Crystal structure of the uranyl arsenate mineral hügelite, Pb2(UO2)3O2(AsO4)2(H2O)5, revisited: a correct unit cell, twinning and hydrogen bonding

Plášil, J.; Petříček, V.; Škácha, P.

doi:10.1107/S2052520621004091

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STRUCTURAL SCIENCE
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ISSN: 2052-5206

Volume 77| Part 3| June 2021| Pages 378-383

https://doi.org/10.1107/S2052520621004091

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Crystal structure of the uranyl arsenate mineral hügelite, Pb₂(UO₂)₃O₂(AsO₄)₂(H₂O)₅, revisited: a correct unit cell, twinning and hydrogen bonding

Jakub Plášil,^a ^* Václav Petříček ^a and Pavel Škácha ^b

^aInstitute of Physics ASCR, v.v.i., Na Slovance 2, Praha 8, 18221, Czech Republic, and ^bDepartment of Mineralogy and Petrology, National Museum, Cirkusová 1740, Praha 9, 19300, Czech Republic
^*Correspondence e-mail: plasil@fzu.cz

Edited by R. Černý, University of Geneva, Switzerland (Received 25 February 2021; accepted 16 April 2021; online 14 May 2021)

Revisiting the structure of uranyl arsenate mineral hügelite provided some corrections to the available structural data. The previous twinning model (by reticular merohedry) in hügelite has been corrected. Twinning of the monoclinic unit cell [a = 7.0189 (7) Å, b = 17.1374 (10) Å, c = 8.1310 (10) Å and β = 108.904 (10)°], which can be expressed as a mirror in [100], leads to a pseudo-orthorhombic unit cell (a = 7.019 Å, b = 17.137 Å, c = 61.539 Å and β = 90.02°), which is eight times larger, with respect to the unit-cell volume, than a real cell. Moreover, the unit cell of chosen here and the unit cell given by the previous structure description both lead to the same supercell. A new structure refinement undertaken on an untwinned crystal of hügelite resulted in R = 4.82% for 12 864 reflections with I_obs > 3σ(I) and GOF = 1.12. The hydrogen-bonding scheme has been proposed for hügelite for the first time.

Keywords: hügelite; uranyl arsenate; crystal structure; twinning; JANA2006; reticular merohedry.

CCDC reference: 2078490

1. Introduction

Uranyl arsenates are, along with uranyl phosphates, the most common alteration products after oxidation weathering of uraninite (Finch & Murakami, 1999 ; Krivovichev & Plášil, 2013 ; Plášil, 2014 ). They occur in the uppermost oxidized parts of uranium deposits, surviving the near-surface or surface conditions due to their very low solubility in aqueous solutions (e.g. Vochten & Goeminne, 1984 ; Gorman-Lewis et al., 2009 ; Maher et al., 2013 ). The most common uranyl arsenates comprise minerals of the well-known autunite group: a Cu-member zeunerite, Cu[(UO₂)(AsO₄)]₂(H₂O)₁₂, and a Ca-member uranospinite, Ca[(UO₂)(AsO₄)]₂(H₂O)₁₀. The mineral hügelite, Pb₂[(UO₂)₃O₂(AsO₄)₂](H₂O)₅, was described originally as a lead–zinc vanadate hydrate (Dürrfeld, 1913 ), but was redetermined later (Walenta & Wimmenauer, 1961 ) as a lead uranyl arsenate hydrate, structurally related to dumontite, Pb₂[(UO₂)₃O₂(PO₄)₂]·5H₂O (Piret & Piret-Meunier, 1988 ). Later on, it was investigated again, from the material originating from the type locality, which is the Michael Mine at Weiler, near Lahr in the Black Forest, Baden–Württemberg, Germany (Walenta, 1979 ). This study updated morphological crystallographic data and physical and optical properties, providing a new formula, Pb₂(UO₂)₃(AsO₄)₂(OH)₄·3H₂O, and produced new crystallographic data. According to that study, hügelite is monoclinic, space group P2₁/m or P2₁, with a = 8.13 Å, b = 17.27 Å, c = 7.01 Å, β = 109°, Z = 2 and D_calc = 5.80 Mg m⁻³. In 2003, Locock & Burns (2003 ) undertook a modern crystallographic study based on a crystal originating from `Geroldseck, Baden', Germany. Based on the diffraction experiment using a four-circle diffractometer with a CCD detector, they inferred hügelite to be monoclinic, twinned by pseudomerohedry, with unit-cell parameters a = 31.066 (3) Å, b = 17.303 (2) Å, c = 7.043 (1) Å, β = 96.492 (2)°, V = 3761.6 (1) Å³, Z = 8 and D_calc = 5.74 Mg m⁻³. Thus, the unit-cell reported by them is twice as large as the original description. They reported that the crystal was twinned by pseudomerohedry, giving a very large pseudo-orthorhombic C-centred cell with the dimensions (transformed settings) a = 7.043 Å, b = 61.733 Å, c = 17.303 Å and γ = 90.02°. They further commented on and judged this twinning model, and presented a final refinement with a reasonable R₁ value of 3.3%, nevertheless with a very low value of goodness-of-fit, S = 0.68 (thus, we assume the authors overestimated their data quality). We notice that Bruker SHELXTL Version 5 was used in the aforementioned study.

The new find of the rare mineral hügelite from the small uranium deposit Labská, Krkonoše Mts. (Czechia), prompted us to perform a new diffraction experiment, which revealed that the actual twinning in hügelite is different from the description presented by Locock & Burns (2003). Here we report on the results of our analysis that might help to understand the nature of the twinning in this mineral, as well as helping in future analyses of similarly twinned crystal structures.

2. Methodology

2.1. Sample

The hügelite crystal used in this study was extracted from a specimen collected by Pavel Škácha from the Labská uranium deposit. This small uranium deposit is located approximately 5 km to the south of the town of Špindlerův Mlýn in the Krkonoše Mountains (Eastern Bohemia, Czechia). Hügelite forms elongated prismatic crystals apparently flattened on one of the prismatic faces. Crystals reach maximally up to 1 mm across (Fig. 1). They are dark orange in colour. Hügelite was found on a few specimens only, associated with more abundant dumontite. Phosphuranylite and saleéite were also identified in the association.

Figure 1
An aggregate of the tabular yellow crystals of hügelite from the Labská deposit. Field of view 7 mm (photo by P. Škácha).

2.2. Single-crystal X-ray diffraction

We studied two tiny crystals of hügelite from the Labská deposit. While the first crystal (hereafter denoted Labská I) of approximate dimensions 0.038 × 0.013 × 0.007 mm was later found to be affected by twinning, the second crystal (Labská II), having similar, but somewhat larger, dimensions (0.067 × 0.018 × 0.005 mm) was found later on to be untwinned. Diffraction experiments were carried out at room temperature with a Rigaku SuperNova single-crystal diffractometer. The diffraction experiment was carried out using Mo Kα radiation (λ = 0.71073 Å) from a micro-focus X-ray tube collimated and monochromated by mirror optics and detected by an Atlas S2 CCD detector.

For both experiments, ω-rotational scans (of frame width 1°) were adopted and a full sphere of the diffraction data was collected. For the larger crystal, Labská II, an increased counting time per frame, equal to 840 s (compared to 400 s for Labská I), a high-sensitivity mode of the CCD detector (binning of pixels 2×2, with a high-gain option) and high-redundancy of the data set (∼7) were used to reveal even weak reflections.

The diffraction experiment for Labská I, as expected, due to previous results given by Locock & Burns (2003), provided a particularly complicated diffraction pattern, caused by twinning due to reticular merohedry (Petříček et al., 2016 ). The studied crystal was found to be monoclinic, but with different unit-cell parameters than given by Locock & Burns (2003). Actually, the unit-cell parameters found are a = 7.0189 (7) Å, b = 17.1374 (10) Å, c = 8.1310 (10) Å and β = 108.904 (10)°, with V = 925.29 (15) Å³ and Z = 2 (Table 1). The reticular twin (diffraction type II) was found by the routine implemented in the JANA2006 program (Petříček et al., 2014 ). The twin operation is a mirror in the [100] direction; the second twin domain can be obtained by the matrix (−1 0 0 | 0 1 0 | 0.75 0 1), simulating a pseudo-orthorhombic supercell, which is eight times larger than a real (sub)cell (a = 7.019 Å, b = 17.137 Å, c = 61.539 Å and β = 90.02°). Therefore, during the data reduction, each twin domain was integrated alone and later imported into the JANA2006 program utilizing the already known twin matrix that helped to define the orientation of each unit cell, thus resolving fully overlapped reflections. Those reflections, present in both data blocks, were included only one time to avoid their multiple occurrences in the refinement. The refinement in JANA2006 including the twin model led to reasonable values of the twin fractions, i.e. 0.877 (1):0.123 (1) (Table 1); noticeably, the second twin domain is rather weak. The refinement, which took into account twinning, improved/smoothed slightly the difference Fourier; nevertheless, there are still false maxima due to poorly fitted absorption (apparent in the vicinity of the U atoms). The fact that intensities (and namely those of the contributing second domain) are quite weak resulted in the refinement converging to higher R = 7.58% for 2110 reflections with I > 3σ(I) (GOF = 1.63); noticeably, on first sight, we have also to take into account a different approach to the weighting scheme of the current refinement and a criterion for observed intensities.

Table 1
Details of the data collection and refinement for the two different crystals of hügelite from the Labská deposit

	Labská I	Labská II
Structural formula	Pb₂(UO₂)₃O₂[(As_0.597P_0.403)O₄)]₂(H₂O)₅	Pb₂(UO₂)₃O₂[(As_0.583P_0.417)O₄)]₂(H₂O)₅
a, b, c (Å), β (°)	7.0189 (7), 17.137 (1), 8.131 (1), 108.90 (1)	7.0258 (3), 17.1769 (5), 8.1463 (7), 108.886 (5)
V (Å³)	925.3 (2)	930.18 (10)
Space group	P2₁/m	P2₁/m
Z	2	2
D_calc (Mg m⁻³) for the above formula	5.667	5.669
Temperature (K)	297	297
Radiation type, wavelength (Å)	Mo Kα, 0.71073	Mo Kα, 0.71073
Crystal dimensions (µm)	38 × 18 × 7	67 × 18 × 5
Limiting θ angles (°)	2.90–29.48	2.38–29.78
Limiting Miller indices	–9 ≤ h ≤ 9, −23 ≤ k ≤ 23, −11 ≤ l ≤ 10	–9 ≤ h ≤ 9, −23 ≤ k ≤ 23, −11 ≤ l ≤ 10
No. of reflections measured	21 107	19 219
No. of unique reflections	4200	19 152
No. of observed reflections (criterion)	2107 [I_obs > 3σ(I)]	12 864 [I_obs > 3σ(I)]
Completeness, R_int	0.93, 0.148	0.92, 0.069
Absorption correction (mm⁻¹), T_min, T_max	46.59, 0.645, 1.000	46.30, 0.501, 1.000
F₀₀₀	1319	1338
Parameters refined, restraints, constraints	134, 0, 13	141, 3, 27
R, wR (obs)	0.0763, 0.1837	0.0482, 0.1181
R, wR (all)	0.1591, 0.2263	0.0750, 0.1373
GOF obs, GOF all	1.67, 1.49	1.12, 1.07
Δρ_min, Δρ_max (e Å⁻³)	−4.02, 6.61 (0.6 Å to U1)	−4.02, 5.04 (0.8 Å to U1)
Weighting scheme	w = 1/[σ²(I) + 0.0036I²]	w = 1/[σ²(I) + 0.0036I²]
Twin fractions 1, 2	0.8734 (12), 0.1266 (12)
Twin matrix
	$[\left({\matrix{ 1 & 0 & 0 \cr 0 & 1 & 0 \cr {0.75} & 0 & { - 1} \cr } } \right)]$

The diffraction experiment for Labská II provided a similar unit cell, with a = 7.0258 (3) Å, b = 17.1769 (5) Å, c = 8.1463 (7) Å and β = 108.886 (5)°, with V = 930.18 (6) Å³ and Z = 2 (Table 1). The second experiment indicated that the crystal is less affected by the twinning than the first crystal; the current unit cell indexed 82% of all observed reflections compared to 29% indexed from the first experiment. The reciprocal space projections and reconstructions did not reveal any important contribution of the second domain; this was also proven later from the refinement. The second refinement in JANA2006 converged to excellent agreement factors (Table 1). It is noteworthy that the GOF for the Labská II refinement is 1.07 for all 19 152 reflections.

Structure solution for the Labská I crystal was carried out using the intrinsic phasing algorithm of the SHELXT program (Sheldrick, 2015 ); refinement of Labská II was carried out using the model obtained for Labská I. Details of the data collection and refinement for both crystals are given in Table 1, final atomic coordinates and displacement parameters in Table 2, selected interatomic distances and hydrogen-bond parameters in Table 3, and a bond-valence analysis in Table 4. The bond-valence analysis was made following the procedure of Brown (2002 , 2009 ) using bond-valence parameters provided by Gagné & Hawthorne (2015 ). The formula of the crystal studied, based on refined occupancies and bond-valence calculations, is Pb₂(UO₂)₃O₂[(As_0.583P_0.417)O₄)]₂(H₂O)₅ (Z = 2 and D_calc = 5.669 Mg m⁻³).

Table 2
Atomic coordinates, isotropic and equivalent displacement parameters (Å) and site occupancies for the crystal structure of hügelite (Labská II)

Atom	x/a	y/b	z/c	U_iso*/U_eq
U1	0.20432 (12)	0.64347 (4)	0.41418 (11)	0.0148 (3)
U2	0.70073 (18)	0.75	0.40346 (17)	0.0179 (4)
Pb	0.63490 (15)	0.39415 (5)	0.05046 (13)	0.0277 (4)
As**	0.6916 (4)	0.55246 (16)	0.3866 (4)	0.0148 (11)
O1	1.008 (3)	0.75	0.380 (3)	0.016 (5)
O2	0.390 (3)	0.75	0.417 (3)	0.016 (5)
O3	0.807 (4)	0.75	0.632 (3)	0.032 (9)
O4	0.146 (3)	0.6333 (9)	0.184 (2)	0.022 (6)
O5	1.165 (4)	0.75	0.918 (3)	0.036 (10)
O6	0.590 (4)	0.75	0.170 (3)	0.025 (9)
O7	0.262 (3)	0.6491 (8)	0.646 (2)	0.028 (7)
O8	0.542 (3)	0.6162 (9)	0.435 (3)	0.033 (7)
O9	0.585 (3)	0.5111 (10)	0.203 (2)	0.035 (7)
O10	0.288 (4)	0.3429 (15)	0.088 (3)	0.067 (12)
O11	0.863 (3)	0.6154 (10)	0.374 (3)	0.037 (8)
O12	0.999 (3)	0.4474 (12)	0.137 (3)	0.044 (8)
O13	0.781 (2)	0.4928 (8)	0.543 (2)	0.021 (6)
H1o5	1.076 (9)	0.75	0.962 (10)	0.0315*
H2o5	1.123 (12)	0.75	0.8153 (17)	0.0315*
H1o10	0.2364	0.3051	0.03525	0.0778*
H2o10	0.2463	0.3656	0.1567	0.0778*
H1o12	1.0882	0.4218	0.1242	0.0534*
H2o12	1.0236	0.4910	0.1855	0.0534*
Note: (**) occupancy 0.597 (16) As/0.403 (16) P.

Table 3
Selected interatomic distances (Å) and hydrogen-bond geometry (Å, °) in the structure of hügelite (Labská II)

U1—O4	1.808 (5)	U2—O1	2.238 (7)	Pb—O4^iv	2.835 (6)
U1—O7	1.811 (6)	U2—O2	2.228 (6)	Pb—O5^v	2.809 (3)
U1—O1ⁱ	2.245 (4)	U2—O3	1.796 (8)	Pb—O6^vi	3.169 (4)
U1—O2	2.242 (4)	U2—O6	1.799 (7)	Pb—O7ⁱⁱ	2.455 (5)
U1—O8	2.387 (5)	U2—O8	2.611 (5)	Pb—O9	2.447 (6)
U1—O11ⁱ	2.366 (5)	U2—O8ⁱⁱⁱ	2.611 (5)	Pb—O9^iv	2.664 (5)
U1—O13ⁱⁱ	2.362 (5)	U2—O11	2.638 (5)	Pb—O10	2.670 (7)
〈U1—O_uranyl〉	1.810	U2—O11ⁱⁱⁱ	2.638 (5)	Pb—O12	2.585 (5)
〈U1—O_eq〉	2.320	〈U2—O_uranyl〉	1.798	〈Pb—O〉	2.704
		〈U2—O_eq〉	2.494
		As/P—O8	1.629 (6)
		As/P—O9	1.617 (5)
		As/P—O11	1.640 (5)
		As/P—O13	1.589 (5)
		〈As/P—O〉	1.619

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H1o5⋯O10^xv	0.82 (2)	2.96 (6)	3.78 (1)	136 (4)
O5—H2o5⋯O3^v	0.820 (16)	2.23 (6)	2.838 (9)	131 (7)
O10—H1o10⋯O6^vi	0.82	2.55	2.973 (10)	113
O10—H2o10⋯O12ⁱ	0.82	2.21	2.876 (9)	138
O12—H1o12⋯O10^viii	0.82	2.06	2.876 (9)	172
O12—H2o12⋯O13^vii	0.82	2.22	2.746 (8)	122
Symmetry codes: (i) ; (ii) −x + 1, −y + 1, −z + 1; (iii) x, −y + $[3 \over 2]$ , z; (iv) −x + 1, −y + 1, −z; (v) −x + 2, y − $[1 \over 2]$ , −z + 1; (vi) $[-x+1, y-{\script{1\over 2}}, -z]$ ; (vii) ; (viii) x+1, y, z; (xv) x+1, y, z+1.

Table 4
Bond-valence analysis (all values given in valence units, v.u.) for hügelite

The bond-valence parameters are taken from Gagné & Hawthorne (2015).

	U1	U2	As	Pb	H1O5	H2O5	H1O10	H2O10	H1O12	H2O12	sum^–H	sum^+H*
O1	0.66	0.67									1.32
O2	0.66	0.68									1.34
O3		1.70				0.20					1.70	1.90
O4	1.65			0.16						0.20	1.82	2.02
O5				0.17	0.80	0.80					0.17	1.77
O6		1.69		0.08			0.20				1.76	1.96
O7	1.64			0.38							2.03	2.03
O8	0.49	0.30	1.27								2.06	2.06
O9			1.31	0.63							1.94	1.94
O10				0.24	0.20		0.80	0.80	0.20		0.24	2.04
O11	0.51	0.29	1.23								2.03	2.03
O12				0.29				0.20	0.80	0.80	0.29	2.09
O13	0.51		1.42								1.93	1.93
Sum	6.12	5.91	5.23	1.95	1.00	1.00	1.00	1.00	1.00	1.00
Note: (*) idealized bond strengths taken from Brown (2002).

Twin contributions were evaluated visually using the reciprocal layers (Fig. 2) reconstructed from the CCD frames (UNWARP tool within the CrysAlis software; Rigaku OD, 2019 $[Rigaku (2019). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, Oxfordshire, England.]$ ) and by computer methods using the program JANA2006 (Fig. 3). Twinning and the extra reflections due to twinning are easily visible for the Labská I crystal at the h0l and hk2 layers, for instance, while Labská II provided unbiased frames (Fig. 3). The presence of additional reflections can bias the indexing algorithms, because it simulates the larger unit-cell parameter. While the refinement of the Labská I crystal returned the refined twin fractions 0.877 (1) and 0.123 (1) (Table 1), the second crystal showed a negligible contribution of twinning only when a mirror operation was taken into account, Tw_vol1/Tw_vol2 = 0.9994 (5)/0.0006 (5).

Figure 2
Twinning in hügelite, showing the reciprocal space reconstruction for the twinned (Labská I) and untwinned (Labská II) crystals. The twin contribution is easily visible in the case of the h0l layer. The biased intensities are apparent for the hk2 layer.

Figure 3
Twinning in hügelite, showing (a) the reciprocal space reconstructed from the intensity data in JANA2006 displaying the contribution of the second domain (green). The correct unit-cell vectors are displayed as red and green rectangles. The choice for the centred cell of Locock & Burns (2003

) is given in the black dashed lines. (b) The reciprocal space reconstruction of the corresponding h0l layer.

3. Results

Our description of the twinning in hügelite leaves the structure model proposed by Locock & Burns (2003) unchanged. The structure possesses uranyl–arsenate sheets with a phosphuranylite topology (Burns, 2005 ; Lussier et al., 2016 ), with Pb²⁺ cations located in the interlayer space between the infinite sheets (Fig. 4).

Figure 4
The crystal structure of hügelite projected down the monoclinic b axis. UO₇ bipyramids are shown in transparent yellow, UO₈ bipyramids are opaque yellow, (As/P)O₄ tetrahedra are green, Pb atoms are dark gray (shown as displacement ellipsoids at the 75% probability level), H atoms are light gray and O atoms are red. The unit-cell edges are outlined with solid black lines. H⋯A bonds have been omitted for clarity.

3.1. Twinning in hügelite

The twin operation, i.e. a mirror in [100], leads to a rather large supercell, with V ∼ 7400 Å³. There is a clear relationship between the unit cell derived by Locock & Burns (2003) and the supercell found in our study. The cell of Locock & Burns (2003) is half the volume of the supercell of our choice: our cell thus represents a real cell of hügelite, while the cell of Locock & Burns is a result of twinning (Fig. 3); the unit cell of Locock & Burns (2003) (a = 30.993 Å, b = 17.159 Å, c = 7.022 Å and β = 96.44), when applied a mirror in (001), leads to the same supercell as in the current study. The correct description of twinning in hügelite confirmed the originally reported unit cell (Walenta, 1979), having a unit-cell volume of ∼930 Å³. The correct unit cell of hügelite (V ∼ 930 Å³), when compared to dumontite (V ∼ 920 Å³), confirms that these two minerals are isotypic As- and P-dominant analogs, respectively. The increase of the unit-cell volume towards the As end member (hügelite), due to the larger effective ionic radius of As⁵⁺ compared to P⁵⁺, is apparent. It should be noted that the currently investigated crystal of hügelite is not an end member of the solid-solution series, based on the site-scattering refinement (Tables 1 and 2).

3.2. Hydrogen bonding in hügelite

Although hügelite is a highly absorbing substance, even for Mo X-rays (μ = 46.30 mm⁻¹), final difference-Fourier calculations revealed few maxima assignable to H atoms around those O atoms that belong, according to the bond-valence analysis, to H₂O groups. Because it was impossible to freely refine all the parameters of the H atoms, they were refined using restrictions available in JANA2006 for the hydrogen-bond geometry. Therefore, the scheme presented should be considered as an approximation at best. We also have to emphasize that the higher BV sums for both H atoms and the donor O atoms resulted from the used restraint on the A—H bond length taken as 0.82 Å as a conservative value for the hydrogen-bond length from X-ray analysis.

The hydrogen-bonding scheme can be deduced from the results of the bond-valence analysis (Table 4). There are three symmetrically independent H₂O sites (corresponding to O5, O10 and O12), indicating five H₂O molecules per unit cell for Z = 2. While atom O5 seems to be three-coordinated (one bond from Pb1 and two bonds to H1O5 and H2O5), atoms O10 and O12 are five- and four-coordinated, respectively. According to the terminology introduced by Schindler & Hawthorne (see, for example, Schindler & Hawthorne, 2008 ), O5 represents the transformer H₂O group, while O10 represents an inverse transformer and O12 represents a nontransformer H₂O group. Therefore, the current results are in contrast to the theoretical predictions made by Schindler & Hawthorne (2008), who concluded that hügelite should contain five inverse transformer (H₂O) groups, based on the bond-valence approach. The above-mentioned scheme should be taken as a best-available model only. Due to underbonding of the O1 U_eq and O2 U_eq atoms (with corresponding low BV sums; Table 4), we can speculate about a somewhat different configuration, involving also the two O atoms U_eq. Nevertheless, for such a task, employment of advanced theoretical approaches, as used recently for the uranyl phosphate mineral phurcalite (Plášil et al., 2020 ), would be necessary.

4. Implications – processing the data using JANA2006 to reveal the nature of twinning

Despite the fact that we did not have an original reflection file for the refinement of Locock & Burns (2003), the software we used for the structure analysis, JANA2006, enables us to perform a check for twinning in their structure, based on the available crystallographic information file (CIF). We have to emphasize here that the warning for the hidden translation symmetry in the CIF file of Locock & Burns (2003) was also indicated by PLATON ADDSYM (a quick test in IUCr checkCIF), returning the B Alert: `PLAT113_ALERT_2_B ADDSYM Suggests Possible Pseudo/New Space Group P2₁/m Check Note: (Pseudo) Lattice Translation Implemented'. The entire procedure we followed in JANA2006 is displayed in Fig. 5. The first step involves a calculation of the theoretical reflection file (Mo Kα, full sphere) based on the atom positions in the CIF of Locock & Burns (2003). The next step involves the calculation of the Patterson map. As the autoconvolution of the electron density itself, it provides important information of the real metrics and can thus reveal the real periodicity features underlying the data. This analysis showed three pronounced Patterson maxima; from them, assuming the omnipresent inversion in the Patterson map, we obtained three translation vectors: (0, 0, 0), (− $[1 \over 4]$ , 0, $[1 \over 4]$ ), ( $[1 \over 2]$ , 0, $[1 \over 2]$ ), ( $[1 \over 4]$ , 0, − $[1 \over 4]$ ). Those were used for the unit-cell transformation by the matrix | $[1 \over 4]$ 0 − $[1 \over 4]$ | 0 1 0 | 0 0 1 |. After axis transformation (a→c), we obtained the following cell: a = 7.043 Å, b = 17.30 Å, c = 8.1554 Å, α = 90°, β = 108.879° and γ = 90°. During the next step, the creation of the refinement reflection file (even if from the simulated data), there were 24 reflections found that violated the translation symmetry. Nevertheless, they were weak. The structure after the transformation into the smaller cell shows few atoms projected into very close positions (<0.5 Å). Merging the 24 atoms and refinement of the simulated structure led then to reasonably low R values (∼4.2% for 2771 reflections). The test for twinning by reticular merohedry/pseudomerohedry (Petříček et al., 2016) readily revealed an orthorhombic supercell (7.043 Å, 17.302 Å, 61.733 Å, 90°, 89.98°, 90°), with a unit-cell volume eight times larger than the real cell. This supercell is a result of the twinning that can be described as a mirror in (100) of the a = 7.043 Å, b = 17.302 Å, c = 8.1554 Å, α = 90°, β = 108.879° and γ = 90° cell. Fig. 3(a) displays a pattern of the eight times larger cell; from this point of view, the cell choice of Locock & Burns (2003) is reasonable and is due to twinning, which had been present in their crystal without any shadow of a doubt.

Figure 5
Diagram displaying the procedure for twin-testing in JANA2006.

Supporting information

CCDC reference: 2078490

Crystal structure: contains datablock global. DOI: https://doi.org/10.1107/S2052520621004091/ra5095sup1.cif

CIF file for the Labska I crystal (twinned). DOI: https://doi.org/10.1107/S2052520621004091/ra5095sup2.txt

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2052520621004091/ra5095Isup3.hkl

Computing details top

Data collection: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018); cell refinement: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018); data reduction: CrysAlis PRO 1.171.39.46 (Rigaku OD, 2018).

(global) top

Crystal data top

Pb₂U₃As_.201O₂₁P_0.799H₁₀	F(000) = 1338
M_r = 1587.7	D_x = 5.669 Mg m⁻³
Monoclinic, P12₁/m1	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 7003 reflections
a = 7.0258 (3) Å	θ = 2.7–29.3°
b = 17.1769 (5) Å	µ = 46.30 mm⁻¹
c = 8.1463 (7) Å	T = 297 K
β = 108.886 (5)°	Prismatic, yellow
V = 930.18 (10) Å³	0.07 × 0.02 × 0.01 mm
Z = 2

Data collection top

SuperNova, Dual, Cu at home/near, AtlasS2 diffractometer	19152 independent reflections
Radiation source: X-ray tube	12864 reflections with I > 3σ(I)
Mirror monochromator	R_int = 0.069
Detector resolution: 10.4054 pixels mm^-1	θ_max = 29.8°, θ_min = 2.4°
ω scans	h = −9→9
Absorption correction: multi-scan CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	k = −23→23
T_min = 0.501, T_max = 1	l = −11→10
19219 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.048	Hydrogen site location: difference Fourier map
wR(F²) = 0.137	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0036I²)
19152 reflections	(Δ/σ)_max = 0.016
141 parameters	Δρ_max = 5.04 e Å⁻³
3 restraints	Δρ_min = −4.02 e Å⁻³
27 constraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
U1	0.20433 (3)	0.643329 (14)	0.41403 (4)	0.01152 (9)
U2	0.70080 (5)	0.75	0.40310 (5)	0.01446 (13)
Pb	0.63520 (4)	0.394231 (17)	0.05030 (4)	0.02458 (11)
As	0.69116 (12)	0.55223 (5)	0.38661 (13)	0.0122 (4)	0.583 (5)
P	0.69116 (12)	0.55223 (5)	0.38661 (13)	0.0122 (4)	0.417 (5)
O1	1.0114 (9)	0.75	0.3837 (9)	0.018 (2)
O2	0.3903 (8)	0.75	0.4195 (9)	0.014 (2)
O3	0.8069 (9)	0.75	0.6354 (10)	0.027 (3)
O4	0.1462 (7)	0.6320 (3)	0.1824 (7)	0.0220 (19)
O5	1.1685 (10)	0.75	0.9215 (10)	0.026 (3)
O6	0.5906 (9)	0.75	0.1706 (9)	0.020 (3)
O7	0.2622 (7)	0.6501 (3)	0.6470 (7)	0.0222 (19)
O8	0.5439 (7)	0.6152 (3)	0.4342 (8)	0.028 (2)
O9	0.5839 (7)	0.5119 (3)	0.2001 (7)	0.030 (2)
O10	0.2938 (9)	0.3432 (5)	0.0899 (9)	0.065 (4)
O11	0.8630 (7)	0.6144 (3)	0.3737 (8)	0.030 (2)
O12	0.9983 (7)	0.4479 (2)	0.1406 (9)	0.044 (3)
O13	0.7802 (6)	0.4928 (3)	0.5421 (7)	0.0210 (19)
H1o5	1.076 (9)	0.75	0.962 (10)	0.0315*
H2o5	1.123 (12)	0.75	0.8153 (17)	0.0315*
H1o10	0.2364	0.3051	0.0353	0.0778*
H2o10	0.2463	0.3656	0.1567	0.0778*
H1o12	1.0882	0.4218	0.1242	0.0534*
H2o12	1.0236	0.4910	0.1855	0.0534*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.00715 (13)	0.01164 (13)	0.01755 (16)	−0.00017 (9)	0.00645 (10)	−0.00019 (11)
U2	0.00681 (17)	0.01711 (19)	0.0206 (2)	0	0.00602 (15)	0
Pb	0.02451 (16)	0.02622 (17)	0.02344 (19)	0.00249 (12)	0.00834 (12)	0.00213 (13)
As	0.0067 (5)	0.0104 (5)	0.0194 (7)	0.0007 (3)	0.0042 (4)	0.0000 (4)
P	0.0067 (5)	0.0104 (5)	0.0194 (7)	0.0007 (3)	0.0042 (4)	0.0000 (4)
O1	0.015 (3)	0.017 (4)	0.020 (4)	0	0.004 (3)	0
O2	0.011 (3)	0.015 (3)	0.018 (4)	0	0.007 (3)	0
O3	0.021 (4)	0.033 (4)	0.027 (5)	0	0.008 (3)	0
O4	0.028 (3)	0.032 (3)	0.008 (3)	−0.005 (2)	0.009 (2)	−0.005 (2)
O5	0.030 (4)	0.036 (5)	0.014 (5)	0	0.009 (3)	0
O6	0.017 (3)	0.035 (4)	0.004 (4)	0	0.000 (3)	0
O7	0.021 (3)	0.023 (3)	0.023 (3)	0.001 (2)	0.008 (2)	0.004 (2)
O8	0.017 (3)	0.021 (3)	0.052 (4)	0.003 (2)	0.017 (3)	0.002 (3)
O9	0.038 (3)	0.021 (3)	0.030 (4)	0.012 (2)	0.009 (3)	0.008 (3)
O10	0.047 (4)	0.079 (6)	0.081 (7)	0.003 (4)	0.038 (4)	−0.009 (5)
O11	0.015 (2)	0.020 (3)	0.060 (5)	−0.004 (2)	0.016 (3)	0.007 (3)
O12	0.041 (3)	0.036 (4)	0.060 (5)	−0.006 (3)	0.022 (3)	−0.013 (4)
O13	0.026 (3)	0.011 (2)	0.028 (4)	0.002 (2)	0.013 (2)	−0.001 (2)

Geometric parameters (Å, º) top

U1—O1ⁱ	2.245 (4)	O4—H2o10^xiv	3.2097
U1—O2	2.242 (4)	O4—H1o12^iv	2.6721
U1—O4	1.808 (5)	O4—H2o12ⁱ	2.5728
U1—O7	1.811 (6)	O5—O6^xv	3.003 (8)
U1—O8	2.387 (5)	O5—O7^viii	3.055 (9)
U1—O11ⁱ	2.366 (5)	O5—O7^ix	3.055 (9)
U1—O13ⁱⁱ	2.362 (5)	O5—H1o5	0.82 (8)
U1—H2o12ⁱ	3.2237	O5—H2o5	0.820 (16)
U2—As	3.3996 (9)	O5—H1o10^xi	3.1236
U2—Asⁱⁱⁱ	3.3996 (9)	O5—H1o10ⁱⁱ	3.1236
U2—P	3.3996 (9)	O5—H2o10^xi	3.4114
U2—Pⁱⁱⁱ	3.3996 (9)	O5—H2o10ⁱⁱ	3.4114
U2—O1	2.238 (7)	O5—H1o12^xii	3.415
U2—O2	2.228 (6)	O5—H1o12^vii	3.415
U2—O3	1.796 (8)	O6—O8	3.246 (8)
U2—O6	1.799 (7)	O6—O8ⁱⁱⁱ	3.246 (8)
U2—O8	2.611 (5)	O6—O10^x	2.973 (10)
U2—O8ⁱⁱⁱ	2.611 (5)	O6—O10^iv	2.973 (10)
U2—O11	2.638 (5)	O6—O11	3.127 (6)
U2—O11ⁱⁱⁱ	2.638 (5)	O6—O11ⁱⁱⁱ	3.127 (6)
Pb—O4^iv	2.835 (6)	O6—H1o5^xiii	3.46 (5)
Pb—O5^v	2.809 (3)	O6—H1o10^x	2.5508
Pb—O6^vi	3.169 (4)	O6—H1o10^iv	2.5508
Pb—O7ⁱⁱ	2.455 (5)	O7—O7ⁱⁱⁱ	3.432 (7)
Pb—O9	2.447 (6)	O7—O8	3.082 (9)
Pb—O9^iv	2.664 (5)	O7—O9ⁱⁱ	3.097 (7)
Pb—O10	2.670 (7)	O7—O10ⁱⁱ	3.164 (7)
Pb—O12	2.585 (5)	O7—O11ⁱ	3.026 (6)
Pb—H1o5^v	3.22 (4)	O7—O12ⁱⁱ	3.351 (9)
Pb—H2o5^v	3.00 (4)	O7—O13ⁱⁱ	2.861 (7)
Pb—H1o10	3.1607	O7—H2o5ⁱ	2.58 (5)
Pb—H2o10	3.1607	O7—H2o10ⁱⁱ	3.3138
Pb—H1o12	3.0784	O8—O9	2.686 (8)
Pb—H2o12	3.0784	O8—O11	2.446 (8)
As—P	0	O8—O13	2.647 (6)
As—O8	1.629 (6)	O8—O13ⁱⁱ	2.991 (7)
As—O9	1.617 (5)	O8—H2o10ⁱⁱ	3.1955
As—O11	1.640 (5)	O9—O9^iv	3.114 (8)
As—O13	1.589 (5)	O9—O10	3.490 (9)
As—H2o12	3.4234	O9—O11	2.673 (7)
As—H2o12^vii	3.4922	O9—O12	3.291 (8)
P—O8	1.629 (6)	O9—O13	2.699 (7)
P—O9	1.617 (5)	O9—H2o10	3.3949
P—O11	1.640 (5)	O9—H2o12	3.1495
P—O13	1.589 (5)	O10—O10^xvi	3.201 (11)
P—H2o12	3.4234	O10—O12ⁱ	2.876 (9)
P—H2o12^vii	3.4922	O10—H1o5^xvii	2.96 (5)
O1—O2^viii	2.583 (9)	O10—H1o10	0.82
O1—O3	2.860 (12)	O10—H1o10^xvi	2.5937
O1—O4^viii	2.950 (8)	O10—H2o10	0.82
O1—O4^ix	2.950 (8)	O10—H1o12ⁱ	2.0611
O1—O6	2.904 (8)	O10—H2o12ⁱ	3.4085
O1—O7^viii	2.864 (7)	O11—O13	2.664 (8)
O1—O7^ix	2.864 (7)	O11—O13^vii	3.005 (6)
O1—O11	2.543 (6)	O11—H1o10^iv	3.4639
O1—O11ⁱⁱⁱ	2.543 (6)	O11—H2o12	3.0388
O1—H2o5	3.345 (18)	O12—O12^xviii	2.913 (9)
O1—H1o10^x	3.4246	O12—O13^vii	2.746 (8)
O1—H1o10^iv	3.4246	O12—H1o5^v	3.498 (16)
O2—O3	2.886 (8)	O12—H1o10^viii	3.2372
O2—O4	2.939 (6)	O12—H2o10^viii	2.2143
O2—O4ⁱⁱⁱ	2.939 (6)	O12—H1o12	0.82
O2—O6	2.817 (11)	O12—H1o12^xviii	3.0309
O2—O7	2.876 (8)	O12—H2o12	0.82
O2—O7ⁱⁱⁱ	2.876 (8)	O12—H2o12^xviii	2.8137
O2—O8	2.540 (5)	O13—O13^vii	3.383 (7)
O2—O8ⁱⁱⁱ	2.540 (5)	O13—H1o12^vii	2.9619
O3—O5	2.838 (9)	O13—H2o12^vii	2.2188
O3—O8	3.082 (6)	H1o5—H2o5	1.34 (10)
O3—O8ⁱⁱⁱ	3.082 (6)	H1o5—H1o10^xi	2.3981
O3—O10^xi	3.016 (11)	H1o5—H1o10ⁱⁱ	2.3981
O3—O10ⁱⁱ	3.016 (11)	H1o5—H2o10^xi	2.9302
O3—O11	3.267 (9)	H1o5—H2o10ⁱⁱ	2.9302
O3—O11ⁱⁱⁱ	3.267 (9)	H1o5—H1o12^xii	3.1629
O3—H1o5	2.72 (6)	H1o5—H1o12^vii	3.1629
O3—H2o5	2.23 (6)	H2o5—H1o10^xi	3.2774
O3—H1o10^xi	2.9512	H2o5—H1o10ⁱⁱ	3.2774
O3—H1o10ⁱⁱ	2.9512	H2o5—H2o10^xi	3.3332
O3—H2o10^xi	2.7132	H2o5—H2o10ⁱⁱ	3.3332
O3—H2o10ⁱⁱ	2.7132	H2o5—H1o12^xii	3.4094
O3—H1o12^xii	3.4853	H2o5—H1o12^vii	3.4094
O3—H1o12^vii	3.4853	H1o10—H1o10^xvi	1.8918
O4—O5^xiii	2.977 (8)	H1o10—H2o10	1.4203
O4—O8	2.896 (6)	H1o10—H2o10^xvi	3.0869
O4—O10^xiv	3.197 (7)	H1o10—H1o12ⁱ	2.4728
O4—O11ⁱ	2.914 (9)	H2o10—H1o12ⁱ	1.4298
O4—O12ⁱ	3.311 (6)	H2o10—H2o12ⁱ	2.7175
O4—O12^iv	2.847 (8)	H1o12—H1o12^xviii	3.3514
O4—O13ⁱⁱ	3.024 (7)	H1o12—H2o12	1.4203
O4—H1o5^xiii	2.65 (5)	H1o12—H2o12^xviii	2.8187
O4—H1o10^xiv	2.9077	H2o12—H2o12^xviii	2.9484

O1ⁱ—U1—O2	70.27 (18)	O7ⁱⁱ—O9—O10	57.05 (16)
O1ⁱ—U1—O4	92.8 (2)	O7ⁱⁱ—O9—O11	106.1 (2)
O1ⁱ—U1—O7	89.2 (2)	O7ⁱⁱ—O9—O12	63.19 (17)
O1ⁱ—U1—O8	136.64 (18)	O7ⁱⁱ—O9—O13	58.68 (17)
O1ⁱ—U1—O11ⁱ	66.88 (18)	O7ⁱⁱ—O9—H2o10	61.18
O1ⁱ—U1—O13ⁱⁱ	145.20 (19)	O7ⁱⁱ—O9—H2o12	72.18
O1ⁱ—U1—H2o12ⁱ	119.2	O8—O9—O9^iv	137.6 (2)
O2—U1—O4	92.4 (2)	O8—O9—O10	123.0 (3)
O2—U1—O7	89.7 (2)	O8—O9—O11	54.3 (2)
O2—U1—O8	66.47 (17)	O8—O9—O12	128.8 (2)
O2—U1—O11ⁱ	137.09 (17)	O8—O9—O13	58.89 (19)
O2—U1—O13ⁱⁱ	143.86 (16)	O8—O9—H2o10	109.45
O2—U1—H2o12ⁱ	142.43	O8—O9—H2o12	115.56
O4—U1—O7	177.5 (2)	O9^iv—O9—O10	68.27 (19)
O4—U1—O8	86.2 (2)	O9^iv—O9—O11	127.2 (3)
O4—U1—O11ⁱ	87.5 (2)	O9^iv—O9—O12	81.7 (2)
O4—U1—O13ⁱⁱ	92.0 (2)	O9^iv—O9—O13	163.4 (3)
O4—U1—H2o12ⁱ	52.83	O9^iv—O9—H2o10	77.2
O7—U1—O8	93.5 (2)	O9^iv—O9—H2o12	89.4
O7—U1—O11ⁱ	91.9 (2)	O10—O9—O11	161.9 (3)
O7—U1—O13ⁱⁱ	85.5 (2)	O10—O9—O12	99.0 (2)
O7—U1—H2o12ⁱ	124.75	O10—O9—O13	103.0 (2)
O8—U1—O11ⁱ	155.90 (17)	O10—O9—H2o10	13.59
O8—U1—O13ⁱⁱ	78.08 (17)	O10—O9—H2o12	113.21
O8—U1—H2o12ⁱ	94.24	O11—O9—O12	76.46 (19)
O11ⁱ—U1—O13ⁱⁱ	78.93 (16)	O11—O9—O13	59.5 (2)
O11ⁱ—U1—H2o12ⁱ	63.71	O11—O9—H2o10	155.58
O13ⁱⁱ—U1—H2o12ⁱ	43.49	O11—O9—H2o12	62.28
As—U2—Asⁱⁱⁱ	175.64 (3)	O12—O9—O13	86.0 (2)
As—U2—P	0	O12—O9—H2o10	111.03
As—U2—Pⁱⁱⁱ	175.64 (3)	O12—O9—H2o12	14.41
As—U2—O1	90.264 (18)	O13—O9—H2o10	97.11
As—U2—O2	89.714 (18)	O13—O9—H2o12	81.11
As—U2—O3	92.167 (18)	H2o10—O9—H2o12	124.92
As—U2—O6	87.829 (18)	Pb—O10—O3^xvii	134.4 (2)
As—U2—O8	27.68 (12)	Pb—O10—O4^xiv	125.3 (3)
As—U2—O8ⁱⁱⁱ	152.38 (12)	Pb—O10—O6^vi	68.1 (2)
As—U2—O11	28.07 (12)	Pb—O10—O7ⁱⁱ	48.88 (14)
As—U2—O11ⁱⁱⁱ	151.95 (13)	Pb—O10—O9	44.38 (15)
Asⁱⁱⁱ—U2—P	175.64 (3)	Pb—O10—O10^xvi	109.2 (3)
Asⁱⁱⁱ—U2—Pⁱⁱⁱ	0	Pb—O10—O12ⁱ	122.0 (3)
Asⁱⁱⁱ—U2—O1	90.264 (18)	Pb—O10—H1o5^xvii	160.3 (14)
Asⁱⁱⁱ—U2—O2	89.714 (18)	Pb—O10—H1o10	120
Asⁱⁱⁱ—U2—O3	92.167 (18)	Pb—O10—H1o10^xvi	113.43
Asⁱⁱⁱ—U2—O6	87.829 (18)	Pb—O10—H2o10	120
Asⁱⁱⁱ—U2—O8	152.38 (12)	Pb—O10—H1o12ⁱ	119.84
Asⁱⁱⁱ—U2—O8ⁱⁱⁱ	27.68 (12)	Pb—O10—H2o12ⁱ	111.81
Asⁱⁱⁱ—U2—O11	151.95 (13)	O3^xvii—O10—O4^xiv	100.3 (2)
Asⁱⁱⁱ—U2—O11ⁱⁱⁱ	28.07 (12)	O3^xvii—O10—O6^vi	115.3 (3)
P—U2—Pⁱⁱⁱ	175.64 (3)	O3^xvii—O10—O7ⁱⁱ	86.2 (2)
P—U2—O1	90.264 (18)	O3^xvii—O10—O9	120.5 (3)
P—U2—O2	89.714 (18)	O3^xvii—O10—O10^xvi	57.9 (2)
P—U2—O3	92.167 (18)	O3^xvii—O10—O12ⁱ	82.6 (3)
P—U2—O6	87.829 (18)	O3^xvii—O10—H1o5^xvii	54.0 (14)
P—U2—O8	27.68 (12)	O3^xvii—O10—H1o10	77.67
P—U2—O8ⁱⁱⁱ	152.38 (12)	O3^xvii—O10—H1o10^xvi	62.96
P—U2—O11	28.07 (12)	O3^xvii—O10—H2o10	60.91
P—U2—O11ⁱⁱⁱ	151.95 (13)	O3^xvii—O10—H1o12ⁱ	84.49
Pⁱⁱⁱ—U2—O1	90.264 (18)	O3^xvii—O10—H2o12ⁱ	86.79
Pⁱⁱⁱ—U2—O2	89.714 (18)	O4^xiv—O10—O6^vi	90.2 (2)
Pⁱⁱⁱ—U2—O3	92.167 (18)	O4^xiv—O10—O7ⁱⁱ	170.1 (3)
Pⁱⁱⁱ—U2—O6	87.829 (18)	O4^xiv—O10—O9	114.9 (2)
Pⁱⁱⁱ—U2—O8	152.38 (12)	O4^xiv—O10—O10^xvi	97.7 (2)
Pⁱⁱⁱ—U2—O8ⁱⁱⁱ	27.68 (12)	O4^xiv—O10—O12ⁱ	55.61 (19)
Pⁱⁱⁱ—U2—O11	151.95 (13)	O4^xiv—O10—H1o5^xvii	50.8 (10)
Pⁱⁱⁱ—U2—O11ⁱⁱⁱ	28.07 (12)	O4^xiv—O10—H1o10	62.3
O1—U2—O2	179.4 (2)	O4^xiv—O10—H1o10^xvi	87.16
O1—U2—O3	89.6 (3)	O4^xiv—O10—H2o10	83.54
O1—U2—O6	91.3 (3)	O4^xiv—O10—H1o12ⁱ	56.22
O1—U2—O8	117.31 (11)	O4^xiv—O10—H2o12ⁱ	64.78
O1—U2—O8ⁱⁱⁱ	117.31 (11)	O6^vi—O10—O7ⁱⁱ	93.8 (2)
O1—U2—O11	62.23 (11)	O6^vi—O10—O9	111.0 (3)
O1—U2—O11ⁱⁱⁱ	62.23 (11)	O6^vi—O10—O10^xvi	57.4 (2)
O2—U2—O3	91.0 (3)	O6^vi—O10—O12ⁱ	144.7 (3)
O2—U2—O6	88.1 (3)	O6^vi—O10—H1o5^xvii	92.2 (14)
O2—U2—O8	62.74 (11)	O6^vi—O10—H1o10	51.94
O2—U2—O8ⁱⁱⁱ	62.74 (11)	O6^vi—O10—H1o10^xvi	54.02
O2—U2—O11	117.73 (11)	O6^vi—O10—H2o10	171.74
O2—U2—O11ⁱⁱⁱ	117.73 (11)	O6^vi—O10—H1o12ⁱ	144.57
O3—U2—O6	179.1 (3)	O6^vi—O10—H2o12ⁱ	149.91
O3—U2—O8	86.67 (17)	O7ⁱⁱ—O10—O9	55.22 (16)
O3—U2—O8ⁱⁱⁱ	86.67 (17)	O7ⁱⁱ—O10—O10^xvi	92.1 (2)
O3—U2—O11	92.95 (17)	O7ⁱⁱ—O10—O12ⁱ	118.6 (3)
O3—U2—O11ⁱⁱⁱ	92.95 (17)	O7ⁱⁱ—O10—H1o5^xvii	138.0 (11)
O6—U2—O8	92.92 (16)	O7ⁱⁱ—O10—H1o10	126.89
O6—U2—O8ⁱⁱⁱ	92.92 (16)	O7ⁱⁱ—O10—H1o10^xvi	102.5
O6—U2—O11	87.47 (17)	O7ⁱⁱ—O10—H2o10	93.28
O6—U2—O11ⁱⁱⁱ	87.47 (17)	O7ⁱⁱ—O10—H1o12ⁱ	117.68
O8—U2—O8ⁱⁱⁱ	124.86 (17)	O7ⁱⁱ—O10—H2o12ⁱ	108.54
O8—U2—O11	55.55 (17)	O9—O10—O10^xvi	146.2 (2)
O8—U2—O11ⁱⁱⁱ	179.41 (13)	O9—O10—O12ⁱ	80.3 (2)
O8ⁱⁱⁱ—U2—O11	179.41 (13)	O9—O10—H1o5^xvii	153.8 (10)
O8ⁱⁱⁱ—U2—O11ⁱⁱⁱ	55.55 (17)	O9—O10—H1o10	161.1
O11—U2—O11ⁱⁱⁱ	124.04 (17)	O9—O10—H1o10^xvi	154.81
O4^iv—Pb—O5^v	63.7 (2)	O9—O10—H2o10	76.62
O4^iv—Pb—O6^vi	77.07 (17)	O9—O10—H1o12ⁱ	78.33
O4^iv—Pb—O7ⁱⁱ	125.15 (15)	O9—O10—H2o12ⁱ	69.18
O4^iv—Pb—O9	131.56 (18)	O10^xvi—O10—O12ⁱ	128.7 (3)
O4^iv—Pb—O9^iv	83.58 (17)	O10^xvi—O10—H1o5^xvii	57.3 (7)
O4^iv—Pb—O10	136.96 (19)	O10^xvi—O10—H1o10	37.05
O4^iv—Pb—O12	63.16 (19)	O10^xvi—O10—H1o10^xvi	10.98
O4^iv—Pb—H1o5^v	51.4 (14)	O10^xvi—O10—H2o10	118.01
O4^iv—Pb—H2o5^v	75.4 (11)	O10^xvi—O10—H1o12ⁱ	130.92
O4^iv—Pb—H1o10	124.23	O10^xvi—O10—H2o12ⁱ	138.16
O4^iv—Pb—H2o10	149.52	O12ⁱ—O10—H1o5^xvii	73.6 (9)
O4^iv—Pb—H1o12	53.54	O12ⁱ—O10—H1o10	109.03
O4^iv—Pb—H2o12	73.49	O12ⁱ—O10—H1o10^xvi	124.01
O5^v—Pb—O6^vi	59.94 (14)	O12ⁱ—O10—H2o10	31.09
O5^v—Pb—O7ⁱⁱ	70.6 (2)	O12ⁱ—O10—H1o12ⁱ	2.21
O5^v—Pb—O9	146.67 (19)	O12ⁱ—O10—H2o12ⁱ	11.43
O5^v—Pb—O9^iv	138.0 (2)	H1o5^xvii—O10—H1o10	40.34
O5^v—Pb—O10	97.9 (2)	H1o5^xvii—O10—H1o10^xvi	50.59
O5^v—Pb—O12	82.99 (15)	H1o5^xvii—O10—H2o10	79.69
O5^v—Pb—H1o5^v	13.4 (12)	H1o5^xvii—O10—H1o12ⁱ	75.65
O5^v—Pb—H2o5^v	15.8 (4)	H1o5^xvii—O10—H2o12ⁱ	84.66
O5^v—Pb—H1o10	88.94	H1o10—O10—H1o10^xvi	26.07
O5^v—Pb—H2o10	106.59	H1o10—O10—H2o10	120
O5^v—Pb—H1o12	70.74	H1o10—O10—H1o12ⁱ	110.69
O5^v—Pb—H2o12	95.29	H1o10—O10—H2o12ⁱ	120.41
O6^vi—Pb—O7ⁱⁱ	104.96 (15)	H1o10^xvi—O10—H2o10	120.04
O6^vi—Pb—O9	143.26 (16)	H1o10^xvi—O10—H1o12ⁱ	126.12
O6^vi—Pb—O9^iv	88.82 (14)	H1o10^xvi—O10—H2o12ⁱ	134.7
O6^vi—Pb—O10	60.5 (2)	H2o10—O10—H1o12ⁱ	31.69
O6^vi—Pb—O12	134.96 (18)	H2o10—O10—H2o12ⁱ	28.65
O6^vi—Pb—H1o5^v	65.6 (8)	H1o12ⁱ—O10—H2o12ⁱ	9.72
O6^vi—Pb—H2o5^v	71.5 (8)	U1^viii—O11—U2	104.48 (18)
O6^vi—Pb—H1o10	47.53	U1^viii—O11—As	149.5 (3)
O6^vi—Pb—H2o10	73.48	U1^viii—O11—P	149.5 (3)
O6^vi—Pb—H1o12	121.8	U1^viii—O11—O1	54.28 (17)
O6^vi—Pb—H2o12	148	U1^viii—O11—O3	95.19 (19)
O7ⁱⁱ—Pb—O9	78.36 (18)	U1^viii—O11—O4^viii	38.30 (13)
O7ⁱⁱ—Pb—O9^iv	149.95 (18)	U1^viii—O11—O6	109.6 (2)
O7ⁱⁱ—Pb—O10	76.12 (18)	U1^viii—O11—O7^viii	36.75 (13)
O7ⁱⁱ—Pb—O12	83.28 (19)	U1^viii—O11—O8	157.6 (3)
O7ⁱⁱ—Pb—H1o5^v	79.0 (14)	U1^viii—O11—O9	138.5 (3)
O7ⁱⁱ—Pb—H2o5^v	55.3 (6)	U1^viii—O11—O13	118.3 (2)
O7ⁱⁱ—Pb—H1o10	81.78	U1^viii—O11—O13^vii	50.48 (13)
O7ⁱⁱ—Pb—H2o10	71.06	U1^viii—O11—H1o10^iv	85.94
O7ⁱⁱ—Pb—H1o12	84.39	U1^viii—O11—H2o12	72.02
O7ⁱⁱ—Pb—H2o12	82.53	U2—O11—As	102.7 (2)
O9—Pb—O9^iv	74.93 (17)	U2—O11—P	102.7 (2)
O9—Pb—O10	85.9 (2)	U2—O11—O1	51.15 (17)
O9—Pb—O12	81.64 (17)	U2—O11—O3	33.30 (12)
O9—Pb—H1o5^v	147.7 (10)	U2—O11—O4^viii	110.3 (2)
O9—Pb—H2o5^v	131.1 (3)	U2—O11—O6	35.09 (13)
O9—Pb—H1o10	98.5	U2—O11—O7^viii	94.53 (18)
O9—Pb—H2o10	73.27	U2—O11—O8	61.67 (17)
O9—Pb—H1o12	94.89	U2—O11—O9	111.42 (19)
O9—Pb—H2o12	68.41	U2—O11—O13	118.2 (3)
O9^iv—Pb—O10	88.40 (19)	U2—O11—O13^vii	150.8 (2)
O9^iv—Pb—O12	105.94 (16)	U2—O11—H1o10^iv	77.06
O9^iv—Pb—H1o5^v	131.0 (14)	U2—O11—H2o12	154.61
O9^iv—Pb—H2o5^v	153.8 (4)	As—O11—P	0
O9^iv—Pb—H1o10	88.75	As—O11—O1	153.8 (3)
O9^iv—Pb—H2o10	88.13	As—O11—O3	100.1 (3)
O9^iv—Pb—H1o12	111.19	As—O11—O4^viii	138.2 (3)
O9^iv—Pb—H2o12	99.95	As—O11—O6	100.5 (2)
O10—Pb—O12	157.7 (2)	As—O11—O7^viii	127.7 (3)
O10—Pb—H1o5^v	110.5 (10)	As—O11—O8	41.38 (18)
O10—Pb—H2o5^v	96.3 (14)	As—O11—O9	34.56 (18)
O10—Pb—H1o10	12.98	As—O11—O13	33.78 (15)
O10—Pb—H2o10	12.98	As—O11—O13^vii	99.4 (2)
O10—Pb—H1o12	159.95	As—O11—H1o10^iv	113.47
O10—Pb—H2o12	149.45	As—O11—H2o12	88.83
O12—Pb—H1o5^v	73.1 (8)	P—O11—O1	153.8 (3)
O12—Pb—H2o5^v	78.5 (13)	P—O11—O3	100.1 (3)
O12—Pb—H1o10	164.7	P—O11—O4^viii	138.2 (3)
O12—Pb—H2o10	146.99	P—O11—O6	100.5 (2)
O12—Pb—H1o12	13.34	P—O11—O7^viii	127.7 (3)
O12—Pb—H2o12	13.34	P—O11—O8	41.38 (18)
H1o5^v—Pb—H2o5^v	24.4 (17)	P—O11—O9	34.56 (18)
H1o5^v—Pb—H1o10	100.66	P—O11—O13	33.78 (15)
H1o5^v—Pb—H2o10	119.79	P—O11—O13^vii	99.4 (2)
H1o5^v—Pb—H1o12	60.2	P—O11—H1o10^iv	113.47
H1o5^v—Pb—H2o12	86.12	P—O11—H2o12	88.83
H2o5^v—Pb—H1o10	90.24	O1—O11—O3	57.4 (2)
H2o5^v—Pb—H2o10	102.06	O1—O11—O4^viii	65.0 (2)
H2o5^v—Pb—H1o12	68.18	O1—O11—O6	60.58 (17)
H2o5^v—Pb—H2o12	89.07	O1—O11—O7^viii	61.18 (18)
H1o10—Pb—H2o10	25.97	O1—O11—O8	112.4 (3)
H1o10—Pb—H1o12	158.37	O1—O11—O9	147.5 (3)
H1o10—Pb—H2o12	161.35	O1—O11—O13	149.0 (3)
H2o10—Pb—H1o12	154.31	O1—O11—O13^vii	104.5 (2)
H2o10—Pb—H2o12	136.95	O1—O11—H1o10^iv	67.52
H1o12—Pb—H2o12	26.68	O1—O11—H2o12	116.07
U2—As—P	0	O3—O11—O4^viii	121.5 (2)
U2—As—O8	48.13 (19)	O3—O11—O6	68.39 (19)
U2—As—O9	117.55 (19)	O3—O11—O7^viii	69.77 (19)
U2—As—O11	49.18 (18)	O3—O11—O8	63.4 (2)
U2—As—O13	127.81 (18)	O3—O11—O9	126.3 (3)
U2—As—H2o12	108.53	O3—O11—O13	97.5 (3)
U2—As—H2o12^vii	100.1	O3—O11—O13^vii	123.8 (2)
P—As—O8	0	O3—O11—H1o10^iv	108.28
P—As—O9	0	O3—O11—H2o12	165.81
P—As—O11	0	O4^viii—O11—O6	92.7 (2)
P—As—O13	0	O4^viii—O11—O7^viii	75.02 (18)
P—As—H2o12	0	O4^viii—O11—O8	159.4 (3)
P—As—H2o12^vii	0	O4^viii—O11—O9	107.2 (3)
O8—As—O9	111.7 (3)	O4^viii—O11—O13	131.1 (2)
O8—As—O11	96.9 (3)	O4^viii—O11—O13^vii	61.43 (18)
O8—As—O13	110.7 (3)	O4^viii—O11—H1o10^iv	53.4
O8—As—H2o12	154.49	O4^viii—O11—H2o12	51.16
O8—As—H2o12^vii	96.15	O6—O11—O7^viii	120.1 (2)
O9—As—O11	110.3 (3)	O6—O11—O8	70.0 (2)
O9—As—O13	114.6 (3)	O6—O11—O9	89.55 (18)
O9—As—H2o12	66.5	O6—O11—O13	131.2 (2)
O9—As—H2o12^vii	142.09	O6—O11—O13^vii	154.1 (3)
O11—As—O13	111.2 (2)	O6—O11—H1o10^iv	45.18
O11—As—H2o12	62.56	O6—O11—H2o12	121.07
O11—As—H2o12^vii	90.33	O7^viii—O11—O8	122.8 (3)
O13—As—H2o12	91.75	O7^viii—O11—O9	150.3 (2)
O13—As—H2o12^vii	28.02	O7^viii—O11—O13	94.9 (2)
H2o12—As—H2o12^vii	98.76	O7^viii—O11—O13^vii	56.64 (15)
U2—P—As	0	O7^viii—O11—H1o10^iv	118.48
U2—P—O8	48.13 (19)	O7^viii—O11—H2o12	96.05
U2—P—O9	117.55 (19)	O8—O11—O9	63.1 (2)
U2—P—O11	49.18 (18)	O8—O11—O13	62.2 (2)
U2—P—O13	127.81 (18)	O8—O11—O13^vii	135.2 (3)
U2—P—H2o12	108.53	O8—O11—H1o10^iv	106.2
U2—P—H2o12^vii	100.1	O8—O11—H2o12	128.32
As—P—O8	0	O9—O11—O13	60.74 (19)
As—P—O9	0	O9—O11—O13^vii	97.6 (2)
As—P—O11	0	O9—O11—H1o10^iv	82.48
As—P—O13	0	O9—O11—H2o12	66.57
As—P—H2o12	0	O13—O11—O13^vii	72.99 (19)
As—P—H2o12^vii	0	O13—O11—H1o10^iv	143
O8—P—O9	111.7 (3)	O13—O11—H2o12	83.78
O8—P—O11	96.9 (3)	O13^vii—O11—H1o10^iv	110.96
O8—P—O13	110.7 (3)	O13^vii—O11—H2o12	43.07
O8—P—H2o12	154.49	H1o10^iv—O11—H2o12	77.6
O8—P—H2o12^vii	96.15	Pb—O12—O4^viii	128.14 (18)
O9—P—O11	110.3 (3)	Pb—O12—O4^iv	62.70 (16)
O9—P—O13	114.6 (3)	Pb—O12—O7ⁱⁱ	46.70 (13)
O9—P—H2o12	66.5	Pb—O12—O9	47.35 (13)
O9—P—H2o12^vii	142.09	Pb—O12—O10^viii	115.3 (2)
O11—P—O13	111.2 (2)	Pb—O12—O12^xviii	104.7 (2)
O11—P—H2o12	62.56	Pb—O12—O13^vii	127.3 (3)
O11—P—H2o12^vii	90.33	Pb—O12—H1o5^v	61.9 (10)
O13—P—H2o12	91.75	Pb—O12—H1o10^viii	101.62
O13—P—H2o12^vii	28.02	Pb—O12—H2o10^viii	118.31
H2o12—P—H2o12^vii	98.76	Pb—O12—H1o12	120
U1^viii—O1—U1^ix	109.4 (3)	Pb—O12—H1o12^xviii	96.24
U1^viii—O1—U2	124.06 (17)	Pb—O12—H2o12	120
U1^viii—O1—O2^viii	54.82 (13)	Pb—O12—H2o12^xviii	96.73
U1^viii—O1—O3	110.3 (2)	O4^viii—O12—O4^iv	124.1 (3)
U1^viii—O1—O4^viii	37.73 (13)	O4^viii—O12—O7ⁱⁱ	129.2 (3)
U1^viii—O1—O4^ix	109.3 (3)	O4^viii—O12—O9	85.93 (17)
U1^viii—O1—O6	121.84 (14)	O4^viii—O12—O10^viii	113.3 (2)
U1^viii—O1—O7^viii	39.22 (14)	O4^viii—O12—O12^xviii	53.97 (16)
U1^viii—O1—O7^ix	101.7 (2)	O4^viii—O12—O13^vii	59.03 (15)
U1^viii—O1—O11	58.84 (11)	O4^viii—O12—H1o5^v	165.9 (13)
U1^viii—O1—O11ⁱⁱⁱ	168.0 (3)	O4^viii—O12—H1o10^viii	125.38
U1^viii—O1—H2o5	87.5 (8)	O4^viii—O12—H2o10^viii	112.88
U1^viii—O1—H1o10^x	115.42	O4^viii—O12—H1o12	107.84
U1^viii—O1—H1o10^iv	88.76	O4^viii—O12—H1o12^xviii	49.6
U1^ix—O1—U2	124.06 (17)	O4^viii—O12—H2o12	22.48
U1^ix—O1—O2^viii	54.82 (13)	O4^viii—O12—H2o12^xviii	70.15
U1^ix—O1—O3	110.3 (2)	O4^iv—O12—O7ⁱⁱ	98.29 (19)
U1^ix—O1—O4^viii	109.3 (3)	O4^iv—O12—O9	103.24 (19)
U1^ix—O1—O4^ix	37.73 (13)	O4^iv—O12—O10^viii	67.9 (2)
U1^ix—O1—O6	121.84 (14)	O4^iv—O12—O12^xviii	70.2 (2)
U1^ix—O1—O7^viii	101.7 (2)	O4^iv—O12—O13^vii	166.6 (3)
U1^ix—O1—O7^ix	39.22 (14)	O4^iv—O12—H1o5^v	48.0 (12)
U1^ix—O1—O11	168.0 (3)	O4^iv—O12—H1o10^viii	56.66
U1^ix—O1—O11ⁱⁱⁱ	58.84 (11)	O4^iv—O12—H2o10^viii	77.61
U1^ix—O1—H2o5	87.5 (8)	O4^iv—O12—H1o12	69.49
U1^ix—O1—H1o10^x	88.76	O4^iv—O12—H1o12^xviii	76.63
U1^ix—O1—H1o10^iv	115.42	O4^iv—O12—H2o12	143.99
U2—O1—O2^viii	170.0 (4)	O4^iv—O12—H2o12^xviii	54.06
U2—O1—O3	38.90 (18)	O7ⁱⁱ—O12—O9	55.58 (17)
U2—O1—O4^viii	122.35 (17)	O7ⁱⁱ—O12—O10^viii	107.5 (2)
U2—O1—O4^ix	122.35 (17)	O7ⁱⁱ—O12—O12^xviii	149.3 (2)
U2—O1—O6	38.28 (17)	O7ⁱⁱ—O12—O13^vii	86.4 (2)
U2—O1—O7^viii	108.9 (3)	O7ⁱⁱ—O12—H1o5^v	64.5 (13)
U2—O1—O7^ix	108.9 (3)	O7ⁱⁱ—O12—H1o10^viii	99.88
U2—O1—O11	66.62 (18)	O7ⁱⁱ—O12—H2o10^viii	101.52
U2—O1—O11ⁱⁱⁱ	66.62 (18)	O7ⁱⁱ—O12—H1o12	112.79
U2—O1—H2o5	80.1 (14)	O7ⁱⁱ—O12—H1o12^xviii	136.16
U2—O1—H1o10^x	82.98	O7ⁱⁱ—O12—H2o12	107.37
U2—O1—H1o10^iv	82.98	O7ⁱⁱ—O12—H2o12^xviii	143.4
O2^viii—O1—O3	131.1 (3)	O9—O12—O10^viii	160.8 (2)
O2^viii—O1—O4^viii	63.8 (2)	O9—O12—O12^xviii	98.23 (19)
O2^viii—O1—O4^ix	63.8 (2)	O9—O12—O13^vii	89.8 (2)
O2^viii—O1—O6	151.7 (4)	O9—O12—H1o5^v	106.8 (11)
O2^viii—O1—O7^viii	63.49 (19)	O9—O12—H1o10^viii	148.18
O2^viii—O1—O7^ix	63.49 (19)	O9—O12—H2o10^viii	157.09
O2^viii—O1—O11	113.62 (17)	O9—O12—H1o12	166.23
O2^viii—O1—O11ⁱⁱⁱ	113.62 (17)	O9—O12—H1o12^xviii	82.81
O2^viii—O1—H2o5	89.9 (14)	O9—O12—H2o12	72.91
O2^viii—O1—H1o10^x	106.58	O9—O12—H2o12^xviii	103.52
O2^viii—O1—H1o10^iv	106.58	O10^viii—O12—O12^xviii	94.7 (3)
O3—O1—O4^viii	136.46 (15)	O10^viii—O12—O13^vii	98.7 (2)
O3—O1—O4^ix	136.46 (15)	O10^viii—O12—H1o5^v	54.4 (11)
O3—O1—O6	77.2 (3)	O10^viii—O12—H1o10^viii	13.86
O3—O1—O7^viii	78.1 (2)	O10^viii—O12—H2o10^viii	11.02
O3—O1—O7^ix	78.1 (2)	O10^viii—O12—H1o12	5.57
O3—O1—O11	74.1 (2)	O10^viii—O12—H1o12^xviii	110.35
O3—O1—O11ⁱⁱⁱ	74.1 (2)	O10^viii—O12—H2o12	124.57
O3—O1—H2o5	41.2 (14)	O10^viii—O12—H2o12^xviii	85.36
O3—O1—H1o10^x	120.23	O12^xviii—O12—O13^vii	111.5 (2)
O3—O1—H1o10^iv	120.23	O12^xviii—O12—H1o5^v	116.7 (13)
O4^viii—O1—O4^ix	86.8 (3)	O12^xviii—O12—H1o10^viii	96.96
O4^viii—O1—O6	96.6 (2)	O12^xviii—O12—H2o10^viii	103.43
O4^viii—O1—O7^viii	76.95 (17)	O12^xviii—O12—H1o12	90.34
O4^viii—O1—O7^ix	126.7 (3)	O12^xviii—O12—H1o12^xviii	15.7
O4^viii—O1—O11	63.57 (19)	O12^xviii—O12—H2o12	74.94
O4^viii—O1—O11ⁱⁱⁱ	144.5 (3)	O12^xviii—O12—H2o12^xviii	16.35
O4^viii—O1—H2o5	125.2 (8)	O13^vii—O12—H1o5^v	125.5 (11)
O4^viii—O1—H1o10^x	77.7	O13^vii—O12—H1o10^viii	110.29
O4^viii—O1—H1o10^iv	53.65	O13^vii—O12—H2o10^viii	89.2
O4^ix—O1—O6	96.6 (2)	O13^vii—O12—H1o12	97.13
O4^ix—O1—O7^viii	126.7 (3)	O13^vii—O12—H1o12^xviii	108.54
O4^ix—O1—O7^ix	76.95 (17)	O13^vii—O12—H2o12	43.06
O4^ix—O1—O11	144.5 (3)	O13^vii—O12—H2o12^xviii	126.27
O4^ix—O1—O11ⁱⁱⁱ	63.57 (19)	H1o5^v—O12—H1o10^viii	41.49
O4^ix—O1—H2o5	125.2 (8)	H1o5^v—O12—H2o10^viii	56.48
O4^ix—O1—H1o10^x	53.65	H1o5^v—O12—H1o12	59.57
O4^ix—O1—H1o10^iv	77.7	H1o5^v—O12—H1o12^xviii	124.64
O6—O1—O7^viii	135.1 (2)	H1o5^v—O12—H2o12	168
O6—O1—O7^ix	135.1 (2)	H1o5^v—O12—H2o12^xviii	100.35
O6—O1—O11	69.71 (16)	H1o10^viii—O12—H2o10^viii	21.21
O6—O1—O11ⁱⁱⁱ	69.71 (16)	H1o10^viii—O12—H1o12	18.42
O6—O1—H2o5	118.4 (14)	H1o10^viii—O12—H1o12^xviii	111.91
O6—O1—H1o10^x	46.65	H1o10^viii—O12—H2o12	138.36
O6—O1—H1o10^iv	46.65	H1o10^viii—O12—H2o12^xviii	84.7
O7^viii—O1—O7^ix	73.61 (19)	H2o10^viii—O12—H1o12	13.5
O7^viii—O1—O11	67.76 (16)	H2o10^viii—O12—H1o12^xviii	119.1
O7^viii—O1—O11ⁱⁱⁱ	136.0 (3)	H2o10^viii—O12—H2o12	119.87
O7^viii—O1—H2o5	48.3 (8)	H2o10^viii—O12—H2o12^xviii	95.47
O7^viii—O1—H1o10^x	154.54	H1o12—O12—H1o12^xviii	106.04
O7^viii—O1—H1o10^iv	124.89	H1o12—O12—H2o12	120
O7^ix—O1—O11	136.0 (3)	H1o12—O12—H2o12^xviii	81.98
O7^ix—O1—O11ⁱⁱⁱ	67.76 (16)	H1o12^xviii—O12—H2o12	67.36
O7^ix—O1—H2o5	48.3 (8)	H1o12^xviii—O12—H2o12^xviii	27.81
O7^ix—O1—H1o10^x	124.89	H2o12—O12—H2o12^xviii	91.29
O7^ix—O1—H1o10^iv	154.54	U1ⁱⁱ—O13—As	138.0 (3)
O11—O1—O11ⁱⁱⁱ	132.7 (3)	U1ⁱⁱ—O13—P	138.0 (3)
O11—O1—H2o5	89.3 (6)	U1ⁱⁱ—O13—O4ⁱⁱ	36.68 (12)
O11—O1—H1o10^x	98.65	U1ⁱⁱ—O13—O7ⁱⁱ	39.13 (13)
O11—O1—H1o10^iv	69.16	U1ⁱⁱ—O13—O8	146.1 (2)
O11ⁱⁱⁱ—O1—H2o5	89.3 (6)	U1ⁱⁱ—O13—O8ⁱⁱ	51.33 (13)
O11ⁱⁱⁱ—O1—H1o10^x	69.16	U1ⁱⁱ—O13—O9	105.1 (2)
O11ⁱⁱⁱ—O1—H1o10^iv	98.65	U1ⁱⁱ—O13—O11	147.9 (3)
H2o5—O1—H1o10^x	156.64	U1ⁱⁱ—O13—O11^vii	50.59 (13)
H2o5—O1—H1o10^iv	156.64	U1ⁱⁱ—O13—O12^vii	103.91 (19)
H1o10^x—O1—H1o10^iv	32.07	U1ⁱⁱ—O13—O13^vii	95.91 (17)
U1—O2—U1ⁱⁱⁱ	109.6 (3)	U1ⁱⁱ—O13—H1o12^vii	111.47
U1—O2—U2	125.05 (14)	U1ⁱⁱ—O13—H2o12^vii	89.4
U1—O2—O1ⁱ	54.91 (13)	As—O13—P	0
U1—O2—O3	118.78 (16)	As—O13—O4ⁱⁱ	167.3 (3)
U1—O2—O4	37.92 (13)	As—O13—O7ⁱⁱ	100.2 (3)
U1—O2—O4ⁱⁱⁱ	109.8 (2)	As—O13—O8	35.13 (18)
U1—O2—O6	114.2 (2)	As—O13—O8ⁱⁱ	109.8 (2)
U1—O2—O7	39.04 (14)	As—O13—O9	33.00 (16)
U1—O2—O7ⁱⁱⁱ	101.4 (3)	As—O13—O11	35.02 (15)
U1—O2—O8	59.49 (11)	As—O13—O11^vii	131.3 (3)
U1—O2—O8ⁱⁱⁱ	168.9 (3)	As—O13—O12^vii	117.9 (2)
U1ⁱⁱⁱ—O2—U2	125.05 (14)	As—O13—O13^vii	86.6 (2)
U1ⁱⁱⁱ—O2—O1ⁱ	54.91 (13)	As—O13—H1o12^vii	109.78
U1ⁱⁱⁱ—O2—O3	118.78 (16)	As—O13—H2o12^vii	132.32
U1ⁱⁱⁱ—O2—O4	109.8 (2)	P—O13—O4ⁱⁱ	167.3 (3)
U1ⁱⁱⁱ—O2—O4ⁱⁱⁱ	37.92 (13)	P—O13—O7ⁱⁱ	100.2 (3)
U1ⁱⁱⁱ—O2—O6	114.2 (2)	P—O13—O8	35.13 (18)
U1ⁱⁱⁱ—O2—O7	101.4 (3)	P—O13—O8ⁱⁱ	109.8 (2)
U1ⁱⁱⁱ—O2—O7ⁱⁱⁱ	39.04 (14)	P—O13—O9	33.00 (16)
U1ⁱⁱⁱ—O2—O8	168.9 (3)	P—O13—O11	35.02 (15)
U1ⁱⁱⁱ—O2—O8ⁱⁱⁱ	59.49 (11)	P—O13—O11^vii	131.3 (3)
U2—O2—O1ⁱ	170.6 (4)	P—O13—O12^vii	117.9 (2)
U2—O2—O3	38.47 (19)	P—O13—O13^vii	86.6 (2)
U2—O2—O4	109.6 (2)	P—O13—H1o12^vii	109.78
U2—O2—O4ⁱⁱⁱ	109.6 (2)	P—O13—H2o12^vii	132.32
U2—O2—O6	39.66 (17)	O4ⁱⁱ—O13—O7ⁱⁱ	75.81 (18)
U2—O2—O7	123.73 (19)	O4ⁱⁱ—O13—O8	138.4 (3)
U2—O2—O7ⁱⁱⁱ	123.73 (19)	O4ⁱⁱ—O13—O8ⁱⁱ	57.55 (16)
U2—O2—O8	66.03 (18)	O4ⁱⁱ—O13—O9	139.5 (2)
U2—O2—O8ⁱⁱⁱ	66.03 (18)	O4ⁱⁱ—O13—O11	157.5 (2)
O1ⁱ—O2—O3	150.9 (4)	O4ⁱⁱ—O13—O11^vii	57.80 (18)
O1ⁱ—O2—O4	64.21 (18)	O4ⁱⁱ—O13—O12^vii	69.85 (18)
O1ⁱ—O2—O4ⁱⁱⁱ	64.21 (18)	O4ⁱⁱ—O13—O13^vii	104.74 (17)
O1ⁱ—O2—O6	131.0 (3)	O4ⁱⁱ—O13—H1o12^vii	75.06
O1ⁱ—O2—O7	63.0 (2)	O4ⁱⁱ—O13—H2o12^vii	56.28
O1ⁱ—O2—O7ⁱⁱⁱ	63.0 (2)	O7ⁱⁱ—O13—O8	123.9 (2)
O1ⁱ—O2—O8	114.33 (17)	O7ⁱⁱ—O13—O8ⁱⁱ	63.51 (18)
O1ⁱ—O2—O8ⁱⁱⁱ	114.33 (17)	O7ⁱⁱ—O13—O9	67.63 (19)
O3—O2—O4	131.41 (17)	O7ⁱⁱ—O13—O11	113.4 (3)
O3—O2—O4ⁱⁱⁱ	131.41 (17)	O7ⁱⁱ—O13—O11^vii	62.05 (16)
O3—O2—O6	78.1 (3)	O7ⁱⁱ—O13—O12^vii	138.9 (2)
O3—O2—O7	94.3 (2)	O7ⁱⁱ—O13—O13^vii	84.06 (19)
O3—O2—O7ⁱⁱⁱ	94.3 (2)	O7ⁱⁱ—O13—H1o12^vii	150.03
O3—O2—O8	68.88 (15)	O7ⁱⁱ—O13—H2o12^vii	124.66
O3—O2—O8ⁱⁱⁱ	68.88 (15)	O8—O13—O8ⁱⁱ	96.1 (2)
O4—O2—O4ⁱⁱⁱ	87.2 (2)	O8—O13—O9	60.3 (2)
O4—O2—O6	81.3 (2)	O8—O13—O11	54.84 (19)
O4—O2—O7	76.95 (17)	O8—O13—O11^vii	161.7 (3)
O4—O2—O7ⁱⁱⁱ	126.7 (3)	O8—O13—O12^vii	96.9 (2)
O4—O2—O8	63.32 (15)	O8—O13—O13^vii	113.0 (2)
O4—O2—O8ⁱⁱⁱ	143.9 (3)	O8—O13—H1o12^vii	83.49
O4ⁱⁱⁱ—O2—O6	81.3 (2)	O8—O13—H2o12^vii	110.61
O4ⁱⁱⁱ—O2—O7	126.7 (3)	O8ⁱⁱ—O13—O9	89.8 (2)
O4ⁱⁱⁱ—O2—O7ⁱⁱⁱ	76.95 (17)	O8ⁱⁱ—O13—O11	144.8 (2)
O4ⁱⁱⁱ—O2—O8	143.9 (3)	O8ⁱⁱ—O13—O11^vii	101.63 (19)
O4ⁱⁱⁱ—O2—O8ⁱⁱⁱ	63.32 (15)	O8ⁱⁱ—O13—O12^vii	112.4 (3)
O6—O2—O7	142.87 (14)	O8ⁱⁱ—O13—O13^vii	145.3 (2)
O6—O2—O7ⁱⁱⁱ	142.87 (14)	O8ⁱⁱ—O13—H1o12^vii	105.44
O6—O2—O8	74.4 (2)	O8ⁱⁱ—O13—H2o12^vii	104.65
O6—O2—O8ⁱⁱⁱ	74.4 (2)	O9—O13—O11	59.80 (19)
O7—O2—O7ⁱⁱⁱ	73.3 (2)	O9—O13—O11^vii	114.8 (3)
O7—O2—O8	69.1 (2)	O9—O13—O12^vii	150.6 (2)
O7—O2—O8ⁱⁱⁱ	136.9 (3)	O9—O13—O13^vii	88.7 (2)
O7ⁱⁱⁱ—O2—O8	136.9 (3)	O9—O13—H1o12^vii	142.24
O7ⁱⁱⁱ—O2—O8ⁱⁱⁱ	69.1 (2)	O9—O13—H2o12^vii	164.08
O8—O2—O8ⁱⁱⁱ	131.3 (3)	O11—O13—O11^vii	107.0 (2)
U2—O3—O1	51.5 (2)	O11—O13—O12^vii	92.4 (2)
U2—O3—O2	50.5 (2)	O11—O13—O13^vii	58.16 (17)
U2—O3—O5	145.2 (4)	O11—O13—H1o12^vii	91.64
U2—O3—O8	57.76 (16)	O11—O13—H2o12^vii	104.35
U2—O3—O8ⁱⁱⁱ	57.76 (16)	O11^vii—O13—O12^vii	80.54 (18)
U2—O3—O10^xi	131.7 (2)	O11^vii—O13—O13^vii	48.86 (16)
U2—O3—O10ⁱⁱ	131.7 (2)	O11^vii—O13—H1o12^vii	96
U2—O3—O11	53.75 (18)	O11^vii—O13—H2o12^vii	69.27
U2—O3—O11ⁱⁱⁱ	53.75 (18)	O12^vii—O13—O13^vii	83.51 (19)
U2—O3—H1o5	161.9 (17)	O12^vii—O13—H1o12^vii	15.94
U2—O3—H2o5	132.7 (14)	O12^vii—O13—H2o12^vii	14.62
U2—O3—H1o10^xi	145.91	O13^vii—O13—H1o12^vii	96.62
U2—O3—H1o10ⁱⁱ	145.91	O13^vii—O13—H2o12^vii	83.15
U2—O3—H2o10^xi	124.34	H1o12^vii—O13—H2o12^vii	27.31
U2—O3—H2o10ⁱⁱ	124.34	Pb^xii—H1o5—Pb^vii	100.5 (18)
U2—O3—H1o12^xii	122.16	Pb^xii—H1o5—O3	102.5 (19)
U2—O3—H1o12^vii	122.16	Pb^xii—H1o5—O4^xv	128.9 (19)
O1—O3—O2	102.0 (3)	Pb^xii—H1o5—O4^xix	56.7 (6)
O1—O3—O5	93.7 (3)	Pb^xii—H1o5—O5	53.0 (12)
O1—O3—O8	88.4 (2)	Pb^xii—H1o5—O6^xv	56.5 (9)
O1—O3—O8ⁱⁱⁱ	88.4 (2)	Pb^xii—H1o5—O10^xi	96.4 (3)
O1—O3—O10^xi	145.60 (19)	Pb^xii—H1o5—O10ⁱⁱ	160.4 (15)
O1—O3—O10ⁱⁱ	145.60 (19)	Pb^xii—H1o5—O12^xii	45.0 (3)
O1—O3—O11	48.49 (16)	Pb^xii—H1o5—O12^vii	142 (2)
O1—O3—O11ⁱⁱⁱ	48.49 (16)	Pb^xii—H1o5—H2o5	69 (2)
O1—O3—H1o5	110.4 (16)	Pb^xii—H1o5—H1o10^xi	106.52
O1—O3—H2o5	81.2 (14)	Pb^xii—H1o5—H1o10ⁱⁱ	152.96
O1—O3—H1o10^xi	151.08	Pb^xii—H1o5—H2o10^xi	84.05
O1—O3—H1o10ⁱⁱ	151.08	Pb^xii—H1o5—H2o10ⁱⁱ	159.71
O1—O3—H2o10^xi	130.58	Pb^xii—H1o5—H1o12^xii	57.63
O1—O3—H2o10ⁱⁱ	130.58	Pb^xii—H1o5—H1o12^vii	153.98
O1—O3—H1o12^xii	109.81	Pb^vii—H1o5—O3	102.5 (19)
O1—O3—H1o12^vii	109.81	Pb^vii—H1o5—O4^xv	56.7 (6)
O2—O3—O5	164.2 (4)	Pb^vii—H1o5—O4^xix	128.9 (19)
O2—O3—O8	50.25 (12)	Pb^vii—H1o5—O5	53.0 (12)
O2—O3—O8ⁱⁱⁱ	50.25 (12)	Pb^vii—H1o5—O6^xv	56.5 (9)
O2—O3—O10^xi	91.0 (3)	Pb^vii—H1o5—O10^xi	160.4 (15)
O2—O3—O10ⁱⁱ	91.0 (3)	Pb^vii—H1o5—O10ⁱⁱ	96.4 (3)
O2—O3—O11	85.1 (2)	Pb^vii—H1o5—O12^xii	142 (2)
O2—O3—O11ⁱⁱⁱ	85.1 (2)	Pb^vii—H1o5—O12^vii	45.0 (3)
O2—O3—H1o5	147.5 (17)	Pb^vii—H1o5—H2o5	69 (2)
O2—O3—H2o5	176.8 (14)	Pb^vii—H1o5—H1o10^xi	152.96
O2—O3—H1o10^xi	99.87	Pb^vii—H1o5—H1o10ⁱⁱ	106.52
O2—O3—H1o10ⁱⁱ	99.87	Pb^vii—H1o5—H2o10^xi	159.71
O2—O3—H2o10^xi	93.62	Pb^vii—H1o5—H2o10ⁱⁱ	84.05
O2—O3—H2o10ⁱⁱ	93.62	Pb^vii—H1o5—H1o12^xii	153.98
O2—O3—H1o12^xii	109.31	Pb^vii—H1o5—H1o12^vii	57.63
O2—O3—H1o12^vii	109.31	O3—H1o5—O4^xv	125.6 (11)
O5—O3—O8	131.30 (12)	O3—H1o5—O4^xix	125.6 (11)
O5—O3—O8ⁱⁱⁱ	131.30 (12)	O3—H1o5—O5	90 (5)
O5—O3—O10^xi	75.7 (3)	O3—H1o5—O6^xv	140 (3)
O5—O3—O10ⁱⁱ	75.7 (3)	O3—H1o5—O10^xi	64.0 (11)
O5—O3—O11	105.7 (2)	O3—H1o5—O10ⁱⁱ	64.0 (11)
O5—O3—O11ⁱⁱⁱ	105.7 (2)	O3—H1o5—O12^xii	76.4 (10)
O5—O3—H1o5	16.7 (16)	O3—H1o5—O12^vii	76.4 (10)
O5—O3—H2o5	12.6 (14)	O3—H1o5—H2o5	55 (4)
O5—O3—H1o10^xi	65.28	O3—H1o5—H1o10^xi	70.16
O5—O3—H1o10ⁱⁱ	65.28	O3—H1o5—H1o10ⁱⁱ	70.16
O5—O3—H2o10^xi	75.8	O3—H1o5—H2o10^xi	57.28
O5—O3—H2o10ⁱⁱ	75.8	O3—H1o5—H2o10ⁱⁱ	57.28
O5—O3—H1o12^xii	64.43	O3—H1o5—H1o12^xii	72.26
O5—O3—H1o12^vii	64.43	O3—H1o5—H1o12^vii	72.26
O8—O3—O8ⁱⁱⁱ	97.4 (2)	O4^xv—H1o5—O4^xix	100 (3)
O8—O3—O10^xi	123.3 (3)	O4^xv—H1o5—O5	106 (3)
O8—O3—O10ⁱⁱ	75.6 (2)	O4^xv—H1o5—O6^xv	74.4 (12)
O8—O3—O11	45.21 (16)	O4^xv—H1o5—O10^xi	118 (3)
O8—O3—O11ⁱⁱⁱ	111.5 (3)	O4^xv—H1o5—O10ⁱⁱ	69.2 (11)
O8—O3—H1o5	128.9 (5)	O4^xv—H1o5—O12^xii	152 (3)
O8—O3—H2o5	130.4 (3)	O4^xv—H1o5—O12^vii	53.01 (17)
O8—O3—H1o10^xi	120.24	O4^xv—H1o5—H2o5	124 (2)
O8—O3—H1o10ⁱⁱ	91.27	O4^xv—H1o5—H1o10^xi	105.33
O8—O3—H2o10^xi	134.56	O4^xv—H1o5—H1o10ⁱⁱ	70.16
O8—O3—H2o10ⁱⁱ	66.57	O4^xv—H1o5—H2o10^xi	134.1
O8—O3—H1o12^xii	156.33	O4^xv—H1o5—H2o10ⁱⁱ	70.04
O8—O3—H1o12^vii	69.16	O4^xv—H1o5—H1o12^xii	146.98
O8ⁱⁱⁱ—O3—O10^xi	75.6 (2)	O4^xv—H1o5—H1o12^vii	53.87
O8ⁱⁱⁱ—O3—O10ⁱⁱ	123.3 (3)	O4^xix—H1o5—O5	106 (3)
O8ⁱⁱⁱ—O3—O11	111.5 (3)	O4^xix—H1o5—O6^xv	74.4 (12)
O8ⁱⁱⁱ—O3—O11ⁱⁱⁱ	45.21 (16)	O4^xix—H1o5—O10^xi	69.2 (11)
O8ⁱⁱⁱ—O3—H1o5	128.9 (5)	O4^xix—H1o5—O10ⁱⁱ	118 (3)
O8ⁱⁱⁱ—O3—H2o5	130.4 (3)	O4^xix—H1o5—O12^xii	53.01 (17)
O8ⁱⁱⁱ—O3—H1o10^xi	91.27	O4^xix—H1o5—O12^vii	152 (3)
O8ⁱⁱⁱ—O3—H1o10ⁱⁱ	120.24	O4^xix—H1o5—H2o5	124 (2)
O8ⁱⁱⁱ—O3—H2o10^xi	66.57	O4^xix—H1o5—H1o10^xi	70.16
O8ⁱⁱⁱ—O3—H2o10ⁱⁱ	134.56	O4^xix—H1o5—H1o10ⁱⁱ	105.33
O8ⁱⁱⁱ—O3—H1o12^xii	69.16	O4^xix—H1o5—H2o10^xi	70.04
O8ⁱⁱⁱ—O3—H1o12^vii	156.33	O4^xix—H1o5—H2o10ⁱⁱ	134.1
O10^xi—O3—O10ⁱⁱ	64.1 (3)	O4^xix—H1o5—H1o12^xii	53.87
O10^xi—O3—O11	165.8 (3)	O4^xix—H1o5—H1o12^vii	146.98
O10^xi—O3—O11ⁱⁱⁱ	102.28 (19)	O5—H1o5—O6^xv	50 (4)
O10^xi—O3—H1o5	62.0 (13)	O5—H1o5—O10^xi	136 (4)
O10^xi—O3—H2o5	86.3 (12)	O5—H1o5—O10ⁱⁱ	136 (4)
O10^xi—O3—H1o10^xi	15.75	O5—H1o5—O12^xii	89.0 (19)
O10^xi—O3—H1o10ⁱⁱ	51.52	O5—H1o5—O12^vii	89.0 (19)
O10^xi—O3—H2o10^xi	15.31	O5—H1o5—H2o5	35 (5)
O10^xi—O3—H2o10ⁱⁱ	79.18	O5—H1o5—H1o10^xi	148.7
O10^xi—O3—H1o12^xii	36.06	O5—H1o5—H1o10ⁱⁱ	148.7
O10^xi—O3—H1o12^vii	95.17	O5—H1o5—H2o10^xi	119.97
O10ⁱⁱ—O3—O11	102.28 (19)	O5—H1o5—H2o10ⁱⁱ	119.97
O10ⁱⁱ—O3—O11ⁱⁱⁱ	165.8 (3)	O5—H1o5—H1o12^xii	101.1
O10ⁱⁱ—O3—H1o5	62.0 (13)	O5—H1o5—H1o12^vii	101.1
O10ⁱⁱ—O3—H2o5	86.3 (12)	O6^xv—H1o5—O10^xi	142.9 (13)
O10ⁱⁱ—O3—H1o10^xi	51.52	O6^xv—H1o5—O10ⁱⁱ	142.9 (13)
O10ⁱⁱ—O3—H1o10ⁱⁱ	15.75	O6^xv—H1o5—O12^xii	99.7 (10)
O10ⁱⁱ—O3—H2o10^xi	79.18	O6^xv—H1o5—O12^vii	99.7 (10)
O10ⁱⁱ—O3—H2o10ⁱⁱ	15.31	O6^xv—H1o5—H2o5	85 (4)
O10ⁱⁱ—O3—H1o12^xii	95.17	O6^xv—H1o5—H1o10^xi	143.95
O10ⁱⁱ—O3—H1o12^vii	36.06	O6^xv—H1o5—H1o10ⁱⁱ	143.95
O11—O3—O11ⁱⁱⁱ	91.0 (3)	O6^xv—H1o5—H2o10^xi	137.28
O11—O3—H1o5	116.4 (10)	O6^xv—H1o5—H2o10ⁱⁱ	137.28
O11—O3—H2o5	97.1 (10)	O6^xv—H1o5—H1o12^xii	110.92
O11—O3—H1o10^xi	153.05	O6^xv—H1o5—H1o12^vii	110.92
O11—O3—H1o10ⁱⁱ	115.74	O10^xi—H1o5—O10ⁱⁱ	65.4 (13)
O11—O3—H2o10^xi	178.08	O10^xi—H1o5—O12^xii	52.1 (4)
O11—O3—H2o10ⁱⁱ	87.46	O10^xi—H1o5—O12^vii	115.7 (15)
O11—O3—H1o12^xii	157.24	O10^xi—H1o5—H2o5	109 (4)
O11—O3—H1o12^vii	73.42	O10^xi—H1o5—H1o10^xi	12.79
O11ⁱⁱⁱ—O3—H1o5	116.4 (10)	O10^xi—H1o5—H1o10ⁱⁱ	56.69
O11ⁱⁱⁱ—O3—H2o5	97.1 (10)	O10^xi—H1o5—H2o10^xi	15.98
O11ⁱⁱⁱ—O3—H1o10^xi	115.74	O10^xi—H1o5—H2o10ⁱⁱ	76.73
O11ⁱⁱⁱ—O3—H1o10ⁱⁱ	153.05	O10^xi—H1o5—H1o12^xii	39.15
O11ⁱⁱⁱ—O3—H2o10^xi	87.46	O10^xi—H1o5—H1o12^vii	103.41
O11ⁱⁱⁱ—O3—H2o10ⁱⁱ	178.08	O10ⁱⁱ—H1o5—O12^xii	115.7 (15)
O11ⁱⁱⁱ—O3—H1o12^xii	73.42	O10ⁱⁱ—H1o5—O12^vii	52.1 (4)
O11ⁱⁱⁱ—O3—H1o12^vii	157.24	O10ⁱⁱ—H1o5—H2o5	109 (4)
H1o5—O3—H2o5	29 (2)	O10ⁱⁱ—H1o5—H1o10^xi	56.69
H1o5—O3—H1o10^xi	49.85	O10ⁱⁱ—H1o5—H1o10ⁱⁱ	12.79
H1o5—O3—H1o10ⁱⁱ	49.85	O10ⁱⁱ—H1o5—H2o10^xi	76.73
H1o5—O3—H2o10^xi	65.32	O10ⁱⁱ—H1o5—H2o10ⁱⁱ	15.98
H1o5—O3—H2o10ⁱⁱ	65.32	O10ⁱⁱ—H1o5—H1o12^xii	103.41
H1o5—O3—H1o12^xii	59.81	O10ⁱⁱ—H1o5—H1o12^vii	39.15
H1o5—O3—H1o12^vii	59.81	O12^xii—H1o5—O12^vii	153 (2)
H2o5—O3—H1o10^xi	77.09	O12^xii—H1o5—H2o5	81.3 (15)
H2o5—O3—H1o10ⁱⁱ	77.09	O12^xii—H1o5—H1o10^xi	63.41
H2o5—O3—H2o10^xi	84.2	O12^xii—H1o5—H1o10ⁱⁱ	108.6
H2o5—O3—H2o10ⁱⁱ	84.2	O12^xii—H1o5—H2o10^xi	39.05
H2o5—O3—H1o12^xii	69.3	O12^xii—H1o5—H2o10ⁱⁱ	122.7
H2o5—O3—H1o12^vii	69.3	O12^xii—H1o5—H1o12^xii	12.92
H1o10^xi—O3—H1o10ⁱⁱ	37.39	O12^xii—H1o5—H1o12^vii	146.94
H1o10^xi—O3—H2o10^xi	28.65	O12^vii—H1o5—H2o5	81.3 (15)
H1o10^xi—O3—H2o10ⁱⁱ	65.89	O12^vii—H1o5—H1o10^xi	108.6
H1o10^xi—O3—H1o12^xii	44.22	O12^vii—H1o5—H1o10ⁱⁱ	63.41
H1o10^xi—O3—H1o12^vii	79.98	O12^vii—H1o5—H2o10^xi	122.7
H1o10ⁱⁱ—O3—H2o10^xi	65.89	O12^vii—H1o5—H2o10ⁱⁱ	39.05
H1o10ⁱⁱ—O3—H2o10ⁱⁱ	28.65	O12^vii—H1o5—H1o12^xii	146.94
H1o10ⁱⁱ—O3—H1o12^xii	79.98	O12^vii—H1o5—H1o12^vii	12.92
H1o10ⁱⁱ—O3—H1o12^vii	44.22	H2o5—H1o5—H1o10^xi	120.06
H2o10^xi—O3—H2o10ⁱⁱ	94.07	H2o5—H1o5—H1o10ⁱⁱ	120.06
H2o10^xi—O3—H1o12^xii	22.57	H2o5—H1o5—H2o10^xi	95.44
H2o10^xi—O3—H1o12^vii	108.39	H2o5—H1o5—H2o10ⁱⁱ	95.44
H2o10ⁱⁱ—O3—H1o12^xii	108.39	H2o5—H1o5—H1o12^xii	88.89
H2o10ⁱⁱ—O3—H1o12^vii	22.57	H2o5—H1o5—H1o12^vii	88.89
H1o12^xii—O3—H1o12^vii	115.68	H1o10^xi—H1o5—H1o10ⁱⁱ	46.46
U1—O4—Pb^iv	136.6 (2)	H1o10^xi—H1o5—H2o10^xi	28.76
U1—O4—O1ⁱ	49.46 (17)	H1o10^xi—H1o5—H2o10ⁱⁱ	69.99
U1—O4—O2	49.67 (18)	H1o10^xi—H1o5—H1o12^xii	50.55
U1—O4—O5^xiii	128.7 (3)	H1o10^xi—H1o5—H1o12^vii	95.76
U1—O4—O8	55.32 (17)	H1o10ⁱⁱ—H1o5—H2o10^xi	69.99
U1—O4—O10^xiv	123.4 (3)	H1o10ⁱⁱ—H1o5—H2o10ⁱⁱ	28.76
U1—O4—O11ⁱ	54.21 (18)	H1o10ⁱⁱ—H1o5—H1o12^xii	95.76
U1—O4—O12ⁱ	99.7 (2)	H1o10ⁱⁱ—H1o5—H1o12^vii	50.55
U1—O4—O12^iv	155.4 (3)	H2o10^xi—H1o5—H2o10ⁱⁱ	85.31
U1—O4—O13ⁱⁱ	51.32 (16)	H2o10^xi—H1o5—H1o12^xii	26.79
U1—O4—H1o5^xiii	123.8 (13)	H2o10^xi—H1o5—H1o12^vii	111.81
U1—O4—H1o10^xiv	116.63	H2o10ⁱⁱ—H1o5—H1o12^xii	111.81
U1—O4—H2o10^xiv	137.52	H2o10ⁱⁱ—H1o5—H1o12^vii	26.79
U1—O4—H1o12^iv	151.13	H1o12^xii—H1o5—H1o12^vii	137.76
U1—O4—H2o12ⁱ	93.12	Pb^xii—H2o5—Pb^vii	111 (2)
Pb^iv—O4—O1ⁱ	145.2 (2)	Pb^xii—H2o5—O1	107.2 (11)
Pb^iv—O4—O2	102.8 (2)	Pb^xii—H2o5—O3	124.4 (10)
Pb^iv—O4—O5^xiii	57.73 (17)	Pb^xii—H2o5—O5	69 (2)
Pb^iv—O4—O8	81.42 (19)	Pb^xii—H2o5—O7^viii	118 (3)
Pb^iv—O4—O10^xiv	99.7 (2)	Pb^xii—H2o5—O7^ix	51.5 (8)
Pb^iv—O4—O11ⁱ	162.3 (2)	Pb^xii—H2o5—H1o5	87.1 (16)
Pb^iv—O4—O12ⁱ	89.97 (19)	Pb^xii—H2o5—H1o10^xi	92.26
Pb^iv—O4—O12^iv	54.13 (16)	Pb^xii—H2o5—H1o10ⁱⁱ	121.04
Pb^iv—O4—O13ⁱⁱ	112.60 (19)	Pb^xii—H2o5—H2o10^xi	81.06
Pb^iv—O4—H1o5^xiii	71.9 (16)	Pb^xii—H2o5—H2o10ⁱⁱ	145.83
Pb^iv—O4—H1o10^xiv	104.2	Pb^xii—H2o5—H1o12^xii	56.96
Pb^iv—O4—H2o10^xiv	85.84	Pb^xii—H2o5—H1o12^vii	151.95
Pb^iv—O4—H1o12^iv	67.9	Pb^vii—H2o5—O1	107.2 (11)
Pb^iv—O4—H2o12ⁱ	96.49	Pb^vii—H2o5—O3	124.4 (10)
O1ⁱ—O4—O2	52.02 (18)	Pb^vii—H2o5—O5	69 (2)
O1ⁱ—O4—O5^xiii	91.7 (2)	Pb^vii—H2o5—O7^viii	51.5 (8)
O1ⁱ—O4—O8	94.8 (2)	Pb^vii—H2o5—O7^ix	118 (3)
O1ⁱ—O4—O10^xiv	83.2 (2)	Pb^vii—H2o5—H1o5	87.1 (16)
O1ⁱ—O4—O11ⁱ	51.39 (17)	Pb^vii—H2o5—H1o10^xi	121.04
O1ⁱ—O4—O12ⁱ	124.5 (2)	Pb^vii—H2o5—H1o10ⁱⁱ	92.26
O1ⁱ—O4—O12^iv	139.7 (2)	Pb^vii—H2o5—H2o10^xi	145.83
O1ⁱ—O4—O13ⁱⁱ	94.8 (2)	Pb^vii—H2o5—H2o10ⁱⁱ	81.06
O1ⁱ—O4—H1o5^xiii	80.1 (15)	Pb^vii—H2o5—H1o12^xii	151.95
O1ⁱ—O4—H1o10^xiv	71.55	Pb^vii—H2o5—H1o12^vii	56.96
O1ⁱ—O4—H2o10^xiv	97.36	O1—H2o5—O3	57.6 (4)
O1ⁱ—O4—H1o12^iv	123.04	O1—H2o5—O5	171 (7)
O1ⁱ—O4—H2o12ⁱ	118.18	O1—H2o5—O7^viii	56.0 (5)
O2—O4—O5^xiii	81.1 (2)	O1—H2o5—O7^ix	56.0 (5)
O2—O4—O8	51.61 (15)	O1—H2o5—H1o5	154 (5)
O2—O4—O10^xiv	126.2 (2)	O1—H2o5—H1o10^xi	116.34
O2—O4—O11ⁱ	94.3 (2)	O1—H2o5—H1o10ⁱⁱ	116.34
O2—O4—O12ⁱ	145.4 (2)	O1—H2o5—H2o10^xi	98.59
O2—O4—O12^iv	153.8 (3)	O1—H2o5—H2o10ⁱⁱ	98.59
O2—O4—O13ⁱⁱ	94.46 (19)	O1—H2o5—H1o12^xii	100.78
O2—O4—H1o5^xiii	81.9 (11)	O1—H2o5—H1o12^vii	100.78
O2—O4—H1o10^xiv	111.82	O3—H2o5—O5	131 (7)
O2—O4—H2o10^xiv	135.43	O3—H2o5—O7^viii	96.8 (5)
O2—O4—H1o12^iv	154.77	O3—H2o5—O7^ix	96.8 (5)
O2—O4—H2o12ⁱ	140.24	O3—H2o5—H1o5	96 (5)
O5^xiii—O4—O8	108.2 (2)	O3—H2o5—H1o10^xi	61.37
O5^xiii—O4—O10^xiv	71.1 (2)	O3—H2o5—H1o10ⁱⁱ	61.37
O5^xiii—O4—O11ⁱ	130.9 (2)	O3—H2o5—H2o10^xi	54.08
O5^xiii—O4—O12ⁱ	131.6 (2)	O3—H2o5—H2o10ⁱⁱ	54.08
O5^xiii—O4—O12^iv	75.8 (2)	O3—H2o5—H1o12^xii	72.99
O5^xiii—O4—O13ⁱⁱ	167.5 (2)	O3—H2o5—H1o12^vii	72.99
O5^xiii—O4—H1o5^xiii	15.3 (15)	O5—H2o5—O7^viii	118 (4)
O5^xiii—O4—H1o10^xiv	64.1	O5—H2o5—O7^ix	118 (4)
O5^xiii—O4—H2o10^xiv	66.8	O5—H2o5—H1o5	35 (4)
O5^xiii—O4—H1o12^iv	74.16	O5—H2o5—H1o10^xi	72.05
O5^xiii—O4—H2o12ⁱ	137.99	O5—H2o5—H1o10ⁱⁱ	72.05
O8—O4—O10^xiv	177.8 (3)	O5—H2o5—H2o10^xi	88.48
O8—O4—O11ⁱ	106.3 (2)	O5—H2o5—H2o10ⁱⁱ	88.48
O8—O4—O12ⁱ	100.19 (19)	O5—H2o5—H1o12^xii	83.49
O8—O4—O12^iv	125.5 (2)	O5—H2o5—H1o12^vii	83.49
O8—O4—O13ⁱⁱ	60.65 (16)	O7^viii—H2o5—O7^ix	83.4 (18)
O8—O4—H1o5^xiii	118.8 (11)	O7^viii—H2o5—H1o5	136.1 (9)
O8—O4—H1o10^xiv	163.42	O7^viii—H2o5—H1o10^xi	149.31
O8—O4—H2o10^xiv	166.91	O7^viii—H2o5—H1o10ⁱⁱ	118.41
O8—O4—H1o12^iv	142.13	O7^viii—H2o5—H2o10^xi	150.53
O8—O4—H2o12ⁱ	98.57	O7^viii—H2o5—H2o10ⁱⁱ	94.46
O10^xiv—O4—O11ⁱ	73.2 (2)	O7^viii—H2o5—H1o12^xii	155.58
O10^xiv—O4—O12ⁱ	81.69 (19)	O7^viii—H2o5—H1o12^vii	76.03
O10^xiv—O4—O12^iv	56.47 (19)	O7^ix—H2o5—H1o5	136.1 (9)
O10^xiv—O4—O13ⁱⁱ	120.3 (2)	O7^ix—H2o5—H1o10^xi	118.41
O10^xiv—O4—H1o5^xiii	60.1 (12)	O7^ix—H2o5—H1o10ⁱⁱ	149.31
O10^xiv—O4—H1o10^xiv	14.46	O7^ix—H2o5—H2o10^xi	94.46
O10^xiv—O4—H2o10^xiv	14.71	O7^ix—H2o5—H2o10ⁱⁱ	150.53
O10^xiv—O4—H1o12^iv	39.87	O7^ix—H2o5—H1o12^xii	76.03
O10^xiv—O4—H2o12ⁱ	83.16	O7^ix—H2o5—H1o12^vii	155.58
O11ⁱ—O4—O12ⁱ	73.1 (2)	H1o5—H2o5—H1o10^xi	39.3
O11ⁱ—O4—O12^iv	110.1 (2)	H1o5—H2o5—H1o10ⁱⁱ	39.3
O11ⁱ—O4—O13ⁱⁱ	60.78 (18)	H1o5—H2o5—H2o10^xi	61.06
O11ⁱ—O4—H1o5^xiii	115.7 (15)	H1o5—H2o5—H2o10ⁱⁱ	61.06
O11ⁱ—O4—H1o10^xiv	73.03	H1o5—H2o5—H1o12^xii	68.05
O11ⁱ—O4—H2o10^xiv	85.19	H1o5—H2o5—H1o12^vii	68.05
O11ⁱ—O4—H1o12^iv	98.23	H1o10^xi—H2o5—H1o10ⁱⁱ	33.55
O11ⁱ—O4—H2o12ⁱ	66.93	H1o10^xi—H2o5—H2o10^xi	24.79
O12ⁱ—O4—O12^iv	55.85 (19)	H1o10^xi—H2o5—H2o10ⁱⁱ	55.67
O12ⁱ—O4—O13ⁱⁱ	51.13 (16)	H1o10^xi—H2o5—H1o12^xii	43.35
O12ⁱ—O4—H1o5^xiii	132.7 (11)	H1o10^xi—H2o5—H1o12^vii	76.84
O12ⁱ—O4—H1o10^xiv	95.45	H1o10ⁱⁱ—H2o5—H2o10^xi	55.67
O12ⁱ—O4—H2o10^xiv	76.73	H1o10ⁱⁱ—H2o5—H2o10ⁱⁱ	24.79
O12ⁱ—O4—H1o12^iv	59.74	H1o10ⁱⁱ—H2o5—H1o12^xii	76.84
O12ⁱ—O4—H2o12ⁱ	7	H1o10ⁱⁱ—H2o5—H1o12^vii	43.35
O12^iv—O4—O13ⁱⁱ	105.6 (2)	H2o10^xi—H2o5—H2o10ⁱⁱ	73.12
O12^iv—O4—H1o5^xiii	79.0 (12)	H2o10^xi—H2o5—H1o12^xii	24.45
O12^iv—O4—H1o10^xiv	68.46	H2o10^xi—H2o5—H1o12^vii	96.93
O12^iv—O4—H2o10^xiv	42.36	H2o10ⁱⁱ—H2o5—H1o12^xii	96.93
O12^iv—O4—H1o12^iv	16.7	H2o10ⁱⁱ—H2o5—H1o12^vii	24.45
O12^iv—O4—H2o12ⁱ	62.31	H1o12^xii—H2o5—H1o12^vii	119.86
O13ⁱⁱ—O4—H1o5^xiii	174.8 (15)	Pb—H1o10—O1^vi	109.31
O13ⁱⁱ—O4—H1o10^xiv	128.2	Pb—H1o10—O3^xvii	118.1
O13ⁱⁱ—O4—H2o10^xiv	122.74	Pb—H1o10—O4^xiv	118.45
O13ⁱⁱ—O4—H1o12^iv	110.77	Pb—H1o10—O5^xvii	166.07
O13ⁱⁱ—O4—H2o12ⁱ	45.83	Pb—H1o10—O6^vi	66.41
H1o5^xiii—O4—H1o10^xiv	50.88	Pb—H1o10—O10	47.02
H1o5^xiii—O4—H2o10^xiv	59.1	Pb—H1o10—O10^xvi	112.48
H1o5^xiii—O4—H1o12^iv	72.94	Pb—H1o10—O11^iv	75.15
H1o5^xiii—O4—H2o12ⁱ	137.54	Pb—H1o10—O12ⁱ	98.64
H1o10^xiv—O4—H2o10^xiv	26.26	Pb—H1o10—H1o5^xvii	173.64
H1o10^xiv—O4—H1o12^iv	52.41	Pb—H1o10—H2o5^xvii	154.88
H1o10^xiv—O4—H2o12ⁱ	96.29	Pb—H1o10—H1o10^xvi	118.98
H2o10^xiv—O4—H1o12^iv	26.15	Pb—H1o10—H2o10	77.02
H2o10^xiv—O4—H2o12ⁱ	79.84	Pb—H1o10—H2o10^xvi	121.33
H1o12^iv—O4—H2o12ⁱ	64.98	Pb—H1o10—H1o12ⁱ	92.74
Pb^xii—O5—Pb^vii	123.8 (2)	O1^vi—H1o10—O3^xvii	130.44
Pb^xii—O5—O3	110.64 (16)	O1^vi—H1o10—O4^xiv	54.8
Pb^xii—O5—O4^xv	132.9 (3)	O1^vi—H1o10—O5^xvii	80.84
Pb^xii—O5—O4^xix	58.59 (13)	O1^vi—H1o10—O6^vi	55.87
Pb^xii—O5—O6^xv	66.00 (12)	O1^vi—H1o10—O10	139.71
Pb^xii—O5—O7^viii	109.8 (3)	O1^vi—H1o10—O10^xvi	84.28
Pb^xii—O5—O7^ix	49.29 (13)	O1^vi—H1o10—O11^iv	43.32
Pb^xii—O5—H1o5	113.6 (12)	O1^vi—H1o10—O12ⁱ	109.5
Pb^xii—O5—H2o5	96 (3)	O1^vi—H1o10—H1o5^xvii	74.33
Pb^xii—O5—H1o10^xi	99.48	O1^vi—H1o10—H2o5^xvii	94.95
Pb^xii—O5—H1o10ⁱⁱ	134.35	O1^vi—H1o10—H1o10^xvi	73.97
Pb^xii—O5—H2o10^xi	82.48	O1^vi—H1o10—H2o10	142.2
Pb^xii—O5—H2o10ⁱⁱ	153.62	O1^vi—H1o10—H2o10^xvi	90.47
Pb^xii—O5—H1o12^xii	58.32	O1^vi—H1o10—H1o12ⁱ	112.92
Pb^xii—O5—H1o12^vii	177.57	O3^xvii—H1o10—O4^xiv	109.06
Pb^vii—O5—O3	110.64 (16)	O3^xvii—H1o10—O5^xvii	55.61
Pb^vii—O5—O4^xv	58.59 (13)	O3^xvii—H1o10—O6^vi	133.64
Pb^vii—O5—O4^xix	132.9 (3)	O3^xvii—H1o10—O10	86.58
Pb^vii—O5—O6^xv	66.00 (12)	O3^xvii—H1o10—O10^xvi	65.52
Pb^vii—O5—O7^viii	49.29 (13)	O3^xvii—H1o10—O11^iv	162.62
Pb^vii—O5—O7^ix	109.8 (3)	O3^xvii—H1o10—O12ⁱ	77.76
Pb^vii—O5—H1o5	113.6 (12)	O3^xvii—H1o10—H1o5^xvii	59.99
Pb^vii—O5—H2o5	96 (3)	O3^xvii—H1o10—H2o5^xvii	41.54
Pb^vii—O5—H1o10^xi	134.35	O3^xvii—H1o10—H1o10^xvi	71.31
Pb^vii—O5—H1o10ⁱⁱ	99.48	O3^xvii—H1o10—H2o10	66.33
Pb^vii—O5—H2o10^xi	153.62	O3^xvii—H1o10—H2o10^xvi	53.35
Pb^vii—O5—H2o10ⁱⁱ	82.48	O3^xvii—H1o10—H1o12ⁱ	79.43
Pb^vii—O5—H1o12^xii	177.57	O4^xiv—H1o10—O5^xvii	59.03
Pb^vii—O5—H1o12^vii	58.32	O4^xiv—H1o10—O6^vi	106.27
O3—O5—O4^xv	110.3 (2)	O4^xiv—H1o10—O10	103.24
O3—O5—O4^xix	110.3 (2)	O4^xiv—H1o10—O10^xvi	122.1
O3—O5—O6^xv	168.7 (4)	O4^xiv—H1o10—O11^iv	53.57
O3—O5—O7^viii	75.3 (2)	O4^xiv—H1o10—O12ⁱ	54.88
O3—O5—O7^ix	75.3 (2)	O4^xiv—H1o10—H1o5^xvii	58.96
O3—O5—H1o5	73 (5)	O4^xiv—H1o10—H2o5^xvii	70.28
O3—O5—H2o5	36 (6)	O4^xiv—H1o10—H1o10^xvi	111.84
O3—O5—H1o10^xi	59.12	O4^xiv—H1o10—H2o10	88.82
O3—O5—H1o10ⁱⁱ	59.12	O4^xiv—H1o10—H2o10^xvi	117.97
O3—O5—H2o10^xi	50.45	O4^xiv—H1o10—H1o12ⁱ	58.89
O3—O5—H2o10ⁱⁱ	50.45	O5^xvii—H1o10—O6^vi	127.37
O3—O5—H1o12^xii	67.02	O5^xvii—H1o10—O10	119.11
O3—O5—H1o12^vii	67.02	O5^xvii—H1o10—O10^xvi	77.3
O4^xv—O5—O4^xix	85.8 (3)	O5^xvii—H1o10—O11^iv	108.78
O4^xv—O5—O6^xv	77.7 (2)	O5^xvii—H1o10—O12ⁱ	68.42
O4^xv—O5—O7^viii	102.33 (15)	O5^xvii—H1o10—H1o5^xvii	7.79
O4^xv—O5—O7^ix	168.1 (3)	O5^xvii—H1o10—H2o5^xvii	14.46
O4^xv—O5—H1o5	59 (3)	O5^xvii—H1o10—H1o10^xvi	72.37
O4^xv—O5—H2o5	131 (2)	O5^xvii—H1o10—H2o10	89.12
O4^xv—O5—H1o10^xi	82.29	O5^xvii—H1o10—H2o10^xvi	66.63
O4^xv—O5—H1o10ⁱⁱ	56.87	O5^xvii—H1o10—H1o12ⁱ	74.19
O4^xv—O5—H2o10^xi	106.89	O6^vi—H1o10—O10	113.4
O4^xv—O5—H2o10ⁱⁱ	59.86	O6^vi—H1o10—O10^xvi	70.61
O4^xv—O5—H1o12^xii	121.22	O6^vi—H1o10—O11^iv	60.4
O4^xv—O5—H1o12^vii	48.83	O6^vi—H1o10—O12ⁱ	148.46
O4^xix—O5—O6^xv	77.7 (2)	O6^vi—H1o10—H1o5^xvii	119.57
O4^xix—O5—O7^viii	168.1 (3)	O6^vi—H1o10—H2o5^xvii	136.52
O4^xix—O5—O7^ix	102.33 (15)	O6^vi—H1o10—H1o10^xvi	68.23
O4^xix—O5—H1o5	59 (3)	O6^vi—H1o10—H2o10	143.37
O4^xix—O5—H2o5	131 (2)	O6^vi—H1o10—H2o10^xvi	83.81
O4^xix—O5—H1o10^xi	56.87	O6^vi—H1o10—H1o12ⁱ	145.96
O4^xix—O5—H1o10ⁱⁱ	82.29	O10—H1o10—O10^xvi	131.97
O4^xix—O5—H2o10^xi	59.86	O10—H1o10—O11^iv	96.51
O4^xix—O5—H2o10ⁱⁱ	106.89	O10—H1o10—O12ⁱ	57.12
O4^xix—O5—H1o12^xii	48.83	O10—H1o10—H1o5^xvii	126.88
O4^xix—O5—H1o12^vii	121.22	O10—H1o10—H2o5^xvii	109.37
O6^xv—O5—O7^viii	95.4 (2)	O10—H1o10—H1o10^xvi	142.95
O6^xv—O5—O7^ix	95.4 (2)	O10—H1o10—H2o10	30
O6^xv—O5—H1o5	118 (5)	O10—H1o10—H2o10^xvi	128.92
O6^xv—O5—H2o5	132 (6)	O10—H1o10—H1o12ⁱ	51.24
O6^xv—O5—H1o10^xi	131.31	O10^xvi—H1o10—O11^iv	121.92
O6^xv—O5—H1o10ⁱⁱ	131.31	O10^xvi—H1o10—O12ⁱ	139.77
O6^xv—O5—H2o10^xi	136.32	O10^xvi—H1o10—H1o5^xvii	72.72
O6^xv—O5—H2o10ⁱⁱ	136.32	O10^xvi—H1o10—H2o5^xvii	75.45
O6^xv—O5—H1o12^xii	116.42	O10^xvi—H1o10—H1o10^xvi	10.98
O6^xv—O5—H1o12^vii	116.42	O10^xvi—H1o10—H2o10	129
O7^viii—O5—O7^ix	68.3 (2)	O10^xvi—H1o10—H2o10^xvi	13.29
O7^viii—O5—H1o5	133 (3)	O10^xvi—H1o10—H1o12ⁱ	143.36
O7^viii—O5—H2o5	48 (4)	O11^iv—H1o10—O12ⁱ	89.52
O7^viii—O5—H1o10^xi	132.25	O11^iv—H1o10—H1o5^xvii	105.53
O7^viii—O5—H1o10ⁱⁱ	109.4	O11^iv—H1o10—H2o5^xvii	122.21
O7^viii—O5—H2o10^xi	124.32	O11^iv—H1o10—H1o10^xvi	113.54
O7^viii—O5—H2o10ⁱⁱ	84.84	O11^iv—H1o10—H2o10	109.03
O7^viii—O5—H1o12^xii	129.55	O11^iv—H1o10—H2o10^xvi	131.59
O7^viii—O5—H1o12^vii	70.5	O11^iv—H1o10—H1o12ⁱ	89.15
O7^ix—O5—H1o5	133 (3)	O12ⁱ—H1o10—H1o5^xvii	75.1
O7^ix—O5—H2o5	48 (4)	O12ⁱ—H1o10—H2o5^xvii	66.05
O7^ix—O5—H1o10^xi	109.4	O12ⁱ—H1o10—H1o10^xvi	139.27
O7^ix—O5—H1o10ⁱⁱ	132.25	O12ⁱ—H1o10—H2o10	34.33
O7^ix—O5—H2o10^xi	84.84	O12ⁱ—H1o10—H2o10^xvi	126.5
O7^ix—O5—H2o10ⁱⁱ	124.32	O12ⁱ—H1o10—H1o12ⁱ	6.02
O7^ix—O5—H1o12^xii	70.5	H1o5^xvii—H1o10—H2o5^xvii	20.65
O7^ix—O5—H1o12^vii	129.55	H1o5^xvii—H1o10—H1o10^xvi	66.77
H1o5—O5—H2o5	109 (7)	H1o5^xvii—H1o10—H2o10	96.9
H1o5—O5—H1o10^xi	23.51	H1o5^xvii—H1o10—H2o10^xvi	63.12
H1o5—O5—H1o10ⁱⁱ	23.51	H1o5^xvii—H1o10—H1o12ⁱ	80.97
H1o5—O5—H2o10^xi	48.08	H2o5^xvii—H1o10—H1o10^xvi	73.23
H1o5—O5—H2o10ⁱⁱ	48.08	H2o5^xvii—H1o10—H2o10	79.8
H1o5—O5—H1o12^xii	65.35	H2o5^xvii—H1o10—H2o10^xvi	63.08
H1o5—O5—H1o12^vii	65.35	H2o5^xvii—H1o10—H1o12ⁱ	71.17
H2o5—O5—H1o10^xi	93.49	H1o10^xvi—H1o10—H2o10	137.05
H2o5—O5—H1o10ⁱⁱ	93.49	H1o10^xvi—H1o10—H2o10^xvi	18.27
H2o5—O5—H2o10^xi	77.62	H1o10^xvi—H1o10—H1o12ⁱ	144.16
H2o5—O5—H2o10ⁱⁱ	77.62	H2o10—H1o10—H2o10^xvi	118.78
H2o5—O5—H1o12^xii	82.71	H2o10—H1o10—H1o12ⁱ	29.93
H2o5—O5—H1o12^vii	82.71	H2o10^xvi—H1o10—H1o12ⁱ	130.09
H1o10^xi—O5—H1o10ⁱⁱ	35.25	Pb—H2o10—O3^xvii	126.23
H1o10^xi—O5—H2o10^xi	24.6	Pb—H2o10—O4^xiv	109.91
H1o10^xi—O5—H2o10ⁱⁱ	56.17	Pb—H2o10—O5^xvii	143.27
H1o10^xi—O5—H1o12^xii	44.16	Pb—H2o10—O7ⁱⁱ	44.5
H1o10^xi—O5—H1o12^vii	78.81	Pb—H2o10—O8ⁱⁱ	97
H1o10ⁱⁱ—O5—H2o10^xi	56.17	Pb—H2o10—O9	43.65
H1o10ⁱⁱ—O5—H2o10ⁱⁱ	24.6	Pb—H2o10—O10	47.02
H1o10ⁱⁱ—O5—H1o12^xii	78.81	Pb—H2o10—O12ⁱ	128.16
H1o10ⁱⁱ—O5—H1o12^vii	44.16	Pb—H2o10—H1o5^xvii	131.32
H2o10^xi—O5—H2o10ⁱⁱ	71.18	Pb—H2o10—H2o5^xvii	150.78
H2o10^xi—O5—H1o12^xii	24.18	Pb—H2o10—H1o10	77.02
H2o10^xi—O5—H1o12^vii	95.36	Pb—H2o10—H1o10^xvi	89.54
H2o10ⁱⁱ—O5—H1o12^xii	95.36	Pb—H2o10—H1o12ⁱ	122.21
H2o10ⁱⁱ—O5—H1o12^vii	24.18	Pb—H2o10—H2o12ⁱ	118.26
H1o12^xii—O5—H1o12^vii	119.53	O3^xvii—H2o10—O4^xiv	107.05
U2—O6—Pb^x	124.30 (16)	O3^xvii—H2o10—O5^xvii	53.75
U2—O6—Pb^iv	124.30 (16)	O3^xvii—H2o10—O7ⁱⁱ	88.38
U2—O6—O1	50.4 (2)	O3^xvii—H2o10—O8ⁱⁱ	62.25
U2—O6—O2	52.2 (2)	O3^xvii—H2o10—O9	135.18
U2—O6—O5^xiii	134.9 (4)	O3^xvii—H2o10—O10	103.77
U2—O6—O8	53.47 (16)	O3^xvii—H2o10—O12ⁱ	103.84
U2—O6—O8ⁱⁱⁱ	53.47 (16)	O3^xvii—H2o10—H1o5^xvii	57.4
U2—O6—O10^x	128.9 (2)	O3^xvii—H2o10—H2o5^xvii	41.72
U2—O6—O10^iv	128.9 (2)	O3^xvii—H2o10—H1o10	85.02
U2—O6—O11	57.44 (15)	O3^xvii—H2o10—H1o10^xvi	60.77
U2—O6—O11ⁱⁱⁱ	57.44 (15)	O3^xvii—H2o10—H1o12ⁱ	110.69
U2—O6—H1o5^xiii	122.9 (14)	O3^xvii—H2o10—H2o12ⁱ	109.05
U2—O6—H1o10^x	123.91	O4^xiv—H2o10—O5^xvii	53.34
U2—O6—H1o10^iv	123.91	O4^xiv—H2o10—O7ⁱⁱ	152.54
Pb^x—O6—Pb^iv	102.83 (16)	O4^xiv—H2o10—O8ⁱⁱ	150.91
Pb^x—O6—O1	124.41 (13)	O4^xiv—H2o10—O9	117.18
Pb^x—O6—O2	97.69 (17)	O4^xiv—H2o10—O10	81.75
Pb^x—O6—O5^xiii	54.05 (9)	O4^xiv—H2o10—O12ⁱ	60.03
Pb^x—O6—O8	142.6 (2)	O4^xiv—H2o10—H1o5^xvii	50.86
Pb^x—O6—O8ⁱⁱⁱ	71.28 (11)	O4^xiv—H2o10—H2o5^xvii	66.16
Pb^x—O6—O10^x	51.41 (15)	O4^xiv—H2o10—H1o10	64.92
Pb^x—O6—O10^iv	102.6 (2)	O4^xiv—H2o10—H1o10^xvi	79.22
Pb^x—O6—O11	172.3 (3)	O4^xiv—H2o10—H1o12ⁱ	55.45
Pb^x—O6—O11ⁱⁱⁱ	79.99 (9)	O4^xiv—H2o10—H2o12ⁱ	72.88
Pb^x—O6—H1o5^xiii	58.0 (5)	O5^xvii—H2o10—O7ⁱⁱ	137.43
Pb^x—O6—H1o10^x	66.06	O5^xvii—H2o10—O8ⁱⁱ	109.41
Pb^x—O6—H1o10^iv	100.02	O5^xvii—H2o10—O9	167.46
Pb^iv—O6—O1	124.41 (13)	O5^xvii—H2o10—O10	96.27
Pb^iv—O6—O2	97.69 (17)	O5^xvii—H2o10—O12ⁱ	75.66
Pb^iv—O6—O5^xiii	54.05 (9)	O5^xvii—H2o10—H1o5^xvii	11.95
Pb^iv—O6—O8	71.28 (11)	O5^xvii—H2o10—H2o5^xvii	13.9
Pb^iv—O6—O8ⁱⁱⁱ	142.6 (2)	O5^xvii—H2o10—H1o10	66.28
Pb^iv—O6—O10^x	102.6 (2)	O5^xvii—H2o10—H1o10^xvi	57.2
Pb^iv—O6—O10^iv	51.41 (15)	O5^xvii—H2o10—H1o12ⁱ	78.05
Pb^iv—O6—O11	79.99 (9)	O5^xvii—H2o10—H2o12ⁱ	89.8
Pb^iv—O6—O11ⁱⁱⁱ	172.3 (3)	O7ⁱⁱ—H2o10—O8ⁱⁱ	56.49
Pb^iv—O6—H1o5^xiii	58.0 (5)	O7ⁱⁱ—H2o10—O9	54.97
Pb^iv—O6—H1o10^x	100.02	O7ⁱⁱ—H2o10—O10	72.41
Pb^iv—O6—H1o10^iv	66.06	O7ⁱⁱ—H2o10—O12ⁱ	139.24
O1—O6—O2	102.6 (3)	O7ⁱⁱ—H2o10—H1o5^xvii	132.64
O1—O6—O5^xiii	174.7 (4)	O7ⁱⁱ—H2o10—H2o5^xvii	129.13
O1—O6—O8	84.60 (18)	O7ⁱⁱ—H2o10—H1o10	94.88
O1—O6—O8ⁱⁱⁱ	84.60 (18)	O7ⁱⁱ—H2o10—H1o10^xvi	89.39
O1—O6—O10^x	88.1 (2)	O7ⁱⁱ—H2o10—H1o12ⁱ	140.32
O1—O6—O10^iv	88.1 (2)	O7ⁱⁱ—H2o10—H2o12ⁱ	124.19
O1—O6—O11	49.71 (12)	O8ⁱⁱ—H2o10—O9	75.17
O1—O6—O11ⁱⁱⁱ	49.71 (12)	O8ⁱⁱ—H2o10—O10	126.19
O1—O6—H1o5^xiii	173.3 (14)	O8ⁱⁱ—H2o10—O12ⁱ	94.83
O1—O6—H1o10^x	77.49	O8ⁱⁱ—H2o10—H1o5^xvii	117.32
O1—O6—H1o10^iv	77.49	O8ⁱⁱ—H2o10—H2o5^xvii	95.52
O2—O6—O5^xiii	82.7 (3)	O8ⁱⁱ—H2o10—H1o10	134.69
O2—O6—O8	48.92 (15)	O8ⁱⁱ—H2o10—H1o10^xvi	112.75
O2—O6—O8ⁱⁱⁱ	48.92 (15)	O8ⁱⁱ—H2o10—H1o12ⁱ	101.03
O2—O6—O10^x	146.01 (18)	O8ⁱⁱ—H2o10—H2o12ⁱ	84.95
O2—O6—O10^iv	146.01 (18)	O9—H2o10—O10	89.79
O2—O6—O11	89.0 (2)	O9—H2o10—O12ⁱ	92.49
O2—O6—O11ⁱⁱⁱ	89.0 (2)	O9—H2o10—H1o5^xvii	167.3
O2—O6—H1o5^xiii	70.7 (14)	O9—H2o10—H2o5^xvii	165.23
O2—O6—H1o10^x	158.22	O9—H2o10—H1o10	119.31
O2—O6—H1o10^iv	158.22	O9—H2o10—H1o10^xvi	132.76
O5^xiii—O6—O8	99.1 (2)	O9—H2o10—H1o12ⁱ	89.68
O5^xiii—O6—O8ⁱⁱⁱ	99.1 (2)	O9—H2o10—H2o12ⁱ	78.85
O5^xiii—O6—O10^x	87.5 (2)	O10—H2o10—O12ⁱ	137.89
O5^xiii—O6—O10^iv	87.5 (2)	O10—H2o10—H1o5^xvii	84.33
O5^xiii—O6—O11	131.22 (12)	O10—H2o10—H2o5^xvii	104.99
O5^xiii—O6—O11ⁱⁱⁱ	131.22 (12)	O10—H2o10—H1o10	30
O5^xiii—O6—H1o5^xiii	12.0 (14)	O10—H2o10—H1o10^xvi	46.67
O5^xiii—O6—H1o10^x	97.61	O10—H2o10—H1o12ⁱ	130.77
O5^xiii—O6—H1o10^iv	97.61	O10—H2o10—H2o12ⁱ	143.04
O8—O6—O8ⁱⁱⁱ	91.0 (2)	O12ⁱ—H2o10—H1o5^xvii	84.46
O8—O6—O10^x	164.9 (3)	O12ⁱ—H2o10—H2o5^xvii	76.66
O8—O6—O10^iv	101.41 (19)	O12ⁱ—H2o10—H1o10	124.46
O8—O6—O11	45.10 (15)	O12ⁱ—H2o10—H1o10^xvi	130.66
O8—O6—O11ⁱⁱⁱ	110.9 (2)	O12ⁱ—H2o10—H1o12ⁱ	7.69
O8—O6—H1o5^xiii	90.7 (10)	O12ⁱ—H2o10—H2o12ⁱ	15.17
O8—O6—H1o10^x	150.62	H1o5^xvii—H2o10—H2o5^xvii	23.5
O8—O6—H1o10^iv	110.03	H1o5^xvii—H2o10—H1o10	54.34
O8ⁱⁱⁱ—O6—O10^x	101.41 (19)	H1o5^xvii—H2o10—H1o10^xvi	46.88
O8ⁱⁱⁱ—O6—O10^iv	164.9 (3)	H1o5^xvii—H2o10—H1o12ⁱ	85.71
O8ⁱⁱⁱ—O6—O11	110.9 (2)	H1o5^xvii—H2o10—H2o12ⁱ	99.22
O8ⁱⁱⁱ—O6—O11ⁱⁱⁱ	45.10 (15)	H2o5^xvii—H2o10—H1o10	75.4
O8ⁱⁱⁱ—O6—H1o5^xiii	90.7 (10)	H2o5^xvii—H2o10—H1o10^xvi	61.25
O8ⁱⁱⁱ—O6—H1o10^x	110.03	H2o5^xvii—H2o10—H1o12ⁱ	80.76
O8ⁱⁱⁱ—O6—H1o10^iv	150.62	H2o5^xvii—H2o10—H2o12ⁱ	89.05
O10^x—O6—O10^iv	65.1 (3)	H1o10—H2o10—H1o10^xvi	24.68
O10^x—O6—O11	121.1 (3)	H1o10—H2o10—H1o12ⁱ	120.37
O10^x—O6—O11ⁱⁱⁱ	73.4 (2)	H1o10—H2o10—H2o12ⁱ	137.79
O10^x—O6—H1o5^xiii	97.6 (12)	H1o10^xvi—H2o10—H1o12ⁱ	130.26
O10^x—O6—H1o10^x	14.66	H1o10^xvi—H2o10—H2o12ⁱ	145.76
O10^x—O6—H1o10^iv	55.37	H1o12ⁱ—H2o10—H2o12ⁱ	17.49
O10^iv—O6—O11	73.4 (2)	Pb—H1o12—O3^v	89.83
O10^iv—O6—O11ⁱⁱⁱ	121.1 (3)	Pb—H1o12—O4^iv	58.57
O10^iv—O6—H1o5^xiii	97.6 (12)	Pb—H1o12—O5^v	50.93
O10^iv—O6—H1o10^x	55.37	Pb—H1o12—O10^viii	126.74
O10^iv—O6—H1o10^iv	14.66	Pb—H1o12—O12	46.66
O11—O6—O11ⁱⁱⁱ	96.32 (19)	Pb—H1o12—O12^xviii	91.02
O11—O6—H1o5^xiii	128.5 (4)	Pb—H1o12—O13^vii	104.57
O11—O6—H1o10^x	106.5	Pb—H1o12—H1o5^v	62.17
O11—O6—H1o10^iv	74.42	Pb—H1o12—H2o5^v	54.86
O11ⁱⁱⁱ—O6—H1o5^xiii	128.5 (4)	Pb—H1o12—H1o10^viii	108.95
O11ⁱⁱⁱ—O6—H1o10^x	74.42	Pb—H1o12—H2o10^viii	128.64
O11ⁱⁱⁱ—O6—H1o10^iv	106.5	Pb—H1o12—H1o12^xviii	81.26
H1o5^xiii—O6—H1o10^x	108.7	Pb—H1o12—H2o12	76.66
H1o5^xiii—O6—H1o10^iv	108.7	Pb—H1o12—H2o12^xviii	86.31
H1o10^x—O6—H1o10^iv	43.53	O3^v—H1o12—O4^iv	100.77
U1—O7—Pbⁱⁱ	157.8 (3)	O3^v—H1o12—O5^v	48.55
U1—O7—O1ⁱ	51.60 (17)	O3^v—H1o12—O10^viii	59.45
U1—O7—O2	51.24 (17)	O3^v—H1o12—O12	113.94
U1—O7—O5ⁱ	140.8 (2)	O3^v—H1o12—O12^xviii	169.22
U1—O7—O7ⁱⁱⁱ	93.7 (2)	O3^v—H1o12—O13^vii	87.57
U1—O7—O8	50.62 (17)	O3^v—H1o12—H1o5^v	47.94
U1—O7—O9ⁱⁱ	107.1 (2)	O3^v—H1o12—H2o5^v	37.72
U1—O7—O10ⁱⁱ	123.4 (3)	O3^v—H1o12—H1o10^viii	56.35
U1—O7—O11ⁱ	51.39 (17)	O3^v—H1o12—H2o10^viii	46.74
U1—O7—O12ⁱⁱ	122.3 (2)	O3^v—H1o12—H1o12^xviii	171.01
U1—O7—O13ⁱⁱ	55.39 (17)	O3^v—H1o12—H2o12	123.02
U1—O7—H2o5ⁱ	127.2 (6)	O3^v—H1o12—H2o12^xviii	154.13
U1—O7—H2o10ⁱⁱ	110.24	O4^iv—H1o12—O5^v	57.01
Pbⁱⁱ—O7—O1ⁱ	147.9 (3)	O4^iv—H1o12—O10^viii	83.91
Pbⁱⁱ—O7—O2	141.3 (2)	O4^iv—H1o12—O12	93.81
Pbⁱⁱ—O7—O5ⁱ	60.12 (16)	O4^iv—H1o12—O12^xviii	70.67
Pbⁱⁱ—O7—O7ⁱⁱⁱ	108.07 (19)	O4^iv—H1o12—O13^vii	160.73
Pbⁱⁱ—O7—O8	118.11 (18)	O4^iv—H1o12—H1o5^v	53.19
Pbⁱⁱ—O7—O9ⁱⁱ	50.70 (14)	O4^iv—H1o12—H2o5^v	70.77
Pbⁱⁱ—O7—O10ⁱⁱ	55.00 (17)	O4^iv—H1o12—H1o10^viii	68.7
Pbⁱⁱ—O7—O11ⁱ	125.2 (2)	O4^iv—H1o12—H2o10^viii	98.41
Pbⁱⁱ—O7—O12ⁱⁱ	50.02 (14)	O4^iv—H1o12—H1o12^xviii	73.55
Pbⁱⁱ—O7—O13ⁱⁱ	102.72 (19)	O4^iv—H1o12—H2o12	116.57
Pbⁱⁱ—O7—H2o5ⁱ	73.2 (4)	O4^iv—H1o12—H2o12^xviii	55.8
Pbⁱⁱ—O7—H2o10ⁱⁱ	64.44	O5^v—H1o12—O10^viii	77.74
O1ⁱ—O7—O2	53.48 (19)	O5^v—H1o12—O12	94.76
O1ⁱ—O7—O5ⁱ	89.2 (2)	O5^v—H1o12—O12^xviii	125.68
O1ⁱ—O7—O7ⁱⁱⁱ	53.20 (13)	O5^v—H1o12—O13^vii	121.69
O1ⁱ—O7—O8	92.7 (2)	O5^v—H1o12—H1o5^v	13.55
O1ⁱ—O7—O9ⁱⁱ	152.8 (2)	O5^v—H1o12—H2o5^v	13.8
O1ⁱ—O7—O10ⁱⁱ	135.9 (2)	O5^v—H1o12—H1o10^viii	61.65
O1ⁱ—O7—O11ⁱ	51.06 (14)	O5^v—H1o12—H2o10^viii	77.77
O1ⁱ—O7—O12ⁱⁱ	112.4 (2)	O5^v—H1o12—H1o12^xviii	123.22
O1ⁱ—O7—O13ⁱⁱ	100.3 (2)	O5^v—H1o12—H2o12	122.97
O1ⁱ—O7—H2o5ⁱ	75.7 (5)	O5^v—H1o12—H2o12^xviii	112.16
O1ⁱ—O7—H2o10ⁱⁱ	134.64	O10^viii—H1o12—O12	172.21
O2—O7—O5ⁱ	108.9 (2)	O10^viii—H1o12—O12^xviii	112.04
O2—O7—O7ⁱⁱⁱ	53.37 (16)	O10^viii—H1o12—O13^vii	115.15
O2—O7—O8	50.33 (16)	O10^viii—H1o12—H1o5^v	65.2
O2—O7—O9ⁱⁱ	130.8 (2)	O10^viii—H1o12—H2o5^v	79.02
O2—O7—O10ⁱⁱ	88.2 (2)	O10^viii—H1o12—H1o10^viii	18.07
O2—O7—O11ⁱ	93.2 (2)	O10^viii—H1o12—H2o10^viii	17.54
O2—O7—O12ⁱⁱ	165.9 (2)	O10^viii—H1o12—H1o12^xviii	125.58
O2—O7—O13ⁱⁱ	99.5 (2)	O10^viii—H1o12—H2o12	156.09
O2—O7—H2o5ⁱ	101.4 (8)	O10^viii—H1o12—H2o12^xviii	103.36
O2—O7—H2o10ⁱⁱ	82.24	O12—H1o12—O12^xviii	73.96
O5ⁱ—O7—O7ⁱⁱⁱ	55.83 (16)	O12—H1o12—O13^vii	66.92
O5ⁱ—O7—O8	148.3 (2)	O12—H1o12—H1o5^v	107.51
O5ⁱ—O7—O9ⁱⁱ	109.9 (2)	O12—H1o12—H2o5^v	93.19
O5ⁱ—O7—O10ⁱⁱ	83.2 (2)	O12—H1o12—H1o10^viii	155.56
O5ⁱ—O7—O11ⁱ	106.5 (2)	O12—H1o12—H2o10^viii	158.81
O5ⁱ—O7—O12ⁱⁱ	67.72 (18)	O12—H1o12—H1o12^xviii	60.36
O5ⁱ—O7—O13ⁱⁱ	150.0 (3)	O12—H1o12—H2o12	30
O5ⁱ—O7—H2o5ⁱ	13.7 (7)	O12—H1o12—H2o12^xviii	81.28
O5ⁱ—O7—H2o10ⁱⁱ	97.47	O12^xviii—H1o12—O13^vii	102.61
O7ⁱⁱⁱ—O7—O8	101.2 (2)	O12^xviii—H1o12—H1o5^v	123.85
O7ⁱⁱⁱ—O7—O9ⁱⁱ	153.96 (19)	O12^xviii—H1o12—H2o5^v	138.22
O7ⁱⁱⁱ—O7—O10ⁱⁱ	87.91 (19)	O12^xviii—H1o12—H1o10^viii	113.38
O7ⁱⁱⁱ—O7—O11ⁱ	101.70 (17)	O12^xviii—H1o12—H2o10^viii	126.5
O7ⁱⁱⁱ—O7—O12ⁱⁱ	120.2 (2)	O12^xviii—H1o12—H1o12^xviii	13.6
O7ⁱⁱⁱ—O7—O13ⁱⁱ	149.1 (2)	O12^xviii—H1o12—H2o12	67.56
O7ⁱⁱⁱ—O7—H2o5ⁱ	48.3 (9)	O12^xviii—H1o12—H2o12^xviii	15.57
O7ⁱⁱⁱ—O7—H2o10ⁱⁱ	94.66	O13^vii—H1o12—H1o5^v	130.41
O8—O7—O9ⁱⁱ	81.2 (2)	O13^vii—H1o12—H2o5^v	108.51
O8—O7—O10ⁱⁱ	73.5 (2)	O13^vii—H1o12—H1o10^viii	129.4
O8—O7—O11ⁱ	99.1 (2)	O13^vii—H1o12—H2o10^viii	99.91
O8—O7—O12ⁱⁱ	138.6 (2)	O13^vii—H1o12—H1o12^xviii	95.82
O8—O7—O13ⁱⁱ	60.30 (18)	O13^vii—H1o12—H2o12	45.79
O8—O7—H2o5ⁱ	148.4 (12)	O13^vii—H1o12—H2o12^xviii	118.17
O8—O7—H2o10ⁱⁱ	59.82	H1o5^v—H1o12—H2o5^v	23.05
O9ⁱⁱ—O7—O10ⁱⁱ	67.73 (19)	H1o5^v—H1o12—H1o10^viii	48.49
O9ⁱⁱ—O7—O11ⁱ	103.50 (19)	H1o5^v—H1o12—H2o10^viii	67.49
O9ⁱⁱ—O7—O12ⁱⁱ	61.24 (17)	H1o5^v—H1o12—H1o12^xviii	125.27
O9ⁱⁱ—O7—O13ⁱⁱ	53.69 (16)	H1o5^v—H1o12—H2o12	136.34
O9ⁱⁱ—O7—H2o5ⁱ	121.8 (4)	H1o5^v—H1o12—H2o12^xviii	108.78
O9ⁱⁱ—O7—H2o10ⁱⁱ	63.85	H2o5^v—H1o12—H1o10^viii	65.48
O10ⁱⁱ—O7—O11ⁱ	169.0 (3)	H2o5^v—H1o12—H2o10^viii	74.79
O10ⁱⁱ—O7—O12ⁱⁱ	104.6 (2)	H2o5^v—H1o12—H1o12^xviii	133.47
O10ⁱⁱ—O7—O13ⁱⁱ	107.7 (2)	H2o5^v—H1o12—H2o12	118.04
O10ⁱⁱ—O7—H2o5ⁱ	94.4 (13)	H2o5^v—H1o12—H2o12^xviii	125.53
O10ⁱⁱ—O7—H2o10ⁱⁱ	14.3	H1o10^viii—H1o12—H2o10^viii	29.71
O11ⁱ—O7—O12ⁱⁱ	75.34 (19)	H1o10^viii—H1o12—H1o12^xviii	125.57
O11ⁱ—O7—O13ⁱⁱ	61.31 (16)	H1o10^viii—H1o12—H2o12	174.12
O11ⁱ—O7—H2o5ⁱ	96.0 (14)	H1o10^viii—H1o12—H2o12^xviii	100.97
O11ⁱ—O7—H2o10ⁱⁱ	155.73	H2o10^viii—H1o12—H1o12^xviii	140
O12ⁱⁱ—O7—O13ⁱⁱ	82.43 (19)	H2o10^viii—H1o12—H2o12	144.9
O12ⁱⁱ—O7—H2o5ⁱ	72.2 (11)	H2o10^viii—H1o12—H2o12^xviii	119.9
O12ⁱⁱ—O7—H2o10ⁱⁱ	111.58	H1o12^xviii—H1o12—H2o12	56.14
O13ⁱⁱ—O7—H2o5ⁱ	150.0 (15)	H1o12^xviii—H1o12—H2o12^xviii	24.74
O13ⁱⁱ—O7—H2o10ⁱⁱ	95.78	H2o12—H1o12—H2o12^xviii	80.88
H2o5ⁱ—O7—H2o10ⁱⁱ	108.22	U1^viii—H2o12—Pb	141.52
U1—O8—U2	104.96 (18)	U1^viii—H2o12—As	71.14
U1—O8—As	144.7 (3)	U1^viii—H2o12—As^vii	66.72
U1—O8—P	144.7 (3)	U1^viii—H2o12—P	71.14
U1—O8—O2	54.04 (16)	U1^viii—H2o12—P^vii	66.72
U1—O8—O3	107.4 (2)	U1^viii—H2o12—O4^viii	34.05
U1—O8—O4	38.52 (13)	U1^viii—H2o12—O9	95.38
U1—O8—O6	97.07 (18)	U1^viii—H2o12—O10^viii	126.31
U1—O8—O7	35.92 (12)	U1^viii—H2o12—O11	44.27
U1—O8—O9	114.6 (2)	U1^viii—H2o12—O12	168.23
U1—O8—O11	161.4 (3)	U1^viii—H2o12—O12^xviii	97.66
U1—O8—O13	133.5 (3)	U1^viii—H2o12—O13^vii	47.11
U1—O8—O13ⁱⁱ	50.59 (13)	U1^viii—H2o12—H2o10^viii	124.28
U1—O8—H2o10ⁱⁱ	99.46	U1^viii—H2o12—H1o12	140.49
U2—O8—As	104.2 (3)	U1^viii—H2o12—H1o12^xviii	91.67
U2—O8—P	104.2 (3)	U1^viii—H2o12—H2o12^xviii	113.55
U2—O8—O2	51.24 (16)	Pb—H2o12—As	70.98
U2—O8—O3	35.57 (15)	Pb—H2o12—As^vii	113.46
U2—O8—O4	100.61 (19)	Pb—H2o12—P	70.98
U2—O8—O6	33.62 (11)	Pb—H2o12—P^vii	113.46
U2—O8—O7	104.5 (2)	Pb—H2o12—O4^viii	139.96
U2—O8—O9	111.9 (3)	Pb—H2o12—O9	46.25
U2—O8—O11	62.78 (17)	Pb—H2o12—O10^viii	90.61
U2—O8—O13	119.8 (2)	Pb—H2o12—O11	97.25
U2—O8—O13ⁱⁱ	155.5 (2)	Pb—H2o12—O12	46.66
U2—O8—H2o10ⁱⁱ	86.75	Pb—H2o12—O12^xviii	95.3
As—O8—P	0	Pb—H2o12—O13^vii	128.14
As—O8—O2	152.5 (4)	Pb—H2o12—H2o10^viii	90.54
As—O8—O3	107.9 (2)	Pb—H2o12—H1o12	76.66
As—O8—O4	116.0 (3)	Pb—H2o12—H1o12^xviii	90.5
As—O8—O6	96.2 (3)	Pb—H2o12—H2o12^xviii	84.1
As—O8—O7	146.7 (3)	As—H2o12—As^vii	81.24
As—O8—O9	34.01 (16)	As—H2o12—P	0
As—O8—O11	41.73 (18)	As—H2o12—P^vii	81.24
As—O8—O13	34.15 (17)	As—H2o12—O4^viii	89.9
As—O8—O13ⁱⁱ	99.1 (2)	As—H2o12—O9	28.09
As—O8—H2o10ⁱⁱ	101.7	As—H2o12—O10^viii	148.75
P—O8—O2	152.5 (4)	As—H2o12—O11	28.62
P—O8—O3	107.9 (2)	As—H2o12—O12	114.13
P—O8—O4	116.0 (3)	As—H2o12—O12^xviii	119.99
P—O8—O6	96.2 (3)	As—H2o12—O13^vii	77.42
P—O8—O7	146.7 (3)	As—H2o12—H2o10^viii	141.83
P—O8—O9	34.01 (16)	As—H2o12—H1o12	140.43
P—O8—O11	41.73 (18)	As—H2o12—H1o12^xviii	103.27
P—O8—O13	34.15 (17)	As—H2o12—H2o12^xviii	126.21
P—O8—O13ⁱⁱ	99.1 (2)	As^vii—H2o12—P	81.24
P—O8—H2o10ⁱⁱ	101.7	As^vii—H2o12—P^vii	0
O2—O8—O3	60.87 (17)	As^vii—H2o12—O4^viii	97.14
O2—O8—O4	65.07 (18)	As^vii—H2o12—O9	103.87
O2—O8—O6	56.7 (2)	As^vii—H2o12—O10^viii	83.54
O2—O8—O7	60.6 (2)	As^vii—H2o12—O11	80.31
O2—O8—O9	135.2 (3)	As^vii—H2o12—O12	103
O2—O8—O11	113.5 (3)	As^vii—H2o12—O12^xviii	149.31
O2—O8—O13	162.0 (3)	As^vii—H2o12—O13^vii	19.66
O2—O8—O13ⁱⁱ	104.3 (2)	As^vii—H2o12—H2o10^viii	75.96
O2—O8—H2o10ⁱⁱ	90.06	As^vii—H2o12—H1o12	91.56
O3—O8—O4	125.3 (2)	As^vii—H2o12—H1o12^xviii	155.53
O3—O8—O6	69.19 (19)	As^vii—H2o12—H2o12^xviii	152.03
O3—O8—O7	86.5 (2)	P—H2o12—P^vii	81.24
O3—O8—O9	133.7 (3)	P—H2o12—O4^viii	89.9
O3—O8—O11	71.4 (2)	P—H2o12—O9	28.09
O3—O8—O13	102.52 (18)	P—H2o12—O10^viii	148.75
O3—O8—O13ⁱⁱ	140.3 (3)	P—H2o12—O11	28.62
O3—O8—H2o10ⁱⁱ	51.18	P—H2o12—O12	114.13
O4—O8—O6	75.02 (19)	P—H2o12—O12^xviii	119.99
O4—O8—O7	74.41 (18)	P—H2o12—O13^vii	77.42
O4—O8—O9	82.0 (2)	P—H2o12—H2o10^viii	141.83
O4—O8—O11	126.5 (3)	P—H2o12—H1o12	140.43
O4—O8—O13	132.2 (2)	P—H2o12—H1o12^xviii	103.27
O4—O8—O13ⁱⁱ	61.79 (16)	P—H2o12—H2o12^xviii	126.21
O4—O8—H2o10ⁱⁱ	137.93	P^vii—H2o12—O4^viii	97.14
O6—O8—O7	117.0 (2)	P^vii—H2o12—O9	103.87
O6—O8—O9	86.9 (2)	P^vii—H2o12—O10^viii	83.54
O6—O8—O11	64.9 (2)	P^vii—H2o12—O11	80.31
O6—O8—O13	126.8 (3)	P^vii—H2o12—O12	103
O6—O8—O13ⁱⁱ	136.6 (2)	P^vii—H2o12—O12^xviii	149.31
O6—O8—H2o10ⁱⁱ	120.36	P^vii—H2o12—O13^vii	19.66
O7—O8—O9	139.6 (2)	P^vii—H2o12—H2o10^viii	75.96
O7—O8—O11	155.7 (3)	P^vii—H2o12—H1o12	91.56
O7—O8—O13	114.6 (3)	P^vii—H2o12—H1o12^xviii	155.53
O7—O8—O13ⁱⁱ	56.19 (17)	P^vii—H2o12—H2o12^xviii	152.03
O7—O8—H2o10ⁱⁱ	63.69	O4^viii—H2o12—O9	103.23
O9—O8—O11	62.6 (2)	O4^viii—H2o12—O10^viii	119.06
O9—O8—O13	60.79 (19)	O4^viii—H2o12—O11	61.91
O9—O8—O13ⁱⁱ	83.8 (2)	O4^viii—H2o12—O12	150.51
O9—O8—H2o10ⁱⁱ	133.61	O4^viii—H2o12—O12^xviii	63.62
O11—O8—O13	62.9 (2)	O4^viii—H2o12—O13^vii	77.89
O11—O8—O13ⁱⁱ	140.9 (3)	O4^viii—H2o12—H2o10^viii	122.76
O11—O8—H2o10ⁱⁱ	93.86	O4^viii—H2o12—H1o12	129.66
O13—O8—O13ⁱⁱ	83.93 (19)	O4^viii—H2o12—H1o12^xviii	59.21
O13—O8—H2o10ⁱⁱ	73.01	O4^viii—H2o12—H2o12^xviii	79.52
O13ⁱⁱ—O8—H2o10ⁱⁱ	95.76	O9—H2o12—O10^viii	135.97
Pb—O9—Pb^iv	105.1 (2)	O9—H2o12—O11	51.15
Pb—O9—As	136.3 (3)	O9—H2o12—O12	92.68
Pb—O9—P	136.3 (3)	O9—H2o12—O12^xviii	103.8
Pb—O9—O7ⁱⁱ	50.94 (14)	O9—H2o12—O13^vii	104.34
Pb—O9—O8	165.0 (3)	O9—H2o12—H2o10^viii	133.85
Pb—O9—O9^iv	55.71 (15)	O9—H2o12—H1o12	122.53
Pb—O9—O10	49.74 (16)	O9—H2o12—H1o12^xviii	88.89
Pb—O9—O11	127.3 (2)	O9—H2o12—H2o12^xviii	103.92
Pb—O9—O12	51.00 (13)	O10^viii—H2o12—O11	163.77
Pb—O9—O13	107.8 (2)	O10^viii—H2o12—O12	44.01
Pb—O9—H2o10	63.08	O10^viii—H2o12—O12^xviii	85.78
Pb—O9—H2o12	65.34	O10^viii—H2o12—O13^vii	96.33
Pb^iv—O9—As	116.0 (3)	O10^viii—H2o12—H2o10^viii	8.32
Pb^iv—O9—P	116.0 (3)	O10^viii—H2o12—H1o12	14.18
Pb^iv—O9—O7ⁱⁱ	153.1 (2)	O10^viii—H2o12—H1o12^xviii	101.88
Pb^iv—O9—O8	88.64 (19)	O10^viii—H2o12—H2o12^xviii	74.32
Pb^iv—O9—O9^iv	49.36 (13)	O11—H2o12—O12	142.5
Pb^iv—O9—O10	99.26 (17)	O11—H2o12—O12^xviii	107.49
Pb^iv—O9—O11	98.6 (2)	O11—H2o12—O13^vii	67.66
Pb^iv—O9—O12	114.1 (2)	O11—H2o12—H2o10^viii	156.19
Pb^iv—O9—O13	147.1 (3)	O11—H2o12—H1o12	167.06
Pb^iv—O9—H2o10	99.03	O11—H2o12—H1o12^xviii	92.27
Pb^iv—O9—H2o12	111.77	O11—H2o12—H2o12^xviii	120.49
As—O9—P	0	O12—H2o12—O12^xviii	88.71
As—O9—O7ⁱⁱ	90.6 (2)	O12—H2o12—O13^vii	122.32
As—O9—O8	34.28 (16)	O12—H2o12—H2o10^viii	44.96
As—O9—O9^iv	160.6 (3)	O12—H2o12—H1o12	30
As—O9—O10	130.8 (3)	O12—H2o12—H1o12^xviii	97.07
As—O9—O11	35.12 (19)	O12—H2o12—H2o12^xviii	72.57
As—O9—O12	96.7 (2)	O12^xviii—H2o12—O13^vii	136.37
As—O9—O13	32.36 (15)	O12^xviii—H2o12—H2o10^viii	94.07
As—O9—H2o10	120.82	O12^xviii—H2o12—H1o12	84.63
As—O9—H2o12	85.41	O12^xviii—H2o12—H1o12^xviii	16.74
P—O9—O7ⁱⁱ	90.6 (2)	O12^xviii—H2o12—H2o12^xviii	16.14
P—O9—O8	34.28 (16)	O13^vii—H2o12—H2o10^viii	89.85
P—O9—O9^iv	160.6 (3)	O13^vii—H2o12—H1o12	106.9
P—O9—O10	130.8 (3)	O13^vii—H2o12—H1o12^xviii	137.02
P—O9—O11	35.12 (19)	O13^vii—H2o12—H2o12^xviii	147.08
P—O9—O12	96.7 (2)	H2o10^viii—H2o12—H1o12	17.61
P—O9—O13	32.36 (15)	H2o10^viii—H2o12—H1o12^xviii	110.19
P—O9—H2o10	120.82	H2o10^viii—H2o12—H2o12^xviii	82.58
P—O9—H2o12	85.41	H1o12—H2o12—H1o12^xviii	99.12
O7ⁱⁱ—O9—O8	114.3 (3)	H1o12—H2o12—H2o12^xviii	70.72
O7ⁱⁱ—O9—O9^iv	105.5 (2)	H1o12^xviii—H2o12—H2o12^xviii	28.4

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H1O5···O10	0.82 (2)	2.96 (6)	3.78 (1)	136 (4)
O5—H2o5···O3	0.820 (16)	2.23 (6)	2.838 (9)	131 (7)
O10—H1o10···O6^vi	0.82	2.55	2.973 (10)	113.40
O10—H2o10···O12ⁱ	0.82	2.21	2.876 (9)	137.89
O12—H1o12···O10^viii	0.82	2.06	2.876 (9)	172.21
O12—H2o12···O13^vii	0.82	2.22	2.746 (8)	122.32

Symmetry codes: (i) x−1, y, z; (vi) −x+1, y−1/2, −z; (vii) −x+2, −y+1, −z+1; (viii) x+1, y, z.

Acknowledgements

We thank two anonymous reviewers as well as the co-editor Radovan Černý for comments which helped in improving the manuscript.

Funding information

The following funding is acknowledged: Czech Science Foundation (GACR 20-11949S) (grant No. 20-11949S to Institute of Physics ASCR, v.v.i.); Ministry of Culture of the Czech Republic (long-term project DKRVO 2019-2023/1.II.c; National Museum, 00023272) for PŠ.

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