Penta­aqua­(1H-benzimidazole-5,6-di­carboxyl­ato-κN 3)cobalt(II) penta­hydrate

Wen-Dong Song; Hao Wang; Shi-Jie Li; Pei-Wen Qin; Shi-Wei Hu

doi:10.1107/S1600536809019904

. 2009 May 29;65(Pt 6):m702. doi: 10.1107/S1600536809019904

Pentaaqua(1H-benzimidazole-5,6-dicarboxylato-κN ³)cobalt(II) pentahydrate

Wen-Dong Song ^a,^*, Hao Wang ^a, Shi-Jie Li ^a, Pei-Wen Qin ^a, Shi-Wei Hu ^a

PMCID: PMC2969642 PMID: 21583056

Abstract

In the title mononuclear complex, [Co(C₉H₄N₂O₄)(H₂O)₅]·5H₂O, the Co^II atom exhibits a distorted octahedral geometry involving an N atom of a 1H-benzimidazole-5,6-dicarboxylate ligand and five water O atoms. A supramolecular network is generated through intermolecular O—H⋯O hydrogen-bonding interactions involving the coordinated and uncoordinated water molecules and the carboxyl O atoms of the organic ligand. An intermolecular N—H⋯O hydrogen bond is also observed.

Related literature

For the crystal structures of related compounds, see: Gao et al. (2008 ▶); Lo et al. (2007 ▶); Yao et al. (2008 ▶).

Experimental

Crystal data

[Co(C₉H₄N₂O₄)(H₂O)₅]·5H₂O
M _r = 443.23
Triclinic,
a = 6.8454 (14) Å
b = 11.480 (2) Å
c = 12.408 (3) Å
α = 78.02 (3)°
β = 78.57 (3)°
γ = 74.80 (3)°
V = 909.7 (4) Å³
Z = 2
Mo Kα radiation
μ = 1.02 mm⁻¹
T = 293 K
0.31 × 0.26 × 0.21 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T _min = 0.744, T _max = 0.815
7307 measured reflections
3269 independent reflections
2010 reflections with I > 2σ(I)
R _int = 0.050

Refinement

R[F ² > 2σ(F ²)] = 0.048
wR(F ²) = 0.148
S = 1.19
3269 reflections
235 parameters
30 restraints
H-atom parameters constrained
Δρ_max = 0.85 e Å⁻³
Δρ_min = −1.00 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPII (Johnson, 1976 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809019904/rz2326sup1.cif

e-65-0m702-sup1.cif^{(18.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809019904/rz2326Isup2.hkl

e-65-0m702-Isup2.hkl^{(160.3KB, 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
N2—H2⋯O10Wⁱ	0.86	1.99	2.822 (8)	162
O1W—H1W⋯O3ⁱⁱ	0.84	1.78	2.603 (7)	169
O1W—H2W⋯O6Wⁱⁱⁱ	0.84	1.95	2.789 (9)	175
O2W—H4W⋯O8W	0.84	1.90	2.726 (9)	165
O2W—H3W⋯O4ⁱⁱ	0.84	1.78	2.614 (7)	173
O3W—H5W⋯O10W^iv	0.84	1.93	2.752 (8)	167
O3W—H6W⋯O6W^v	0.84	1.92	2.758 (8)	177
O4W—H7W⋯O7Wⁱⁱⁱ	0.84	2.05	2.827 (7)	154
O4W—H8W⋯O1^iv	0.84	1.96	2.801 (8)	176
O5W—H9W⋯O7W	0.84	1.92	2.734 (9)	162
O5W—H10W⋯O2^vi	0.84	1.88	2.700 (7)	164
O6W—H12W⋯O1^vi	0.84	1.98	2.812 (6)	171
O6W—H11W⋯O2W	0.84	2.06	2.865 (6)	161
O7W—H13W⋯O8W	0.84	1.89	2.721 (8)	168
O7W—H14W⋯O2ⁱ	0.84	1.91	2.737 (8)	168
O8W—H15W⋯O1W^vii	0.84	2.05	2.860 (7)	163
O8W—H16W⋯O9W	0.84	1.88	2.699 (7)	166
O9W—H17W⋯O4^vii	0.84	1.93	2.766 (9)	172
O9W—H18W⋯O3	0.84	1.93	2.771 (8)	175
O10W—H20W⋯O1	0.87	1.89	2.747 (7)	168
O10W—H19W⋯O2^vii	0.87	2.54	3.191 (9)	133

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

Acknowledgments

The authors acknowledge Guang Dong Ocean University for support of this work.

supplementary crystallographic information

Comment

In the structural investigation of 1H-benzimidazole-5,6-dicarboxylate complexes, it has been found that the 1H-benzimidazole-5,6-dicarboxylic acid can function as a multidentate ligand (Gao et al., 2008; Lo et al., 2007; Yao et al., 2008), with versatile binding and coordination modes. In this paper, we report the crystal structure of the title compound, a new cobalt(II) complex obtained by the reaction of the 1H-benzimidazole-5,6-dicarboxylic acid and cobalt chloride in alkaline aqueous solution.

As illustrated in Figure 1, the cobalt(II) atom is six-coordinated by one N atom from a 1H-benzimidazole-5,6-dicarboxylate ligand and five O atoms from five water molecules, displaying a distorted octahedral geometry. The O1/O2/C7 and O3/O4/C8 carboxylate groups are tilted with respect to the plane of the benzimidazole ring system by 36.0 (3) and 68.1 (2)°, respectively. Intermolecular O—H···O hydrogen bonding interactions (Table 1) form a three-dimensional supramolecular network involving the coordinated and uncoordinated water molecules as donors and the carboxylate O atoms of the organic ligand as acceptors (Fig. 2). An intermolecular N—H···O hydrogen bond is also observed.

Experimental

A mixture of cobalt chloride (1 mmol), 1H-benzimidazole-5,6-dicarboxylic acid (1 mmol), NaOH (1.5 mmol) and H₂O (12 ml) was placed in a 23 ml Teflon reactor, heated to 433 K for three days and then cooled to room temperature at a rate of 10 K h^-1. The crystals obtained were washed with water and dryed in air.