Poly[(μ4-3-carb­oxy­benzoato-κ5 O 1:O 1,O 1′:O 1′:O 3)(quinolin-8-olato-κ2 N,O)lead(II)]

Akbar Ghaemi; Zohreh Dadkhah; Seik Weng Ng; Edward R T Tiekink

doi:10.1107/S160053681105495X

. 2012 Jan 7;68(Pt 2):m97–m98. doi: 10.1107/S160053681105495X

Poly[(μ₄-3-carboxybenzoato-κ⁵ O ¹:O ¹,O ^1′:O ^1′:O ³)(quinolin-8-olato-κ² N,O)lead(II)]

Akbar Ghaemi ^a,^‡, Zohreh Dadkhah ^a, Seik Weng Ng ^b,^c, Edward R T Tiekink ^b,^*

PMCID: PMC3274846 PMID: 22346895

Abstract

The asymmetric unit of the title complex, [Pb(C₈H₅O₄)(C₉H₆NO)]_n, comprises a Pb^II cation, a quinolin-8-olate anion and a 3-carboxybenzoate anion. The coordination geometry of the Pb^II atom is defined by one N and six O atoms, as well as a stereochemically active lone pair of electrons, and is based on a Ψ-dodecahedron. The quinolin-8-olate is chelating and the 3-carboxybenzoate anion forms bonds to four different Pb^II atoms. The benzoate end of the 3-carboxybenzoate ligand chelates one Pb^II atom and simultaneously bridges two Pb^II atoms on either side, forming a chain along the b axis. The carboxyl end of the 3-carboxybenzoate connects to a neighbouring chain by employing its carbonyl atom to form a bond to a Pb^II atom and the hydroxyl group to form a hydrogen bond to a quinolin-8-olate O atom. Thereby, a layer is formed in the bc plane.

Related literature

For background to Pb^II mixed quinolate carboxylate structures, see: Shahverdizadeh et al. (2008 ▶).

Experimental

Crystal data

[Pb(C₈H₅O₄)(C₉H₆NO)]
M _r = 516.46
Monoclinic,
a = 9.0746 (2) Å
b = 7.0262 (2) Å
c = 22.6919 (6) Å
β = 93.185 (3)°
V = 1444.60 (6) Å³
Z = 4
Mo Kα radiation
μ = 11.71 mm⁻¹
T = 100 K
0.25 × 0.20 × 0.15 mm

Data collection

Agilent SuperNova Dual diffractometer with an Atlas detector
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010 ▶) T _min = 0.158, T _max = 0.273
9690 measured reflections
3325 independent reflections
3035 reflections with I > 2σ(I)
R _int = 0.029

Refinement

R[F ² > 2σ(F ²)] = 0.021
wR(F ²) = 0.049
S = 1.01
3325 reflections
221 parameters
1 restraint
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.92 e Å⁻³
Δρ_min = −1.27 e Å⁻³

Data collection: CrysAlis PRO (Agilent, 2010 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S160053681105495X/qm2046sup1.cif

e-68-00m97-sup1.cif^{(23.4KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681105495X/qm2046Isup2.hkl

e-68-00m97-Isup2.hkl^{(163.1KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Pb—O1	2.608 (2)
Pb—O1ⁱ	2.746 (2)
Pb—O2ⁱⁱ	2.578 (2)
Pb—O2ⁱ	2.809 (2)
Pb—O3ⁱⁱⁱ	2.840 (3)
Pb—O5	2.318 (2)
Pb—N1	2.468 (3)

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

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H1⋯O5ⁱⁱⁱ	0.84 (1)	1.74 (3)	2.539 (4)	158 (6)

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Symmetry code: (iii) Inline graphic .

Acknowledgments

We gratefully acknowledge practical support of this study by the Islamic Azad University (Saveh Branch), and thank the University of Malaya for supporting the crystallographic facility.

supplementary crystallographic information

Comment

Mixed lead(II) complexes of quinolin-8-olate and monofunctional carboxylates have displayed a variety of structural motifs (Shahverdizadeh et al., 2008). In the present report, a 1:1 structure containing quinolin-8-olate and 3-carboxybenzoate is described, (I).

The asymmetric unit of (I) comprises a Pb^II cation, a quinolin-8-olate anion and a 3-carboxybenzoate anion, Fig. 1. The coordination geometry of the Pb^II atom is defined by a N and six O atoms as well as a stereochemically active lone pair of electrons, and is based on a Ψ-dodecahedron. The quinolin-8-olate anion is chelating, whereas the 3-carboxybenzoate anion is pentadentate, forming bonds to four different Pb^II atoms, Table 1. The benzoate group chelates one Pb^II atom and each of these O atoms forms a bond to a neighbouring Pb^II to form a chain along the b axis. Adjacent chains, along the c axis, are connected by Pb—O(carbonyl) bonds. The hydroxyl group forms a hydrogen bond to the quinolin-8-olate-O atom, Table 2. The result is a layer in the bc plane. Layers stack along the a axis, Fig. 3, with no specific intermolecular interactions between them.

Experimental

The title complex was obtained by the following method. A methanol solution (10 ml) of 8-hydroxyquinoline (0.145 g, 1 mmol) was added to an aqueous solution (2 ml) of Pb(NO₃)₂ (0.331 g, 1 mmol). The mixture was stirred for 10 min. To this solution, was added a DMF solution (5 ml) of isophthalic acid (0.084 g, 0.5 mmol) slowly at room temperature. This mixture was filtered. After keeping the filtrate in air, crystals were formed at the bottom of the vessel upon slow evaporation of the solvents at room temperature. M.pt. 558 K (dec.). Yield: 65%.