Poly[(μ-4,4′-bipyridine)(μ-naph­tha­lene-1,4-dicarboxyl­ato)iron(II)]

Jan Boeckmann; Inke Jess; Christian Näther

doi:10.1107/S1600536808042992

. 2008 Dec 20;65(Pt 1):m122. doi: 10.1107/S1600536808042992

Poly[(μ-4,4′-bipyridine)(μ-naphthalene-1,4-dicarboxylato)iron(II)]

Jan Boeckmann ^a, Inke Jess ^a, Christian Näther ^a,^*

PMCID: PMC2968022 PMID: 21581486

Abstract

The asymmetric unit of the title compound, [Fe(C₁₂H₆O₄)(C₁₀H₈N₂)], consists of two independent Fe(II) atoms, two naphthalene-1,4-dicarboxylate anions and two 4,4′-bipyridine ligands. The Fe(II) atoms are each coordinated by four O atoms of the naphthalene-1,4-dicarboxylate anions and two N atoms of the 4,4′-bipyridine ligands within a distorted octahedron. Two Fe(II) atoms are bridged via the carboxylate groups of two symmetry-related anions into dimers, which are further connected into chains. These chains are linked by additional anions into layers that are finally connected by the 4,4′-bipyridine ligands into a three-dimensional coordination network.

Related literature

For a related structure, see: Zheng et al. (2005 ▶).

Experimental

Crystal data

[Fe(C₁₂H₆O₄)(C₁₀H₈N₂)]
M _r = 426.20
Monoclinic,
a = 10.5169 (4) Å
b = 29.8928 (10) Å
c = 11.5578 (4) Å
β = 93.178 (3)°
V = 3627.9 (2) Å³
Z = 8
Mo Kα radiation
μ = 0.87 mm⁻¹
T = 293 (2) K
0.09 × 0.09 × 0.08 mm

Data collection

STOE IPDS-2 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe, 2008 ▶) T _min = 0.923, T _max = 0.933
21152 measured reflections
7116 independent reflections
5305 reflections with I > 2σ(I)
R _int = 0.050

Refinement

R[F ² > 2σ(F ²)] = 0.067
wR(F ²) = 0.141
S = 1.14
7116 reflections
523 parameters
H-atom parameters constrained
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.36 e Å⁻³

Data collection: X-AREA (Stoe, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2008 ▶) and XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: XCIF in SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808042992/ng2529sup1.cif

e-65-0m122-sup1.cif^{(27.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808042992/ng2529Isup2.hkl

e-65-0m122-Isup2.hkl^{(348.2KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Fe1—O4ⁱ	2.056 (3)
Fe1—O1	2.057 (3)
Fe1—O14	2.215 (3)
Fe1—N2ⁱⁱ	2.220 (3)
Fe1—N1	2.227 (4)
Fe1—O13	2.283 (3)
Fe2—O3ⁱ	2.020 (3)
Fe2—O2	2.048 (3)
Fe2—O11ⁱⁱⁱ	2.147 (4)
Fe2—N12^iv	2.207 (4)
Fe2—N11	2.246 (4)
Fe2—O12ⁱⁱⁱ	2.332 (4)

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

Acknowledgments

This work was supported by the state of Schleswig-Holstein. We thank Professor Dr Wolfgang Bensch for the facility to use his equipment.

supplementary crystallographic information

Comment

The structure determination of the title compound was performed as a part of a project on the synthesis of new metal organic frameworks. In this project we have reacted iron(II)sulfate with naphthalene-1,4-dicarboxylic acid in sodium hydroxide and water, which leads to the formation of bis(µ₂-4,4'-bipyridine)-bis(µ₂-naphthalene-1,4-dicarboxylate)diiron(II).

In the crystal structure of the title compound each of the two crystallographically iron atoms are surrounded by two N atoms of two symmetry related 4,4'-bipyridine ligands and four O atoms of three naphthalene-1,4-dicarboxylate anions, of which two are related by symmetry. The coordination polyhedron can be described as a distorted octahedra (Fig 1 and tab 1). Two symmetry related anions bridges two different Fe atoms into dimers, which are further connected into chains by these anions (Fig. 2). Such dimers are also found in the structure of [Eu₂(naphthalene-1,4-dicarboxylate)₃(4,4'-bipyridine)_0.5(H₂O)₃]- (4,4'-bipyridine) reported by Zheng et al. (2005). The second crystallographically independent napthalene-1,4-dicarboxylate anion is coordinated with both O atoms of its carboxyl group to the metal centers. These anions entangle the Fe-naphthalene-1,4-dicarboxylate chains into layers which are parallel to the a/b plane. These layers are further linked by the 4,4'-bipyridine ligands into a three-dimensional coordination network (Fig 3).

Experimental

27.9 mg FeSO₄^. 7 H₂O (0.10 mmol), 33.0 mg naphthalene-1,4-dicarboxylic acid (0.15 mmol), 10.4 mg NaOH (0.26 mmol), 20.0 mg 4,4'-Bipyridine (0.10 mmol) and 5 ml of water were transfered into a glass tube and heated to 150° C for 4 d. On cooling yellow platelets of the title compound were obtained.