Poly[bis-(μ(3)-acetato-κO,O':O:O')bis-(μ(2)-acetato-κO,O':O)(μ(2)-2,5-dimethyl-benzene-1,4-diol-κO:O')dilead(II)].

The title compound, [Pb(2)(C(2)H(3)O(2))(4)(C(8)H(10)O(2))](n), has a polymeric structure, with acetatolead(II) chains and 2,5-dimethyl-benzene-1,4-diol mol-ecules 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-dimethyl-benzene-1,4-diol mol-ecule. 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(II)O(6) core with the empty space around the metal ion filled by the stereochemically active 6s(2) 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 6s 2 lone electron pair of the lead(II) ion were discussed by Shimoni-Livny et al. (1998 ▶).

Experimental

Crystal data

[Pb2(C2H3O2)4(C8H10O2)]

M = 788.72

Triclinic,

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 ▶) 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[F 2 > 2σ(F 2)] = 0.017

wR(F 2) = 0.043

S = 1.07

2432 reflections

132 parameters

H-atom parameters constrained

Δρmax = 1.30 e Å−3

Δρmin = −1.67 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2005 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2005 ▶); 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.

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

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

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pb2(C2H3O2)4(C8H10O2)]	Z = 1
Mr = 788.72	F(000) = 362
Triclinic, P1	Dx = 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

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

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(Fo2) + (0.0223P)2 + 0.6288P] where P = (Fo2 + 2Fc2)/3
S = 1.07	(Δ/σ)max = 0.001
2432 reflections	Δρmax = 1.30 e Å−3
132 parameters	Δρmin = −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)

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.

	x	y	z	Uiso*/Ueq
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*

	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)

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—C7iv	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—C5iv	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—C7iv	122.7 (3)
C1—O1—Pb1	94.0 (2)	O5—C5—C6	116.7 (3)
C1—O1—Pb1i	149.3 (2)	C7iv—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)	C5iv—C7—C6	122.0 (3)
O2—C1—C2	119.4 (3)	C5iv—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)	C7iv—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)	C7iv—C5—C6—C8	179.8 (4)
O3—Pb1—O4—C3	1.1 (2)	C5—C6—C7—C5iv	−0.3 (6)
O1—Pb1—O4—C3	29.2 (2)	C8—C6—C7—C5iv	−179.8 (4)

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

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) ; (ii) ; (iii) .

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) .