Hexa-μ2-acetato-1:2κ4 O:O′;1:2κ2 O:O;2:3κ4 O:O′;2:3κ2 O:O-bis­(2-amino-7-chloro-5-methyl-1,8-naphthyridine)-1κN 1,3κN 1-trizinc(II)

Xin-Sheng Li; Juan Mo; Li Yuan; Jian-Hua Liu; Su-Mei Zhang

doi:10.1107/S1600536808024549

. 2008 Aug 6;64(Pt 9):m1128. doi: 10.1107/S1600536808024549

Hexa-μ₂-acetato-1:2κ⁴ O:O′;1:2κ² O:O;2:3κ⁴ O:O′;2:3κ² O:O-bis(2-amino-7-chloro-5-methyl-1,8-naphthyridine)-1κN ¹,3κN ¹-trizinc(II)

Xin-Sheng Li ^a, Juan Mo ^a,^*, Li Yuan ^a, Jian-Hua Liu ^a, Su-Mei Zhang ^a

PMCID: PMC2960502 PMID: 21201587

Abstract

The title complex, [Zn₃(C₂H₃O₂)₆(C₉H₈ClN₃)₂], contains three Zn^II atoms bridged by six acetate ligands. The central Zn^II ion, located on an inversion centre, is surrounded by six O atoms from acetate ligands in a distorted octahedral geometry [Zn—O = 1.9588 (12)–2.1237 (12) Å]. The terminal Zn^II ions are coordinated by one N atom of 2-amino-7-chloro-5-methyl-1,8-naphthyridine and three O atoms of three acetate ligands in a distorted tetrahedral geometry. The separation between the central and terminal Zn^II ions is 3.245 (3) Å.

Related literature

For related literature, see: Baker & Norman (2004 ▶); Lis et al. (2005 ▶); Stadie et al. (2007 ▶).

Experimental

Crystal data

[Zn₃(C₂H₃O₂)₆(C₉H₈ClN₃)₂]
M _r = 937.64
Triclinic,
a = 9.1978 (12) Å
b = 9.2108 (13) Å
c = 12.0457 (16) Å
α = 93.602 (3)°
β = 91.685 (2)°
γ = 118.247 (2)°
V = 895.2 (2) Å³
Z = 1
Mo Kα radiation
μ = 2.21 mm⁻¹
T = 113 (2) K
0.12 × 0.08 × 0.02 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.782, T _max = 0.956
11008 measured reflections
4221 independent reflections
3495 reflections with I > 2σ(I)
R _int = 0.030

Refinement

R[F ² > 2σ(F ²)] = 0.024
wR(F ²) = 0.065
S = 1.01
4221 reflections
253 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.36 e Å⁻³
Δρ_min = −0.65 e Å⁻³

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; 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 ▶); software used to prepare material for publication: XP in SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808024549/hg2413sup1.cif

e-64-m1128-sup1.cif^{(22.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808024549/hg2413Isup2.hkl

e-64-m1128-Isup2.hkl^{(206.8KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Zn1—O3	2.0724 (12)
Zn1—O5	2.0910 (12)
Zn1—O1	2.1237 (12)
Zn2—O3	1.9588 (12)
Zn2—O2	1.9748 (12)
Zn2—N2	2.0379 (14)

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O3—Zn1—O5ⁱ	91.21 (5)
O3—Zn1—O5	88.79 (5)
O3—Zn1—O1ⁱ	89.96 (5)
O5—Zn1—O1ⁱ	93.21 (5)
O3—Zn1—O1	90.04 (5)
O5—Zn1—O1	86.79 (5)

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Symmetry code: (i) Inline graphic .

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H3B⋯O2	0.85 (2)	2.15 (2)	2.921 (2)	150.0 (17)
N3—H3A⋯O5ⁱⁱ	0.87 (2)	2.09 (2)	2.958 (2)	171.0 (19)

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Symmetry code: (ii) Inline graphic .

Acknowledgments

We thank Henan Agricultural University for the generous support of this study.

supplementary crystallographic information

Comment

Acetic acid is versatile ligand which can function in monodentate or bidentate modes in metal complexes (Baker & Norman, 2004; Lis et al., 2005; Stadie et al., 2007). Here, we report the crystal structure of the title compound, (I), in which three Zn^II ions are bridged by three acetic acid ligands.

The middle Zn atom in (I) (Fig. 1) has a distorted octahedral coordination geometry involving six O atoms of six acetic acid ligands. The Zn—O bonds lengths are between 1.9588 (12) and 2.1237 (12)Å (Table 1). The End Zn^II ion is coordinated by one N atom of 2-amino-4-methyl-7-chloro-1,8-naphthyridine and three O atoms of three acetic acid ligands, and has a distorted tetrahedron coordination geometry. The distance of two neighboring Zn^II ions separated by two O atoms of each two acetate bridging ligands and one O atoms of one acetate bridging ligand is 3.245 (3) Å.

Experimental

A 10 ml dichloromethane solution of 2-amino-5-methyl-7-chloro-1,8-naphthyridine (0.039 g, 0.2 mmol) was added to a 20 mL dichloromethane solution of Zn(CH₃COO)₂ (0.055 g, 0.3 mmol) under an N₂ atmosphere. The mixture was stirred for 10 h. Colorless crystals suitable for X-ray diffraction were formed by vapour diffusion of diethyl ethyl ether into dichloromethane solution.