Crystal structure of poly[[{μ2-1,4-bis[(1H-imid­azol-1-yl)methyl]benzene}[μ6-5-(4-carboxylatophenoxy)isophthalato]-μ3-hydroxido-dicobalt(II)] 0.25-hydrate]

Yaping Li; Dajun Sun; Julia Ming; Liying Han; Guanfang Su

doi:10.1107/S1600536814022806

. 2014 Oct 29;70(Pt 11):m376–m377. doi: 10.1107/S1600536814022806

Crystal structure of poly[[{μ₂-1,4-bis[(1H-imidazol-1-yl)methyl]benzene}[μ₆-5-(4-carboxylatophenoxy)isophthalato]-μ₃-hydroxido-dicobalt(II)] 0.25-hydrate]

Yaping Li ^a, Dajun Sun ^b,^*, Julia Ming ^c, Liying Han ^d, Guanfang Su ^a

PMCID: PMC4257313 PMID: 25484783

Abstract

The title coordination polymer, {[Co₂(C₁₅H₇O₇)(OH)(C₁₄H₁₄N₄)]·0.25H₂O}_n, was synthesized under hydrothermal conditions. The asymmetric unit contains two Co²⁺ ions, one L ³⁻ anion originating from 5-(4-carboxyphenoxy)isophthalic acid (H₃ L), one OH⁻ ligand, one 1,4-bis[(1H-imidazol-l-yl)methyl]benzene (bix) ligand and one disordered lattice water molecule (occupancy 0.25). The two Co²⁺ ions have different environments. One has an octahedral O₄N₂ coordination sphere, defined by four O atoms from three carboxylate groups and one OH⁻ ligand, and two N atoms from two symmetry-related bix ligands. The other has a trigonal-bipyramidal O₅ coordination sphere resulting from three carboxylate groups and two OH⁻ ligands. The dihedral angles between the two benzene rings in the L ³⁻ ligand and between the benzene ring and the two imidazole rings in the bix ligand are 67.05 (15), 75.27 (17) and 82.05 (17)°, respectively. Four neighbouring Co²⁺ ions are linked by six carboxylate groups and two μ ₃-OH ligands, forming a butterfly-shaped secondary building unit (SBU). These SBUs are connected by L ³⁻ anions into layers parallel to (1-10). Adjacent layers are cross-linked by the bix ligands, forming a three-dimensional framework that has a bimodal (3,8)-connected tfz-d topology. The disordered lattice water molecule is located in the voids of the framework and has O⋯O and O⋯N contacts of 2.81 (2) and 2.95 (2) Å, suggesting medium-strength hydrogen bonds. The title compound may be a good candidate for artificial eye lenses.

Keywords: crystal structure; Co^II complex; (3,8)-connected tfz-d topology

Related literature

For general background to the properties and applications of compounds with metal-organic framework structures (MOFs), see: Batten & Robson (1998 ▶); Farrusseng et al. (2009 ▶); Iremonger et al. (2013 ▶); Kreno et al. (2012 ▶); Kurmoo (2009 ▶); Song et al. (2013 ▶); Su et al. (2012 ▶); Wong et al. (2006 ▶). For topological analysis of crystal structures, see: Blatov et al. (2010 ▶).

Experimental

Crystal data

[Co₂(C₁₅H₇O₇)(OH)(C₁₄H₁₄N₄)]·0.25H₂O
M _r = 676.87
Triclinic,
a = 10.7381 (6) Å
b = 10.7477 (6) Å
c = 13.5585 (12) Å
α = 95.596 (1)°
β = 91.497 (1)°
γ = 118.728 (1)°
V = 1360.85 (16) Å³
Z = 2
Mo Kα radiation
μ = 1.28 mm⁻¹
T = 173 K
0.19 × 0.16 × 0.15 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2010 ▶) T _min = 0.793, T _max = 0.831
7626 measured reflections
5314 independent reflections
4359 reflections with I > 2σ(I)
R _int = 0.024

Refinement

R[F ² > 2σ(F ²)] = 0.037
wR(F ²) = 0.086
S = 1.04
5314 reflections
396 parameters
1 restraint
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.37 e Å⁻³
Δρ_min = −0.37 e Å⁻³

Data collection: APEX2 (Bruker, 2010 ▶); cell refinement: SAINT (Bruker, 2010 ▶); data reduction: SAINT (Bruker, 2010 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg & Putz, 2010 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S1600536814022806/wm5040sup1.cif

e-70-0m376-sup1.cif^{(28.9KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814022806/wm5040Isup2.hkl

e-70-0m376-Isup2.hkl^{(254.9KB, hkl)}

Click here for additional data file.^{(1.6MB, tif)}

x y z x y z x y z x y z x y z . DOI: 10.1107/S1600536814022806/wm5040fig1.tif

The extended asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 50% probability level. The disordered lattice water molecule has been omitted for clarity. [Symmetry codes: i) 2 − x, 2 − y, 1 − z; ii) 2 − x, 1 − y, 1 − z; iii) −1 + x, −1 + y, z; iv) 2 − x, 2 − y, −z; v) 1 − x, 1 − y, z.]

Click here for additional data file.^{(431.9KB, tif)}

x y z . DOI: 10.1107/S1600536814022806/wm5040fig2.tif

The tetranuclear SBU in the structure of the title compound. [Symmetry code: A) 1 − x,1 − y,-z.]

Click here for additional data file.^{(896.1KB, tif)}

L 3− . DOI: 10.1107/S1600536814022806/wm5040fig3.tif

View of the layered network formed by the SBUs and the L ³⁻ anions.

CCDC reference: 1029647

Additional supporting information: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors acknowledge the financial aid provided by the Natural Science Foundation of Jilin Province (201015168) and a project of the National Development and Reform Commission of Jilin Province.

supplementary crystallographic information

S1. Synthesis and crystallization

A mixture of cobalt acetate tetrahydrate (0.0249 g, 0.1 mmol), 5-(4-carboxyphenoxy)isophthalic acid (H₃L, 0.0151 g, 0.05 mmol), 1,4-bis[(1H-imidazol-l-yl)methyl]benzene (bix) (0.0118 g, 0.05 mmol), water (6 ml) and NaOH (aq, 0.1 molar, 2 ml) was placed in a 20 ml PTFE-lined stainless steel vessel under autogenous pressure, heated at a 413 K for 5 days, and allowed to cool down to room temperature during 30 h. The obtained crystals were collected, washed with water and ethanol, and dried under ambient conditions with a yield of 17% based on cobalt acetate.

S2. Refinement

H atoms attached to C atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with a C—H distance of 0.95 Å (aromatic) and 0.98 Å (methylene), and with U_iso(H) = 1.2U_eq(C). The H atom of the hydroxy group was located from a difference Fourier map and was refined with a distance restraint of 0.85 (2) Å. Additional electron density was found that was assigned to a lattice water molecule. Refinement of its occupancy revealed a considerable under-occupation that was fixed at 0.25 for the final refinement. H atoms of this molecule were not considered in the final model.