Poly[[(μ3-5,6-dicarboxy­bicyclo­[2.2.2]oct-7-ene-2,3-dicarboxyl­ato)(1,10-phenanthroline)copper(II)] monohydrate]

Yun-Yu Liu; Yu-Jiang Zhuo; Xing-Qi Li; Ji-Cheng Ma

doi:10.1107/S1600536808037999

. 2008 Nov 22;64(Pt 12):m1590. doi: 10.1107/S1600536808037999

Poly[[(μ₃-5,6-dicarboxybicyclo[2.2.2]oct-7-ene-2,3-dicarboxylato)(1,10-phenanthroline)copper(II)] monohydrate]

Yun-Yu Liu ^a,^*, Yu-Jiang Zhuo ^a, Xing-Qi Li ^a, Ji-Cheng Ma ^a

PMCID: PMC2960067 PMID: 21581190

Abstract

In the title compound, {[Cu(C₁₂H₁₀O₈)(C₁₂H₈N₂)]·H₂O}_n, the Cu^II ion is five-coordinated by two N atoms from one phenanthroline ligand and three O atoms from three different H₂ L ²⁻ anions (H₄ L is bicyclo[2.2.2]oct-7-ene-2,3,5,6-tetracarboxylic acid) in a distorted square-pyramidal geometry. Each H₂ L ²⁻ ion bridges three Cu^II atoms to form a zigzag sheet parallel to the ab plane. The crystal structure is consolidated by O—H⋯O hydrogen bonds.

Related literature

For general background, see: Yang et al. (2008 ▶).

Experimental

Crystal data

[Cu(C₁₂H₁₀O₈)(C₁₂H₈N₂)]·H₂O
M _r = 543.96
Monoclinic,
a = 6.5900 (4) Å
b = 15.1650 (8) Å
c = 10.7490 (6) Å
β = 95.244 (9)°
V = 1069.73 (10) Å³
Z = 2
Mo Kα radiation
μ = 1.08 mm⁻¹
T = 293 (2) K
0.33 × 0.21 × 0.20 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.696, T _max = 0.803
6580 measured reflections
4555 independent reflections
4343 reflections with I > 2σ(I)
R _int = 0.022

Refinement

R[F ² > 2σ(F ²)] = 0.026
wR(F ²) = 0.065
S = 1.04
4555 reflections
333 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.31 e Å⁻³
Δρ_min = −0.37 e Å⁻³
Absolute structure: Flack (1983 ▶), 1914 Friedel pairs
Flack parameter: 0.008 (8)

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SAINT (Bruker, 1998 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL-Plus (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL-Plus (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808037999/ci2718sup1.cif

e-64-m1590-sup1.cif^{(25.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808037999/ci2718Isup2.hkl

e-64-m1590-Isup2.hkl^{(218.6KB, hkl)}

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

Table 1. Selected bond lengths (Å).

N1—Cu1	2.0072 (17)
N2—Cu1	2.0119 (19)
O2—Cu1	1.9640 (15)
Cu1—O3ⁱ	1.9355 (15)
Cu1—O7ⁱⁱ	2.3398 (18)

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

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯O1W	0.82	1.84	2.567 (2)	148
O8—H8⋯O2ⁱⁱⁱ	0.82	1.79	2.594 (2)	166
O1W—HW11⋯O4^iv	0.82 (3)	1.97 (3)	2.777 (3)	167 (3)
O1W—HW12⋯O1^v	0.82 (2)	2.05 (3)	2.763 (3)	145 (4)

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Symmetry codes: (iii) Inline graphic ; (iv) ; (v) .

Acknowledgments

The authors thank the Science Foundation for Young Teachers of Northeast Normal University (grant Nos. 20080305 and 20080304) for financial support.

supplementary crystallographic information

Comment

Coordination polymers based on poly(carboxylic acids) have been investigated in the area of solid state and material science (Yang et al., 2008). We selected bicyclo[2.2.2]oct-7-ene-2,3,5,6-tetracarboxylic acid (H₄L) as a poly(carboxylic acid) ligand and phenanthroline (phen) as a secondary ligand, generating a new coordination polymer, [Cu(phen)(H₂L)]^.H₂O, which is reported here.

In the title compound, each Cu^II atom is five-coordinated by two N atoms from one phen ligand, and three O atoms from three different H₂L^2- anions in a distorted square-pyramidal geometry (Fig. 1 and Table 1). Each H₂L^2- bridges three Cu^II atoms to form a two-dimensional layer structure (Fig. 2). The O–H···O hydrogen bonds (Table 2) further consolidate the crystal structure.

Experimental

A mixture of H₄L (0.5 mmol), phen (0.5 mmol), NaOH (1 mmol) and CuCl₂^.2H₂O (0.5 mmol) was suspended in deionized water (12 ml) and sealed in a 20-ml Teflon-lined autoclave. The mixture was heated at 373 K for 7 d and then the autoclave was slowly cooled to room temperature. The grown single crystals were collected, washed with deionized water and dried.