Poly[[diaqua­(μ-4,4′-bipyridine N,N′-di­oxide-κ2 O:O′)(μ-terephthalato-κ2 O 1:O 4)cobalt(II)] 4,4′-bipyridine N,N′-dioxide monosolvate]

Xin Ge; Shu-Yan Song

doi:10.1107/S1600536812040056

. 2012 Sep 26;68(Pt 10):m1307. doi: 10.1107/S1600536812040056

Poly[[diaqua(μ-4,4′-bipyridine N,N′-dioxide-κ² O:O′)(μ-terephthalato-κ² O ¹:O ⁴)cobalt(II)] 4,4′-bipyridine N,N′-dioxide monosolvate]

Xin Ge ^a, Shu-Yan Song ^a,^*

PMCID: PMC3470175 PMID: 23125619

Abstract

In the title compound, {[Co(C₈H₄O₄)(C₁₀H₈N₂O₂)(H₂O)₂]·C₁₀H₈N₂O₂}_n, the Co^II atom, lying on an inversion center, is hexacoordinated in a distorted octahedral geometry defined by two O atoms from two terephthalate (tp) ligands, two O atoms from two 4,4′-bipyridine N,N′-dioxide (bpydo) ligands and two water molecules. The coordinated tp and bpydo ligands and uncoordinated bpydo molecule all have an inversion center. The Co^II atoms are connected by the tp and bpydo ligands into a layer parallel to (111). In the crystal, O—H⋯O hydrogen bonds link the uncoordinated bpydo molecules and the layers into a three-dimensional supramolecular structure. Intralayer O—H⋯O hydrogen bonds and π–π interactions [centroid-to-centroid distances = 3.6643 (13) and 3.8048 (13) Å] are also observed.

Related literature

For the design of supramolecular structures containing metal ions and organic ligands, see: Liao et al. (2008 ▶); Wang et al. (2008 ▶). For a related structure, see: Su et al. (2009 ▶).

Experimental

Crystal data

[Co(C₈H₄O₄)(C₁₀H₈N₂O₂)(H₂O)₂]·C₁₀H₈N₂O₂
M _r = 635.44
Triclinic,
a = 7.3883 (10) Å
b = 9.1788 (13) Å
c = 9.8054 (13) Å
α = 81.312 (2)°
β = 82.200 (2)°
γ = 79.301 (2)°
V = 641.92 (15) Å³
Z = 1
Mo Kα radiation
μ = 0.74 mm⁻¹
T = 293 K
0.27 × 0.24 × 0.20 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.825, T _max = 0.866
3574 measured reflections
2516 independent reflections
2340 reflections with I > 2σ(I)
R _int = 0.017

Refinement

R[F ² > 2σ(F ²)] = 0.031
wR(F ²) = 0.081
S = 1.05
2516 reflections
202 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.48 e Å⁻³
Δρ_min = −0.33 e Å⁻³

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

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812040056/hy2589sup1.cif

e-68-m1307-sup1.cif^{(18.7KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812040056/hy2589Isup2.hkl

e-68-m1307-Isup2.hkl^{(123.6KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O2	0.84 (2)	1.92 (2)	2.755 (2)	170 (2)
O5—H5B⋯O3ⁱ	0.85 (2)	1.85 (2)	2.660 (2)	158 (3)

Open in a new tab

Symmetry code: (i) Inline graphic .

Acknowledgments

The authors are grateful for financial aid from the National Natural Science Foundation of China (grant No. 21001101).

supplementary crystallographic information

Comment

Much progress has been achieved in the design of supramolecular structures containing metal–organic molecules during recent years (Liao et al., 2008; Wang et al., 2008). Multifunctional ligands can link metal ions into one-, two- or three-dimensional structures, and in this context, aromatic carboxylates and 4,4'-bipyridine N,N'-dioxide have been used successfully to synthesize such materials.

As shown in Fig. 1, the coordination environment of the Co^II atom, lying on an inversion center, can be described as distorted octahedral, defined by four O atoms in the equatorial plane from two terephthalate (tp) ligands and two 4,4'-bipyridine N,N'-dioxide (bpydo) ligands, and two water molecules in the axial positions. The bond distances and angles are normal (Su et al., 2009). The Co^II atoms are connected by the tp and bpydo ligands, forming a layer structure parallel to (111). O—H···O hydrogen bonds (Table 1) link the uncoordinated bpydo molecules and the layers into a three-dimensional supramolecular structure (Fig. 2). Intralayer O—H···O hydrogen bonds and π–π interactions [centroid–centroid distances = 3.6643 (13) and 3.8048 (13) Å] are also observed.

Experimental

A mixture of terephthalic acid (0.1 mmol, 0.017 g), 4,4'-bipyridine N,N'-dioxide (0.2 mmol, 0.038 g), cobalt nitrate (0.1 mmol, 0.030 g), H₂O (5 ml) and dimethylformamide (15 ml) was stirred at 358 K for 10 min. The mixture was filtrated and pink block crystals of the title compound were isolated after evaporation of the solvent.