Bis[μ-2-(2-carboxyl­atophen­yl)acetato]-κ3 O 1,O 1′:O 2;κ3 O 2:O 1,O 1′-bis­[aqua­(1,10-phenanthroline-κ2 N,N′)nickel(II)]

Feng Li; Huifang Zeng; Zhaowei Yan; Taohai Li

doi:10.1107/S1600536809018339

. 2009 May 23;65(Pt 6):m681. doi: 10.1107/S1600536809018339

Bis[μ-2-(2-carboxylatophenyl)acetato]-κ³ O ¹,O ^1′:O ²;κ³ O ²:O ¹,O ^1′-bis[aqua(1,10-phenanthroline-κ² N,N′)nickel(II)]

Feng Li ^a, Huifang Zeng ^a, Zhaowei Yan ^a, Taohai Li ^a,^*

PMCID: PMC2969824 PMID: 21583040

Abstract

The title compound, [Ni₂(C₉H₆O₄)₂(C₁₂H₈N₂)₂(H₂O)₂], is isostructural with the Zn^II analogue. Each Ni^II atom is coordinated in a distorted octahedral geometry by three O atoms from two homophthalate anions, one aqua O atom and two 1,10-phenanthroline N atoms. The two Ni^II atoms are linked by two bridging homophthalate dianions into a centrosymmetric dinuclear unit. The dinuclear units are linked into one-dimensional ladder-like chains along [100] by O—H⋯O hydrogen bonds between the coordinated water molecules and one of the O atoms of the carboxylatomethyl group.

Related literature

For the Zn^II analogue, see: He et al. (2006 ▶); Sun (2006 ▶).

Experimental

Crystal data

[Ni₂(C₉H₆O₄)₂(C₁₂H₈N₂)₂(H₂O)₂]
M _r = 870.14
Monoclinic,
a = 8.819 (3) Å
b = 19.432 (6) Å
c = 12.898 (3) Å
β = 122.900 (17)°
V = 1855.8 (10) Å³
Z = 2
Mo Kα radiation
μ = 1.08 mm⁻¹
T = 173 K
0.45 × 0.40 × 0.20 mm

Data collection

Rigaku Mercury70 CCD diffractometer
Absorption correction: multi-scan (CrystalClear; Molecular Structure Corporation & Rigaku, 2001 ▶) T _min = 0.618, T _max = 0.806
14201 measured reflections
4232 independent reflections
3900 reflections with I > 2σ(I)
R _int = 0.021

Refinement

R[F ² > 2σ(F ²)] = 0.032
wR(F ²) = 0.083
S = 1.05
4232 reflections
262 parameters
H-atom parameters constrained
Δρ_max = 0.43 e Å⁻³
Δρ_min = −0.35 e Å⁻³

Data collection: CrystalClear (Molecular Structure Corporation & Rigaku, 2001 ▶); 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/S1600536809018339/bi2368sup1.cif

e-65-0m681-sup1.cif^{(23.6KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809018339/bi2368Isup2.hkl

e-65-0m681-Isup2.hkl^{(207.4KB, 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
O1W—H1WA⋯O1ⁱ	0.84	1.87	2.653 (2)	155
O1W—H1WB⋯O4ⁱⁱ	0.83	1.88	2.7108 (17)	175

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

supplementary crystallographic information

Comment

The title compound is isostructural with its Zn^II analogue (He et al., 2006; Sun, 2006). The asymmetric unit consitsts of one Ni^II atom, one 1,10-phenanthroline (phen) ligan, one homophthalate dianion (hpht^2-) and a coordinated water molecule. The Ni^II atom is six-coordinated by two N atoms from phen and four O atoms, three from two hpht^2- anions and one from coordinated H₂O, in a distorted octahedron coordination geometry (Table 1). In the hpht^2- ligand, the carboxylate group coordinates in a monodentate manner to Ni^II while the ethylcarboxylate group coordinates in a bidentate manner to another Ni^II atom. Two hpht^2- ions link two Ni^II atoms to form a dinuclear complex across a centre of inversion. Such units are linked to form one-dimensional ladder-like chains along [100] by O—H···O hydrogen bonds from the coordinated water molecule to one of ethylcarboxyl O atoms. π–π interactions are formed between phen units in adjacent chains.

Experimental

Homophthalic acid (H₂hpht; 0.0275 g, 0.15 mmol), 1,10-phenanthroline (phen; 0.030 g, 0.15 mmol) and Ni(NO₃)₂.6H₂O (0.044 g, 0.15 mmol) were put in 10 ml distilled H₂O and the pH was adjusted to about 4.2 by addind dilute NaOH aqueous solution. The mixture was sealed in a 25 ml Teflon-lined autoclave and heated to 433 K for 3 days, then slowly cooled to room temperature. Red prism crystals were collected and washed with distilled water (yield: 51%)