Dilead(II) oxyhydroxide bromide

Kunisawa, H.; Yamaura, J.; Nomura, T.

doi:10.1107/S241431462600790X

inorganic compounds

IUCrDATA

ISSN: 2414-3146

Volume 11| Part 8| August 2026| x260790

https://doi.org/10.1107/S241431462600790X

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Dilead(II) oxyhydroxide bromide

Hibiki Kunisawa,^a Jun-ichi Yamaura ^b and Toshihiro Nomura ^a ^*

^aDepartment of Physics, Shizuoka University, Shizuoka 422-8529, Japan, and ^bInstitute for Solid State Physics, The University of Tokyo, Kashiwa, Chiba, 277-8581, Japan
^*Correspondence e-mail: [email protected]

Edited by M. Weil, Vienna University of Technology, Austria (Received 17 July 2026; accepted 1 August 2026; online 7 August 2026)

The crystal structure of the title compound, Pb₂O(OH)Br, has been determined by single-crystal X-ray diffraction. The compound crystallizes in the tetragonal space group P4₂/mcm. The structure consists of [PbO₄Br₄] square antiprisms, which form square layers in the ab plane and are stacked alternately along the c-axis direction. The hydroxide site is assigned on the basis of bond-valence-sum calculations.

Keywords: crystal structure; Pb(II); oxyhydroxide; bromide; square antiprismatic coordination.

CCDC reference: 2578647

Structure description

Lead oxyhalides comprise a diverse family of compounds with a variety of crystal structures. Among them, Pb₂O(OH)Cl (Turner et al., 2015 ), Pb₂O(OH)I (Siidra et al., 2013 ), and Pb₃O₂(OH)Br (Krivovichev & Burns, 2001 ) are oxide–hydroxide halides related to the title compound. In this work, we report the crystal structure of Pb₂O(OH)Br determined by single-crystal X-ray diffraction.

The title compound crystallizes in the tetragonal space group P4₂/mcm. We note that the crystal structure of Pb₂O(OH)Br is different from the ones of Pb₂O(OH)Cl (space group Pnma) and Pb₂O(OH)I (space group C2/m). The asymmetric unit contains one Pb site, three O sites (O1, O2 and O3), and one Br site. The divalent Pb cation is coordinated in a square-antiprismatic mode by four O and four Br atoms (Fig. 1 and Table 1). The O₄ and Br₄ squares are parallel, rotated by 45° relative to each other, with the Br₄ square having an edge length approximately √2 times that of the O₄ square. The face-sharing square antiprisms form square layers in the ab plane (Fig. 2). These layers with opposite orientations are alternately stacked along the c axis. Consequently, a Br square layer and an O square layer are formed alternately along the c axis with 45° relative rotation. The Br atom is surrounded by eight Pb cations in a distorted cubic arrangement, while each of the O atoms is surrounded by four Pb cations in a distorted tetrahedral mode (Fig. 3).

Table 1
Selected bond lengths (Å)

Pb—Brⁱ	3.3741 (15)	Pb—O1	2.3101 (6)
Pb—Br	3.3741 (15)	Pb—O2^iv	2.4291 (3)
Pb—Brⁱⁱ	3.6154 (15)	Pb—O2	2.4291 (3)
Pb—Brⁱⁱⁱ	3.6154 (15)	Pb—O3H	2.5426 (6)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) $[y, -x, -z+{\script{1\over 2}}]$ .

Figure 1
(a) Coordination environment of the Pb atom. Displacement ellipsoids are drawn at the 50% probability level; (b) the [PbBr₄O₄] coordination polyhedron viewed along the c axis. [Symmetry codes: (i) x, y − 1, z; (ii) −x + 1, −y + 1, −z; (iii) −x, −y + 1, −z; (iv) y, −x, −z + $[{1\over 2}]$ .]

Figure 2
The crystal structure of Pb₂O(OH)Br with polyhedral representation. (a) Perspective view, projections along (b) the a and (c) the c axes.

Figure 3
Coordination environments of the (a) Br and (b) O atoms. Ellipsoids are drawn at the 50% probability level. [Symmetry codes: (ii) −x + 1, −y + 1, −z; (iii) −x, −y + 1, −z; (iv) y, −x, −z + $[{1\over 2}]$ ; (v) −x + 1, −y + 1, z; (vi) y, −x + 1, z − $[{1\over 2}]$ ; (vii) x, y + 1, −z; (viii) x, y + 1, z; (ix) −x, −y + 1, z; (x) x, y, −z; (xi) y, −x + 1, −z + $[{1\over 2}]$ ; (xv) −y, x, −z + $[{1\over 2}]$ ; (xvi) −y + 1, x, −z + $[{1\over 2}]$ ; (xvii) −x + 1, −y, z; (xix) −x, −y, z.]

Charge neutrality requires the presence of one H atom per formula unit, although the H atom could not be located from difference Fourier maps owing to the presence of the heavy Pb atom. Bond-valence-sum (BVS) calculations (Brown, 2002 ; Brese & O'Keeffe, 1991 ) were therefore carried out to identify the hydroxide site (Table 2). Consistent with the longest Pb—O3 bond length, O3 exhibits the lowest BVS value, supporting its assignment as the hydroxide site. We note that the O2 site cannot be assigned as the hydroxide site because its multiplicity is twice that of the O1 and O3 sites. The off-centered coordination around the Pb²⁺ cation reflects the stereochemical activity of its 6s² electron lone pair.

Table 2
Atomic sites (multiplicity and Wyckoff letter), site symmetries, and bond-valence sums (in valence units)

Pb (8 o)	m	2.16
Br (4 j)	mm2	0.84
O1 (2 d)	$[\overline{4}]$ 2m	2.34
O2 (4 e)	222	1.70
O3H (2 b)	$[\overline{4}]$ 2m	1.25

Synthesis and crystallization

Single crystals of Pb₂O(OH)Br were obtained serendipitously during attempts to synthesize the Br analogues of diaboleite, Pb₂CuCl₂(OH)₄, and cumengeite, Pb₂₁Cu₂₀Cl₄₂(OH)₄₀·6H₂O, (Alun Humphreys et al., 1980 ) under hydrothermal conditions. Pb wire (0.6 g, Nilaco), CuBr₂ (0.2 g, FUJIFILM Wako), and 5 wt% aqueous ammonia (8 ml) were placed in a polymer-lined stainless-steel autoclave and heated at 533 K for 24 h. Yellow, plate-like crystals grew on the surface of the Pb wire, and a suitable crystal was selected for the single-crystal X-ray diffraction measurements.

Refinement

Details of data collection and structure refinement are given in Table 3. The largest residual electron-density peaks are located within 0.9 Å of the Pb atom and are attributed to Fourier termination errors associated with the heavy Pb atom.

Table 3
Experimental details

Crystal data
Chemical formula	Pb₂O(OH)Br
M_r	526.29
Crystal system, space group	Tetragonal, P4₂/mcm
Temperature (K)	296
a, c (Å)	5.8161 (3), 12.8870 (13)
V (Å³)	435.93 (6)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	86.13
Crystal size (mm)	0.10 × 0.08 × 0.01

Data collection
Diffractometer	XtaLAB AFC11 (RCD3): quarter-chi single
Absorption correction	Multi-scan (CrysAlis PRO; Rigaku OD, 2023 )
T_min, T_max	0.542, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	9139, 705, 460
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.882

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.131, 1.12
No. of reflections	705
No. of parameters	18
H-atom treatment	H-atom parameters not defined
Δρ_max, Δρ_min (e Å⁻³)	6.55, −4.22
Computer programs: CrysAlis PRO (Rigaku OD, 2023), SHELXT (Sheldrick, 2015a ), SHELXL (Sheldrick, 2015b ), VESTA (Momma & Izumi, 2011 ), OLEX2 (Dolomanov et al., 2009 ) and publCIF (Westrip, 2010 ).

Structural data

CCDC reference: 2578647

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S241431462600790X/wm4254sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S241431462600790X/wm4254Isup2.hkl

checkCIF report

Computing details top

Dilead(II) oxyhydroxide bromide top

Crystal data top

Pb₂O(OH)Br	D_x = 8.019 Mg m⁻³
M_r = 526.29	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4₂/mcm	Cell parameters from 2463 reflections
a = 5.8161 (3) Å	θ = 3.1–34.3°
c = 12.8870 (13) Å	µ = 86.13 mm⁻¹
V = 435.93 (6) Å³	T = 296 K
Z = 4	Plate, yellow
F(000) = 860	0.10 × 0.08 × 0.01 mm

Data collection top

XtaLAB AFC11 (RCD3): quarter-chi single diffractometer	705 independent reflections
Radiation source: Rotating-anode X-ray tube, Rigaku (Mo) X-ray Source	460 reflections with I > 2σ(I)
Mirror monochromator	R_int = 0.062
Detector resolution: 10.0000 pixels mm^-1	θ_max = 38.8°, θ_min = 3.2°
ω scans	h = −8→10
Absorption correction: multi-scan (CrysAlisPro; Rigaku OD, 2023)	k = −10→10
T_min = 0.542, T_max = 1.000	l = −22→18
9139 measured reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: dual
R[F² > 2σ(F²)] = 0.044	H-atom parameters not defined
wR(F²) = 0.131	w = 1/[σ²(F_o²) + (0.0369P)² + 26.4764P] where P = (F_o² + 2F_c²)/3
S = 1.12	(Δ/σ)_max < 0.001
705 reflections	Δρ_max = 6.55 e Å⁻³
18 parameters	Δρ_min = −4.22 e Å⁻³

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Pb	0.26668 (8)	0.26668 (8)	0.15022 (4)	0.01991 (19)
Br	0.2582 (3)	0.7418 (3)	0.000000	0.0233 (4)
O1	0.500000	0.500000	0.250000	0.018 (7)
O2	0.000000	0.500000	0.250000	0.023 (8)
O3H	0.000000	0.000000	0.250000	0.020 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb	0.0215 (2)	0.0215 (2)	0.0168 (3)	−0.0095 (3)	−0.00071 (12)	−0.00071 (12)
Br	0.0204 (6)	0.0204 (6)	0.0290 (11)	0.0022 (15)	0.000	0.000
O1	0.020 (10)	0.020 (10)	0.015 (16)	0.000	0.000	0.000
O2	0.016 (10)	0.024 (12)	0.03 (2)	0.000	0.000	0.000
O3H	0.022 (11)	0.022 (11)	0.017 (17)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Pb—Brⁱ	3.3741 (15)	Pb—O1	2.3101 (6)
Pb—Br	3.3741 (15)	Pb—O2^iv	2.4291 (3)
Pb—Brⁱⁱ	3.6154 (15)	Pb—O2	2.4291 (3)
Pb—Brⁱⁱⁱ	3.6154 (15)	Pb—O3H	2.5426 (6)

Br—Pb—Brⁱ	72.22 (6)	Pb—O1—Pb^ix	58.337 (6)
Brⁱⁱⁱ—Pb—Brⁱⁱ	71.96 (6)	Pb^xiv—O1—Pb^xvii	94.056 (3)
Br—Pb—Brⁱⁱⁱ	72.039 (8)	Pb^xv—O1—Pb^viii	94.056 (4)
Brⁱ—Pb—Brⁱⁱ	72.039 (8)	Pb—O2—Pb^xi	100.64 (3)
Br—Pb—Brⁱⁱ	112.590 (16)	Pb^xviii—O2—Pb^xix	51.065 (2)
Brⁱ—Pb—Brⁱⁱⁱ	112.590 (16)	Pb^xviii—O2—Pb^xx	92.740 (7)
O1—Pb—Br	81.191 (16)	Pb^viii—O2—Pb^iv	143.039 (7)
O1—Pb—Brⁱ	81.191 (16)	Pb^xvi—O2—Pb^viii	92.740 (7)
O1—Pb—Brⁱⁱ	143.33 (3)	Pb^ix—O2—Pb^xx	55.085 (16)
O1—Pb—Brⁱⁱⁱ	143.33 (3)	Pb^xv—O2—Pb^iv	63.525 (18)
O1—Pb—O2	75.655 (14)	Pb—O2—Pb^xv	112.08 (3)
O1—Pb—O2^iv	75.655 (14)	Pb^xi—O2—Pb^viii	55.085 (16)
O1—Pb—O3H	115.80 (2)	Pb^xviii—O2—Pb^viii	118.901 (6)
O2—Pb—Brⁱⁱⁱ	75.63 (3)	Pb—O2—Pb^xx	148.277 (12)
O2^iv—Pb—Brⁱⁱ	75.63 (3)	Pb^xi—O2—Pb^xv	116.07 (2)
O2^iv—Pb—Br	146.59 (3)	Pb^xix—O2—Pb^xx	143.039 (7)
O2—Pb—Brⁱ	146.59 (3)	Pb^xi—O2—Pb^iv	99.647 (17)
O2—Pb—Brⁱⁱ	138.29 (3)	Pb^v—O2—Pb^iv	92.740 (7)
O2^iv—Pb—Brⁱⁱⁱ	138.29 (3)	Pb—O2—Pb^ix	116.07 (2)
O2—Pb—Br	80.62 (3)	Pb^xxi—O2—Pb^xix	92.740 (7)
O2^iv—Pb—Brⁱ	80.62 (3)	Pb—O2—Pb^viii	99.647 (17)
O2^iv—Pb—O2	115.67 (2)	Pb^ix—O2—Pb^viii	63.525 (19)
O2—Pb—O3H	71.552 (14)	Pb^xi—O2—Pb^ix	112.08 (3)
O2^iv—Pb—O3H	71.552 (14)	Pb^xxi—O2—Pb^viii	95.585 (7)
O3H—Pb—Brⁱⁱ	75.368 (15)	Pb^xix—O2—Pb^viii	149.527 (14)
O3H—Pb—Brⁱⁱⁱ	75.368 (15)	Pb^xv—O2—Pb^xx	99.647 (17)
O3H—Pb—Br	141.34 (3)	Pb^xv—O2—Pb^ix	100.64 (3)
O3H—Pb—Brⁱ	141.34 (3)	Pb^v—O2—Pb^xx	95.585 (8)
Pb^v—Br—Pb^vi	124.37 (4)	Pb^xxi—O2—Pb^xx	51.065 (2)
Pbⁱ—Br—Pb^vii	72.180 (8)	Pb—O2—Pb^iv	55.085 (16)
Pb^viii—Br—Pb^ix	74.70 (4)	Pb—O2—Pb^xviii	106.011 (17)
Pb—Br—Pb^vi	124.37 (4)	Pb^xviii—O2—Pb^iv	95.585 (7)
Pb^x—Br—Pb^ix	107.961 (8)	Pb^xvi—O2—Pb^iv	51.065 (2)
Pbⁱⁱⁱ—Br—Pb^vi	58.241 (14)	Pb^xix—O2—Pb^iv	48.630 (9)
Pb^x—Br—Pb^vii	112.591 (17)	Pb^xi—O2—Pb^xviii	153.350 (11)
Pb^ix—Br—Pb^vi	122.98 (3)	Pb^xi—O2—Pb^v	53.030 (17)
Pb—Br—Pb^viii	112.590 (16)	Pb^v—O2—Pb^xix	118.901 (6)
Pb^v—Br—Pb^xi	54.357 (14)	Pb^xv—O2—Pb^v	153.350 (11)
Pbⁱ—Br—Pb^ix	176.910 (14)	Pb^xv—O2—Pb^xviii	53.030 (17)
Pb—Br—Pb^xi	54.357 (14)	Pb^ix—O2—Pb^v	106.011 (17)
Pb^viii—Br—Pbⁱⁱⁱ	108.04 (6)	Pb^xv—O2—Pb^viii	148.277 (12)
Pb^x—Br—Pb^viii	176.910 (15)	Pb^xviii—O2—Pb^v	147.940 (14)
Pb—Br—Pb^vii	176.910 (15)	Pb^ix—O2—Pb^xviii	55.377 (19)
Pb^v—Br—Pb^viii	72.179 (8)	Pb^xvi—O2—Pb^v	47.339 (10)
Pbⁱ—Br—Pb^viii	107.961 (8)	Pb^v—O2—Pb^viii	51.065 (2)
Pbⁱⁱⁱ—Br—Pb^vii	74.70 (4)	Pb—O2—Pb^xxi	153.350 (11)
Pb^ix—Br—Pb^xi	58.241 (14)	Pb—O2—Pb^xvi	53.029 (17)
Pb^x—Br—Pb^xi	124.37 (4)	Pb^xi—O2—Pb^xxi	106.011 (17)
Pb^vii—Br—Pb^ix	108.04 (6)	Pb^xi—O2—Pb^xx	63.525 (19)
Pb^v—Br—Pbⁱⁱⁱ	176.910 (15)	Pb^xv—O2—Pb^xxi	55.377 (19)
Pb^x—Br—Pb^vi	54.357 (14)	Pb^xi—O2—Pb^xvi	55.377 (19)
Pbⁱ—Br—Pb^xi	124.37 (4)	Pb^ix—O2—Pb^xxi	53.030 (17)
Pbⁱ—Br—Pb^vi	54.357 (14)	Pb^xvi—O2—Pb^xx	118.901 (6)
Pb—Br—Pbⁱⁱⁱ	107.961 (8)	Pb^xviii—O2—Pb^xxi	47.339 (9)
Pb^viii—Br—Pb^vi	122.98 (3)	Pb^xv—O2—Pb^xvi	106.011 (17)
Pbⁱⁱⁱ—Br—Pb^xi	122.98 (3)	Pb^xvi—O2—Pb^xxi	147.940 (14)
Pb^x—Br—Pb^v	107.78 (6)	Pb^viii—O2—Pb^xx	48.630 (8)
Pb^v—Br—Pb^ix	112.591 (17)	Pb^v—O2—Pb^xxi	146.116 (7)
Pb^x—Br—Pbⁱ	69.33 (4)	Pb^ix—O2—Pb^xvi	153.350 (11)
Pb^v—Br—Pb^vii	107.961 (8)	Pb—O2—Pb^xix	63.525 (19)
Pb^v—Br—Pbⁱ	70.02 (4)	Pb^ix—O2—Pb^iv	148.277 (12)
Pbⁱ—Br—Pbⁱⁱⁱ	112.591 (17)	Pb^xi—O2—Pb^xix	148.277 (12)
Pb^x—Br—Pb	70.02 (4)	Pb^xviii—O2—Pb^xvi	146.116 (7)
Pb—Br—Pb^ix	72.179 (8)	Pb^xv—O2—Pb^xix	55.085 (16)
Pb^v—Br—Pb	69.33 (4)	Pb^xxi—O2—Pb^iv	118.901 (6)
Pb^x—Br—Pbⁱⁱⁱ	72.180 (8)	Pb^ix—O2—Pb^xix	99.647 (17)
Pbⁱ—Br—Pb	107.78 (6)	Pb—O2—Pb^v	55.377 (19)
Pb^viii—Br—Pb^vii	64.75 (3)	Pb^xvi—O2—Pb^xix	95.585 (7)
Pb^vi—Br—Pb^xi	178.24 (6)	Pb^xx—O2—Pb^iv	149.527 (14)
Pbⁱⁱⁱ—Br—Pb^ix	64.75 (3)	Pb—O3H—Pb^xix	119.24 (3)
Pb^viii—Br—Pb^xi	58.241 (14)	Pb^ix—O3H—Pb^xvii	121.353 (13)
Pb^vii—Br—Pb^vi	58.241 (14)	Pb^xvi—O3H—Pb^ix	94.262 (4)
Pb^vii—Br—Pb^xi	122.98 (3)	Pb^xviii—O3H—Pb^xvii	148.360 (14)
Pb—O1—Pb^v	112.35 (3)	Pb^xi—O3H—Pb^xviii	94.262 (4)
Pb^iv—O1—Pb^viii	147.401 (13)	Pb^iv—O3H—Pb^ix	152.875 (9)
Pb^xii—O1—Pb^xiii	94.056 (4)	Pb^xv—O3H—Pb^xvii	152.875 (9)
Pb^xiii—O1—Pb^viii	116.547 (13)	Pb—O3H—Pb^xv	104.820 (12)
Pb^xiv—O1—Pb^xv	149.152 (13)	Pb^xix—O3H—Pb^xviii	60.734 (7)
Pb^xi—O1—Pb^xiii	148.721 (10)	Pb^xvi—O3H—Pb^xviii	141.606 (14)
Pb^xvi—O1—Pb^viii	148.721 (10)	Pb—O3H—Pb^ix	60.734 (7)
Pb—O1—Pb^xvi	108.051 (15)	Pb^xix—O3H—Pb^xv	104.820 (12)
Pb^v—O1—Pb^xv	148.721 (10)	Pbⁱⁱ—O3H—Pb^ix	148.360 (14)
Pb^xii—O1—Pb^xv	116.547 (13)	Pb^xix—O3H—Pb^xvii	102.305 (10)
Pb—O1—Pb^xiii	103.228 (10)	Pb^xxii—O3H—Pb^xvii	94.262 (4)
Pb^v—O1—Pb^xvi	108.051 (15)	Pb—O3H—Pb^iv	104.820 (12)
Pb^xvii—O1—Pb^xiii	53.957 (13)	Pb^xxiii—O3H—Pbⁱⁱ	94.262 (4)
Pb^v—O1—Pb^viii	58.337 (6)	Pb—O3H—Pb^xviii	102.305 (10)
Pb^ix—O1—Pb^viii	53.957 (13)	Pb^iv—O3H—Pb^xviii	152.875 (9)
Pb—O1—Pb^xi	108.051 (15)	Pb^xix—O3H—Pb^iv	104.820 (12)
Pb^iv—O1—Pb^xvii	45.493 (14)	Pb^xxiii—O3H—Pb^xviii	50.571 (15)
Pb—O1—Pb^xv	56.043 (19)	Pbⁱⁱ—O3H—Pb^xviii	121.353 (13)
Pb^xi—O1—Pb^xv	58.337 (6)	Pb^xv—O3H—Pb^ix	52.101 (18)
Pb^v—O1—Pb^xi	108.051 (15)	Pb^xv—O3H—Pb^iv	119.24 (3)
Pb^iv—O1—Pb^xv	53.957 (13)	Pb^xxii—O3H—Pb^ix	141.606 (14)
Pb^xvii—O1—Pb^xv	94.056 (4)	Pb^xxiii—O3H—Pb^ix	94.262 (4)
Pb^xvi—O1—Pb^xiii	56.044 (19)	Pb—O3H—Pb^xvii	60.734 (7)
Pb^xvi—O1—Pb^xi	112.35 (3)	Pb—O3H—Pb^xvi	52.101 (18)
Pb^ix—O1—Pb^xiii	149.152 (13)	Pb^xvi—O3H—Pb^xvii	50.571 (15)
Pb^iv—O1—Pb^xiii	94.056 (4)	Pb^xi—O3H—Pb^xvii	94.262 (4)
Pb—O1—Pb^viii	103.228 (10)	Pbⁱⁱ—O3H—Pb^xvii	48.014 (14)
Pb—O1—Pb^xii	148.721 (10)	Pb^xix—O3H—Pb^xvi	152.875 (9)
Pb^xii—O1—Pb^viii	45.493 (14)	Pb^xix—O3H—Pb^xxii	52.101 (18)
Pb^xiv—O1—Pb^viii	94.056 (4)	Pb^xxii—O3H—Pbⁱⁱ	50.571 (15)
Pb^xi—O1—Pb^xvii	148.721 (10)	Pb^xv—O3H—Pb^xxii	102.305 (10)
Pb^v—O1—Pb^xii	56.044 (19)	Pb^xv—O3H—Pb^xvi	102.305 (10)
Pb^v—O1—Pb^ix	103.228 (10)	Pb^iv—O3H—Pb^xxii	60.734 (7)
Pb^ix—O1—Pb^xvii	116.547 (13)	Pb^xv—O3H—Pb^xviii	52.101 (18)
Pb^xvi—O1—Pb^ix	148.721 (10)	Pb^xvi—O3H—Pb^xxii	121.353 (13)
Pb^xvi—O1—Pb^xii	103.228 (10)	Pb^iv—O3H—Pb^xvi	60.734 (7)
Pb^xi—O1—Pb^ix	56.044 (19)	Pb^xi—O3H—Pb^xxii	148.360 (14)
Pb^xvi—O1—Pb^xv	103.228 (10)	Pb^xxii—O3H—Pb^xviii	94.262 (4)
Pb^xii—O1—Pb^ix	94.056 (3)	Pb—O3H—Pb^xxiii	152.876 (9)
Pb^xi—O1—Pb^xii	58.337 (6)	Pb—O3H—Pb^xi	52.101 (18)
Pb^xiv—O1—Pb^ix	147.401 (13)	Pb^xix—O3H—Pb^xxiii	52.101 (18)
Pb^ix—O1—Pb^xv	45.493 (14)	Pb^xix—O3H—Pb^ix	102.305 (10)
Pb—O1—Pb^iv	56.043 (19)	Pb^xv—O3H—Pb^xxiii	60.734 (7)
Pb—O1—Pb^xiv	148.721 (10)	Pb^xix—O3H—Pb^xi	152.875 (9)
Pb^v—O1—Pb^iv	148.721 (10)	Pb^iv—O3H—Pb^xxiii	102.305 (10)
Pb^v—O1—Pb^xiii	58.337 (6)	Pb^xi—O3H—Pb^ix	50.571 (15)
Pb^xvi—O1—Pb^iv	58.337 (6)	Pb^xvi—O3H—Pb^xxiii	148.360 (14)
Pb^v—O1—Pb^xiv	56.044 (19)	Pb^xv—O3H—Pb^xi	60.734 (7)
Pb^xi—O1—Pb^iv	103.228 (10)	Pb^xi—O3H—Pb^xxiii	121.353 (13)
Pb^xiv—O1—Pb^xiii	45.493 (14)	Pb^xviii—O3H—Pb^ix	48.014 (14)
Pb^xii—O1—Pb^iv	149.152 (13)	Pb^xxii—O3H—Pb^xxiii	48.014 (14)
Pb^xvi—O1—Pb^xiv	58.337 (6)	Pb^iv—O3H—Pb^xi	102.305 (10)
Pb^xiv—O1—Pb^iv	116.547 (13)	Pb—O3H—Pbⁱⁱ	102.305 (10)
Pb^xv—O1—Pb^xiii	147.401 (13)	Pb^iv—O3H—Pb^xvii	52.101 (18)
Pb^ix—O1—Pb^iv	94.056 (4)	Pb^xix—O3H—Pbⁱⁱ	60.734 (7)
Pb^xi—O1—Pb^xiv	103.228 (10)	Pb^xvi—O3H—Pb^xi	48.014 (14)
Pb—O1—Pb^xvii	58.337 (6)	Pb^xv—O3H—Pbⁱⁱ	152.875 (9)
Pb^xi—O1—Pb^viii	56.044 (19)	Pb^xxiii—O3H—Pb^xvii	141.606 (14)
Pb^v—O1—Pb^xvii	103.228 (10)	Pb^iv—O3H—Pbⁱⁱ	52.101 (18)
Pb^xii—O1—Pb^xiv	53.957 (13)	Pb—O3H—Pb^xxii	152.876 (9)
Pb^xvi—O1—Pb^xvii	56.044 (19)	Pb^xvi—O3H—Pbⁱⁱ	94.262 (4)
Pb^xvii—O1—Pb^viii	149.152 (13)	Pb^xi—O3H—Pbⁱⁱ	141.606 (14)
Pb^xii—O1—Pb^xvii	147.401 (13)

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

Atomic sites (multiplicity and Wyckoff letter), site symmetries, and bond-valence sums (in valence units) top

Pb (8 o)	m	2.16
Br (4 j)	mm2	0.84
O1 (2 d)	42m	2.34
O2 (4 e)	222	1.70
O3H (2 b)	42m	1.25

Acknowledgements

The XRD experiments were performed as joint research at the Institute for Solid State Physics, University of Tokyo and at the Molecular Structure Analysis Section, Shizuoka Instrumental Analysis Center, Shizuoka University.

Funding information

Funding for this research was provided by: Japan Society for the Promotion of Science.

References

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inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Dilead(II) oxyhydroxide bromide

Structure description

Synthesis and crystallization

Refinement

Structural data

Acknowledgements

Funding information

References

inorganic compounds