Poly[bis­(μ3-acetato-κ4O,O′:O:O′)bis­(μ2-acetato-κ3O,O′:O)(μ2-2,5-dimethyl­benzene-1,4-diol-κ2O:O′)dilead(II)]

Lyczko, K.; Bak, J.

doi:10.1107/S1600536808030535

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 10| October 2008| Pages m1341-m1342

doi:10.1107/S1600536808030535

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Poly[bis(μ₃-acetato-κ⁴O,O′:O:O′)bis(μ₂-acetato-κ³O,O′:O)(μ₂-2,5-dimethylbenzene-1,4-diol-κ²O:O′)dilead(II)]

Krzysztof Lyczko ^a ^* and Joanna Bak ^b

^aInstitute of Nuclear Chemistry and Technology, Dorodna 16, 03-195 Warsaw, Poland, and ^bWarsaw University, Pasteura 1, 02-093 Warsaw, Poland
^*Correspondence e-mail: k.lyczko@op.pl

(Received 3 September 2008; accepted 22 September 2008; online 27 September 2008)

The title compound, [Pb₂(C₂H₃O₂)₄(C₈H₁₀O₂)]_n, has a polymeric structure, with acetatolead(II) chains and 2,5-dimethylbenzene-1,4-diol molecules forming bridges between two Pb^II ions from neighbouring chains. Each Pb^II centre is surrounded by eight O atoms; four belong to bidentate acetate ions, three to neighbouring bridging acetate groups and one to the 2,5-dimethylbenzene-1,4-diol molecule. The Pb^II ions are chelated symmetrically and asymmetrically by acetate ligands. The coordination environment of the Pb^II ion can be described as a hemidirected Pb^IIO₆ core with the empty space around the metal ion filled by the stereochemically active 6s² electron pair and two longer Pb—O contacts. The Pb—O distances are in the range of 2.355 (3)–2.994 (3) Å. Additionally, the crystal structure is stabilized by O—H⋯O hydrogen bonds.

Related literature

Other crystal structures containing polymeric lead(II) acetate were reported by: Rajaram & Rao (1982 ); Bryant et al. (1984 ); Harrowfield et al. (1996 ). Van der Waals radii of lead(II) and oxygen were presented by Bondi (1964 ). The synthesis of the title compound was carried out similarly to the method used for obtaining the bis(2,4-pentanedionato)lead(II) complex described by Lyczko et al. (2006 ). Hemi- and holodirected geometries of lead(II) complexes and the role of the 6s² lone electron pair of the lead(II) ion were discussed by Shimoni-Livny et al. (1998 ).

Experimental

Crystal data

[Pb₂(C₂H₃O₂)₄(C₈H₁₀O₂)]
M_r = 788.72
Triclinic, $[P \overline 1]$
a = 7.4905 (11) Å
b = 7.5526 (10) Å
c = 10.2522 (15) Å
α = 93.043 (11)°
β = 100.787 (12)°
γ = 116.377 (14)°
V = 504.28 (12) Å³
Z = 1
Mo Kα radiation
μ = 16.72 mm⁻¹
T = 100 (2) K
0.35 × 0.26 × 0.14 mm

Data collection

Kuma KM-4 four-circle CCD diffractometer
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005 $[Oxford Diffraction (2005). CrysAlis RED and CrysAlis CCD. Oxford Diffraction Poland, Wrocław, Poland.]$ ) T_min = 0.040, T_max = 0.227
9065 measured reflections
2432 independent reflections
2317 reflections with I > 2σ(I)
R_int = 0.041

Refinement

R[F² > 2σ(F²)] = 0.017
wR(F²) = 0.043
S = 1.07
2432 reflections
132 parameters
H-atom parameters constrained
Δρ_max = 1.30 e Å⁻³
Δρ_min = −1.67 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb1—O3	2.355 (3)
Pb1—O1	2.493 (3)
Pb1—O2	2.499 (3)
Pb1—O1ⁱ	2.618 (2)
Pb1—O4	2.700 (3)
Pb1—O2ⁱⁱ	2.767 (3)
Pb1—O5	2.993 (3)
Pb1—O4ⁱⁱⁱ	2.994 (3)
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x, -y+1, -z; (iii) -x, -y, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯O3ⁱ	0.84	1.87	2.668 (4)	159
Symmetry code: (i) -x+1, -y+1, -z.

Data collection: CrysAlis CCD (Oxford Diffraction, 2005 $[Oxford Diffraction (2005). CrysAlis RED and CrysAlis CCD. Oxford Diffraction Poland, Wrocław, Poland.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2005 $[Oxford Diffraction (2005). CrysAlis RED and CrysAlis CCD. Oxford Diffraction Poland, Wrocław, Poland.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2006 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808030535/nc2114sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808030535/nc2114Isup2.hkl

checkCIF report

Comment top

The aim of this work was to synthesize the complex between Pb^II ions and 3-methyl-2,4-pentanedione. Unexpectedly, under the reaction conditions (see Experimental), instead of the bis(3-methyl-2,4-pentanedionato)lead(II) complex, the title compound was obtained.

The structure of this compound consists of polymeric chains of lead(II) acetate linked via 2,5-dimethylbenzene-1,4-diol molecules, each bridging two Pb^II ions from neighbouring chains. As shown in Fig. 1 the title compound contains eight-coordinated Pb^II ions. Each Pb^II centre binds strongly four O atoms from bidentate acetate ions in a nearly pyramidal configuration with Pb—O bond lengths in the range of 2.355 (3)–2.700 (3) Å, and additionally two O atoms from neighbouring bridging acetate groups of the same chain at 2.618 (2) and 2.766 (3) Å. The Pb^II ions are chelated symmetrically [Pb—O = 2.493 (3) and 2.499 (3) Å] and asymmetrically [2.355 (3) and 2.700 (3) Å] by acetato ligands. The coordination sphere of the metal ion is completed by two additional O atoms at distances of about 2.99 Å, the first from the acetate group of the neighbouring chain and the second from the 2,5-dimethylbenzene-1,4-diol molecule. These two contacts are much longer than the Pb—O bonds in the chelate but shorter than the sum of the van der Waals radii of lead(II) and oxygen (3.44 Å; Bondi, 1964) indicating some weak interactions. The crystal structure is also stabilized by O—H···O hydrogen bonds. The OH groups of the 2,5-dimethylbenzene-1,4-diol molecule form hydrogen bonds with a H···O distance of 1.87 Å to O atoms from neighbouring CH₃COO^- ions (Fig. 2). The resulting coordination sphere of the Pb^II ion in the title compound has a hemidirected geometry (Shimoni-Livny et al., 1998). It contains the Pb^IIO₆ core with the empty space at one side of the metal ion filled by stereochemically active electron pair and two longer Pb—O contacts of 2.993 (3) and 2.994 (3) Å. The 6s² electron pair is located opposite to the shortest Pb—O bond length [2.355 (3) Å] and between two longest Pb—O contacts of about 2.99 Å.

Identical polymeric acetato-lead(II) chains are present in the lead(II) acetate trihydrate structure, where the metal ions are nine-coordinated (Pb^IIO₉) with two bidentate acetate groups, three coordinated water molecules and two bridging distances to O atoms from the neighbouring acetate groups (Rajaram & Rao, 1982; Bryant et al., 1984). In another polymeric structure of lead(II) acetate the Pb^II ions are eight-coordinated with the Pb^IIO₆N₂ core containing in addition two N atoms from two 2-pyridylamine molecules (Harrowfield et al., 1996).

Related literature top

Other crystal structures containing polymeric lead(II) acetate were reported by: Rajaram & Rao (1982); Bryant et al. (1984); Harrowfield et al. (1996). Van der Waals radii of lead(II) and oxygen were presented by Bondi (1964). The synthesis of the title compound was carried out similarly to the method used for obtaining the bis(2,4-pentanedionato)lead(II) complex described by Lyczko et al. (2006). Hemi- and holodirected geometries of lead(II) complexes and the role of the 6s² lone electron pair of the lead(II) ion were discussed by Shimoni-Livny et al. (1998).

Experimental top

The title compound was obtained unintentionally in an attempt to synthesize single crystals of the bis(3-methyl-2,4-pentanedionato)lead(II) complex. Small pieces of lead foil (0.26 g) were heated (~50 °C) for a few weeks in a mixture of 3-methyl-2,4-pentanedione (2 ml) and toluene (2 ml) under reflux. The synthesis was carried out similarly to that used for the preparation of crystals of the bis(2,4-pentanedionato)lead(II) complex (Lyczko et al., 2006). After heating the reaction mixture was stored for a few months until it converted into an orange–brown solid. Colourless crystals of the title compound were separated from the reaction mixture. Analysis, calculated for C₁₆H₂₂O₁₀Pb₂: C 24.36, H 2.81%; found: C 24.14, H 2.88%.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED (Oxford Diffraction, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. A fragment of the polymeric structure of the title compound with labelling showing the environment of the lead atom. Displacement ellipsoids of non-hydrogen atoms are drawn at the 50% probability level. [Symmetry codes: (i) -x + 1, -y + 1, -z; (ii) -x, -y + 1, -z; (iii) -x, -y, -z; (iv) x + 1, -y + 1, -z + 1].
	Fig. 2. A packing diagram of the title compound. Hydrogen bonding is shown as blue dashed lines.

Poly[bis(µ₃-acetato-κ⁴O,O':O:O')bis(µ₂- acetato-κ³O,O':O)(µ₂-2,5-dimethylbenzene-1,4- diol-κ²O:O')dilead(II)] top

Crystal data top

[Pb₂(C₂H₃O₂)₄(C₈H₁₀O₂)]	Z = 1
M_r = 788.72	F(000) = 362
Triclinic, P1	D_x = 2.597 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.4905 (11) Å	Cell parameters from 9065 reflections
b = 7.5526 (10) Å	θ = 3.0–28.7°
c = 10.2522 (15) Å	µ = 16.72 mm⁻¹
α = 93.043 (11)°	T = 100 K
β = 100.787 (12)°	Prismatic, colourless
γ = 116.377 (14)°	0.35 × 0.26 × 0.14 mm
V = 504.28 (12) Å³

Data collection top

Kuma KM-4 four-circle CCD diffractometer	2432 independent reflections
Radiation source: fine-focus sealed tube	2317 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.041
Detector resolution: 8.6479 pixels mm^-1	θ_max = 28.7°, θ_min = 3.1°
ω scans	h = −9→9
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005)	k = −10→10
T_min = 0.040, T_max = 0.227	l = −13→13
9065 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.017	H-atom parameters constrained
wR(F²) = 0.043	w = 1/[σ²(F_o²) + (0.0223P)² + 0.6288P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max = 0.001
2432 reflections	Δρ_max = 1.30 e Å⁻³
132 parameters	Δρ_min = −1.67 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0077 (5)

Crystal data top

[Pb₂(C₂H₃O₂)₄(C₈H₁₀O₂)]	γ = 116.377 (14)°
M_r = 788.72	V = 504.28 (12) Å³
Triclinic, P1	Z = 1
a = 7.4905 (11) Å	Mo Kα radiation
b = 7.5526 (10) Å	µ = 16.72 mm⁻¹
c = 10.2522 (15) Å	T = 100 K
α = 93.043 (11)°	0.35 × 0.26 × 0.14 mm
β = 100.787 (12)°

Data collection top

Kuma KM-4 four-circle CCD diffractometer	2432 independent reflections
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005)	2317 reflections with I > 2σ(I)
T_min = 0.040, T_max = 0.227	R_int = 0.041
9065 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.017	0 restraints
wR(F²) = 0.043	H-atom parameters constrained
S = 1.07	Δρ_max = 1.30 e Å⁻³
2432 reflections	Δρ_min = −1.67 e Å⁻³
132 parameters

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
Pb1	0.205617 (17)	0.362095 (17)	0.046792 (11)	0.00910 (6)
O1	0.4490 (4)	0.6463 (4)	−0.0457 (2)	0.0121 (5)
O2	0.1324 (4)	0.6005 (4)	−0.0858 (3)	0.0154 (5)
O3	0.1663 (4)	0.2264 (4)	−0.1751 (2)	0.0148 (5)
O4	−0.1191 (4)	0.0447 (4)	−0.1145 (3)	0.0214 (6)
C1	0.3154 (5)	0.6990 (5)	−0.0954 (3)	0.0111 (6)
C2	0.3723 (6)	0.8784 (6)	−0.1662 (4)	0.0155 (7)
H2A	0.5180	0.9365	−0.1668	0.023*
H2B	0.3466	0.9780	−0.1192	0.023*
H2C	0.2896	0.8380	−0.2589	0.023*
C3	−0.0132 (5)	0.0788 (6)	−0.1992 (4)	0.0135 (7)
C4	−0.0903 (6)	−0.0587 (6)	−0.3316 (4)	0.0212 (8)
H4A	−0.0509	−0.1658	−0.3216	0.032*
H4B	−0.0301	0.0174	−0.4002	0.032*
H4C	−0.2400	−0.1172	−0.3588	0.032*
C5	0.5070 (5)	0.5941 (5)	0.3871 (3)	0.0124 (7)
O5	0.5039 (4)	0.6836 (4)	0.2743 (3)	0.0166 (5)
H5	0.6216	0.7356	0.2591	0.025*
C6	0.3672 (5)	0.5861 (6)	0.4637 (4)	0.0129 (7)
C7	0.3647 (5)	0.4909 (5)	0.5766 (3)	0.0133 (7)
H7	0.2720	0.4841	0.6303	0.016*
C8	0.2300 (6)	0.6797 (7)	0.4230 (4)	0.0207 (8)
H8A	0.1526	0.6732	0.4914	0.031*
H8B	0.1344	0.6074	0.3366	0.031*
H8C	0.3133	0.8199	0.4145	0.031*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.00762 (8)	0.00740 (8)	0.01117 (8)	0.00219 (6)	0.00281 (5)	0.00244 (5)
O1	0.0087 (12)	0.0098 (12)	0.0179 (12)	0.0040 (10)	0.0032 (9)	0.0049 (10)
O2	0.0082 (12)	0.0150 (13)	0.0246 (14)	0.0054 (11)	0.0062 (10)	0.0077 (11)
O3	0.0130 (12)	0.0112 (12)	0.0157 (12)	0.0012 (11)	0.0048 (9)	0.0017 (10)
O4	0.0123 (13)	0.0247 (16)	0.0203 (14)	0.0021 (12)	0.0053 (10)	0.0018 (12)
C1	0.0119 (16)	0.0087 (16)	0.0123 (16)	0.0048 (14)	0.0025 (12)	0.0006 (13)
C2	0.0098 (17)	0.0120 (18)	0.0240 (19)	0.0034 (15)	0.0051 (14)	0.0091 (15)
C3	0.0107 (17)	0.0115 (17)	0.0151 (16)	0.0037 (15)	−0.0002 (13)	0.0028 (14)
C4	0.023 (2)	0.0139 (19)	0.0179 (18)	0.0035 (17)	0.0004 (15)	−0.0014 (15)
C5	0.0120 (16)	0.0105 (17)	0.0090 (15)	0.0010 (14)	0.0011 (12)	0.0005 (13)
O5	0.0146 (13)	0.0202 (14)	0.0150 (12)	0.0062 (12)	0.0061 (10)	0.0089 (11)
C6	0.0110 (17)	0.0105 (16)	0.0145 (16)	0.0036 (14)	0.0013 (12)	−0.0007 (13)
C7	0.0109 (16)	0.0128 (17)	0.0133 (16)	0.0029 (14)	0.0038 (12)	0.0001 (14)
C8	0.0190 (19)	0.025 (2)	0.0224 (19)	0.0138 (18)	0.0055 (15)	0.0065 (16)

Geometric parameters (Å, º) top

Pb1—O3	2.355 (3)	C2—H2C	0.9800
Pb1—O1	2.493 (3)	C3—C4	1.509 (5)
Pb1—O2	2.499 (3)	C4—H4A	0.9800
Pb1—O1ⁱ	2.618 (2)	C4—H4B	0.9800
Pb1—O4	2.700 (3)	C4—H4C	0.9800
Pb1—O2ⁱⁱ	2.767 (3)	C5—O5	1.372 (4)
Pb1—O5	2.993 (3)	C5—C7^iv	1.384 (5)
Pb1—O4ⁱⁱⁱ	2.994 (3)	C5—C6	1.405 (5)
O1—C1	1.267 (4)	O5—H5	0.8400
O1—Pb1ⁱ	2.618 (2)	C6—C7	1.393 (5)
O2—C1	1.263 (4)	C6—C8	1.499 (5)
O3—C3	1.275 (4)	C7—C5^iv	1.384 (5)
O4—C3	1.245 (4)	C7—H7	0.9500
C1—C2	1.500 (5)	C8—H8A	0.9800
C2—H2A	0.9800	C8—H8B	0.9800
C2—H2B	0.9800	C8—H8C	0.9800

O3—Pb1—O1	75.58 (9)	O4—C3—O3	121.2 (3)
O3—Pb1—O2	77.94 (9)	O4—C3—C4	120.8 (3)
O1—Pb1—O2	52.08 (8)	O3—C3—C4	118.0 (3)
O3—Pb1—O1ⁱ	75.04 (8)	C3—C4—H4A	109.5
O1—Pb1—O1ⁱ	66.16 (9)	C3—C4—H4B	109.5
O2—Pb1—O1ⁱ	116.77 (8)	H4A—C4—H4B	109.5
O3—Pb1—O4	50.93 (8)	C3—C4—H4C	109.5
O1—Pb1—O4	121.84 (8)	H4A—C4—H4C	109.5
O2—Pb1—O4	91.50 (9)	H4B—C4—H4C	109.5
O1ⁱ—Pb1—O4	111.98 (8)	O5—C5—C7^iv	122.7 (3)
C1—O1—Pb1	94.0 (2)	O5—C5—C6	116.7 (3)
C1—O1—Pb1ⁱ	149.3 (2)	C7^iv—C5—C6	120.6 (3)
Pb1—O1—Pb1ⁱ	113.84 (9)	C5—O5—H5	109.5
C1—O2—Pb1	93.8 (2)	C7—C6—C5	117.4 (3)
C3—O3—Pb1	101.7 (2)	C7—C6—C8	122.9 (3)
C3—O4—Pb1	86.2 (2)	C5—C6—C8	119.8 (3)
O2—C1—O1	120.1 (3)	C5^iv—C7—C6	122.0 (3)
O2—C1—C2	119.4 (3)	C5^iv—C7—H7	119.0
O1—C1—C2	120.6 (3)	C6—C7—H7	119.0
C1—C2—H2A	109.5	C6—C8—H8A	109.5
C1—C2—H2B	109.5	C6—C8—H8B	109.5
H2A—C2—H2B	109.5	H8A—C8—H8B	109.5
C1—C2—H2C	109.5	C6—C8—H8C	109.5
H2A—C2—H2C	109.5	H8A—C8—H8C	109.5
H2B—C2—H2C	109.5	H8B—C8—H8C	109.5

O3—Pb1—O1—C1	86.8 (2)	O2—Pb1—O4—C3	74.2 (2)
O2—Pb1—O1—C1	1.04 (19)	O1ⁱ—Pb1—O4—C3	−45.6 (2)
O1ⁱ—Pb1—O1—C1	166.6 (3)	Pb1—O2—C1—O1	1.9 (3)
O4—Pb1—O1—C1	64.6 (2)	Pb1—O2—C1—C2	−178.1 (3)
O3—Pb1—O1—Pb1ⁱ	−79.76 (11)	Pb1—O1—C1—O2	−1.9 (3)
O2—Pb1—O1—Pb1ⁱ	−165.57 (16)	Pb1ⁱ—O1—C1—O2	153.6 (3)
O1ⁱ—Pb1—O1—Pb1ⁱ	0.0	Pb1—O1—C1—C2	178.1 (3)
O4—Pb1—O1—Pb1ⁱ	−101.97 (11)	Pb1ⁱ—O1—C1—C2	−26.4 (6)
O3—Pb1—O2—C1	−82.0 (2)	Pb1—O4—C3—O3	−1.8 (3)
O1—Pb1—O2—C1	−1.05 (19)	Pb1—O4—C3—C4	175.7 (3)
O1ⁱ—Pb1—O2—C1	−15.8 (2)	Pb1—O3—C3—O4	2.1 (4)
O4—Pb1—O2—C1	−131.5 (2)	Pb1—O3—C3—C4	−175.4 (3)
O1—Pb1—O3—C3	−156.6 (2)	O5—C5—C6—C7	178.3 (3)
O2—Pb1—O3—C3	−103.1 (2)	C7^iv—C5—C6—C7	0.3 (6)
O1ⁱ—Pb1—O3—C3	134.7 (2)	O5—C5—C6—C8	−2.3 (5)
O4—Pb1—O3—C3	−1.1 (2)	C7^iv—C5—C6—C8	179.8 (4)
O3—Pb1—O4—C3	1.1 (2)	C5—C6—C7—C5^iv	−0.3 (6)
O1—Pb1—O4—C3	29.2 (2)	C8—C6—C7—C5^iv	−179.8 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O3ⁱ	0.84	1.87	2.668 (4)	159

Symmetry code: (i) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula	[Pb₂(C₂H₃O₂)₄(C₈H₁₀O₂)]
M_r	788.72
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	7.4905 (11), 7.5526 (10), 10.2522 (15)
α, β, γ (°)	93.043 (11), 100.787 (12), 116.377 (14)
V (Å³)	504.28 (12)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	16.72
Crystal size (mm)	0.35 × 0.26 × 0.14

Data collection
Diffractometer	Kuma KM-4 four-circle CCD diffractometer
Absorption correction	Analytical (CrysAlis RED; Oxford Diffraction, 2005)
T_min, T_max	0.040, 0.227
No. of measured, independent and observed [I > 2σ(I)] reflections	9065, 2432, 2317
R_int	0.041
(sin θ/λ)_max (Å⁻¹)	0.676

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.017, 0.043, 1.07
No. of reflections	2432
No. of parameters	132
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.30, −1.67

Computer programs: CrysAlis CCD (Oxford Diffraction, 2005), CrysAlis RED (Oxford Diffraction, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), Mercury (Macrae et al., 2006).

Selected bond lengths (Å) top

Pb1—O3	2.355 (3)	Pb1—O4	2.700 (3)
Pb1—O1	2.493 (3)	Pb1—O2ⁱⁱ	2.767 (3)
Pb1—O2	2.499 (3)	Pb1—O5	2.993 (3)
Pb1—O1ⁱ	2.618 (2)	Pb1—O4ⁱⁱⁱ	2.994 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O3ⁱ	0.84	1.87	2.668 (4)	159.3

Symmetry code: (i) −x+1, −y+1, −z.

Acknowledgements

The authors thank Warsaw University and the Institute of Nuclear Chemistry and Technology for financial support.

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