Tetra­aqua­bis[4-(imidazol-1-yl-κN 3)benzoato]manganese(II)

Lei Zhu; Dabin Wang; Hongyan Xu

doi:10.1107/S1600536810012638

. 2010 Apr 10;66(Pt 5):m513. doi: 10.1107/S1600536810012638

Tetraaquabis[4-(imidazol-1-yl-κN ³)benzoato]manganese(II)

Lei Zhu ^a, Dabin Wang ^b, Hongyan Xu ^b,^*

PMCID: PMC2979258 PMID: 21579010

Abstract

In the title compound, [Mn(C₁₀H₇N₂O₂)₂(H₂O)₄], the Mn^II atom, lying on an inversion center, has an octahedral environment with four coordinated water molecules in the equatorial plane and two N atoms from two 4-(imidazol-1-yl)benzoate ligands at the axial sites. The complex molecules are connected into a three-dimensional network by extensive hydrogen bonds between the water molecules and the carboxylate O atoms.

Related literature

For the good coordination ability and diverse coordination modes of ligands containing imidazole and carboxylate groups, see: Fan et al. (2004 ▶); Sun et al. (2005 ▶). For the construction of metal–organic frameworks using ligands based on imidazolyl and carboxylate groups as building blocks, see: Carlucci et al. (2008 ▶); Zhang et al. (2007 ▶).

Experimental

Crystal data

[Mn(C₁₀H₇N₂O₂)₂(H₂O)₄]
M _r = 501.36
Monoclinic,
a = 12.278 (12) Å
b = 11.026 (11) Å
c = 7.978 (7) Å
β = 96.91 (2)°
V = 1072.2 (18) Å³
Z = 2
Mo Kα radiation
μ = 0.67 mm⁻¹
T = 293 K
0.28 × 0.14 × 0.10 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.536, T _max = 1.000
7972 measured reflections
2444 independent reflections
2131 reflections with I > 2σ(I)
R _int = 0.023

Refinement

R[F ² > 2σ(F ²)] = 0.032
wR(F ²) = 0.113
S = 0.91
2444 reflections
195 parameters
All H-atom parameters refined
Δρ_max = 0.36 e Å⁻³
Δρ_min = −0.23 e Å⁻³

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; 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: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810012638/hy2292sup1.cif

e-66-0m513-sup1.cif^{(14.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810012638/hy2292Isup2.hkl

e-66-0m513-Isup2.hkl^{(120.1KB, 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
O3—H13⋯O1ⁱ	0.85 (2)	2.02 (2)	2.837 (3)	161 (2)
O3—H14⋯O2ⁱⁱ	0.79 (3)	1.90 (3)	2.688 (3)	179 (2)
O4—H11⋯O1ⁱⁱⁱ	0.90 (2)	1.82 (2)	2.702 (3)	168 (2)
O4—H12⋯O1ⁱ	0.87 (2)	1.86 (2)	2.694 (3)	158.9 (19)

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

Acknowledgments

The authors thank the National Natural Science Foundation of China and the State Key Laboratory of Structural Chemistry for financial support.

supplementary crystallographic information

Comment

Over past few years, considerable effort was paied in the study of metal-organic frameworks (MOFs) owing to their intriguing structural diversity and potential application in adsorption, molecular recognition, catalysis and maganetism. The field of molecular magnets has attracted great interest from different horizons for many years. In this context, the ligand containing imidazole and carboxylate groups is of special interest due to its good coordination ability and diverse coordination modes (Fan et al., 2004; Sun et al., 2005). However, the reports of ligands based on imidazole and carboxylate groups as building blocks for the construction of MOFs (Carlucci et al., 2008; Zhang et al., 2007) are still rare. In this paper, we report the synthesis and structural characterzation of the title compound.

As shown in Fig. 1, the molecular structure of the title compound is a momonuclear Mn^II complex and the dihedral angle between the imidazolyl ring and the benzene ring of the 4-(imidazol-1-yl)benzoate is 6.3 (2)°. The Mn^II ion is coordinated by four water molecules and two N atoms from two different 4-(imidazol-1-yl)benzoate ligands, forming a distorted octahedral coordination environment. The Mn—N and Mn—O bond distances are 2.238 (2) Å and 2.149 (2) and 2.189 (3) Å, respectively. The related hydrogen-bonding geometry is given in Table 1. A l l values involved with hydrogen bonds fall in a normal range. The intermolecular O—H···O hydrogen-bonding interactions between the coordinated water molecules and carboxylate O atoms of 4-(imidazol-1-yl)benzoate ligands lead to the formation of a three-dimensional network structure as shown in Fig. 2.

Experimental

A 10 ml aqueous solution of 4-(imidazole-1-yl)benzoic acid (0.038 g, 0.20 mmol) was slowly added into the manganese(II) perchlorate (0.663 g, 0.30 mmol) solution in methanol (10 ml). The mixed solution was stirred for 20 min and then HClO₄ solution was added dropwise with constant stirring until the mixed solution was clear. The resulting solution was filtered and the slow evaporation of filtrate in air gave rise to the desirable products, which were subsequently washed twice with Et₂O (yield 38%).