catena-Poly[[bis­(3-methyl­benzoato-κ2 O,O′)lead(II)]-μ-4,4′-bipyridine-κ2 N:N′]

Jian-Ying Xie; Fu Huang

doi:10.1107/S1600536811035021

. 2011 Sep 3;67(Pt 10):m1326. doi: 10.1107/S1600536811035021

catena-Poly[[bis(3-methylbenzoato-κ² O,O′)lead(II)]-μ-4,4′-bipyridine-κ² N:N′]

Jian-Ying Xie ^a, Fu Huang ^a,^*

PMCID: PMC3201505 PMID: 22065196

Abstract

In the title complex, [Pb(C₈H₇O₂)₂(C₁₀H₈N₂)]_n, the Pb^II atom is located on a twofold rotation axis and is six-coordinated by four carboxylate O atoms from two 3-methylbenzoate ligands and two N atoms from two 4,4′-bipyridine (4,4′-bpy) ligands, displaying a hemi-directed coordination. The 4,4′-bpy ligand has an inversion center at the mid-point of the central C—C bond. The Pb^II atoms are linked by bidentate bridging 4,4′-bpy into a chain along [101]. These chains are further connected into layers via C—H⋯O hydrogen bonds.

Related literature

For general background to 3-methylbenzoate complexes, see: Wang et al. (2002 ▶); Zhao et al. (2009 ▶) and to 4,4′-bipyridine complexes, see: Biradha et al. (2006 ▶). For hemi- and holo-directed geometries of lead(II) complexes, see: Shimoni-Livny et al. (1998 ▶).

Experimental

Crystal data

[Pb(C₈H₇O₂)₂(C₁₀H₈N₂)]
M _r = 633.65
Monoclinic,
a = 20.506 (8) Å
b = 5.534 (2) Å
c = 20.219 (8) Å
β = 103.507 (7)°
V = 2231.0 (15) Å³
Z = 4
Mo Kα radiation
μ = 7.60 mm⁻¹
T = 296 K
0.30 × 0.27 × 0.21 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.129, T _max = 0.215
8381 measured reflections
2402 independent reflections
2153 reflections with I > 2σ(I)
R _int = 0.025

Refinement

R[F ² > 2σ(F ²)] = 0.017
wR(F ²) = 0.042
S = 1.01
2402 reflections
151 parameters
H-atom parameters constrained
Δρ_max = 0.38 e Å⁻³
Δρ_min = −0.50 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811035021/hy2458sup1.cif

e-67-m1326-sup1.cif^{(21.5KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811035021/hy2458Isup2.hkl

e-67-m1326-Isup2.hkl^{(118.1KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Pb1—O1	2.4803 (19)
Pb1—O2	2.4148 (19)
Pb1—N1	2.893 (2)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C13—H13⋯O1ⁱ	0.93	2.54	3.461 (4)	172

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors acknowledge Guangdong Ocean University for supporting this work.

supplementary crystallographic information

Comment

In the structural investigation of 3-methylbenzoate complexes, it has been found that 3-methylbenzoic acid functions as a multidentate ligand (Wang et al., 2002; Zhao et al., 2009), with versatile binding and coordination modes. As is well known, 4,4'-bipyridine (4,4'-bpy) ligand may act in bidentate bridging or monodentate terminal mode (Biradha et al., 2006). In this paper, we report the crystal structure of the title compound, a new Pb(II) complex obtained by the reaction of 3-methylbenzoic acid, 4,4'-bpy and lead acetate in an alkaline aqueous solution.

As depicted in Fig. 1, the Pb^II atom is located on a twofold rotation axis and is coordinated by four O atoms from two 3-methylbenzoate ligands and two N atoms from two µ-4,4'-bpy ligand (Table 1). The coordination environment of the Pb^II atom is hemidirected (Shimoni-Livny et al., 1998). The 3-methylbenzoate ligand adopting bidentate coordination mode chelate the Pb^II atom, which can be regarded as a knot. The 4,4'-bpy ligand bridges two neighboring knots, forming a one-dimensional chain along [1 0 1] (Fig. 2). The distance between two knots is 12.882 (3) Å. These chains are further assembled via C—H···O hydrogen bonds (Table 2) into a layered network (Fig. 3).

Experimental

A mixture of lead acetate (1 mmol, 0.325 g), 3-methylbenzoic acid (1 mmol, 0.136 g), 4,4'-bpy (1 mmol, 0.156 g), NaOH (1.5 mmol, 0.06 g) and H₂O (12 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 433 K for 3 days and then cooled to room temperature at a rate of 10 K h^-1. Colorless crystals obtained were washed with water and dried in air.