)
O324—As4—Pb18^vii	50.4 (8)	Pb23^v—O324—Pb27	87.3 (6)
O110—As4—Pb18^vii	138.1 (8)	Pb21^vii—O324—Pb27	77.1 (5)
O315—As4—Pb18^vii	108.3 (9)	As4—O324—Pb14	65.5 (8)
O22—As4—Pb18^vii	55.6 (8)	Pb18^vii—O324—Pb14	115.6 (7)
Pb21^vii—As4—Pb18^vii	76.67 (9)	Pb23^v—O324—Pb14	75.5 (6)
O324—As4—Pb15^x	106.1 (9)	Pb21^vii—O324—Pb14	141.0 (8)
O110—As4—Pb15^x	137.5 (8)	Pb27—O324—Pb14	64.4 (4)

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

(Mim173K)

Crystal data

As4Cl1.33O16Pb6.67	F(000) = 2488
Mr = 1984.21	Dx = 7.322 Mg m^−3
Monoclinic, P1121/b	Ag Kα radiation, λ = 0.56087 Å
a = 10.2378 (3) Å	Cell parameters from 17310 reflections
b = 20.4573 (7) Å	θ = 1.8–29.4°
c = 7.4457 (2) Å	µ = 37.69 mm^−1
β = 90°	T = 288 K
V = 1349.96 (9) Å^3	Fragment, pale-orange
Z = 3	0.10 × 0.06 × 0.04 mm

Data collection

XtaLAB Synergy, Dualflex, Hypix diffractometer	5136 independent reflections
Radiation source: micro-focus sealed X-ray tube	4525 reflections with I > 2σ(I)
Detector resolution: 10.000 pixels mm^-1	Rint = 0.046
o scan	θmax = 25.6°, θmin = 1.8°
Absorption correction: multi-scan SCALE 3 ABSPACK	h = −15→15
Tmin = 0.376, Tmax = 1.00	k = −31→31
22378 measured reflections	l = −11→11

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.039	Secondary atom site location: Difmap
wR(F^2) = 0.086	w = 1/[σ^2(Fo^2) + (0.0142P)^2 + 76.360P] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max = 0.001
5136 reflections	Δρmax = 4.44 e Å^−3
192 parameters	Δρmin = −5.28 e Å^−3

Special details

Experimental. CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pb1A	0.67171 (4)	0.41433 (2)	0.00758 (5)	0.00962 (8)
Pb1B	0.33841 (4)	0.58049 (2)	0.50637 (5)	0.00904 (7)
Pb2A	0.00320 (4)	0.37496 (2)	0.23784 (5)	0.01039 (11)	0.993 (3)
Pb2B	0.24970 (4)	0.37335 (2)	0.74304 (6)	0.01133 (8)
Pb2C	0.24669 (4)	0.74878 (2)	0.27201 (5)	0.00880 (7)
AsA	0.38556 (11)	0.45478 (5)	0.25233 (13)	0.00502 (16)
AsB	0.40951 (11)	0.26187 (5)	0.75359 (13)	0.00529 (16)
AsC	0.02343 (11)	0.55758 (5)	0.24594 (12)	0.00474 (16)
O1A	0.4937 (9)	0.4140 (4)	0.2474 (10)	0.0096 (13)
O1B	0.3269 (9)	0.6663 (4)	0.7503 (10)	0.0103 (13)
O1C	0.8333 (8)	0.5036 (4)	0.2509 (10)	0.0080 (12)
O2A	0.4877 (9)	0.5489 (4)	0.2195 (12)	0.0138 (15)
O2B	0.6016 (18)	0.3060 (9)	0.721 (2)	0.013 (3)*	0.54 (2)
O2B1	0.4065 (18)	0.1968 (9)	0.292 (2)	0.013 (3)*	0.54 (2)
O2C	0.1088 (9)	0.5059 (4)	0.2825 (11)	0.0131 (14)
O3A	0.2495 (9)	0.4183 (5)	0.0944 (11)	0.0136 (15)
O3B	0.666 (3)	0.7071 (10)	0.085 (2)	0.018 (3)	0.523 (17)
O3B1	0.604 (3)	0.7094 (11)	0.046 (3)	0.018 (3)	0.477 (17)
O3C	0.0847 (10)	0.6001 (5)	0.0444 (11)	0.0163 (16)
O3D	0.2985 (10)	0.4430 (5)	0.4542 (11)	0.0154 (16)
O3E	0.663 (2)	0.7075 (9)	0.398 (2)	0.011 (2)*	0.523 (17)
O3E1	0.385 (2)	0.2994 (9)	0.556 (2)	0.011 (2)*	0.477 (17)
O3F	0.0870 (11)	0.6260 (5)	0.4033 (11)	0.0176 (17)
Cl	0.0080 (3)	0.24987 (15)	0.4909 (3)	0.0138 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1A	0.01215 (16)	0.01590 (16)	0.00455 (13)	0.00983 (14)	−0.00073 (11)	−0.00077 (11)
Pb1B	0.01191 (16)	0.01350 (15)	0.00450 (13)	0.00844 (13)	0.00023 (11)	0.00038 (11)
Pb2A	0.00828 (17)	0.00731 (16)	0.01649 (19)	0.00459 (12)	0.00143 (12)	0.00215 (12)
Pb2B	0.00617 (14)	0.00727 (14)	0.01954 (17)	0.00262 (11)	0.00056 (12)	0.00194 (12)
Pb2C	0.00615 (14)	0.00901 (14)	0.01116 (14)	0.00373 (11)	−0.00139 (11)	0.00213 (11)
AsA	0.0040 (4)	0.0059 (4)	0.0053 (3)	0.0026 (3)	0.0001 (3)	0.0002 (3)
AsB	0.0049 (4)	0.0052 (4)	0.0058 (4)	0.0026 (3)	0.0004 (3)	−0.0003 (3)
AsC	0.0041 (4)	0.0047 (3)	0.0051 (4)	0.0020 (3)	0.0007 (3)	0.0003 (3)
O1A	0.009 (3)	0.014 (3)	0.009 (3)	0.008 (3)	0.001 (2)	0.003 (3)
O1B	0.014 (3)	0.006 (3)	0.012 (3)	0.005 (3)	0.000 (3)	−0.004 (2)
O1C	0.004 (3)	0.009 (3)	0.008 (3)	0.001 (2)	0.001 (2)	0.002 (2)
O2A	0.010 (3)	0.009 (3)	0.020 (4)	0.003 (3)	0.003 (3)	0.004 (3)
O2C	0.012 (3)	0.011 (3)	0.019 (4)	0.007 (3)	−0.003 (3)	0.002 (3)
O3A	0.010 (3)	0.019 (4)	0.012 (3)	0.006 (3)	−0.006 (3)	−0.006 (3)
O3B	0.037 (10)	0.012 (4)	0.013 (6)	0.018 (6)	0.014 (6)	0.004 (4)
O3B1	0.037 (10)	0.012 (4)	0.013 (6)	0.018 (6)	0.014 (6)	0.004 (4)
O3C	0.012 (4)	0.026 (4)	0.014 (3)	0.012 (3)	0.008 (3)	0.012 (3)
O3D	0.021 (4)	0.017 (4)	0.015 (3)	0.014 (3)	0.010 (3)	0.008 (3)
O3F	0.020 (4)	0.012 (3)	0.014 (4)	0.003 (3)	0.005 (3)	−0.007 (3)
Cl	0.0131 (10)	0.0132 (10)	0.0112 (10)	0.0038 (8)	0.0028 (8)	−0.0013 (8)

Geometric parameters (Å, º)

Pb1A—O1B^i	2.449 (8)	Pb2C—O3E^vii	8.234 (15)
Pb1A—O1C	2.515 (7)	AsA—O3A	1.685 (8)
Pb1A—O1A	2.549 (8)	AsA—O2A	1.687 (8)
Pb1A—O2B1^ii	2.562 (16)	AsA—O1A	1.688 (8)
Pb1A—O3C^iii	2.682 (9)	AsA—O3D	1.702 (8)
Pb1A—O2A^iii	2.704 (9)	AsB—O3B1^i	1.637 (19)
Pb1A—O3B1^iii	2.72 (2)	AsB—O3E^i	1.640 (16)
Pb1A—O2C^iii	2.951 (9)	AsB—O2B1^ix	1.659 (16)
Pb1A—O3B^iii	3.16 (2)	AsB—O1B^x	1.697 (7)
Pb1A—O3A^iii	3.191 (9)	AsB—O3B^i	1.711 (17)
Pb1A—Pb1B^i	3.6235 (5)	AsB—O2B	1.721 (16)
Pb1B—O1A^i	2.477 (8)	AsB—O3E1	1.737 (17)
Pb1B—O1C^i	2.508 (7)	AsC—O3F	1.685 (8)
Pb1B—O1B	2.570 (7)	AsC—O3C	1.690 (8)
Pb1B—O2C	2.653 (8)	AsC—O1C^xi	1.691 (7)
Pb1B—O3D	2.660 (8)	AsC—O2C	1.699 (8)
Pb1B—O2B^i	2.686 (16)	O1A—Pb1B^i	2.477 (7)
Pb1B—O3E1^i	2.702 (19)	O1B—AsB^xii	1.697 (7)
Pb1B—O2A	2.881 (9)	O1B—Pb1A^i	2.449 (8)
Pb1B—O3E	3.129 (18)	O1C—AsC^xiii	1.691 (7)
Pb1B—O3F	3.237 (11)	O1C—Pb1B^i	2.508 (7)
Pb1B—Pb1A^i	3.6235 (5)	O2A—Pb2B^i	2.357 (8)
Pb2A—O2C	2.356 (8)	O2A—Pb1A^iii	2.704 (9)
Pb2A—O3C^iv	2.438 (8)	O2B—O2B1^ix	0.530 (18)
Pb2A—O3A	2.459 (9)	O2B—Pb2C^i	2.328 (16)
Pb2A—O3F^v	2.824 (8)	O2B—Pb1B^i	2.686 (16)
Pb2A—O1B^v	3.047 (8)	O2B1—O2B^ii	0.530 (18)
Pb2A—O3D	3.075 (10)	O2B1—AsB^ii	1.659 (16)
Pb2A—Cl	3.198 (3)	O2B1—Pb2C^xiv	2.403 (16)
Pb2B—O2A^i	2.357 (8)	O2B1—Pb1A^ix	2.562 (16)
Pb2B—O3E^i	2.475 (17)	O3B—O3B1	0.72 (3)
Pb2B—O3D	2.489 (8)	O3B—AsB^i	1.711 (17)
Pb2B—O3B^i	2.55 (2)	O3B—Pb2C^xv	2.500 (17)
Pb2B—O3A^vi	2.773 (8)	O3B—Pb2B^i	2.55 (2)
Pb2B—O1C^i	3.034 (8)	O3B1—AsB^i	1.637 (19)
Pb2B—Cl	3.126 (3)	O3B1—Pb2C^xv	2.432 (19)
Pb2C—O2B^i	2.328 (16)	O3B1—Pb1A^iii	2.72 (2)
Pb2C—O2B1^vii	2.403 (16)	O3C—Pb2A^iv	2.438 (8)
Pb2C—O3F	2.414 (9)	O3C—Pb1A^iii	2.682 (9)
Pb2C—O3B1^viii	2.432 (19)	O3E—O3E1^i	0.556 (19)
Pb2C—O3B^viii	2.500 (17)	O3E—AsB^i	1.640 (16)
Pb2C—O3E1^vii	2.749 (17)	O3E—Pb2B^i	2.475 (17)
Pb2C—O1A^vii	3.047 (8)	O3E1—O3E^i	0.556 (19)
Pb2C—O3C	3.134 (10)	O3E1—Pb1B^i	2.702 (19)
Pb2C—Cl^vii	3.140 (3)	O3E1—Pb2C^xiv	2.749 (17)
O1B^i—Pb1A—O1C	74.7 (2)	O1C^i—Pb2B—Cl	104.02 (15)
O1B^i—Pb1A—O1A	74.2 (3)	O2B^i—Pb2C—O2B1^vii	12.7 (4)
O1C—Pb1A—O1A	73.0 (2)	O2B^i—Pb2C—O3F	76.0 (5)
O1B^i—Pb1A—O2B1^ii	88.2 (4)	O2B1^vii—Pb2C—O3F	82.9 (4)
O1C—Pb1A—O2B1^ii	153.5 (4)	O2B^i—Pb2C—O3B1^viii	72.4 (7)
O1A—Pb1A—O2B1^ii	122.1 (4)	O2B1^vii—Pb2C—O3B1^viii	82.8 (7)
O1B^i—Pb1A—O3C^iii	73.3 (3)	O3F—Pb2C—O3B1^viii	90.3 (5)
O1C—Pb1A—O3C^iii	82.8 (3)	O2B^i—Pb2C—O3B^viii	87.1 (6)
O1A—Pb1A—O3C^iii	143.5 (2)	O2B1^vii—Pb2C—O3B^viii	98.3 (6)
O2B1^ii—Pb1A—O3C^iii	72.9 (4)	O3F—Pb2C—O3B^viii	86.1 (5)
O1B^i—Pb1A—O2A^iii	148.8 (3)	O3B1^viii—Pb2C—O3B^viii	16.8 (6)
O1C—Pb1A—O2A^iii	121.2 (2)	O2B^i—Pb2C—O3E1^vii	81.8 (6)
O1A—Pb1A—O2A^iii	84.8 (2)	O2B1^vii—Pb2C—O3E1^vii	69.8 (6)
O2B1^ii—Pb1A—O2A^iii	83.7 (4)	O3F—Pb2C—O3E1^vii	134.7 (4)
O3C^iii—Pb1A—O2A^iii	131.6 (3)	O3B1^viii—Pb2C—O3E1^vii	119.7 (8)
O1B^i—Pb1A—O3B1^iii	80.4 (5)	O3B^viii—Pb2C—O3E1^vii	131.9 (7)
O1C—Pb1A—O3B1^iii	141.3 (4)	O2B^i—Pb2C—O1A^vii	98.7 (4)
O1A—Pb1A—O3B1^iii	72.1 (4)	O2B1^vii—Pb2C—O1A^vii	96.4 (4)
O2B1^ii—Pb1A—O3B1^iii	50.5 (5)	O3F—Pb2C—O1A^vii	158.0 (3)
O3C^iii—Pb1A—O3B1^iii	117.8 (5)	O3B1^viii—Pb2C—O1A^vii	67.8 (5)
O2A^iii—Pb1A—O3B1^iii	71.2 (5)	O3B^viii—Pb2C—O1A^vii	72.3 (5)
O1B^i—Pb1A—O2C^iii	130.7 (3)	O3E1^vii—Pb2C—O1A^vii	63.6 (4)
O1C—Pb1A—O2C^iii	94.8 (2)	O2B^i—Pb2C—O3C	72.6 (4)
O1A—Pb1A—O2C^iii	149.3 (2)	O2B1^vii—Pb2C—O3C	67.0 (4)
O2B1^ii—Pb1A—O2C^iii	81.1 (4)	O3F—Pb2C—O3C	57.0 (2)
O3C^iii—Pb1A—O2C^iii	57.5 (2)	O3B1^viii—Pb2C—O3C	136.8 (5)
O2A^iii—Pb1A—O2C^iii	77.7 (2)	O3B^viii—Pb2C—O3C	140.8 (4)
O3B1^iii—Pb1A—O2C^iii	123.8 (4)	O3E1^vii—Pb2C—O3C	78.9 (4)
O1B^i—Pb1A—O3B^iii	90.3 (4)	O1A^vii—Pb2C—O3C	142.5 (2)
O1C—Pb1A—O3B^iii	142.3 (3)	O2B^i—Pb2C—Cl^vii	136.6 (4)
O1A—Pb1A—O3B^iii	69.7 (3)	O2B1^vii—Pb2C—Cl^vii	125.8 (4)
O2B1^ii—Pb1A—O3B^iii	55.4 (5)	O3F—Pb2C—Cl^vii	97.8 (3)
O3C^iii—Pb1A—O3B^iii	126.4 (4)	O3B1^viii—Pb2C—Cl^vii	151.0 (5)
O2A^iii—Pb1A—O3B^iii	60.5 (4)	O3B^viii—Pb2C—Cl^vii	135.9 (5)
O3B1^iii—Pb1A—O3B^iii	11.1 (5)	O3E1^vii—Pb2C—Cl^vii	72.6 (4)
O2C^iii—Pb1A—O3B^iii	120.3 (3)	O1A^vii—Pb2C—Cl^vii	100.33 (15)
O1B^i—Pb1A—O3A^iii	144.5 (2)	O3C—Pb2C—Cl^vii	68.54 (16)
O1C—Pb1A—O3A^iii	70.8 (2)	O2B^i—Pb2C—O3E^vii	117.6 (4)
O1A—Pb1A—O3A^iii	88.0 (2)	O2B1^vii—Pb2C—O3E^vii	113.3 (4)
O2B1^ii—Pb1A—O3A^iii	127.0 (4)	O3F—Pb2C—O3E^vii	160.6 (2)
O3C^iii—Pb1A—O3A^iii	109.5 (2)	O3B1^viii—Pb2C—O3E^vii	81.5 (5)
O2A^iii—Pb1A—O3A^iii	54.3 (2)	O3B^viii—Pb2C—O3E^vii	81.1 (4)
O3B1^iii—Pb1A—O3A^iii	123.5 (5)	O3E1^vii—Pb2C—O3E^vii	63.8 (4)
O2C^iii—Pb1A—O3A^iii	61.2 (2)	O1A^vii—Pb2C—O3E^vii	19.9 (2)
O3B^iii—Pb1A—O3A^iii	112.4 (4)	O3C—Pb2C—O3E^vii	138.00 (19)
O1B^i—Pb1A—Pb1B^i	45.12 (17)	Cl^vii—Pb2C—O3E^vii	81.75 (14)
O1C—Pb1A—Pb1B^i	43.75 (16)	O3A—AsA—O2A	107.9 (4)
O1A—Pb1A—Pb1B^i	43.08 (17)	O3A—AsA—O1A	111.6 (4)
O2B1^ii—Pb1A—Pb1B^i	130.6 (4)	O2A—AsA—O1A	112.1 (4)
O3C^iii—Pb1A—Pb1B^i	100.90 (18)	O3A—AsA—O3D	107.2 (4)
O2A^iii—Pb1A—Pb1B^i	125.90 (19)	O2A—AsA—O3D	105.7 (4)
O3B1^iii—Pb1A—Pb1B^i	98.1 (4)	O1A—AsA—O3D	112.1 (4)
O2C^iii—Pb1A—Pb1B^i	137.73 (16)	O3B1^i—AsB—O3E^i	111.0 (10)
O3B^iii—Pb1A—Pb1B^i	101.9 (3)	O3B1^i—AsB—O2B1^ix	86.4 (11)
O3A^iii—Pb1A—Pb1B^i	101.64 (14)	O3E^i—AsB—O2B1^ix	122.6 (8)
O1A^i—Pb1B—O1C^i	74.3 (2)	O3B1^i—AsB—O1B^x	110.2 (7)
O1A^i—Pb1B—O1B	73.4 (3)	O3E^i—AsB—O1B^x	111.6 (6)
O1C^i—Pb1B—O1B	72.7 (2)	O2B1^ix—AsB—O1B^x	112.0 (6)
O1A^i—Pb1B—O2C	152.3 (2)	O3B1^i—AsB—O3B^i	24.8 (9)
O1C^i—Pb1B—O2C	86.7 (2)	O3E^i—AsB—O3B^i	88.2 (10)
O1B—Pb1B—O2C	120.4 (3)	O2B1^ix—AsB—O3B^i	107.4 (10)
O1A^i—Pb1B—O3D	83.8 (3)	O1B^x—AsB—O3B^i	112.4 (7)
O1C^i—Pb1B—O3D	72.3 (2)	O3B1^i—AsB—O2B	102.6 (11)
O1B—Pb1B—O3D	142.2 (2)	O3E^i—AsB—O2B	108.6 (8)
O2C—Pb1B—O3D	71.1 (3)	O2B1^ix—AsB—O2B	17.9 (6)
O1A^i—Pb1B—O2B^i	125.1 (4)	O1B^x—AsB—O2B	112.5 (6)
O1C^i—Pb1B—O2B^i	145.7 (4)	O3B^i—AsB—O2B	120.8 (9)
O1B—Pb1B—O2B^i	85.7 (4)	O3B1^i—AsB—O3E1	124.0 (10)
O2C—Pb1B—O2B^i	81.6 (4)	O3E^i—AsB—O3E1	18.7 (7)
O3D—Pb1B—O2B^i	132.0 (4)	O2B1^ix—AsB—O3E1	107.4 (9)
O1A^i—Pb1B—O3E1^i	72.4 (4)	O1B^x—AsB—O3E1	113.3 (6)
O1C^i—Pb1B—O3E1^i	143.4 (4)	O3B^i—AsB—O3E1	103.9 (10)
O1B—Pb1B—O3E1^i	83.4 (4)	O2B—AsB—O3E1	91.7 (9)
O2C—Pb1B—O3E1^i	129.7 (4)	O3F—AsC—O3C	107.5 (5)
O3D—Pb1B—O3E1^i	118.2 (4)	O3F—AsC—O1C^xi	111.6 (4)
O2B^i—Pb1B—O3E1^i	54.8 (5)	O3C—AsC—O1C^xi	111.4 (4)
O1A^i—Pb1B—O2A	97.2 (3)	O3F—AsC—O2C	107.5 (5)
O1C^i—Pb1B—O2A	130.5 (2)	O3C—AsC—O2C	106.8 (4)
O1B—Pb1B—O2A	152.6 (2)	O1C^xi—AsC—O2C	111.9 (4)
O2C—Pb1B—O2A	79.7 (3)	AsA—O1A—Pb1B^i	125.0 (4)
O3D—Pb1B—O2A	58.2 (2)	AsA—O1A—Pb1A	131.2 (4)
O2B^i—Pb1B—O2A	78.9 (4)	Pb1B^i—O1A—Pb1A	92.3 (3)
O3E1^i—Pb1B—O2A	69.2 (4)	AsB^xii—O1B—Pb1A^i	128.4 (4)
O1A^i—Pb1B—O3E	74.2 (3)	AsB^xii—O1B—Pb1B	127.4 (4)
O1C^i—Pb1B—O3E	147.5 (3)	Pb1A^i—O1B—Pb1B	92.4 (2)
O1B—Pb1B—O3E	90.4 (4)	AsC^xiii—O1C—Pb1B^i	130.3 (4)
O2C—Pb1B—O3E	125.6 (3)	AsC^xiii—O1C—Pb1A	125.6 (4)
O3D—Pb1B—O3E	112.2 (4)	Pb1B^i—O1C—Pb1A	92.3 (2)
O2B^i—Pb1B—O3E	55.4 (4)	AsA—O2A—Pb2B^i	126.8 (5)
O3E1^i—Pb1B—O3E	7.0 (5)	AsA—O2A—Pb1A^iii	107.0 (4)
O2A—Pb1B—O3E	62.2 (3)	Pb2B^i—O2A—Pb1A^iii	122.0 (3)
O1A^i—Pb1B—O3F	142.8 (2)	AsA—O2A—Pb1B	93.1 (3)
O1C^i—Pb1B—O3F	89.0 (2)	Pb2B^i—O2A—Pb1B	108.4 (3)
O1B—Pb1B—O3F	69.9 (2)	Pb1A^iii—O2A—Pb1B	86.6 (2)
O2C—Pb1B—O3F	54.1 (2)	O2B1^ix—O2B—AsB	74 (3)
O3D—Pb1B—O3F	123.1 (3)	O2B1^ix—O2B—Pb2C^i	92 (3)
O2B^i—Pb1B—O3F	58.2 (4)	AsB—O2B—Pb2C^i	127.4 (8)
O3E1^i—Pb1B—O3F	108.7 (4)	O2B1^ix—O2B—Pb1B^i	132 (3)
O2A—Pb1B—O3F	118.4 (2)	AsB—O2B—Pb1B^i	104.4 (7)
O3E—Pb1B—O3F	111.5 (3)	Pb2C^i—O2B—Pb1B^i	120.7 (7)
O1A^i—Pb1B—Pb1A^i	44.66 (18)	O2B^ii—O2B1—AsB^ii	88 (3)
O1C^i—Pb1B—Pb1A^i	43.91 (17)	O2B^ii—O2B1—Pb2C^xiv	75 (3)
O1B—Pb1B—Pb1A^i	42.48 (18)	AsB^ii—O2B1—Pb2C^xiv	126.3 (8)
O2C—Pb1B—Pb1A^i	127.89 (19)	O2B^ii—O2B1—Pb1A^ix	124 (3)
O3D—Pb1B—Pb1A^i	100.68 (18)	AsB^ii—O2B1—Pb1A^ix	109.3 (8)
O2B^i—Pb1B—Pb1A^i	127.1 (3)	Pb2C^xiv—O2B1—Pb1A^ix	122.5 (6)
O3E1^i—Pb1B—Pb1A^i	100.1 (4)	AsC—O2C—Pb2A	126.8 (4)
O2A—Pb1B—Pb1A^i	140.63 (17)	AsC—O2C—Pb1B	109.0 (4)
O3E—Pb1B—Pb1A^i	105.4 (3)	Pb2A—O2C—Pb1B	120.9 (3)
O3F—Pb1B—Pb1A^i	100.96 (14)	AsA—O3A—Pb2A	109.1 (4)
O2C—Pb2A—O3C^iv	83.8 (3)	O3B1—O3B—AsB^i	72 (2)
O2C—Pb2A—O3A	81.2 (3)	O3B1—O3B—Pb2C^xv	76 (2)
O3C^iv—Pb2A—O3A	88.3 (3)	AsB^i—O3B—Pb2C^xv	131.8 (9)
O2C—Pb2A—O3F^v	80.6 (3)	O3B1—O3B—Pb2B^i	147 (3)
O3C^iv—Pb2A—O3F^v	131.5 (3)	AsB^i—O3B—Pb2B^i	104.4 (8)
O3A—Pb2A—O3F^v	133.3 (3)	Pb2C^xv—O3B—Pb2B^i	121.6 (7)
O2C—Pb2A—O1B^v	97.2 (2)	O3B—O3B1—AsB^i	83 (2)
O3C^iv—Pb2A—O1B^v	67.0 (2)	O3B—O3B1—Pb2C^xv	87 (2)
O3A—Pb2A—O1B^v	155.1 (2)	AsB^i—O3B1—Pb2C^xv	142.2 (12)
O3F^v—Pb2A—O1B^v	69.9 (3)	O3B—O3B1—Pb1A^iii	122 (3)
O2C—Pb2A—O3D	67.9 (2)	AsB^i—O3B1—Pb1A^iii	103.5 (10)
O3C^iv—Pb2A—O3D	137.6 (3)	Pb2C^xv—O3B1—Pb1A^iii	112.5 (8)
O3A—Pb2A—O3D	57.7 (2)	AsC—O3C—Pb2A^iv	142.4 (5)
O3F^v—Pb2A—O3D	75.6 (3)	AsC—O3C—Pb1A^iii	101.4 (4)
O1B^v—Pb2A—O3D	144.4 (2)	Pb2A^iv—O3C—Pb1A^iii	111.1 (3)
O2C—Pb2A—Cl	130.1 (2)	AsC—O3C—Pb2C	84.2 (4)
O3C^iv—Pb2A—Cl	146.1 (2)	Pb2A^iv—O3C—Pb2C	109.5 (3)
O3A—Pb2A—Cl	96.9 (2)	Pb1A^iii—O3C—Pb2C	96.6 (3)
O3F^v—Pb2A—Cl	64.7 (2)	AsA—O3D—Pb2B	141.7 (5)
O1B^v—Pb2A—Cl	102.71 (15)	AsA—O3D—Pb1B	100.8 (4)
O3D—Pb2A—Cl	69.41 (16)	Pb2B—O3D—Pb1B	111.1 (3)
O2A^i—Pb2B—O3E^i	80.1 (4)	AsA—O3D—Pb2A	85.9 (3)
O2A^i—Pb2B—O3D	83.2 (3)	Pb2B—O3D—Pb2A	108.9 (3)
O3E^i—Pb2B—O3D	88.8 (4)	Pb1B—O3D—Pb2A	98.7 (3)
O2A^i—Pb2B—O3B^i	74.7 (5)	O3E1^i—O3E—AsB^i	91 (3)
O3E^i—Pb2B—O3B^i	55.2 (5)	O3E1^i—O3E—Pb2B^i	131 (3)
O3D—Pb2B—O3B^i	140.0 (4)	AsB^i—O3E—Pb2B^i	110.2 (8)
O2A^i—Pb2B—O3A^vi	81.7 (3)	O3E1^i—O3E—Pb1B	36 (2)
O3E^i—Pb2B—O3A^vi	133.1 (4)	AsB^i—O3E—Pb1B	90.0 (7)
O3D—Pb2B—O3A^vi	131.2 (3)	Pb2B^i—O3E—Pb1B	98.2 (5)
O3B^i—Pb2B—O3A^vi	78.4 (4)	O3E^i—O3E1—AsB	71 (3)
O2A^i—Pb2B—O1C^i	97.9 (2)	O3E^i—O3E1—Pb1B^i	137 (3)
O3E^i—Pb2B—O1C^i	155.0 (4)	AsB—O3E1—Pb1B^i	103.3 (8)
O3D—Pb2B—O1C^i	66.2 (2)	O3E^i—O3E1—Pb2C^xiv	103 (3)
O3B^i—Pb2B—O1C^i	148.6 (4)	AsB—O3E1—Pb2C^xiv	138.4 (8)
O3A^vi—Pb2B—O1C^i	70.3 (2)	Pb1B^i—O3E1—Pb2C^xiv	107.4 (6)
O2A^i—Pb2B—Cl	142.2 (2)	AsC—O3F—Pb2C	111.2 (4)
O3E^i—Pb2B—Cl	67.0 (4)	AsC—O3F—Pb1B	87.6 (4)
O3D—Pb2B—Cl	78.1 (2)	Pb2C—O3F—Pb1B	100.0 (3)
O3B^i—Pb2B—Cl	99.6 (5)	Pb2B—Cl—Pb2A	91.73 (7)
O3A^vi—Pb2B—Cl	134.65 (18)

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

(Mim273K)

Crystal data

As3ClO12Pb5	F(000) = 2488
Mr = 1488.16	Dx = 7.300 Mg m^−3
Monoclinic, P1121/b	Ag Kα radiation, λ = 0.56087 Å
a = 10.2398 (4) Å	Cell parameters from 14002 reflections
b = 20.4774 (9) Å	θ = 3.1–28.9°
c = 7.4554 (3) Å	µ = 37.57 mm^−1
β = 90°	T = 273 K
V = 1354.10 (12) Å^3	Fragment, pale-orange
Z = 4	0.10 × 0.06 × 0.04 mm

Data collection

XtaLAB Synergy, Dualflex, Hypix diffractometer	4531 reflections with I > 2σ(I)
Radiation source: micro-focus sealed X-ray tube	Rint = 0.047
o scan	θmax = 26.4°, θmin = 1.8°
Absorption correction: multi-scan SCALE 3 ABSPACK	h = −16→16
Tmin = 0.433, Tmax = 1.000	k = −32→32
27265 measured reflections	l = −10→11
5414 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.032	Secondary atom site location: difference Fourier map
wR(F^2) = 0.071	w = 1/[σ^2(Fo^2) + (0.0218P)^2 + 19.508P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
5414 reflections	Δρmax = 2.96 e Å^−3
190 parameters	Δρmin = −4.32 e Å^−3

Special details

Experimental. CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1A	0.67071 (3)	0.41445 (2)	0.00751 (4)	0.01422 (6)
Pb1B	0.33731 (3)	0.58067 (2)	0.50632 (4)	0.01408 (6)
Pb2A	0.00408 (3)	0.37537 (2)	0.23830 (4)	0.01546 (6)
Pb2B	0.25092 (3)	0.37315 (2)	0.74157 (4)	0.01629 (6)
Pb2C	0.24636 (3)	0.74840 (2)	0.27105 (4)	0.01397 (6)
AsA	0.38479 (7)	0.45467 (4)	0.25265 (9)	0.00821 (11)
AsB	0.40963 (8)	0.26244 (4)	0.75337 (9)	0.00848 (11)
AsC	0.02396 (8)	0.55778 (4)	0.24628 (9)	0.00804 (11)
O1A	0.4938 (6)	0.4145 (3)	0.2486 (8)	0.0156 (10)
O1B	0.3290 (7)	0.6676 (3)	0.7495 (8)	0.0161 (10)
O1C	0.8351 (6)	0.5032 (3)	0.2504 (7)	0.0157 (10)
O2A	0.4866 (6)	0.5489 (3)	0.2252 (9)	0.0205 (12)
O2B	0.5995 (7)	0.3059 (4)	0.7543 (13)	0.038 (2)
O2C	0.1103 (7)	0.5066 (3)	0.2799 (9)	0.0186 (11)
O3A	0.2505 (7)	0.4195 (4)	0.0927 (9)	0.0228 (13)
O3B	0.6381 (13)	0.7073 (4)	0.0628 (12)	0.057 (3)
O3C	0.0862 (7)	0.6017 (4)	0.0479 (9)	0.0228 (12)
O3D	0.2947 (8)	0.4413 (4)	0.4515 (9)	0.0273 (14)
O3E	0.6416 (10)	0.7029 (4)	0.4204 (12)	0.042 (2)
O3F	0.0864 (8)	0.6251 (3)	0.4046 (9)	0.0246 (13)
Cl	0.0067 (2)	0.24994 (10)	0.4915 (3)	0.0185 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1A	0.01742 (12)	0.01922 (12)	0.00870 (11)	0.01116 (10)	−0.00050 (8)	−0.00052 (8)
Pb1B	0.01702 (12)	0.01834 (12)	0.00881 (11)	0.01028 (10)	−0.00005 (8)	0.00003 (8)
Pb2A	0.01342 (11)	0.01135 (11)	0.02230 (14)	0.00672 (9)	0.00174 (9)	0.00220 (8)
Pb2B	0.01072 (11)	0.01229 (11)	0.02464 (14)	0.00484 (9)	0.00104 (9)	0.00196 (9)
Pb2C	0.01153 (10)	0.01385 (11)	0.01752 (12)	0.00709 (9)	−0.00148 (9)	0.00191 (8)
AsA	0.0072 (2)	0.0088 (3)	0.0093 (3)	0.0045 (2)	0.0000 (2)	0.0002 (2)
AsB	0.0083 (3)	0.0081 (3)	0.0095 (3)	0.0044 (2)	0.0007 (2)	−0.0001 (2)
AsC	0.0076 (3)	0.0076 (3)	0.0086 (3)	0.0036 (2)	0.0004 (2)	0.00012 (19)
O1A	0.012 (2)	0.019 (2)	0.019 (3)	0.010 (2)	0.0010 (19)	0.0023 (19)
O1B	0.021 (3)	0.006 (2)	0.020 (3)	0.0054 (19)	0.002 (2)	0.0013 (17)
O1C	0.009 (2)	0.016 (2)	0.014 (3)	−0.0001 (19)	−0.0012 (18)	−0.0011 (18)
O2A	0.010 (2)	0.010 (2)	0.036 (4)	0.0010 (19)	−0.001 (2)	0.006 (2)
O2B	0.009 (2)	0.020 (3)	0.088 (7)	0.009 (2)	−0.003 (3)	−0.002 (3)
O2C	0.017 (2)	0.009 (2)	0.032 (3)	0.008 (2)	−0.005 (2)	0.0004 (19)
O3A	0.016 (3)	0.029 (3)	0.024 (3)	0.012 (2)	−0.010 (2)	−0.014 (2)
O3B	0.092 (8)	0.021 (3)	0.037 (5)	0.013 (4)	0.049 (5)	0.000 (3)
O3C	0.015 (3)	0.036 (3)	0.016 (3)	0.012 (3)	0.007 (2)	0.014 (2)
O3D	0.040 (4)	0.035 (3)	0.019 (3)	0.028 (3)	0.017 (3)	0.013 (2)
O3E	0.060 (5)	0.021 (3)	0.044 (5)	0.020 (3)	−0.041 (4)	−0.009 (3)
O3F	0.025 (3)	0.013 (2)	0.023 (3)	0.000 (2)	0.005 (2)	−0.010 (2)
Cl	0.0190 (8)	0.0165 (7)	0.0178 (8)	0.0073 (7)	0.0011 (6)	−0.0007 (6)

Geometric parameters (Å, º)

Pb1A—O1B^i	2.472 (5)	Pb2C—O2B^i	2.349 (6)
Pb1A—O1C	2.522 (5)	Pb2C—O3B^vii	2.425 (7)
Pb1A—O1A	2.552 (6)	Pb2C—O3F	2.432 (6)
Pb1A—O3C^ii	2.701 (6)	Pb2C—O1A^viii	3.066 (6)
Pb1A—O2A^ii	2.716 (6)	Pb2C—O3C	3.092 (7)
Pb1A—O2B^iii	2.723 (8)	Pb2C—Cl^viii	3.152 (2)
Pb1A—O2C^ii	2.934 (6)	Pb2C—O3E^viii	8.210 (7)
Pb1A—O3B^ii	2.934 (10)	AsA—O3A	1.686 (6)
Pb1A—O3A^ii	3.166 (7)	AsA—O1A	1.686 (5)
Pb1A—Pb1B^i	3.6280 (4)	AsA—O2A	1.686 (5)
Pb1B—O1A^i	2.483 (6)	AsA—O3D	1.694 (6)
Pb1B—O1C^i	2.515 (6)	AsB—O3B^i	1.674 (7)
Pb1B—O1B	2.572 (6)	AsB—O3E^i	1.682 (7)
Pb1B—O2C	2.651 (6)	AsB—O1B^ix	1.688 (5)
Pb1B—O3D	2.695 (6)	AsB—O2B	1.686 (6)
Pb1B—O2B^i	2.844 (8)	AsC—O1C^x	1.682 (5)
Pb1B—O2A	2.854 (7)	AsC—O3F	1.680 (6)
Pb1B—O3E	2.931 (9)	AsC—O3C	1.682 (6)
Pb1B—O3F	3.216 (8)	AsC—O2C	1.694 (5)
Pb1B—Pb1A^i	3.6280 (4)	O1A—Pb1B^i	2.483 (6)
Pb2A—O2C	2.362 (5)	O1B—AsB^xi	1.688 (5)
Pb2A—O3C^iv	2.462 (6)	O1B—Pb1A^i	2.472 (5)
Pb2A—O3A	2.466 (7)	O1C—AsC^xii	1.682 (5)
Pb2A—O3F^v	2.817 (6)	O1C—Pb1B^i	2.515 (5)
Pb2A—O3D	3.031 (8)	O2A—Pb2B^i	2.354 (6)
Pb2A—O1B^v	3.069 (6)	O2A—Pb1A^ii	2.716 (6)
Pb2A—Cl	3.1981 (19)	O2B—Pb2C^i	2.349 (6)
Pb2B—O2A^i	2.354 (6)	O2B—Pb1A^vi	2.723 (8)
Pb2B—O3D	2.490 (6)	O3B—AsB^i	1.674 (7)
Pb2B—O3E^i	2.610 (9)	O3B—Pb2C^xiii	2.425 (7)
Pb2B—O3A^vi	2.786 (6)	O3C—Pb2A^iv	2.462 (6)
Pb2B—O3B^i	2.830 (12)	O3C—Pb1A^ii	2.701 (6)
Pb2B—O1C^i	3.069 (6)	O3E—AsB^i	1.682 (7)
Pb2B—Cl	3.1292 (19)	O3E—Pb2B^i	2.610 (9)
O1B^i—Pb1A—O1C	74.72 (19)	O3A—Pb2A—Cl	97.85 (16)
O1B^i—Pb1A—O1A	74.10 (18)	O3F^v—Pb2A—Cl	64.79 (14)
O1C—Pb1A—O1A	73.26 (18)	O3D—Pb2A—Cl	69.38 (12)
O1B^i—Pb1A—O3C^ii	73.42 (19)	O1B^v—Pb2A—Cl	101.90 (10)
O1C—Pb1A—O3C^ii	82.7 (2)	O2A^i—Pb2B—O3D	83.5 (2)
O1A—Pb1A—O3C^ii	143.63 (18)	O2A^i—Pb2B—O3E^i	76.9 (2)
O1B^i—Pb1A—O2A^ii	149.13 (18)	O3D—Pb2B—O3E^i	85.5 (2)
O1C—Pb1A—O2A^ii	122.30 (19)	O2A^i—Pb2B—O3A^vi	82.3 (2)
O1A—Pb1A—O2A^ii	86.03 (19)	O3D—Pb2B—O3A^vi	131.0 (2)
O3C^ii—Pb1A—O2A^ii	130.25 (19)	O3E^i—Pb2B—O3A^vi	135.4 (2)
O1B^i—Pb1A—O2B^iii	92.5 (2)	O2A^i—Pb2B—O3B^i	71.7 (2)
O1C—Pb1A—O2B^iii	153.64 (19)	O3D—Pb2B—O3B^i	139.6 (2)
O1A—Pb1A—O2B^iii	126.0 (2)	O3E^i—Pb2B—O3B^i	58.6 (2)
O3C^ii—Pb1A—O2B^iii	71.4 (2)	O3A^vi—Pb2B—O3B^i	77.5 (2)
O2A^ii—Pb1A—O2B^iii	80.1 (2)	O2A^i—Pb2B—O1C^i	98.03 (18)
O1B^i—Pb1A—O2C^ii	130.51 (18)	O3D—Pb2B—O1C^i	66.43 (18)
O1C—Pb1A—O2C^ii	94.37 (17)	O3E^i—Pb2B—O1C^i	151.9 (2)
O1A—Pb1A—O2C^ii	149.44 (16)	O3A^vi—Pb2B—O1C^i	69.54 (17)
O3C^ii—Pb1A—O2C^ii	57.22 (16)	O3B^i—Pb2B—O1C^i	146.60 (18)
O2A^ii—Pb1A—O2C^ii	77.10 (17)	O2A^i—Pb2B—Cl	142.26 (17)
O2B^iii—Pb1A—O2C^ii	76.3 (2)	O3D—Pb2B—Cl	77.38 (19)
O1B^i—Pb1A—O3B^ii	85.4 (2)	O3E^i—Pb2B—Cl	69.42 (16)
O1C—Pb1A—O3B^ii	142.04 (19)	O3A^vi—Pb2B—Cl	134.28 (13)
O1A—Pb1A—O3B^ii	70.29 (19)	O3B^i—Pb2B—Cl	103.26 (18)
O3C^ii—Pb1A—O3B^ii	122.4 (2)	O1C^i—Pb2B—Cl	103.51 (11)
O2A^ii—Pb1A—O3B^ii	65.5 (2)	O2B^i—Pb2C—O3B^vii	86.1 (4)
O2B^iii—Pb1A—O3B^ii	56.5 (2)	O2B^i—Pb2C—O3F	78.8 (2)
O2C^ii—Pb1A—O3B^ii	122.7 (2)	O3B^vii—Pb2C—O3F	88.3 (2)
O1B^i—Pb1A—O3A^ii	144.75 (17)	O2B^i—Pb2C—O1A^viii	98.2 (2)
O1C—Pb1A—O3A^ii	71.07 (17)	O3B^vii—Pb2C—O1A^viii	69.5 (2)
O1A—Pb1A—O3A^ii	88.04 (17)	O3F—Pb2C—O1A^viii	157.81 (19)
O3C^ii—Pb1A—O3A^ii	109.83 (17)	O2B^i—Pb2C—O3C	69.6 (2)
O2A^ii—Pb1A—O3A^ii	54.60 (16)	O3B^vii—Pb2C—O3C	140.2 (2)
O2B^iii—Pb1A—O3A^ii	122.2 (2)	O3F—Pb2C—O3C	57.08 (18)
O2C^ii—Pb1A—O3A^ii	61.41 (16)	O1A^viii—Pb2C—O3C	142.68 (15)
O3B^ii—Pb1A—O3A^ii	117.3 (2)	O2B^i—Pb2C—Cl^viii	131.7 (2)
O1B^i—Pb1A—Pb1B^i	45.11 (13)	O3B^vii—Pb2C—Cl^viii	142.2 (3)
O1C—Pb1A—Pb1B^i	43.84 (13)	O3F—Pb2C—Cl^viii	98.07 (18)
O1A—Pb1A—Pb1B^i	43.16 (13)	O1A^viii—Pb2C—Cl^viii	100.09 (11)
O3C^ii—Pb1A—Pb1B^i	101.01 (14)	O3C—Pb2C—Cl^viii	68.78 (12)
O2A^ii—Pb1A—Pb1B^i	127.30 (14)	O2B^i—Pb2C—O3E^viii	117.10 (18)
O2B^iii—Pb1A—Pb1B^i	135.60 (18)	O3B^vii—Pb2C—O3E^viii	81.95 (18)
O2C^ii—Pb1A—Pb1B^i	137.39 (12)	O3F—Pb2C—O3E^viii	160.51 (15)
O3B^ii—Pb1A—Pb1B^i	99.92 (16)	O1A^viii—Pb2C—O3E^viii	21.23 (13)
O3A^ii—Pb1A—Pb1B^i	101.73 (12)	O3C—Pb2C—O3E^viii	136.86 (13)
O1A^i—Pb1B—O1C^i	74.56 (18)	Cl^viii—Pb2C—O3E^viii	79.97 (8)
O1A^i—Pb1B—O1B	73.58 (19)	O3A—AsA—O1A	112.2 (3)
O1C^i—Pb1B—O1B	73.12 (18)	O3A—AsA—O2A	108.0 (3)
O1A^i—Pb1B—O2C	152.26 (17)	O1A—AsA—O2A	112.0 (3)
O1C^i—Pb1B—O2C	87.30 (19)	O3A—AsA—O3D	106.7 (4)
O1B—Pb1B—O2C	121.47 (19)	O1A—AsA—O3D	112.1 (3)
O1A^i—Pb1B—O3D	84.0 (2)	O2A—AsA—O3D	105.5 (3)
O1C^i—Pb1B—O3D	72.49 (19)	O3B^i—AsB—O3E^i	105.3 (5)
O1B—Pb1B—O3D	142.79 (18)	O3B^i—AsB—O1B^ix	111.7 (3)
O2C—Pb1B—O3D	70.5 (2)	O3E^i—AsB—O1B^ix	113.5 (3)
O1A^i—Pb1B—O2B^i	126.91 (19)	O3B^i—AsB—O2B	105.9 (5)
O1C^i—Pb1B—O2B^i	147.78 (19)	O3E^i—AsB—O2B	107.5 (4)
O1B—Pb1B—O2B^i	89.4 (2)	O1B^ix—AsB—O2B	112.3 (3)
O2C—Pb1B—O2B^i	78.97 (19)	O1C^x—AsC—O3F	111.8 (3)
O3D—Pb1B—O2B^i	127.7 (2)	O1C^x—AsC—O3C	112.0 (3)
O1A^i—Pb1B—O2A	96.17 (18)	O3F—AsC—O3C	107.0 (3)
O1C^i—Pb1B—O2A	130.32 (18)	O1C^x—AsC—O2C	111.6 (3)
O1B—Pb1B—O2A	151.89 (17)	O3F—AsC—O2C	107.6 (3)
O2C—Pb1B—O2A	79.54 (18)	O3C—AsC—O2C	106.6 (3)
O3D—Pb1B—O2A	57.92 (17)	AsA—O1A—Pb1B^i	125.8 (3)
O2B^i—Pb1B—O2A	75.84 (19)	AsA—O1A—Pb1A	131.0 (3)
O1A^i—Pb1B—O3E	72.84 (19)	Pb1B^i—O1A—Pb1A	92.17 (18)
O1C^i—Pb1B—O3E	145.56 (19)	AsB^xi—O1B—Pb1A^i	128.7 (3)
O1B—Pb1B—O3E	87.2 (2)	AsB^xi—O1B—Pb1B	128.4 (3)
O2C—Pb1B—O3E	127.1 (2)	Pb1A^i—O1B—Pb1B	91.97 (17)
O3D—Pb1B—O3E	114.3 (2)	AsC^xii—O1C—Pb1B^i	130.4 (3)
O2B^i—Pb1B—O3E	56.10 (19)	AsC^xii—O1C—Pb1A	126.7 (3)
O2A—Pb1B—O3E	64.7 (2)	Pb1B^i—O1C—Pb1A	92.17 (17)
O1A^i—Pb1B—O3F	143.25 (17)	AsA—O2A—Pb2B^i	127.4 (3)
O1C^i—Pb1B—O3F	88.62 (18)	AsA—O2A—Pb1A^ii	106.3 (3)
O1B—Pb1B—O3F	70.30 (17)	Pb2B^i—O2A—Pb1A^ii	120.9 (2)
O2C—Pb1B—O3F	54.25 (15)	AsA—O2A—Pb1B	94.4 (3)
O3D—Pb1B—O3F	122.31 (19)	Pb2B^i—O2A—Pb1B	109.2 (2)
O2B^i—Pb1B—O3F	59.70 (17)	Pb1A^ii—O2A—Pb1B	86.95 (17)
O2A—Pb1B—O3F	119.08 (17)	AsB—O2B—Pb2C^i	128.3 (4)
O3E—Pb1B—O3F	111.43 (17)	AsB—O2B—Pb1A^vi	101.6 (3)
O1A^i—Pb1B—Pb1A^i	44.67 (13)	Pb2C^i—O2B—Pb1A^vi	118.2 (3)
O1C^i—Pb1B—Pb1A^i	43.99 (12)	AsC—O2C—Pb2A	126.8 (3)
O1B—Pb1B—Pb1A^i	42.92 (12)	AsC—O2C—Pb1B	108.6 (3)
O2C—Pb1B—Pb1A^i	128.79 (14)	Pb2A—O2C—Pb1B	120.5 (2)
O3D—Pb1B—Pb1A^i	100.77 (14)	AsA—O3A—Pb2A	108.2 (3)
O2B^i—Pb1B—Pb1A^i	131.24 (17)	AsB^i—O3B—Pb2C^xiii	140.7 (4)
O2A—Pb1B—Pb1A^i	139.63 (12)	AsC—O3C—Pb2A^iv	141.8 (3)
O3E—Pb1B—Pb1A^i	102.93 (16)	AsC—O3C—Pb1A^ii	101.3 (3)
O3F—Pb1B—Pb1A^i	101.28 (11)	Pb2A^iv—O3C—Pb1A^ii	110.4 (2)
O2C—Pb2A—O3C^iv	84.3 (2)	AsC—O3C—Pb2C	85.5 (3)
O2C—Pb2A—O3A	80.5 (2)	Pb2A^iv—O3C—Pb2C	110.4 (2)
O3C^iv—Pb2A—O3A	87.8 (2)	Pb1A^ii—O3C—Pb2C	97.32 (19)
O2C—Pb2A—O3F^v	81.0 (2)	AsA—O3D—Pb2B	141.4 (3)
O3C^iv—Pb2A—O3F^v	131.7 (2)	AsA—O3D—Pb1B	100.0 (3)
O3A—Pb2A—O3F^v	133.7 (2)	Pb2B—O3D—Pb1B	110.5 (3)
O2C—Pb2A—O3D	68.48 (18)	AsA—O3D—Pb2A	87.0 (3)
O3C^iv—Pb2A—O3D	138.43 (18)	Pb2B—O3D—Pb2A	110.1 (2)
O3A—Pb2A—O3D	58.03 (19)	Pb1B—O3D—Pb2A	98.9 (2)
O3F^v—Pb2A—O3D	75.75 (18)	AsB^i—O3E—Pb2B^i	102.0 (4)
O2C—Pb2A—O1B^v	97.84 (17)	AsB^i—O3E—Pb1B	96.1 (3)
O3C^iv—Pb2A—O1B^v	67.10 (17)	Pb2B^i—O3E—Pb1B	100.2 (2)
O3A—Pb2A—O1B^v	154.84 (19)	AsC—O3F—Pb2C	110.3 (3)
O3F^v—Pb2A—O1B^v	69.80 (18)	AsC—O3F—Pb1B	87.9 (3)
O3D—Pb2A—O1B^v	144.62 (16)	Pb2C—O3F—Pb1B	99.9 (2)
O2C—Pb2A—Cl	130.72 (15)	Pb2B—Cl—Pb2A	91.61 (5)
O3C^iv—Pb2A—Cl	145.02 (16)

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

(Mim288K)

Crystal data

As2Cl0.67O8Pb3.33	F(000) = 2488
Mr = 992.11	Dx = 7.283 Mg m^−3
Monoclinic, P1121/b	Ag Kα radiation, λ = 0.56087 Å
a = 10.2552 (3) Å	Cell parameters from 14405 reflections
b = 20.4913 (6) Å	θ = 1.8–29.3°
c = 7.4576 (2) Å	µ = 37.74 mm^−1
β = 90°	T = 288 K
V = 1357.29 (7) Å^3	Fragment, pale-orange
Z = 6	0.10 × 0.06 × 0.04 mm

Data collection

XtaLAB Synergy, Dualflex, Hypix diffractometer	5638 independent reflections
Radiation source: micro-focus sealed X-ray tube	4670 reflections with I > 2σ(I)
Detector resolution: 10.0000 pixels mm^-1	Rint = 0.048
o scan	θmax = 26.4°, θmin = 1.8°
Absorption correction: multi-scan SCALE 3 ABSPACK	h = −15→16
Tmin = 0.377, Tmax = 1.000	k = −32→32
27930 measured reflections	l = −11→11

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.033	Secondary atom site location: Difmap
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0292P)^2 + 12.8986P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
5638 reflections	Δρmax = 4.21 e Å^−3
190 parameters	Δρmin = −4.54 e Å^−3

Special details

Experimental. CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1A	0.67046 (3)	0.41450 (2)	0.00749 (3)	0.01478 (6)
Pb1B	0.33702 (3)	0.58073 (2)	0.50634 (3)	0.01464 (6)
Pb2A	0.00428 (3)	0.37550 (2)	0.23855 (4)	0.01599 (6)
Pb2B	0.25128 (3)	0.37313 (2)	0.74136 (4)	0.01681 (6)
Pb2C	0.24624 (3)	0.74829 (2)	0.27066 (3)	0.01463 (6)
AsA	0.38458 (8)	0.45465 (4)	0.25276 (8)	0.00851 (11)
AsB	0.40972 (8)	0.26269 (4)	0.75316 (8)	0.00866 (11)
AsC	0.02424 (8)	0.55791 (4)	0.24647 (8)	0.00825 (11)
O1A	0.4931 (7)	0.4151 (4)	0.2490 (7)	0.0170 (10)
O1B	0.3298 (8)	0.6686 (3)	0.7513 (7)	0.0182 (11)
O1C	0.8350 (6)	0.5028 (3)	0.2501 (6)	0.0150 (10)
O2A	0.4864 (7)	0.5492 (3)	0.2256 (8)	0.0209 (11)
O2B	0.5989 (7)	0.3064 (4)	0.7530 (11)	0.0352 (19)
O2C	0.1101 (7)	0.5067 (3)	0.2787 (9)	0.0210 (12)
O3A	0.2508 (8)	0.4202 (4)	0.0930 (8)	0.0277 (14)
O3B	0.6370 (12)	0.7070 (4)	0.0642 (11)	0.058 (3)
O3C	0.0866 (7)	0.6026 (4)	0.0476 (8)	0.0246 (13)
O3D	0.2933 (8)	0.4407 (4)	0.4499 (8)	0.0278 (14)
O3E	0.6434 (10)	0.7033 (4)	0.4188 (10)	0.041 (2)
O3F	0.0864 (7)	0.6247 (3)	0.4064 (8)	0.0230 (13)
Cl	0.0061 (2)	0.24971 (10)	0.4912 (2)	0.0189 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1A	0.01836 (13)	0.01946 (12)	0.00899 (10)	0.01131 (10)	−0.00049 (8)	−0.00040 (8)
Pb1B	0.01777 (13)	0.01896 (12)	0.00901 (10)	0.01056 (10)	−0.00010 (8)	0.00002 (8)
Pb2A	0.01417 (12)	0.01185 (11)	0.02275 (12)	0.00710 (9)	0.00186 (9)	0.00238 (8)
Pb2B	0.01090 (11)	0.01298 (11)	0.02536 (13)	0.00507 (9)	0.00134 (9)	0.00205 (8)
Pb2C	0.01209 (11)	0.01435 (11)	0.01866 (11)	0.00752 (9)	−0.00153 (8)	0.00194 (8)
AsA	0.0077 (3)	0.0091 (2)	0.0095 (2)	0.0047 (2)	0.00026 (19)	0.00028 (19)
AsB	0.0088 (3)	0.0082 (2)	0.0096 (2)	0.0047 (2)	0.00063 (19)	−0.00004 (19)
AsC	0.0074 (3)	0.0079 (2)	0.0091 (2)	0.0036 (2)	0.00033 (19)	−0.00007 (19)
O1A	0.019 (3)	0.026 (3)	0.016 (2)	0.019 (2)	0.0023 (18)	0.0009 (18)
O1B	0.029 (3)	0.009 (2)	0.015 (2)	0.008 (2)	0.0032 (19)	0.0012 (16)
O1C	0.004 (2)	0.019 (2)	0.016 (2)	0.0014 (18)	0.0004 (16)	−0.0006 (17)
O2A	0.013 (3)	0.011 (2)	0.036 (3)	0.004 (2)	0.000 (2)	0.005 (2)
O2B	0.010 (3)	0.019 (3)	0.081 (6)	0.010 (2)	−0.004 (3)	−0.004 (3)
O2C	0.019 (3)	0.010 (2)	0.038 (3)	0.010 (2)	−0.006 (2)	0.002 (2)
O3A	0.022 (3)	0.042 (4)	0.023 (3)	0.019 (3)	−0.011 (2)	−0.016 (3)
O3B	0.096 (8)	0.017 (3)	0.046 (4)	0.016 (4)	0.057 (5)	0.006 (3)
O3C	0.018 (3)	0.040 (3)	0.017 (2)	0.016 (3)	0.004 (2)	0.017 (2)
O3D	0.041 (4)	0.037 (3)	0.021 (3)	0.031 (3)	0.020 (3)	0.014 (2)
O3E	0.062 (5)	0.024 (3)	0.040 (4)	0.024 (3)	−0.040 (4)	−0.009 (3)
O3F	0.023 (3)	0.014 (2)	0.021 (3)	0.001 (2)	0.005 (2)	−0.0096 (19)
Cl	0.0197 (8)	0.0179 (7)	0.0180 (7)	0.0086 (7)	0.0011 (6)	0.0001 (6)

Geometric parameters (Å, º)

Pb1A—O1B^i	2.476 (5)	Pb2C—O2B^i	2.364 (7)
Pb1A—O1C	2.518 (5)	Pb2C—O3B^vii	2.443 (7)
Pb1A—O1A	2.565 (5)	Pb2C—O3F	2.445 (6)
Pb1A—O2A^ii	2.713 (6)	Pb2C—O1A^viii	3.077 (6)
Pb1A—O3C^ii	2.715 (6)	Pb2C—O3C	3.078 (7)
Pb1A—O2B^iii	2.725 (7)	Pb2C—Cl^viii	3.1548 (19)
Pb1A—O3B^ii	2.929 (10)	Pb2C—O3E^viii	8.219 (6)
Pb1A—O2C^ii	2.931 (6)	AsA—O1A	1.672 (6)
Pb1A—O3A^ii	3.156 (7)	AsA—O3A	1.683 (6)
Pb1A—Pb1B^i	3.6288 (3)	AsA—O3D	1.689 (6)
Pb1B—O1A^i	2.495 (6)	AsA—O2A	1.691 (5)
Pb1B—O1C^i	2.515 (5)	AsB—O3B^i	1.663 (7)
Pb1B—O1B	2.591 (5)	AsB—O3E^i	1.675 (6)
Pb1B—O2C	2.659 (6)	AsB—O1B^ix	1.677 (5)
Pb1B—O3D	2.706 (6)	AsB—O2B	1.682 (7)
Pb1B—O2B^i	2.829 (8)	AsC—O3F	1.682 (5)
Pb1B—O2A	2.853 (6)	AsC—O1C^x	1.688 (5)
Pb1B—O3E	2.952 (9)	AsC—O2C	1.691 (6)
Pb1B—O3F	3.208 (7)	AsC—O3C	1.692 (5)
Pb1B—Pb1A^i	3.6289 (3)	O1A—Pb1B^i	2.495 (5)
Pb2A—O2C	2.362 (5)	O1B—AsB^xi	1.677 (5)
Pb2A—O3C^iv	2.458 (5)	O1B—Pb1A^i	2.476 (5)
Pb2A—O3A	2.468 (7)	O1C—AsC^xii	1.688 (5)
Pb2A—O3F^v	2.805 (6)	O1C—Pb1B^i	2.515 (5)
Pb2A—O3D	3.016 (8)	O2A—Pb2B^i	2.356 (6)
Pb2A—O1B^v	3.077 (7)	O2A—Pb1A^ii	2.713 (6)
Pb2A—Cl	3.2004 (17)	O2B—Pb2C^i	2.364 (7)
Pb2B—O2A^i	2.356 (6)	O2B—Pb1A^vi	2.725 (7)
Pb2B—O3D	2.497 (6)	O3B—AsB^i	1.663 (7)
Pb2B—O3E^i	2.596 (9)	O3B—Pb2C^xiii	2.443 (7)
Pb2B—O3A^vi	2.795 (6)	O3C—Pb2A^iv	2.458 (5)
Pb2B—O3B^i	2.828 (11)	O3C—Pb1A^ii	2.715 (6)
Pb2B—O1C^i	3.082 (6)	O3E—AsB^i	1.675 (6)
Pb2B—Cl	3.1370 (18)	O3E—Pb2B^i	2.596 (9)
O1B^i—Pb1A—O1C	75.05 (18)	O3A—Pb2A—Cl	98.06 (17)
O1B^i—Pb1A—O1A	74.70 (19)	O3F^v—Pb2A—Cl	65.07 (14)
O1C—Pb1A—O1A	73.38 (18)	O3D—Pb2A—Cl	69.47 (12)
O1B^i—Pb1A—O2A^ii	149.0 (2)	O1B^v—Pb2A—Cl	101.72 (10)
O1C—Pb1A—O2A^ii	122.64 (19)	O2A^i—Pb2B—O3D	83.9 (2)
O1A—Pb1A—O2A^ii	85.94 (18)	O2A^i—Pb2B—O3E^i	77.1 (2)
O1B^i—Pb1A—O3C^ii	72.96 (19)	O3D—Pb2B—O3E^i	85.7 (2)
O1C—Pb1A—O3C^ii	82.7 (2)	O2A^i—Pb2B—O3A^vi	82.4 (2)
O1A—Pb1A—O3C^ii	143.70 (17)	O3D—Pb2B—O3A^vi	130.9 (2)
O2A^ii—Pb1A—O3C^ii	130.30 (18)	O3E^i—Pb2B—O3A^vi	135.46 (19)
O1B^i—Pb1A—O2B^iii	92.3 (2)	O2A^i—Pb2B—O3B^i	71.4 (2)
O1C—Pb1A—O2B^iii	153.6 (2)	O3D—Pb2B—O3B^i	139.6 (2)
O1A—Pb1A—O2B^iii	126.1 (2)	O3E^i—Pb2B—O3B^i	58.2 (2)
O2A^ii—Pb1A—O2B^iii	79.7 (2)	O3A^vi—Pb2B—O3B^i	77.9 (2)
O3C^ii—Pb1A—O2B^iii	71.4 (2)	O2A^i—Pb2B—O1C^i	98.17 (18)
O1B^i—Pb1A—O3B^ii	85.3 (2)	O3D—Pb2B—O1C^i	66.52 (17)
O1C—Pb1A—O3B^ii	142.38 (18)	O3E^i—Pb2B—O1C^i	152.25 (18)
O1A—Pb1A—O3B^ii	70.60 (19)	O3A^vi—Pb2B—O1C^i	69.23 (17)
O2A^ii—Pb1A—O3B^ii	65.3 (2)	O3B^i—Pb2B—O1C^i	146.66 (17)
O3C^ii—Pb1A—O3B^ii	122.0 (2)	O2A^i—Pb2B—Cl	142.31 (16)
O2B^iii—Pb1A—O3B^ii	56.2 (2)	O3D—Pb2B—Cl	77.07 (18)
O1B^i—Pb1A—O2C^ii	130.13 (19)	O3E^i—Pb2B—Cl	69.37 (16)
O1C—Pb1A—O2C^ii	94.19 (17)	O3A^vi—Pb2B—Cl	134.19 (15)
O1A—Pb1A—O2C^ii	149.27 (17)	O3B^i—Pb2B—Cl	103.35 (18)
O2A^ii—Pb1A—O2C^ii	77.27 (17)	O1C^i—Pb2B—Cl	103.44 (10)
O3C^ii—Pb1A—O2C^ii	57.30 (16)	O2B^i—Pb2C—O3B^vii	85.7 (3)
O2B^iii—Pb1A—O2C^ii	76.20 (19)	O2B^i—Pb2C—O3F	78.6 (2)
O3B^ii—Pb1A—O2C^ii	122.62 (18)	O3B^vii—Pb2C—O3F	88.1 (2)
O1B^i—Pb1A—O3A^ii	145.34 (16)	O2B^i—Pb2C—O1A^viii	98.5 (2)
O1C—Pb1A—O3A^ii	71.29 (17)	O3B^vii—Pb2C—O1A^viii	69.5 (2)
O1A—Pb1A—O3A^ii	87.87 (18)	O3F—Pb2C—O1A^viii	157.54 (17)
O2A^ii—Pb1A—O3A^ii	54.68 (16)	O2B^i—Pb2C—O3C	70.0 (2)
O3C^ii—Pb1A—O3A^ii	110.11 (18)	O3B^vii—Pb2C—O3C	140.46 (19)
O2B^iii—Pb1A—O3A^ii	121.86 (19)	O3F—Pb2C—O3C	57.52 (17)
O3B^ii—Pb1A—O3A^ii	117.3 (2)	O1A^viii—Pb2C—O3C	142.68 (14)
O2C^ii—Pb1A—O3A^ii	61.41 (16)	O2B^i—Pb2C—Cl^viii	132.14 (19)
O1B^i—Pb1A—Pb1B^i	45.55 (12)	O3B^vii—Pb2C—Cl^viii	142.2 (3)
O1C—Pb1A—Pb1B^i	43.82 (11)	O3F—Pb2C—Cl^viii	98.25 (17)
O1A—Pb1A—Pb1B^i	43.41 (12)	O1A^viii—Pb2C—Cl^viii	99.94 (10)
O2A^ii—Pb1A—Pb1B^i	127.54 (14)	O3C—Pb2C—Cl^viii	68.60 (11)
O3C^ii—Pb1A—Pb1B^i	100.82 (12)	O2B^i—Pb2C—O3E^viii	117.09 (18)
O2B^iii—Pb1A—Pb1B^i	135.82 (16)	O3B^vii—Pb2C—O3E^viii	81.77 (17)
O3B^ii—Pb1A—Pb1B^i	100.20 (14)	O3F—Pb2C—O3E^viii	160.36 (14)
O2C^ii—Pb1A—Pb1B^i	137.17 (12)	O1A^viii—Pb2C—O3E^viii	20.82 (13)
O3A^ii—Pb1A—Pb1B^i	101.89 (11)	O3C—Pb2C—O3E^viii	136.81 (11)
O1A^i—Pb1B—O1C^i	74.64 (18)	Cl^viii—Pb2C—O3E^viii	80.18 (8)
O1A^i—Pb1B—O1B	73.91 (19)	O1A—AsA—O3A	112.7 (3)
O1C^i—Pb1B—O1B	73.12 (18)	O1A—AsA—O3D	112.3 (3)
O1A^i—Pb1B—O2C	152.06 (18)	O3A—AsA—O3D	106.2 (4)
O1C^i—Pb1B—O2C	87.52 (18)	O1A—AsA—O2A	111.9 (3)
O1B—Pb1B—O2C	121.7 (2)	O3A—AsA—O2A	107.7 (3)
O1A^i—Pb1B—O3D	83.8 (2)	O3D—AsA—O2A	105.7 (3)
O1C^i—Pb1B—O3D	72.71 (18)	O3B^i—AsB—O3E^i	104.9 (5)
O1B—Pb1B—O3D	143.03 (16)	O3B^i—AsB—O1B^ix	112.3 (3)
O2C—Pb1B—O3D	70.2 (2)	O3E^i—AsB—O1B^ix	112.9 (3)
O1A^i—Pb1B—O2B^i	126.8 (2)	O3B^i—AsB—O2B	105.8 (5)
O1C^i—Pb1B—O2B^i	148.0 (2)	O3E^i—AsB—O2B	107.8 (4)
O1B—Pb1B—O2B^i	89.40 (19)	O1B^ix—AsB—O2B	112.5 (3)
O2C—Pb1B—O2B^i	79.02 (18)	O3F—AsC—O1C^x	112.0 (3)
O3D—Pb1B—O2B^i	127.46 (19)	O3F—AsC—O2C	107.5 (3)
O1A^i—Pb1B—O2A	95.70 (18)	O1C^x—AsC—O2C	111.3 (3)
O1C^i—Pb1B—O2A	130.49 (17)	O3F—AsC—O3C	107.1 (3)
O1B—Pb1B—O2A	151.62 (18)	O1C^x—AsC—O3C	111.9 (3)
O2C—Pb1B—O2A	79.52 (19)	O2C—AsC—O3C	106.7 (3)
O3D—Pb1B—O2A	57.90 (16)	AsA—O1A—Pb1B^i	126.4 (3)
O2B^i—Pb1B—O2A	75.66 (18)	AsA—O1A—Pb1A	131.3 (3)
O1A^i—Pb1B—O3E	72.84 (18)	Pb1B^i—O1A—Pb1A	91.64 (19)
O1C^i—Pb1B—O3E	145.59 (17)	AsB^xi—O1B—Pb1A^i	129.6 (3)
O1B—Pb1B—O3E	87.3 (2)	AsB^xi—O1B—Pb1B	128.1 (3)
O2C—Pb1B—O3E	126.85 (18)	Pb1A^i—O1B—Pb1B	91.45 (18)
O3D—Pb1B—O3E	114.2 (2)	AsC^xii—O1C—Pb1B^i	130.3 (3)
O2B^i—Pb1B—O3E	55.91 (18)	AsC^xii—O1C—Pb1A	127.0 (3)
O2A—Pb1B—O3E	64.34 (19)	Pb1B^i—O1C—Pb1A	92.28 (17)
O1A^i—Pb1B—O3F	143.55 (16)	AsA—O2A—Pb2B^i	127.2 (3)
O1C^i—Pb1B—O3F	88.33 (17)	AsA—O2A—Pb1A^ii	106.2 (3)
O1B—Pb1B—O3F	70.34 (17)	Pb2B^i—O2A—Pb1A^ii	121.0 (2)
O2C—Pb1B—O3F	54.29 (15)	AsA—O2A—Pb1B	94.5 (2)
O3D—Pb1B—O3F	122.03 (19)	Pb2B^i—O2A—Pb1B	109.3 (2)
O2B^i—Pb1B—O3F	60.19 (17)	Pb1A^ii—O2A—Pb1B	87.06 (18)
O2A—Pb1B—O3F	119.33 (16)	AsB—O2B—Pb2C^i	128.1 (4)
O3E—Pb1B—O3F	111.77 (17)	AsB—O2B—Pb1A^vi	101.7 (3)
O1A^i—Pb1B—Pb1A^i	44.94 (12)	Pb2C^i—O2B—Pb1A^vi	117.7 (3)
O1C^i—Pb1B—Pb1A^i	43.90 (12)	AsC—O2C—Pb2A	127.1 (3)
O1B—Pb1B—Pb1A^i	43.00 (12)	AsC—O2C—Pb1B	108.4 (3)
O2C—Pb1B—Pb1A^i	128.98 (14)	Pb2A—O2C—Pb1B	120.2 (2)
O3D—Pb1B—Pb1A^i	100.92 (12)	AsA—O3A—Pb2A	108.3 (3)
O2B^i—Pb1B—Pb1A^i	131.32 (15)	AsB^i—O3B—Pb2C^xiii	140.6 (4)
O2A—Pb1B—Pb1A^i	139.49 (12)	AsC—O3C—Pb2A^iv	141.7 (3)
O3E—Pb1B—Pb1A^i	103.06 (13)	AsC—O3C—Pb1A^ii	100.7 (3)
O3F—Pb1B—Pb1A^i	101.17 (10)	Pb2A^iv—O3C—Pb1A^ii	110.4 (2)
O2C—Pb2A—O3C^iv	84.4 (2)	AsC—O3C—Pb2C	85.7 (3)
O2C—Pb2A—O3A	80.3 (2)	Pb2A^iv—O3C—Pb2C	111.0 (2)
O3C^iv—Pb2A—O3A	87.8 (2)	Pb1A^ii—O3C—Pb2C	97.44 (19)
O2C—Pb2A—O3F^v	81.1 (2)	AsA—O3D—Pb2B	141.2 (3)
O3C^iv—Pb2A—O3F^v	131.6 (2)	AsA—O3D—Pb1B	99.9 (3)
O3A—Pb2A—O3F^v	133.84 (19)	Pb2B—O3D—Pb1B	110.1 (2)
O2C—Pb2A—O3D	68.81 (19)	AsA—O3D—Pb2A	87.6 (3)
O3C^iv—Pb2A—O3D	138.68 (18)	Pb2B—O3D—Pb2A	110.5 (2)
O3A—Pb2A—O3D	57.85 (18)	Pb1B—O3D—Pb2A	99.0 (2)
O3F^v—Pb2A—O3D	76.05 (17)	AsB^i—O3E—Pb2B^i	102.6 (4)
O2C—Pb2A—O1B^v	98.14 (18)	AsB^i—O3E—Pb1B	95.4 (3)
O3C^iv—Pb2A—O1B^v	66.84 (17)	Pb2B^i—O3E—Pb1B	100.1 (2)
O3A—Pb2A—O1B^v	154.62 (17)	AsC—O3F—Pb2C	109.5 (3)
O3F^v—Pb2A—O1B^v	69.93 (17)	AsC—O3F—Pb1B	88.1 (3)
O3D—Pb2A—O1B^v	145.16 (14)	Pb2C—O3F—Pb1B	99.8 (2)
O2C—Pb2A—Cl	131.13 (15)	Pb2B—Cl—Pb2A	91.48 (4)
O3C^iv—Pb2A—Cl	144.45 (16)

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

(Mim353K)

Crystal data

As4Cl1.33O16Pb6.67	F(000) = 2488
Mr = 1984.21	Dx = 7.277 Mg m^−3
Monoclinic, P1121/b	Ag Kα radiation, λ = 0.56087 Å
a = 10.2544 (4) Å	Cell parameters from 12252 reflections
b = 20.5052 (7) Å	θ = 3.0–29.3°
c = 7.4568 (2) Å	µ = 37.71 mm^−1
β = 90°	T = 353 K
V = 1358.26 (10) Å^3	Fragment, pale orange
Z = 3	0.10 × 0.06 × 0.04 mm

Data collection

XtalLAB, Synergy, Dualflex, Hypix diffractometer	4410 reflections with I > 2σ(I)
Radiation source: micro-focus sealed X-ray tube	Rint = 0.038
o scan	θmax = 26.4°, θmin = 1.8°
Absorption correction: multi-scan SCALE ABSPACK	h = −15→16
Tmin = 0.170, Tmax = 1.000	k = −32→32
24325 measured reflections	l = −11→11
5534 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.029	Secondary atom site location: Difmap
wR(F^2) = 0.069	w = 1/[σ^2(Fo^2) + (0.0266P)^2 + 2.914P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
5534 reflections	Δρmax = 4.22 e Å^−3
190 parameters	Δρmin = −3.78 e Å^−3

Special details

Experimental. CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1A	0.67002 (2)	0.41498 (2)	0.00739 (3)	0.01771 (5)
Pb1B	0.33661 (2)	0.58138 (2)	0.50620 (3)	0.01775 (5)
Pb2A	0.00487 (3)	0.37582 (2)	0.24120 (3)	0.01947 (5)
Pb2B	0.25167 (3)	0.37313 (2)	0.74208 (3)	0.01994 (5)
Pb2C	0.24637 (3)	0.74805 (2)	0.26755 (3)	0.01802 (5)
AsA	0.38396 (6)	0.45453 (3)	0.25219 (7)	0.01005 (10)
AsB	0.40948 (6)	0.26279 (3)	0.75257 (7)	0.01001 (9)
AsC	0.02470 (6)	0.55805 (3)	0.24698 (7)	0.00995 (10)
O1A	0.4924 (6)	0.4150 (3)	0.2484 (6)	0.0203 (9)
O1B	0.3299 (6)	0.6688 (2)	0.7502 (6)	0.0194 (9)
O1C	0.8362 (5)	0.5036 (3)	0.2503 (6)	0.0201 (9)
O2A	0.4851 (5)	0.5492 (3)	0.2317 (7)	0.0273 (12)
O2B	0.5997 (6)	0.3064 (3)	0.7510 (8)	0.0336 (15)
O2C	0.1105 (6)	0.5071 (3)	0.2756 (7)	0.0257 (11)
O3A	0.2546 (6)	0.4219 (3)	0.0880 (8)	0.0332 (13)
O3B	0.6382 (8)	0.7066 (3)	0.0641 (9)	0.0466 (18)
O3C	0.0877 (5)	0.6039 (3)	0.0510 (7)	0.0305 (12)
O3D	0.2877 (7)	0.4383 (4)	0.4468 (8)	0.0378 (14)
O3E	0.6420 (8)	0.7033 (3)	0.4203 (9)	0.0419 (16)
O3F	0.0869 (6)	0.6236 (3)	0.4105 (7)	0.0287 (12)
Cl	0.00464 (16)	0.24939 (8)	0.4928 (2)	0.0221 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1A	0.02182 (11)	0.02153 (11)	0.01121 (10)	0.01190 (9)	−0.00023 (7)	−0.00020 (7)
Pb1B	0.02094 (11)	0.02182 (11)	0.01131 (10)	0.01130 (9)	−0.00017 (7)	−0.00020 (7)
Pb2A	0.01694 (10)	0.01326 (9)	0.02841 (13)	0.00770 (8)	0.00165 (8)	0.00218 (8)
Pb2B	0.01318 (10)	0.01521 (9)	0.02963 (13)	0.00574 (8)	0.00170 (7)	0.00188 (8)
Pb2C	0.01512 (10)	0.01667 (9)	0.02396 (11)	0.00920 (8)	−0.00141 (7)	0.00189 (8)
AsA	0.0086 (2)	0.0102 (2)	0.0116 (2)	0.00493 (17)	0.00000 (16)	0.00009 (17)
AsB	0.0101 (2)	0.0088 (2)	0.0116 (2)	0.00508 (17)	0.00041 (16)	0.00009 (17)
AsC	0.0089 (2)	0.0087 (2)	0.0116 (2)	0.00393 (17)	0.00050 (16)	0.00044 (17)
O1A	0.025 (2)	0.030 (2)	0.017 (2)	0.022 (2)	−0.0021 (15)	−0.0019 (16)
O1B	0.027 (2)	0.0083 (16)	0.020 (2)	0.0074 (16)	0.0022 (16)	0.0032 (14)
O1C	0.0102 (19)	0.022 (2)	0.021 (2)	0.0025 (16)	0.0006 (14)	−0.0017 (16)
O2A	0.013 (2)	0.0096 (18)	0.053 (4)	0.0017 (16)	−0.0036 (19)	0.0031 (19)
O2B	0.011 (2)	0.018 (2)	0.072 (5)	0.0080 (18)	0.000 (2)	−0.001 (2)
O2C	0.022 (2)	0.0134 (19)	0.044 (3)	0.0112 (18)	−0.0058 (19)	0.0004 (18)
O3A	0.027 (3)	0.047 (3)	0.032 (3)	0.024 (3)	−0.017 (2)	−0.024 (2)
O3B	0.073 (4)	0.022 (3)	0.038 (3)	0.019 (3)	0.040 (3)	0.002 (2)
O3C	0.019 (2)	0.047 (3)	0.023 (3)	0.014 (2)	0.0048 (18)	0.022 (2)
O3D	0.055 (4)	0.053 (4)	0.029 (3)	0.044 (3)	0.023 (3)	0.025 (3)
O3E	0.061 (4)	0.025 (3)	0.038 (3)	0.021 (3)	−0.034 (3)	−0.005 (2)
O3F	0.025 (2)	0.020 (2)	0.026 (3)	0.0001 (19)	0.0076 (19)	−0.0100 (18)
Cl	0.0225 (7)	0.0214 (7)	0.0228 (8)	0.0112 (6)	0.0006 (5)	−0.0011 (5)

Geometric parameters (Å, º)

Pb1A—O1B^i	2.493 (4)	Pb2C—O2B^i	2.349 (5)
Pb1A—O1C	2.528 (4)	Pb2C—O3B^vii	2.461 (6)
Pb1A—O1A	2.559 (5)	Pb2C—O3F	2.480 (5)
Pb1A—O2A^ii	2.724 (5)	Pb2C—O3C	3.031 (6)
Pb1A—O3C^ii	2.734 (5)	Pb2C—O1A^viii	3.077 (5)
Pb1A—O2B^iii	2.744 (6)	Pb2C—Cl^viii	3.1595 (15)
Pb1A—O2C^ii	2.912 (5)	Pb2C—O3E^viii	8.230 (5)
Pb1A—O3B^ii	2.935 (7)	AsA—O1A	1.672 (5)
Pb1A—O3A^ii	3.115 (6)	AsA—O3A	1.679 (5)
Pb1A—Pb1B^i	3.6291 (3)	AsA—O2A	1.689 (5)
Pb1B—O1A^i	2.509 (4)	AsA—O3D	1.692 (5)
Pb1B—O1C^i	2.528 (4)	AsB—O3E^i	1.671 (5)
Pb1B—O1B	2.579 (5)	AsB—O3B^i	1.676 (5)
Pb1B—O2C	2.669 (5)	AsB—O1B^ix	1.677 (4)
Pb1B—O3D	2.754 (6)	AsB—O2B	1.692 (5)
Pb1B—O2B^i	2.810 (6)	AsC—O3C	1.683 (5)
Pb1B—O2A	2.820 (6)	AsC—O1C^x	1.682 (5)
Pb1B—O3E	2.941 (7)	AsC—O2C	1.683 (5)
Pb1B—O3F	3.167 (6)	AsC—O3F	1.686 (5)
Pb1B—Pb1A^i	3.6291 (3)	O1A—Pb1B^i	2.509 (4)
Pb2A—O2C	2.360 (5)	O1B—AsB^xi	1.677 (4)
Pb2A—O3C^iv	2.493 (5)	O1B—Pb1A^i	2.493 (4)
Pb2A—O3A	2.517 (6)	O1C—AsC^xii	1.682 (5)
Pb2A—O3F^v	2.765 (5)	O1C—Pb1B^i	2.528 (4)
Pb2A—O3D	2.948 (7)	O2A—Pb2B^i	2.359 (5)
Pb2A—O1B^v	3.080 (5)	O2A—Pb1A^ii	2.724 (5)
Pb2A—Cl	3.1993 (15)	O2B—Pb2C^i	2.349 (5)
Pb2B—O2A^i	2.359 (5)	O2B—Pb1A^vi	2.744 (6)
Pb2B—O3D	2.505 (5)	O3B—AsB^i	1.676 (5)
Pb2B—O3E^i	2.612 (7)	O3B—Pb2C^xiii	2.461 (5)
Pb2B—O3A^vi	2.762 (5)	O3C—Pb2A^iv	2.493 (5)
Pb2B—O3B^i	2.807 (8)	O3C—Pb1A^ii	2.734 (5)
Pb2B—O1C^i	3.078 (5)	O3E—AsB^i	1.671 (5)
Pb2B—Cl	3.1446 (15)	O3E—Pb2B^i	2.612 (7)
O1B^i—Pb1A—O1C	75.16 (16)	O3A—Pb2A—Cl	99.17 (14)
O1B^i—Pb1A—O1A	74.70 (16)	O3F^v—Pb2A—Cl	65.80 (12)
O1C—Pb1A—O1A	73.78 (15)	O3D—Pb2A—Cl	69.48 (11)
O1B^i—Pb1A—O2A^ii	149.50 (15)	O1B^v—Pb2A—Cl	101.40 (8)
O1C—Pb1A—O2A^ii	123.33 (16)	O2A^i—Pb2B—O3D	84.2 (2)
O1A—Pb1A—O2A^ii	87.02 (16)	O2A^i—Pb2B—O3E^i	76.36 (18)
O1B^i—Pb1A—O3C^ii	72.83 (15)	O3D—Pb2B—O3E^i	85.30 (18)
O1C—Pb1A—O3C^ii	83.24 (17)	O2A^i—Pb2B—O3A^vi	82.89 (18)
O1A—Pb1A—O3C^ii	144.01 (15)	O3D—Pb2B—O3A^vi	131.0 (2)
O2A^ii—Pb1A—O3C^ii	128.96 (16)	O3E^i—Pb2B—O3A^vi	135.94 (16)
O1B^i—Pb1A—O2B^iii	92.10 (16)	O2A^i—Pb2B—O3B^i	72.15 (18)
O1C—Pb1A—O2B^iii	153.14 (16)	O3D—Pb2B—O3B^i	140.19 (16)
O1A—Pb1A—O2B^iii	126.23 (16)	O3E^i—Pb2B—O3B^i	58.63 (18)
O2A^ii—Pb1A—O2B^iii	79.09 (16)	O3A^vi—Pb2B—O3B^i	78.19 (16)
O3C^ii—Pb1A—O2B^iii	70.31 (17)	O2A^i—Pb2B—O1C^i	98.57 (15)
O1B^i—Pb1A—O2C^ii	129.59 (16)	O3D—Pb2B—O1C^i	66.67 (15)
O1C—Pb1A—O2C^ii	93.79 (15)	O3E^i—Pb2B—O1C^i	151.94 (15)
O1A—Pb1A—O2C^ii	149.76 (15)	O3A^vi—Pb2B—O1C^i	68.89 (15)
O2A^ii—Pb1A—O2C^ii	76.88 (15)	O3B^i—Pb2B—O1C^i	146.75 (14)
O3C^ii—Pb1A—O2C^ii	56.94 (14)	O2A^i—Pb2B—Cl	141.51 (14)
O2B^iii—Pb1A—O2C^ii	76.01 (15)	O3D—Pb2B—Cl	75.85 (17)
O1B^i—Pb1A—O3B^ii	85.27 (18)	O3E^i—Pb2B—Cl	69.57 (12)
O1C—Pb1A—O3B^ii	142.51 (15)	O3A^vi—Pb2B—Cl	134.68 (12)
O1A—Pb1A—O3B^ii	70.31 (15)	O3B^i—Pb2B—Cl	103.34 (13)
O2A^ii—Pb1A—O3B^ii	65.42 (17)	O1C^i—Pb2B—Cl	103.02 (9)
O3C^ii—Pb1A—O3B^ii	121.34 (17)	O2B^i—Pb2C—O3B^vii	85.5 (2)
O2B^iii—Pb1A—O3B^ii	56.59 (15)	O2B^i—Pb2C—O3F	77.91 (19)
O2C^ii—Pb1A—O3B^ii	122.94 (15)	O3B^vii—Pb2C—O3F	87.04 (19)
O1B^i—Pb1A—O3A^ii	145.04 (14)	O2B^i—Pb2C—O3C	70.49 (16)
O1C—Pb1A—O3A^ii	71.04 (15)	O3B^vii—Pb2C—O3C	140.36 (15)
O1A—Pb1A—O3A^ii	87.43 (16)	O3F—Pb2C—O3C	57.92 (15)
O2A^ii—Pb1A—O3A^ii	54.96 (13)	O2B^i—Pb2C—O1A^viii	98.87 (16)
O3C^ii—Pb1A—O3A^ii	111.11 (15)	O3B^vii—Pb2C—O1A^viii	69.02 (16)
O2B^iii—Pb1A—O3A^ii	122.39 (16)	O3F—Pb2C—O1A^viii	156.05 (15)
O2C^ii—Pb1A—O3A^ii	62.35 (14)	O3C—Pb2C—O1A^viii	143.76 (12)
O3B^ii—Pb1A—O3A^ii	117.04 (17)	O2B^i—Pb2C—Cl^viii	133.18 (15)
O1B^i—Pb1A—Pb1B^i	45.27 (11)	O3B^vii—Pb2C—Cl^viii	141.27 (18)
O1C—Pb1A—Pb1B^i	44.12 (10)	O3F—Pb2C—Cl^viii	98.97 (14)
O1A—Pb1A—Pb1B^i	43.73 (10)	O3C—Pb2C—Cl^viii	68.88 (10)
O2A^ii—Pb1A—Pb1B^i	128.99 (12)	O1A^viii—Pb2C—Cl^viii	100.22 (9)
O3C^ii—Pb1A—Pb1B^i	100.94 (11)	O2B^i—Pb2C—O3E^viii	117.49 (14)
O2B^iii—Pb1A—Pb1B^i	135.48 (12)	O3B^vii—Pb2C—O3E^viii	81.52 (13)
O2C^ii—Pb1A—Pb1B^i	136.91 (10)	O3F—Pb2C—O3E^viii	159.75 (12)
O3B^ii—Pb1A—Pb1B^i	100.11 (12)	O3C—Pb2C—O3E^viii	137.37 (10)
O3A^ii—Pb1A—Pb1B^i	101.73 (10)	O1A^viii—Pb2C—O3E^viii	20.92 (10)
O1A^i—Pb1B—O1C^i	74.64 (16)	Cl^viii—Pb2C—O3E^viii	80.21 (6)
O1A^i—Pb1B—O1B	74.08 (16)	O1A—AsA—O3A	112.3 (2)
O1C^i—Pb1B—O1B	73.71 (15)	O1A—AsA—O2A	112.3 (3)
O1A^i—Pb1B—O2C	151.81 (16)	O3A—AsA—O2A	107.5 (3)
O1C^i—Pb1B—O2C	87.67 (16)	O1A—AsA—O3D	112.5 (2)
O1B—Pb1B—O2C	122.28 (16)	O3A—AsA—O3D	106.2 (3)
O1A^i—Pb1B—O3D	84.35 (18)	O2A—AsA—O3D	105.5 (3)
O1C^i—Pb1B—O3D	71.88 (16)	O3E^i—AsB—O3B^i	105.2 (4)
O1B—Pb1B—O3D	143.11 (15)	O3E^i—AsB—O1B^ix	113.3 (2)
O2C—Pb1B—O3D	69.16 (17)	O3B^i—AsB—O1B^ix	112.1 (2)
O1A^i—Pb1B—O2B^i	126.89 (16)	O3E^i—AsB—O2B	107.2 (3)
O1C^i—Pb1B—O2B^i	148.33 (16)	O3B^i—AsB—O2B	106.4 (3)
O1B—Pb1B—O2B^i	89.35 (15)	O1B^ix—AsB—O2B	112.2 (3)
O2C—Pb1B—O2B^i	78.94 (15)	O3C—AsC—O1C^x	112.1 (2)
O3D—Pb1B—O2B^i	127.34 (16)	O3C—AsC—O2C	106.5 (3)
O1A^i—Pb1B—O2A	94.88 (15)	O1C^x—AsC—O2C	111.7 (2)
O1C^i—Pb1B—O2A	129.38 (15)	O3C—AsC—O3F	107.2 (3)
O1B—Pb1B—O2A	151.65 (14)	O1C^x—AsC—O3F	111.7 (2)
O2C—Pb1B—O2A	79.37 (15)	O2C—AsC—O3F	107.3 (3)
O3D—Pb1B—O2A	57.72 (14)	AsA—O1A—Pb1B^i	126.7 (2)
O2B^i—Pb1B—O2A	76.39 (15)	AsA—O1A—Pb1A	131.1 (2)
O1A^i—Pb1B—O3E	72.67 (16)	Pb1B^i—O1A—Pb1A	91.46 (15)
O1C^i—Pb1B—O3E	145.56 (15)	AsB^xi—O1B—Pb1A^i	129.3 (2)
O1B—Pb1B—O3E	87.11 (17)	AsB^xi—O1B—Pb1B	128.6 (2)
O2C—Pb1B—O3E	126.71 (16)	Pb1A^i—O1B—Pb1B	91.35 (15)
O3D—Pb1B—O3E	114.88 (18)	AsC^xii—O1C—Pb1B^i	130.2 (2)
O2B^i—Pb1B—O3E	56.08 (15)	AsC^xii—O1C—Pb1A	127.2 (2)
O2A—Pb1B—O3E	64.58 (16)	Pb1B^i—O1C—Pb1A	91.75 (15)
O1A^i—Pb1B—O3F	143.57 (14)	AsA—O2A—Pb2B^i	127.4 (3)
O1C^i—Pb1B—O3F	88.08 (15)	AsA—O2A—Pb1A^ii	105.2 (2)
O1B—Pb1B—O3F	70.32 (14)	Pb2B^i—O2A—Pb1A^ii	119.82 (19)
O2C—Pb1B—O3F	54.58 (14)	AsA—O2A—Pb1B	96.3 (2)
O3D—Pb1B—O3F	120.87 (16)	Pb2B^i—O2A—Pb1B	110.56 (19)
O2B^i—Pb1B—O3F	60.75 (14)	Pb1A^ii—O2A—Pb1B	87.43 (15)
O2A—Pb1B—O3F	120.37 (14)	AsB—O2B—Pb2C^i	128.3 (3)
O3E—Pb1B—O3F	112.43 (14)	AsB—O2B—Pb1A^vi	101.0 (2)
O1A^i—Pb1B—Pb1A^i	44.82 (11)	Pb2C^i—O2B—Pb1A^vi	117.4 (2)
O1C^i—Pb1B—Pb1A^i	44.14 (10)	AsC—O2C—Pb2A	127.6 (3)
O1B—Pb1B—Pb1A^i	43.38 (10)	AsC—O2C—Pb1B	107.6 (2)
O2C—Pb1B—Pb1A^i	129.46 (12)	Pb2A—O2C—Pb1B	119.60 (19)
O3D—Pb1B—Pb1A^i	100.79 (12)	AsA—O3A—Pb2A	105.8 (3)
O2B^i—Pb1B—Pb1A^i	131.63 (12)	AsB^i—O3B—Pb2C^xiii	140.0 (3)
O2A—Pb1B—Pb1A^i	138.43 (11)	AsC—O3C—Pb2A^iv	141.3 (3)
O3E—Pb1B—Pb1A^i	102.89 (12)	AsC—O3C—Pb1A^ii	100.5 (2)
O3F—Pb1B—Pb1A^i	101.17 (9)	Pb2A^iv—O3C—Pb1A^ii	109.46 (19)
O2C—Pb2A—O3C^iv	84.32 (19)	AsC—O3C—Pb2C	87.2 (2)
O2C—Pb2A—O3A	79.62 (18)	Pb2A^iv—O3C—Pb2C	111.52 (19)
O3C^iv—Pb2A—O3A	86.64 (17)	Pb1A^ii—O3C—Pb2C	98.04 (15)
O2C—Pb2A—O3F^v	81.73 (17)	AsA—O3D—Pb2B	140.8 (3)
O3C^iv—Pb2A—O3F^v	131.43 (19)	AsA—O3D—Pb1B	98.7 (2)
O3A—Pb2A—O3F^v	135.17 (16)	Pb2B—O3D—Pb1B	109.1 (2)
O2C—Pb2A—O3D	69.91 (16)	AsA—O3D—Pb2A	89.4 (3)
O3C^iv—Pb2A—O3D	139.11 (15)	Pb2B—O3D—Pb2A	112.0 (2)
O3A—Pb2A—O3D	58.50 (17)	Pb1B—O3D—Pb2A	99.36 (16)
O3F^v—Pb2A—O3D	76.85 (15)	AsB^i—O3E—Pb2B^i	101.8 (3)
O2C—Pb2A—O1B^v	98.32 (15)	AsB^i—O3E—Pb1B	95.6 (3)
O3C^iv—Pb2A—O1B^v	66.85 (14)	Pb2B^i—O3E—Pb1B	100.20 (17)
O3A—Pb2A—O1B^v	153.46 (15)	AsC—O3F—Pb2C	107.6 (2)
O3F^v—Pb2A—O1B^v	69.55 (14)	AsC—O3F—Pb1B	88.9 (2)
O3D—Pb2A—O1B^v	145.76 (13)	Pb2C—O3F—Pb1B	99.81 (16)
O2C—Pb2A—Cl	132.41 (13)	Pb2B—Cl—Pb2A	91.07 (4)
O3C^iv—Pb2A—Cl	143.26 (14)

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

(Mim393K)

Crystal data

As3ClO12Pb5	Dx = 7.256 Mg m^−3
Mr = 1488.16	Ag Kα radiation, λ = 0.56087 Å
Hexagonal, P63/m	Cell parameters from 7991 reflections
a = 10.2722 (3) Å	θ = 2.8–29.2°
c = 7.4537 (3) Å	µ = 37.60 mm^−1
V = 681.13 (5) Å^3	T = 393 K
Z = 2	Fragment, pale-orange
F(000) = 1244	0.10 × 0.06 × 0.04 mm

Data collection

XtaLAB Synergy, Dualflex, Hypix diffractometer	1202 independent reflections
Radiation source: micro-focus sealed X-ray tube	1060 reflections with I > 2σ(I)
Detector resolution: 0.0000 pixels mm^-1	Rint = 0.038
o scan	θmax = 29.2°, θmin = 1.8°
Absorption correction: multi-scan SCALE 3 ABSPACK	h = −15→17
Tmin = 0.367, Tmax = 1.000	k = −17→17
11659 measured reflections	l = −12→12

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.027	Secondary atom site location: Difmap
wR(F^2) = 0.059	w = 1/[σ^2(Fo^2) + (0.0248P)^2 + 4.3496P] where P = (Fo^2 + 2Fc^2)/3
S = 1.15	(Δ/σ)max < 0.001
1202 reflections	Δρmax = 2.41 e Å^−3
39 parameters	Δρmin = −3.93 e Å^−3

Special details

Experimental. CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.3333	0.6667	0.50673 (4)	0.02062 (8)
Pb2	0.00503 (3)	0.25169 (3)	0.2500	0.02343 (8)
As3	0.38361 (6)	0.40888 (7)	0.2500	0.01097 (10)
O1	0.4935 (6)	0.3303 (7)	0.2500	0.0217 (10)
O2	0.4853 (7)	0.5985 (6)	0.2500	0.0384 (17)
O3	0.2691 (7)	0.3587 (7)	0.0720 (7)	0.0481 (15)
Cl	0.0000	0.0000	0.0000	0.0261 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.02495 (10)	0.02495 (10)	0.01198 (11)	0.01247 (5)	0.000	0.000
Pb2	0.01882 (12)	0.01445 (11)	0.03684 (15)	0.00819 (9)	0.000	0.000
As3	0.0098 (2)	0.0113 (2)	0.0123 (2)	0.00559 (19)	0.000	0.000
O1	0.025 (2)	0.033 (3)	0.019 (2)	0.024 (2)	0.000	0.000
O2	0.017 (2)	0.013 (2)	0.080 (5)	0.004 (2)	0.000	0.000
O3	0.055 (3)	0.070 (4)	0.044 (3)	0.050 (3)	−0.037 (3)	−0.040 (3)
Cl	0.0253 (8)	0.0253 (8)	0.0276 (14)	0.0127 (4)	0.000	0.000

Geometric parameters (Å, º)

Pb1—O1^i	2.530 (3)	Pb2—O3	2.710 (7)
Pb1—O1^ii	2.530 (4)	Pb2—O3^vi	2.710 (7)
Pb1—O1^iii	2.530 (3)	As3—O2	1.689 (6)
Pb1—O2^iv	2.771 (4)	As3—O3^vi	1.674 (4)
Pb1—O2^v	2.771 (4)	As3—O3	1.674 (4)
Pb1—O2	2.771 (4)	As3—O1	1.684 (5)
Pb1—Pb1^vi	3.8272 (6)	O1—Pb1^iii	2.530 (3)
Pb1—O3^vii	13.435 (5)	O1—Pb1^x	2.530 (3)
Pb2—O2^v	2.352 (6)	O2—Pb2^iv	2.352 (6)
Pb2—O3^viii	2.629 (5)	O2—Pb1^vi	2.771 (4)
Pb2—O3^ix	2.629 (5)	O3—Pb2^xi	2.629 (5)
O1^i—Pb1—O1^ii	74.30 (13)	O2^v—Pb2—O3^viii	84.28 (15)
O1^i—Pb1—O1^iii	74.30 (13)	O2^v—Pb2—O3^ix	84.28 (15)
O1^ii—Pb1—O1^iii	74.30 (13)	O3^viii—Pb2—O3^ix	131.8 (3)
O1^i—Pb1—O2^iv	90.95 (12)	O2^v—Pb2—O3	74.44 (17)
O1^ii—Pb1—O2^iv	150.75 (17)	O3^viii—Pb2—O3	81.64 (8)
O1^iii—Pb1—O2^iv	126.57 (17)	O3^ix—Pb2—O3	138.46 (16)
O1^i—Pb1—O2^v	126.57 (17)	O2^v—Pb2—O3^vi	74.44 (17)
O1^ii—Pb1—O2^v	90.95 (12)	O3^viii—Pb2—O3^vi	138.46 (15)
O1^iii—Pb1—O2^v	150.75 (17)	O3^ix—Pb2—O3^vi	81.64 (8)
O2^iv—Pb1—O2^v	77.57 (13)	O3—Pb2—O3^vi	58.62 (19)
O1^i—Pb1—O2	150.75 (17)	O2—As3—O3^vi	106.8 (3)
O1^ii—Pb1—O2	126.57 (17)	O2—As3—O3	106.8 (3)
O1^iii—Pb1—O2	90.95 (12)	O3^vi—As3—O3	104.8 (5)
O2^iv—Pb1—O2	77.57 (13)	O2—As3—O1	112.1 (3)
O2^v—Pb1—O2	77.57 (13)	O3^vi—As3—O1	112.86 (19)
O1^i—Pb1—Pb1^vi	135.79 (8)	O3—As3—O1	112.86 (19)
O1^ii—Pb1—Pb1^vi	135.79 (8)	As3—O1—Pb1^iii	129.05 (14)
O1^iii—Pb1—Pb1^vi	135.79 (8)	As3—O1—Pb1^x	129.05 (14)
O2^iv—Pb1—Pb1^vi	46.33 (9)	Pb1^iii—O1—Pb1^x	91.57 (16)
O2^v—Pb1—Pb1^vi	46.33 (9)	As3—O2—Pb2^iv	128.2 (3)
O2—Pb1—Pb1^vi	46.33 (9)	As3—O2—Pb1	100.9 (2)
O1^i—Pb1—O3^vii	119.20 (9)	Pb2^iv—O2—Pb1	115.53 (16)
O1^ii—Pb1—O3^vii	69.83 (14)	As3—O2—Pb1^vi	100.9 (2)
O1^iii—Pb1—O3^vii	49.78 (12)	Pb2^iv—O2—Pb1^vi	115.53 (16)
O2^iv—Pb1—O3^vii	138.52 (11)	Pb1—O2—Pb1^vi	87.34 (17)
O2^v—Pb1—O3^vii	101.65 (12)	As3—O3—Pb2^xi	137.9 (3)
O2—Pb1—O3^vii	62.16 (10)	As3—O3—Pb2	98.3 (3)
Pb1^vi—Pb1—O3^vii	103.52 (2)	Pb2^xi—O3—Pb2	115.74 (19)

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