Bis[μ-3-(2-hydroxy­ethyl)-2-methyl-4-oxo-4H-pyrido[1,2-a]pyrimidin-9-olato-κ3 N,O:O]bis[aquachloridocopper(II)]

Ying Deng; Zhong-Shu Li; Bai-Wang Sun

doi:10.1107/S1600536808028687

. 2008 Sep 13;64(Pt 10):m1262. doi: 10.1107/S1600536808028687

Bis[μ-3-(2-hydroxyethyl)-2-methyl-4-oxo-4H-pyrido[1,2-a]pyrimidin-9-olato-κ³ N,O:O]bis[aquachloridocopper(II)]

Ying Deng ^a, Zhong-Shu Li ^a, Bai-Wang Sun ^a,^*

PMCID: PMC2959477 PMID: 21201016

Abstract

In the dinuclear centrosymmetric copper(II) title compound, [Cu₂(C₁₁H₁₁N₂O₂)₂Cl₂(H₂O)₂], each Cu^II ion has a slightly distorted trigonal-bipyramidal geometry and is coordinated by one N and one O atom from one 3-(2-hydroxyethyl)-2-methyl-4-oxopyrido[1,2-a]pyrimidin-9-olate ligand, another O atom from the second ligand, one water molecule and one Cl atom. The crystal structure involves intermolecular C—H⋯Cl, O—H⋯Cl and O—H⋯O hydrogen bonds

Related literature

For related literature, see: Bayot et al. (2006 ▶); Chen et al. (2007 ▶); Sun et al. (2008 ▶); Wu et al. (2006 ▶).

Experimental

Crystal data

[Cu₂(C₁₁H₁₁N₂O₂)₂Cl₂(H₂O)₂]
M _r = 672.45
Monoclinic,
a = 9.391 (3) Å
b = 11.322 (3) Å
c = 11.905 (4) Å
β = 102.414 (18)°
V = 1236.2 (6) Å³
Z = 2
Mo Kα radiation
μ = 1.99 mm⁻¹
T = 293 (2) K
0.25 × 0.12 × 0.08 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T _min = 0.890, T _max = 1.000 (expected range = 0.759–0.853)
12472 measured reflections
2826 independent reflections
2249 reflections with I > 2σ(I)
R _int = 0.056

Refinement

R[F ² > 2σ(F ²)] = 0.045
wR(F ²) = 0.115
S = 1.01
2826 reflections
176 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.49 e Å⁻³
Δρ_min = −0.47 e Å⁻³

Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; 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/S1600536808028687/sg2256sup1.cif

e-64-m1262-sup1.cif^{(19.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808028687/sg2256Isup2.hkl

e-64-m1262-Isup2.hkl^{(138.8KB, 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—H5C⋯O2ⁱ	0.82	2.13	2.742 (4)	131
O5—H5D⋯O1ⁱⁱ	0.96	2.11	2.788 (4)	127
O2—H2A⋯Cl1ⁱⁱⁱ	0.75 (6)	2.37 (6)	3.078 (4)	158 (6)
C9—H9A⋯Cl1	0.96	2.49	3.275 (4)	139
C3—H3A⋯Cl1^iv	0.93	2.72	3.387 (4)	130

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

supplementary crystallographic information

Comment

In the past decade, much attention has been paid to the design and synthesis of self-assembling systems with organic ligands containing N and O donors (Bayot et al., 2006; Chen et al., 2007). Quinolin-8-ol is one such ligand and several crystal structures of complexes containing it have been reported (Wu et al., 2006). Our group has recently reported a new manganese compound with this 3-(2-hydroxyethyl)-2-methyl-4-oxopyrido[1,2-a]pyrimidin-9-olate ligands (Sun et al., 2008). We report here the synthesis and crystal structure of the title complex, (I) (Fig. 1). In (I), each Cu(II) ion has a slightly distorted trigonal–bipyramidal geometry and is coordinated by one N atoms and one O atom from one 3-(2-hydroxyethyl)-2-methyl-4-oxopyrido[1,2-a]pyrimidin-9-olate ligand, the another O atom of the second 3-(2-hydroxyethyl)-2-methyl-4-oxopyrido[1,2-a]pyrimidin-9-olate ligand, together with one water molecule and one Cl atom (Fig. 1). The bond lengths and angles are shown in Table 1. In the crystal structure, the intermolecular O—H···O hydrogen bonds connect the molecules of (I) into a two-dimensional layer along the [010] axis, Fig. 2. Two neighboring net framework layers are interconnected through intermolecular C—H···Cl, O—H···Cl hydrogen bonds forming a three-dimensionnal framework along the [100] axis, Fig. 3, Table 2.

Experimental

All chemicals used (reagent grade) were commercially available. a aqueous solution (5 ml) of CuCl₂ (28 mg, 0.1 mmol) was added with constant stirring to a ethanol solution (10 ml) containing 3-(2-hydroxyethyl)-2-methyl-9-hydroxylpyrido[1,2-a] pyrimidin-4-one (22 mg, 0.1 mmol) then filtered off. After a few days, colorless well shaped single crystals in the form of prisms deposited in the other liquid. They were separated off, washed with cold ethanol and dried in air at room temperature.