catena-Poly[[diaqua­[1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-1,4-dihydro­quinoline-3-carboxyl­ato-κ2 O,O′]nickel(II)]-μ-4,4′-oxydibenzoato-κ2 O:O′]

Jun Hong

doi:10.1107/S1600536807062216

. 2007 Dec 6;64(Pt 1):m17. doi: 10.1107/S1600536807062216

catena-Poly[[diaqua[1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-1,4-dihydroquinoline-3-carboxylato-κ² O,O′]nickel(II)]-μ-4,4′-oxydibenzoato-κ² O:O′]

Jun Hong ^a,^*

PMCID: PMC2914909 PMID: 21200518

Abstract

In the title compound, [Ni(C₁₆H₁₈FN₃O₃)(C₁₄H₈O₅)(H₂O)₂]_n, the Ni^II atom exhibits a distorted octahedral geometry that is defined by four O atoms and two water molecules. Ni atoms are connected via the 4,4′-oxydibenzoate anions into a one-dimensional chain running along the crystallographic [ Inline graphic 30] direction. In the crystal structure, the one-dimensional chains are connected via N—H⋯O and O—H⋯O hydrogen bonding to form a three-dimensional supramolecular network.

Related literature

For general background, see: Xiao et al. (2005 ▶). For a related structure, see: An et al. (2005 ▶).

Experimental

Crystal data

[Ni(C₁₆H₁₈FN₃O₃)(C₁₄H₈O₅)(H₂O)₂]
M _r = 670.28
Triclinic,
a = 10.105 (2) Å
b = 12.230 (2) Å
c = 13.052 (3) Å
α = 72.50 (3)°
β = 73.13 (3)°
γ = 77.57 (3)°
V = 1457.7 (5) Å³
Z = 2
Mo Kα radiation
μ = 0.74 mm⁻¹
T = 298 (2) K
0.32 × 0.24 × 0.22 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.798, T _max = 0.855
11571 measured reflections
5134 independent reflections
4210 reflections with I > 2σ(I)
R _int = 0.027

Refinement

R[F ² > 2σ(F ²)] = 0.040
wR(F ²) = 0.112
S = 1.02
5134 reflections
406 parameters
H-atom parameters constrained
Δρ_max = 0.73 e Å⁻³
Δρ_min = −0.42 e Å⁻³

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL-Plus (Sheldrick, 1990 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807062216/im2047sup1.cif

e-64-00m17-sup1.cif^{(24KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807062216/im2047Isup2.hkl

e-64-00m17-Isup2.hkl^{(251.4KB, 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
O2W—H4⋯O2	0.85	1.93	2.695 (3)	149
O2W—H4⋯O1	0.85	2.55	2.965 (3)	111
N3—H3B⋯O2ⁱ	0.90	1.82	2.714 (3)	170
N3—H3C⋯O8ⁱⁱ	0.90	1.85	2.719 (3)	162
O1W—H1⋯O1ⁱⁱⁱ	0.85	2.03	2.761 (3)	144
O1W—H2⋯O4^iv	0.85	1.99	2.834 (3)	173
O2W—H3⋯O5^v	0.85	1.82	2.615 (3)	155

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

Acknowledgments

The author thanks Jilin Normal University for supporting this work.

supplementary crystallographic information

Comment

Norfloxacin [1-Ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(piperazin-1-yl)quinoline-3-carboxylic acid, Hcf] is a member of a class of quinolones that is used to treat infections (Xiao et al. 2005; An et al. 2005), As a part of our ongoing investigations in this field we report here the crystal structure of the title compound. In the crystal structure of the title compound, the Ni atoms are coordinated by three oxygen atoms of two Hcf ligand and one 4,4'-oxy-bisbenzoate, one oxygen atom from one symmetry related 4,4'-oxy-bisbenzoate and two water molecules within a distorted octahedral geometry (Figure 1). The nickel atoms are linked by the 4,4'-oxy-bisbenzoate anions into a one-dimensional chain running along crystallographic [-1, 1.5, 0] direction. The adjacent chains are further extended into a two-dimensional supramolecular network by N—H···O and O—H···O hydrogen bonds(Tab. 1).

Experimental

Compound (I) was prepared by a hydrothermal method. A mixture of Ni(NO₃)₂.6H₂O (0.15 g 0.5 mmol), norfloxacin (0.16 g 0.5 mmol), 4,4'-oxy-bisbenzoic acid (0.13 g 0.5 mmol) and water (10 ml) was stirred for 20 min and then transferred to a 23 ml Teflon reactor. The reactor was kept at 433 K for 72 h under autogenous pressure. Single crystals of (I) were obtained after cooling to room temperature.