catena-Poly[[(benzoato-κ2 O,O′)(2,2′-bipyridine-κ2 N,N′)lead(II)]-μ3-nitrato-κ4 O:O,O′:O′′]

Juan Yang; Jun Dai; Xiaohan Wang

doi:10.1107/S160053681004907X

. 2010 Nov 27;66(Pt 12):m1686. doi: 10.1107/S160053681004907X

catena-Poly[[(benzoato-κ² O,O′)(2,2′-bipyridine-κ² N,N′)lead(II)]-μ₃-nitrato-κ⁴ O:O,O′:O′′]

Juan Yang ^a,^*, Jun Dai ^b, Xiaohan Wang ^b

PMCID: PMC3011738 PMID: 21589342

Abstract

In the title coordination polymer, [Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]_n, the Pb^II ion is eight-coordinated by two N atoms from one 2,2′-bipyridine ligand, two O atoms from one benzoate anion and four O atoms from three nitrate groups (one chelating, two bridging) in a distorted dodecahedral geometry. Adjacent Pb^II ions are linked by bridging nitrate O atoms through the central Pb₂O₂ and Pb₂O₄N₂ cores, resulting in an infinite chain structure along the b axis. The crystal structure is stabilized by π–π stacking interactions between 2,2′-bipyridine and benzoate ligands belonging to neighboring chains, with shortest centroid–centroid distances of 3.685 (8) and 3.564 (8) Å.

Related literature

For applications of complexes containing Pb(II), see: Fan & Zhu (2006 ▶); Hamilton et al. (2004 ▶); Alvarado et al. (2005 ▶). For the use of aromatic carboxylate and 2,2′-bipyridine-like ligands in the preparation of metal-organic complexes, see: Wang et al. (2006 ▶); Masaoka et al. (2001 ▶); Hagrman & Zubieta (2000 ▶); Li et al. (2002 ▶).

Experimental

Crystal data

[Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]
M _r = 546.49
Triclinic,
a = 6.5389 (11) Å
b = 8.5052 (14) Å
c = 15.548 (3) Å
α = 84.566 (3)°
β = 86.593 (3)°
γ = 83.729 (2)°
V = 854.6 (3) Å³
Z = 2
Mo Kα radiation
μ = 9.91 mm⁻¹
T = 296 K
0.23 × 0.21 × 0.15 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T _min = 0.118, T _max = 0.226
4385 measured reflections
2981 independent reflections
2769 reflections with I > 2σ(I)
R _int = 0.030

Refinement

R[F ² > 2σ(F ²)] = 0.037
wR(F ²) = 0.099
S = 1.02
2981 reflections
235 parameters
H-atom parameters constrained
Δρ_max = 2.70 e Å⁻³
Δρ_min = −2.79 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 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053681004907X/gk2325sup1.cif

e-66-m1686-sup1.cif^{(18KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053681004907X/gk2325Isup2.hkl

e-66-m1686-Isup2.hkl^{(146.3KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Pb1—O1	2.432 (5)
Pb1—N2	2.441 (6)
Pb1—N1	2.471 (5)
Pb1—O2	2.619 (6)
Pb1—O4	2.871 (6)
Pb1—O3	2.928 (6)
Pb1—O3ⁱ	2.893 (6)
Pb1—O5ⁱⁱ	2.887 (7)

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

The authors acknowledge financial support by the Doctoral Foundation of Henan Polytechnic University (B2008-58 648265).

supplementary crystallographic information

Comment

Complexes containing Pb(II) ion have recently attracted considerable interest not only because of the variety of their architectures, but also because of their potential applications, especially in environmental protection and in systems with different biological properties (Fan & Zhu, 2006; Hamilton et al., 2004; Alvarado et al., 2005). As an important family of multidentate O-donor ligands, aromatic carboxylate ligands have been extensively employed in the preparation of metal-organic complexes because of their potential properties and intriguing structural topologies (Wang et al., 2006; Masaoka et al., 2001). To our knowledge, carboxylate coordinates metal in various ways, for example, in the mode of monodentate, bidentate chelating, bidentate bridging or chelating-bridging. It is well known that the introduction of chelate ligands such as 2,2'-bipyridine are capable of passivating metal sites via the N donors of the organic groups and may induce new structural evolution (Hagrman et al., 2000; Li et al., 2002). Herein, we report the structure of the title polymer.

The asymmetric unit of the title compound, [Pb(C₁₀H₈N₂)(C₇H₅O₂)(NO₃)], contains a Pb^II cation, one 2,2'-bipyridine ligand, one benzoate and one nitrate ligand, as illustrated in in Fig.1. The Pb^II atom is eight-coordinated by two N atoms from one 2,2'-bipyridine ligand, two O atoms from one benzoate anion and four O atoms from three chelating-bridging nitrate ligands in a distorted dodecahedron geometry. The O3 and O5 atoms of bridging nitrato ligands link the adjacent Pb^II ions through the central Pb₂O₂ and Pb₂O₄N₂ cores, resulting in an infinite chain structure along the b axis (Fig.2). The excellent coordinating ability and large conjugated systems of 2,2'-bipyridine and benzoato ligands allow to form π..π interactions. The chains are extended into the framework through π..π stacking interactions between the ligands belonging to the neighboring chains, with the shortest centroid-centroid distance of 3.685 (8) and 3.564 (8)Å.

Experimental

A mixture of Pb(NO₃)₂ (0.09 g, 0.27 mmol), benzoic acid (0.102 g, 0.84 mmol), 2,2'-bipyridine (0.065 g, 0.41 mmol) and distilled water (10 ml) was sealed in a 25 ml Teflon-lined stainless autoclave. The mixture was heated at 403 K for 6 days to give the colorless crystals suitable for X-ray diffraction analysis.