Poly[[tris­(N,N-dimethyl­formamide)(μ4-5-nitro­isophthalato)(μ3-5-nitro­isophthalato)dicobalt(II)] N,N-dimethyl­formamide monosolvate]

Meng Su; Zhan-Dong Huang; Huang Sun; Guang Yang; Seik Weng Ng

doi:10.1107/S1600536810035270

. 2010 Sep 8;66(Pt 10):m1220–m1221. doi: 10.1107/S1600536810035270

Poly[[tris(N,N-dimethylformamide)(μ₄-5-nitroisophthalato)(μ₃-5-nitroisophthalato)dicobalt(II)] N,N-dimethylformamide monosolvate]

Meng Su ^a, Zhan-Dong Huang ^a, Huang Sun ^a, Guang Yang ^a, Seik Weng Ng ^b,^*

PMCID: PMC2983205 PMID: 21587377

Abstract

In the polymeric title compound, [Co₂(C₃H₇NO)₃(C₈H₃NO₆)₂]·C₃H₇NO, one 5-nitroisophthalate dianion has its two carboxylate groups chelating to one Co^II atom while simultaneously coordinating to another metal atom in a μ₄-bridging mode. The other 5-nitroisophthalte dianion has one carboxylate group chelating to a metal atom whereas the other bridges two metal atoms in a μ₃-bridging mode. Both metal atoms show an octahedral coordination. The polymer adopts a layer motif, with the lattice dimethylformamide molecules occupying the space between adjacent layers.

Related literature

For adducts of cobalt 5-nitroisophthalate, see: Chen et al. (2006 ▶); Du et al. (2008 ▶); Guo et al. (2006 ▶); Liu et al. (2008 ▶); Luo et al. (2003 ▶); Wang et al. (2008 ▶, 2009 ▶); Xie et al. (2006 ▶); Ye et al. (2008a ▶,b ▶); Yuan et al. (2009 ▶); Zhou et al. (2004 ▶).

Experimental

Crystal data

[Co₂(C₃H₇NO)₃(C₈H₃NO₆)₂]·C₃H₇NO
M _r = 828.47
Monoclinic,
a = 10.0833 (12) Å
b = 17.0887 (19) Å
c = 21.074 (2) Å
β = 92.910 (2)°
V = 3626.7 (7) Å³
Z = 4
Mo Kα radiation
μ = 0.99 mm⁻¹
T = 293 K
0.40 × 0.30 × 0.30 mm

Data collection

Bruker SMART diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.796, T _max = 1
21143 measured reflections
7876 independent reflections
5128 reflections with I > 2σ(I)
R _int = 0.036

Refinement

R[F ² > 2σ(F ²)] = 0.048
wR(F ²) = 0.132
S = 0.99
7876 reflections
477 parameters
54 restraints
H-atom parameters constrained
Δρ_max = 0.57 e Å⁻³
Δρ_min = −0.45 e Å⁻³

Data collection: SMART (Bruker, 1999 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: OLEX (Dolomanov et al., 2003 ▶) and X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810035270/bt5344sup1.cif

e-66-m1220-sup1.cif^{(30.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810035270/bt5344Isup2.hkl

e-66-m1220-Isup2.hkl^{(385.3KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Co1—O1	2.001 (2)
Co1—O3ⁱ	2.247 (2)
Co1—O4ⁱ	2.058 (2)
Co1—O7	2.383 (3)
Co1—O8	2.082 (3)
Co1—O10ⁱⁱ	2.008 (2)
Co2—O2	2.042 (2)
Co2—O7	2.091 (2)
Co2—O9ⁱⁱ	2.082 (2)
Co2—O13	2.139 (3)
Co2—O14	2.100 (2)
Co2—O15	2.063 (2)

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

Acknowledgments

We thank the National Science Foundation of China (No. J0830412) and the University of Malaya for supporting this study.

supplementary crystallographic information

Comment

Cobalt 5-nitroisophthalate forms a number of adducts with neutral ligands (Chen et al., 2006; Du et al., 2008; Guo et al., 2006; Liu et al., 2008; Luo et al., 2003; Wang et al., 2008; Wang et al., 2009; Xie et al., 2006; Ye et al., 2008a; Ye et al., 2008b; Yuan et al., 2009; Zhou et al., 2004). The structure of the parent coordination polymer has not been reported. The attempt to synthesize this compound by using DMF as the solvent gave instead the DMF-coordinated polymer, who crystallizes as a DMF solvate (Scheme I).

In polymeric Co₂(DFM)₃(C₈H₃NO₆)₂^.DMF, the 5-nitroisophthalate units show different binding modes. With one dianion, each carboxyl –CO₂ fragment chelate to one cobalt(II) atom while simultaneously coordinating to another metal atom, i.e., this dianion functions in a µ₄-bridging mode. With the other, one carboxyl fragment chelates to a metal atom whereas the other bridges two metal atoms, the dianion functioning in a µ₃-bridging mode. Both metal atoms show octahedral coordination. Of the two indepent metal atoms, one is coordinated by three DMF molecules. The bridging mode exercised by the dianion gives rise to a layer motif (Fig. 1). The lattice DMF molecules occupy the space between adjacent layers.

Experimental

Cobalt(II) nitrate hexahydrate (0.5 mmol, 0.146 g) and 5-nitroisophthalic acid (0.5 mmol, 0.106 g) were dissolved in DMF (2 ml); triethylamine was allowed to diffuse into the solution. Purple crystals were obtained in 30% yield after one week.