catena-Poly[[[aqua­[(2-hydroxy­phen­yl)acetato-κ2O,O′]lead(II)]-μ3-[(2-hydroxy­phen­yl)acetato-κ4O:O,O′:O′]] monohydrate]

Xiao, J.-X.; Wu, X.-G.; Qin, L.

doi:10.1107/S1600536810004162

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 3| March 2010| Pages m273-m274

doi:10.1107/S1600536810004162

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catena-Poly[[[aqua[(2-hydroxyphenyl)acetato-κ²O,O′]lead(II)]-μ₃-[(2-hydroxyphenyl)acetato-κ⁴O:O,O′:O′]] monohydrate]

Jun-Xia Xiao,^a ^* Xian-Ge Wu ^a and Liang Qin ^a

^aSchool of Chemistry and Chemical Engineering, Zhaoqing University, Zhaoqing 526061, People's Republic of China
^*Correspondence e-mail: xiaojx090@126.com

(Received 18 January 2010; accepted 2 February 2010; online 6 February 2010)

In the title complex, {[Pb(C₈H₇O₃)₂(H₂O)]·H₂O}_n, the Pb^II atom is seven-coordinated by six carboxylate O atoms from four different 2-hydroxyphenylacetate (2-dph) ligands and one water molecule, displaying a hemidirected irregular geometry, with the empty side of the metal ion capped by a benzene ring forming a Pb⋯π contact [Pb⋯centroid distance = 3.342 (2) Å]. One 2-dph ligand functions in a bridging mode and connects Pb ions into a linear chain. The crystal packing is governed by intra- and intermolecular O—H⋯O hydrogen bonds.

Related literature

For general background to hydroxyphenylacetate complexes, see: Liwporncharoenvong et al. (2002 ); Nie & Li (2009 ). For general background to hemi- and holodirected geometries of lead(II) complexes, see: Shimoni-Livny et al. (1998 ).

Experimental

Crystal data

[Pb(C₈H₇O₃)₂(H₂O)]·H₂O
M_r = 545.50
Triclinic, $[P \overline 1]$
a = 7.4610 (15) Å
b = 10.721 (2) Å
c = 11.701 (2) Å
α = 109.72 (3)°
β = 90.10 (3)°
γ = 102.92 (3)°
V = 855.7 (3) Å³
Z = 2
Mo Kα radiation
μ = 9.90 mm⁻¹
T = 293 K
0.30 × 0.26 × 0.22 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ) T_min = 0.075, T_max = 0.126
6821 measured reflections
3076 independent reflections
2951 reflections with I > 2σ(I)
R_int = 0.056

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.084
S = 1.05
3076 reflections
228 parameters
6 restraints
H-atom parameters constrained
Δρ_max = 2.77 e Å⁻³
Δρ_min = −1.58 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb1—O1	2.701 (5)
Pb1—O2	2.527 (4)
Pb1—O3	2.453 (3)
Pb1—O3ⁱ	2.662 (4)
Pb1—O4	2.508 (4)
Pb1—O4ⁱⁱ	2.772 (4)
Pb1—O1W	2.687 (4)
Symmetry codes: (i) -x+2, -y, -z+1; (ii) -x+1, -y, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯O2Wⁱⁱⁱ	0.82	1.80	2.618 (6)	173
O6—H6⋯O5ⁱ	0.82	1.93	2.698 (6)	156
O1W—H1W⋯O1ⁱⁱ	0.84	2.31	3.089 (6)	154
O1W—H2W⋯O2ⁱ	0.84	2.16	2.900 (6)	147
O2W—H3W⋯O1^iv	0.84	1.88	2.715 (6)	172
O2W—H4W⋯O6^v	0.84	2.05	2.788 (7)	146
Symmetry codes: (i) -x+2, -y, -z+1; (ii) -x+1, -y, -z+1; (iii) x+1, y, z+1; (iv) -x+1, -y+1, -z+1; (v) x, y+1, z.

Data collection: CrystalStructure (Rigaku/MSC, 2002 ); cell refinement: CrystalStructure; data reduction: CrystalStructure; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976 ) and DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810004162/hy2276sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810004162/hy2276Isup2.hkl

checkCIF report

Comment top

In the structural investigation of hydroxyphenylacetate complexes, it has been found that the hydroxyphenylacelic acid functions as a multidentate ligand (Liwporncharoenvong et al., 2002; Nie & Li, 2009), with versatile binding and coordination modes. However, the structures of 2-hydroxyphenylacetate (2-dph) complexes have not been reported to date. In this paper, we report the crystal structure of the title compound, a new Pb complex obtained by the reaction of 2-Hdph and lead acetate in an alkaline aqueous solution.

As depicted in Fig. 1, the Pb^II atom is coordinated by six O atoms from four 2-dph ligands and one water molecule (Table 1). The coordination environment of the Pb^II atom can be described as a hemidirected irregular geometry, with the empty sapce around the meal ion filled by the stereochemically active 6 s² electron pair (Shimoni-Livny et al., 1998) and a Pb···π contact [Pb1···Cg1ⁱ = 3.342 (2) Å, Cg1 is the centroid of the C11–C16 ring. Symmetry code: (i) 2-x, -y, 1-z]. The 2-dph ligands exhibit two types of coordination modes: one acts as bidentate chelating ligand; the other acts as a tetradentate chelate-bridging ligand to coordinate three Pb^II ions. The carboxylate groups of the tetradentate ligands connect Pb^II ions into a Pb–carboxylate linear chain, with Pb···Pb separations of 4.330 (2) and 4.381 (3) Å (Fig. 2). The crystal packing is governed by intra- and intermolecular O—H···O hydrogen bonding interactions involving the hydroxy and carboxylate groups of the 2-dph ligands, coordinated and uncoordinated water molecules (Table 2).

Related literature top

For general background to hydroxyphenylacetate complexes, see: Liwporncharoenvong et al. (2002); Nie & Li (2009). For general background to hemi- and holodirected geometries of lead(II) complexes, see: Shimoni-Livny et al. (1998).

Experimental top

The title compound was prepared by the addition of a stoichiometric amount of lead acetate (1 mmol, 0.325 g) to a hot aqueous solution (25 ml) of 2-Hdph (1 mmol, 0.152 g). The pH value was then adjusted to 7.0 to 8.0 with NaOH (1 mmol, 0.04 g). The resulting solution was filtered, and colorless single crystals were obtained at room temperature over several days.

Computing details top

Data collection: CrystalStructure (Rigaku/MSC, 2002); cell refinement: CrystalStructure (Rigaku/MSC, 2002); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of the title compound, together with symmetry-related atoms to complete the coordination environment. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) 2-x, -y, 1-z; (ii) 1-x, -y, 1-z.]
	Fig. 2. A polyhedral view of the Pb–carboxylate chain along the a axis. H atoms have been omitted for clarity.

catena-Poly[[[aqua[(2-hydroxyphenyl)acetato- κ²O,O']lead(II)]-µ₃-[(2-hydroxyphenyl)acetato- κ⁴O:O,O':O']] monohydrate] top

Crystal data top

[Pb(C₈H₇O₃)₂(H₂O)]·H₂O	Z = 2
M_r = 545.50	F(000) = 520
Triclinic, P1	D_x = 2.117 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.4610 (15) Å	Cell parameters from 2895 reflections
b = 10.721 (2) Å	θ = 2.4–27.9°
c = 11.701 (2) Å	µ = 9.90 mm⁻¹
α = 109.72 (3)°	T = 293 K
β = 90.10 (3)°	Block, colorless
γ = 102.92 (3)°	0.30 × 0.26 × 0.22 mm
V = 855.7 (3) Å³

Data collection top

Rigaku/MSC Mercury CCD diffractometer	3076 independent reflections
Radiation source: fine-focus sealed tube	2951 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.056
ω scans	θ_max = 25.2°, θ_min = 3.1°
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	h = −8→8
T_min = 0.075, T_max = 0.126	k = −12→12
6821 measured reflections	l = −14→14

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.084	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0431P)²] where P = (F_o² + 2F_c²)/3
3076 reflections	(Δ/σ)_max = 0.003
228 parameters	Δρ_max = 2.77 e Å⁻³
6 restraints	Δρ_min = −1.58 e Å⁻³

Crystal data top

[Pb(C₈H₇O₃)₂(H₂O)]·H₂O	γ = 102.92 (3)°
M_r = 545.50	V = 855.7 (3) Å³
Triclinic, P1	Z = 2
a = 7.4610 (15) Å	Mo Kα radiation
b = 10.721 (2) Å	µ = 9.90 mm⁻¹
c = 11.701 (2) Å	T = 293 K
α = 109.72 (3)°	0.30 × 0.26 × 0.22 mm
β = 90.10 (3)°

Data collection top

Rigaku/MSC Mercury CCD diffractometer	3076 independent reflections
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	2951 reflections with I > 2σ(I)
T_min = 0.075, T_max = 0.126	R_int = 0.056
6821 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	6 restraints
wR(F²) = 0.084	H-atom parameters constrained
S = 1.05	Δρ_max = 2.77 e Å⁻³
3076 reflections	Δρ_min = −1.58 e Å⁻³
228 parameters

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

	x	y	z	U_iso*/U_eq
Pb1	0.76187 (2)	0.029805 (17)	0.601979 (13)	0.02638 (11)
O1	0.6798 (6)	0.2761 (5)	0.6889 (4)	0.0433 (10)
O2	0.9615 (6)	0.2666 (4)	0.6423 (4)	0.0439 (10)
O6	0.7995 (6)	−0.2407 (5)	0.1437 (5)	0.0487 (11)
H6	0.8311	−0.3082	0.1465	0.073*
O5	1.1923 (6)	0.5007 (4)	0.8890 (3)	0.0413 (9)
H5	1.2721	0.5388	0.9460	0.062*
C1	0.8449 (8)	0.3338 (6)	0.6845 (5)	0.0320 (12)
C2	0.9012 (8)	0.4889 (6)	0.7318 (6)	0.0435 (14)
H2A	0.8219	0.5223	0.6892	0.052*
H2B	0.8802	0.5217	0.8175	0.052*
C3	1.0981 (8)	0.5484 (5)	0.7178 (5)	0.0392 (13)
C4	1.1459 (10)	0.6010 (6)	0.6257 (6)	0.0471 (15)
H4	1.0530	0.6059	0.5753	0.056*
C5	1.3273 (10)	0.6461 (7)	0.6070 (6)	0.0512 (17)
H5A	1.3558	0.6801	0.5442	0.061*
C6	1.4641 (10)	0.6410 (7)	0.6797 (6)	0.0531 (17)
H6A	1.5865	0.6687	0.6652	0.064*
C7	1.4221 (9)	0.5938 (6)	0.7770 (6)	0.0443 (14)
H7	1.5162	0.5935	0.8289	0.053*
C8	1.2403 (8)	0.5481 (5)	0.7949 (5)	0.0340 (12)
C9	0.7658 (7)	0.0291 (5)	0.3582 (5)	0.0269 (11)
C10	0.7743 (8)	0.0257 (7)	0.2278 (5)	0.0324 (12)
H10A	0.6655	−0.0388	0.1794	0.039*
H10B	0.7718	0.1151	0.2260	0.039*
C11	0.9411 (7)	−0.0131 (6)	0.1715 (4)	0.0296 (12)
C12	0.9491 (7)	−0.1495 (6)	0.1294 (4)	0.0300 (12)
C13	1.1053 (8)	−0.1886 (7)	0.0786 (5)	0.0407 (14)
H13	1.1097	−0.2799	0.0523	0.049*
C14	1.2530 (9)	−0.0917 (8)	0.0675 (6)	0.0448 (16)
H14	1.3572	−0.1176	0.0332	0.054*
C15	1.2474 (9)	0.0435 (7)	0.1069 (5)	0.0478 (18)
H15	1.3478	0.1088	0.0996	0.057*
C16	1.0910 (9)	0.0828 (6)	0.1580 (5)	0.0390 (14)
H16	1.0871	0.1741	0.1833	0.047*
O3	0.9083 (5)	0.0283 (4)	0.4142 (3)	0.0339 (9)
O4	0.6204 (5)	0.0363 (4)	0.4101 (3)	0.0366 (9)
O1W	0.6888 (6)	−0.2332 (5)	0.4561 (4)	0.0531 (12)
H2W	0.7696	−0.2339	0.4061	0.080*
H1W	0.5860	−0.2720	0.4161	0.080*
O2W	0.4261 (6)	0.6318 (6)	0.0817 (4)	0.0617 (14)
H3W	0.3977	0.6548	0.1537	0.093*
H4W	0.5291	0.6783	0.0746	0.093*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.01845 (15)	0.03419 (16)	0.02621 (15)	0.00640 (11)	0.00500 (9)	0.00999 (11)
O1	0.029 (2)	0.046 (2)	0.049 (2)	0.005 (2)	0.0044 (18)	0.013 (2)
O2	0.031 (2)	0.034 (2)	0.063 (3)	0.0088 (19)	0.017 (2)	0.012 (2)
O6	0.031 (2)	0.041 (2)	0.075 (3)	0.006 (2)	0.004 (2)	0.022 (2)
O5	0.041 (2)	0.042 (2)	0.041 (2)	0.006 (2)	0.0043 (17)	0.0162 (19)
C1	0.026 (3)	0.038 (3)	0.030 (3)	0.006 (3)	0.002 (2)	0.010 (2)
C2	0.029 (3)	0.035 (3)	0.063 (4)	0.008 (3)	0.005 (3)	0.014 (3)
C3	0.034 (3)	0.025 (3)	0.055 (3)	0.005 (3)	0.003 (3)	0.010 (3)
C4	0.061 (4)	0.035 (3)	0.047 (3)	0.013 (3)	0.003 (3)	0.015 (3)
C5	0.055 (4)	0.043 (3)	0.055 (4)	0.002 (3)	0.010 (3)	0.023 (3)
C6	0.043 (4)	0.047 (4)	0.064 (4)	0.002 (3)	0.022 (3)	0.018 (3)
C7	0.031 (3)	0.044 (3)	0.056 (4)	0.005 (3)	0.002 (3)	0.018 (3)
C8	0.029 (3)	0.030 (3)	0.040 (3)	0.006 (2)	0.004 (2)	0.009 (2)
C9	0.022 (3)	0.028 (2)	0.029 (2)	0.006 (2)	0.003 (2)	0.009 (2)
C10	0.027 (3)	0.052 (3)	0.025 (3)	0.018 (3)	0.010 (2)	0.016 (2)
C11	0.029 (3)	0.040 (3)	0.017 (2)	0.014 (3)	0.0021 (19)	0.003 (2)
C12	0.026 (3)	0.036 (3)	0.022 (2)	0.006 (2)	0.0002 (19)	0.003 (2)
C13	0.039 (3)	0.048 (3)	0.039 (3)	0.021 (3)	0.008 (3)	0.013 (3)
C14	0.035 (3)	0.068 (4)	0.038 (3)	0.025 (3)	0.016 (3)	0.018 (3)
C15	0.033 (4)	0.061 (5)	0.048 (4)	0.000 (4)	0.007 (3)	0.024 (4)
C16	0.047 (4)	0.038 (3)	0.026 (2)	0.004 (3)	0.005 (2)	0.008 (2)
O3	0.0205 (19)	0.057 (2)	0.0277 (17)	0.0135 (18)	0.0076 (14)	0.0173 (17)
O4	0.0182 (19)	0.052 (2)	0.044 (2)	0.0106 (18)	0.0099 (16)	0.0217 (19)
O1W	0.046 (3)	0.045 (2)	0.057 (3)	0.000 (2)	0.019 (2)	0.011 (2)
O2W	0.036 (3)	0.092 (4)	0.044 (2)	0.018 (3)	0.007 (2)	0.005 (3)

Geometric parameters (Å, º) top

Pb1—O1	2.701 (5)	C6—H6A	0.9300
Pb1—O2	2.527 (4)	C7—C8	1.377 (8)
Pb1—O3	2.453 (3)	C7—H7	0.9300
Pb1—O3ⁱ	2.662 (4)	C9—O3	1.251 (6)
Pb1—O4	2.508 (4)	C9—O4	1.249 (6)
Pb1—O4ⁱⁱ	2.772 (4)	C9—C10	1.515 (7)
Pb1—O1W	2.687 (4)	C10—C11	1.485 (7)
O1—C1	1.259 (7)	C10—H10A	0.9700
O2—C1	1.249 (7)	C10—H10B	0.9700
O6—C12	1.362 (7)	C11—C12	1.392 (8)
O6—H6	0.8200	C11—C16	1.388 (8)
O5—C8	1.377 (7)	C12—C13	1.393 (8)
O5—H5	0.8200	C13—C14	1.375 (9)
C1—C2	1.521 (8)	C13—H13	0.9300
C2—C3	1.499 (8)	C14—C15	1.375 (9)
C2—H2A	0.9700	C14—H14	0.9300
C2—H2B	0.9700	C15—C16	1.396 (9)
C3—C4	1.389 (9)	C15—H15	0.9300
C3—C8	1.393 (8)	C16—H16	0.9300
C4—C5	1.376 (10)	O1W—H2W	0.8401
C4—H4	0.9300	O1W—H1W	0.8400
C5—C6	1.349 (10)	O2W—H3W	0.8365
C5—H5A	0.9300	O2W—H4W	0.8383
C6—C7	1.403 (9)

O3—Pb1—O4	51.86 (12)	C5—C6—C7	120.2 (6)
O3—Pb1—O2	72.89 (14)	C5—C6—H6A	119.9
O4—Pb1—O2	89.65 (15)	C7—C6—H6A	119.9
O3—Pb1—O3ⁱ	64.41 (14)	C8—C7—C6	119.5 (6)
O4—Pb1—O3ⁱ	115.37 (11)	C8—C7—H7	120.2
O2—Pb1—O3ⁱ	80.89 (13)	C6—C7—H7	120.2
O3—Pb1—O1W	74.25 (14)	O5—C8—C7	121.6 (6)
O4—Pb1—O1W	77.54 (15)	O5—C8—C3	117.7 (5)
O2—Pb1—O1W	145.72 (13)	C7—C8—C3	120.7 (6)
O3ⁱ—Pb1—O1W	76.41 (14)	O3—C9—O4	120.4 (5)
O3—Pb1—O1	104.29 (14)	O3—C9—C10	118.9 (4)
O4—Pb1—O1	80.18 (14)	O4—C9—C10	120.6 (5)
O2—Pb1—O1	49.36 (13)	C11—C10—C9	113.5 (4)
O3ⁱ—Pb1—O1	128.80 (13)	C11—C10—H10A	108.9
O1—Pb1—O4ⁱⁱ	76.94 (13)	C9—C10—H10A	108.9
O2—Pb1—O4ⁱⁱ	125.05 (14)	C11—C10—H10B	108.9
O3—Pb1—O4ⁱⁱ	117.78 (12)	C9—C10—H10B	108.9
O3ⁱ—Pb1—O4ⁱⁱ	154.01 (12)	H10A—C10—H10B	107.7
O4—Pb1—O4ⁱⁱ	67.94 (11)	C12—C11—C16	118.2 (5)
O1W—Pb1—O4ⁱⁱ	79.49 (13)	C12—C11—C10	119.8 (5)
O1W—Pb1—O1	152.25 (15)	C16—C11—C10	122.1 (5)
C1—O1—Pb1	90.2 (4)	O6—C12—C11	116.6 (5)
C1—O2—Pb1	98.8 (3)	O6—C12—C13	122.3 (5)
C12—O6—H6	109.5	C11—C12—C13	121.1 (5)
C8—O5—H5	109.5	C14—C13—C12	119.7 (6)
O2—C1—O1	121.5 (5)	C14—C13—H13	120.1
O2—C1—C2	120.0 (5)	C12—C13—H13	120.1
O1—C1—C2	118.5 (5)	C15—C14—C13	120.3 (6)
C3—C2—C1	114.7 (5)	C15—C14—H14	119.9
C3—C2—H2A	108.6	C13—C14—H14	119.9
C1—C2—H2A	108.6	C14—C15—C16	120.0 (6)
C3—C2—H2B	108.6	C14—C15—H15	120.0
C1—C2—H2B	108.6	C16—C15—H15	120.0
H2A—C2—H2B	107.6	C11—C16—C15	120.7 (6)
C4—C3—C8	117.8 (6)	C11—C16—H16	119.6
C4—C3—C2	121.6 (6)	C15—C16—H16	119.6
C8—C3—C2	120.6 (6)	C9—O3—Pb1	95.1 (3)
C5—C4—C3	121.5 (7)	C9—O3—Pb1ⁱ	146.8 (3)
C5—C4—H4	119.2	Pb1—O3—Pb1ⁱ	115.59 (14)
C3—C4—H4	119.2	C9—O4—Pb1	92.5 (3)
C6—C5—C4	120.1 (6)	H2W—O1W—H1W	107.6
C6—C5—H5A	119.9	H3W—O2W—H4W	112.2
C4—C5—H5A	119.9

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+1, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O2Wⁱⁱⁱ	0.82	1.80	2.618 (6)	173
O6—H6···O5ⁱ	0.82	1.93	2.698 (6)	156
O1W—H1W···O1ⁱⁱ	0.84	2.31	3.089 (6)	154
O1W—H2W···O2ⁱ	0.84	2.16	2.900 (6)	147
O2W—H3W···O1^iv	0.84	1.88	2.715 (6)	172
O2W—H4W···O6^v	0.84	2.05	2.788 (7)	146

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+1, −y, −z+1; (iii) x+1, y, z+1; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z.

Experimental details

Crystal data
Chemical formula	[Pb(C₈H₇O₃)₂(H₂O)]·H₂O
M_r	545.50
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	7.4610 (15), 10.721 (2), 11.701 (2)
α, β, γ (°)	109.72 (3), 90.10 (3), 102.92 (3)
V (Å³)	855.7 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	9.90
Crystal size (mm)	0.30 × 0.26 × 0.22

Data collection
Diffractometer	Rigaku/MSC Mercury CCD diffractometer
Absorption correction	Multi-scan (REQAB; Jacobson, 1998)
T_min, T_max	0.075, 0.126
No. of measured, independent and observed [I > 2σ(I)] reflections	6821, 3076, 2951
R_int	0.056
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.084, 1.05
No. of reflections	3076
No. of parameters	228
No. of restraints	6
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.77, −1.58

Computer programs: CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 1999).

Selected bond lengths (Å) top

Pb1—O1	2.701 (5)	Pb1—O4	2.508 (4)
Pb1—O2	2.527 (4)	Pb1—O4ⁱⁱ	2.772 (4)
Pb1—O3	2.453 (3)	Pb1—O1W	2.687 (4)
Pb1—O3ⁱ	2.662 (4)

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+1, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O2Wⁱⁱⁱ	0.82	1.80	2.618 (6)	173
O6—H6···O5ⁱ	0.82	1.93	2.698 (6)	156
O1W—H1W···O1ⁱⁱ	0.84	2.31	3.089 (6)	154
O1W—H2W···O2ⁱ	0.84	2.16	2.900 (6)	147
O2W—H3W···O1^iv	0.84	1.88	2.715 (6)	172
O2W—H4W···O6^v	0.84	2.05	2.788 (7)	146

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+1, −y, −z+1; (iii) x+1, y, z+1; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z.

Acknowledgements

The authors acknowledge the Guangdong Natural Science Foundation (SN. 8452606101000739) for supporting this work.

References

Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Jacobson, R. (1998). REQAB. Molecular Structure Corporation, The Woodlands, Texas, USA. Google Scholar
Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Google Scholar
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