Bis(acetato-κO)[1,2-bis­(2-pyridyl­meth­oxy)benzene-κ4 N,O,O′,N′]copper(II) tetra­hydrate

Shuang Zhang; Yu-Jie Wang; Dong-Sheng Ma; Ying Liu; Jin-Sheng Gao

doi:10.1107/S1600536810021495

. 2010 Jun 16;66(Pt 7):m787. doi: 10.1107/S1600536810021495

Bis(acetato-κO)[1,2-bis(2-pyridylmethoxy)benzene-κ⁴ N,O,O′,N′]copper(II) tetrahydrate

Shuang Zhang ^a, Yu-Jie Wang ^a,^b, Dong-Sheng Ma ^b, Ying Liu ^b, Jin-Sheng Gao ^a,^b,^*

PMCID: PMC3006683 PMID: 21587712

Abstract

In the title compound, [Cu(CH₃COO)₂(C₁₈H₁₆N₂O₂)]·4H₂O, the Cu^II ion is six-coordinated in a Jahn–Teller-distorted octahedral geometry environment defined by four O atoms and two N atoms. A chain structure along [100] is built up by intermolecular O—H⋯O hydrogen bonds involving the uncoordinated water molecules.

Related literature

For the synthesis and general backround to flexible pyridyl-based ligands, see: Liu et al. (2010a ▶,b ▶). For a related structure, see: Zhang et al. (2010 ▶)

Experimental

Crystal data

[Cu(C₂H₃O₂)₂(C₁₈H₁₆N₂O₂)]·4H₂O
M _r = 545.02
Triclinic,
a = 8.0192 (16) Å
b = 11.291 (2) Å
c = 14.117 (3) Å
α = 102.97 (3)°
β = 92.69 (3)°
γ = 93.70 (3)°
V = 1240.5 (4) Å³
Z = 2
Mo Kα radiation
μ = 0.94 mm⁻¹
T = 291 K
0.37 × 0.15 × 0.14 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.726, T _max = 0.880
12216 measured reflections
5621 independent reflections
4677 reflections with I > 2σ(I)
R _int = 0.043

Refinement

R[F ² > 2σ(F ²)] = 0.056
wR(F ²) = 0.169
S = 1.05
5621 reflections
318 parameters
H-atom parameters constrained
Δρ_max = 1.14 e Å⁻³
Δρ_min = −0.44 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810021495/ng2782sup1.cif

e-66-0m787-sup1.cif^{(21.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810021495/ng2782Isup2.hkl

e-66-0m787-Isup2.hkl^{(275.2KB, 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
O10—H67⋯O6ⁱ	0.85	2.40	3.072 (6)	137
O10—H66⋯O9	0.85	2.07	2.913 (6)	169
O9—H64⋯O8ⁱⁱ	0.85	2.26	2.955 (6)	139
O9—H65⋯O8	0.85	2.09	2.828 (6)	145
O8—H63⋯O7ⁱⁱⁱ	0.85	2.06	2.874 (5)	162
O8—H62⋯O7	0.85	1.94	2.784 (5)	176
O7—H61⋯O6^iv	0.85	1.91	2.755 (4)	177
O7—H60⋯O4	0.85	1.94	2.784 (5)	172

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

Acknowledgments

The authors thank the Special Funds for the Research of Scientific and Technological Innovative Talents of Harbin Municipal Science and Technology Bureau (2006RFQXG093, 2009RFXXG027), the Science and Technology Planning Project of Heilongjiang Province (GZ08A401) and Heilongjiang University for supporting this study.

supplementary crystallographic information

Comment

N-Heterocyclic ligands coordinated with transition metal ions can form a variety of topology structures, including macrocycles, polyhedra and linear and helical polymers. Our group has report three kinds of flexible pyridyl-based ligands in previous reports (Liu et al. 20010a; Liu et al. 20010b). As a part of our continuing work for bipyridyl aromatic ligands, we report the crystal structure of the title compound here, and its analogous monohydrate compound also has been reported by our group (Zhang et al. 20010).

1,2-Bis(pyridin-2-ylmethoxy)benzene molecule act as a chelating ligand to coordinate with Cu^II ion forming a discrete strucutre. Two acetate counter ions also coordinate to the center Cu^II ion, resulting the Cu^II ion is six-coordinated in quadrangular bipyramid geometry (Figure 1, Table 1).

A one-dimensional chain structure along [100] direction is built up by intermolecular hydrogen bonds involving the uncoordinated water molecules (Figure 2, Table 2).

Experimental

The 1,2-Bis(pyridin-2-ylmethoxy)benzene was synthesized by the reaction of ο-dihydroxybenzene and 2-chloromethylpyridine hydrochloride under nitrogen atmosphere and alkaline condition (Liu et al., 2010a). Title ligand (0.58 g, 2 mmol) and Cu(CH₃COO)₂.H₂O (0.40 g, 2 mmol) were dissolved in 15 ml e thanol, and then the mixture keep stirring for 30 minute. The resulting solution was filtered, and the filtrate was allowed to stand in a desiccator at room temperature for several days. Bule needle crystals were obtained.