Bis[μ-4-(4-carb­oxy­phen­oxy)phthalato]bis­[triaqua­nickel(II)]

Xue Cai

doi:10.1107/S1600536810049718

. 2010 Dec 11;67(Pt 1):m60. doi: 10.1107/S1600536810049718

Bis[μ-4-(4-carboxyphenoxy)phthalato]bis[triaquanickel(II)]

Xue Cai ^a,^*

PMCID: PMC3050356 PMID: 21522579

Abstract

In the centrosymmetric binuclear title compound, [Ni₂(C₁₅H₈O₇)₂(H₂O)₆], the Ni^II ion is in a distorted octahedral coordination geometry with O₆ donors, three from three water molecules, the others from three carboxylate groups of two ligands. Extensive O—H⋯O hydrogen bonding connects the molecules into a three-dimensional supramolecular structure.

Related literature

For metal-organic coordination polymers, see: Evans et al. (1999 ▶); Li et al. (2008 ▶). For related structures, see: Wang et al. (2010 ▶); Hökelek et al. (2009 ▶).

Experimental

Crystal data

[Ni₂(C₁₅H₈O₇)₂(H₂O)₆]
M _r = 825.90
Monoclinic,
a = 14.4173 (9) Å
b = 9.5002 (6) Å
c = 11.2857 (7) Å
β = 92.632 (1)°
V = 1544.14 (17) Å³
Z = 2
Mo Kα radiation
μ = 1.32 mm⁻¹
T = 298 K
0.18 × 0.12 × 0.05 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) ▶ T _min = 0.798, T _max = 0.937
7457 measured reflections
2716 independent reflections
2245 reflections with I > 2σ(I)
R _int = 0.030

Refinement

R[F ² > 2σ(F ²)] = 0.030
wR(F ²) = 0.069
S = 1.02
2716 reflections
263 parameters
10 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.28 e Å⁻³
Δρ_min = −0.31 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP (Sheldrick, 1998 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810049718/ds2071sup1.cif

e-67-00m60-sup1.cif^{(17.6KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810049718/ds2071Isup2.hkl

e-67-00m60-Isup2.hkl^{(130.6KB, 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
O6—H6A⋯O1ⁱ	0.85 (1)	1.73 (1)	2.579 (3)	176 (4)
O8—H8A⋯O10ⁱⁱ	0.85 (1)	2.41 (3)	2.967 (3)	124 (3)
O8—H8B⋯O2ⁱⁱⁱ	0.86 (1)	2.07 (2)	2.841 (3)	150 (4)
O9—H9B⋯O3^iv	0.84 (1)	2.14 (2)	2.889 (2)	149 (3)
O8—H8A⋯O7^v	0.85 (1)	2.12 (2)	2.867 (3)	146 (3)
O10—H10B⋯O1^vi	0.84 (1)	1.96 (1)	2.770 (3)	164 (3)

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

Acknowledgments

The project was supported by the Excellent Young Scholars of Higher University of Heilongjiang Province, China (1155G57), the Natural Science Foundation of Heilongjiang Province, China (B201016), the Doctoral Research Fund of Mudanjiang Teachers College, China (MSB: 200902) and the Research Fund of Mudanjiang Teachers College, China (KY: 200902).

supplementary crystallographic information

Comment

In the field of supramolecular chemistry and crystal engineering, the design and assembly of metal-organic coordination polymers with appealing structures and properties have stimulated interests of chemists (Evans et al., 1999). The hydrogen bonding interaction often leads to complicated spramolecular structure (Li et al., 2008).

As shown in Fig.1, compound I is a new binuclear neutral complex with a shuttle molecular configuration. The two Ni(II) ions locate in the middle of this molecule. Ni(II) atom is coordinated in a octahedral coordination sphere The bond lengths of Ni—O are similar with the values in those complexes containing Ni—O sgment (Wang et al., 2010). There are rich hydrogen bonding interaction O—H···O in this compound, giving a three-dimensional supramolecular structure.

Experimental

H3L4 (0.0302 g, 0.1 mmol), Ni(OAc)₂.4H₂O (0.0498 g, 0.2 mmol), and H2O (15 ml) was sealed in 25 ml Teflon-lined stainless steel reactor and heated to 120 ^oC. Green block-shaped crystals suitable for X-ray diffraction analysis were separated by filtration with the yield of 37%