Poly[[aqua­(μ5-1H-benzimidazole-5,6-dicarboxyl­ato)(μ4-1H-benzimidazole-5,6-dicarboxyl­ato)dibarium] 4.5-hydrate]

Heng-Qiang Zhang; Xiu-Jun Zheng; Chun-Xiang Zhao; Seik Weng Ng

doi:10.1107/S160053681101590X

. 2011 May 7;67(Pt 6):m671–m672. doi: 10.1107/S160053681101590X

Poly[[aqua(μ₅-1H-benzimidazole-5,6-dicarboxylato)(μ₄-1H-benzimidazole-5,6-dicarboxylato)dibarium] 4.5-hydrate]

Heng-Qiang Zhang ^a, Xiu-Jun Zheng ^b, Chun-Xiang Zhao ^c, Seik Weng Ng ^d,^*

PMCID: PMC3120458 PMID: 21754581

Abstract

The polymeric title compound, {[Ba₂(C₉H₄N₂O₄)₂(H₂O)]·4.5H₂O}_n, adopts a layer structure parallel to (001) in which adjacent Ba^II atoms are connected by two benzimidazole-5,6-dicarboxylate dianions, one functioning in a μ₄-bridging mode and the other in a μ₅-bridging mode. The Ba atom having water in its coordination environment as well as the Ba atom without water exist in a nine-coordinate polyhedron of O atoms; the geometry is difficult to derive. Lattice water molecules occupy the space between layers and interact with the layers through O—H⋯O, O—H⋯N and N—H⋯O hydrogen bonds. ne of the five lattice water molecules is equally disordered around an inversion centre and shows half-occupancy.

Related literature

For the strontium 1H-benzimidazole-5,6-dicarboxylate derivative, see: Song et al. (2009 ▶).

Experimental

Crystal data

[Ba₂(C₉H₄N₂O₄)₂(H₂O)]·4.5H₂O
M _r = 782.05
Triclinic,
a = 6.9331 (4) Å
b = 9.5950 (4) Å
c = 18.0179 (7) Å
α = 103.186 (1)°
β = 92.068 (2)°
γ = 93.032 (2)°
V = 1163.94 (9) Å³
Z = 2
Mo Kα radiation
μ = 3.44 mm⁻¹
T = 293 K
0.33 × 0.24 × 0.21 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.396, T _max = 0.532
11398 measured reflections
5246 independent reflections
4749 reflections with I > 2σ(I)
R _int = 0.025

Refinement

R[F ² > 2σ(F ²)] = 0.028
wR(F ²) = 0.074
S = 1.07
5246 reflections
343 parameters
30 restraints
H-atom parameters constrained
Δρ_max = 1.54 e Å⁻³
Δρ_min = −0.68 e Å⁻³

Data collection: RAPID-AUTO (Rigaku Corporation, 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: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053681101590X/jh2280sup1.cif

e-67-0m671-sup1.cif^{(32.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053681101590X/jh2280Isup2.hkl

e-67-0m671-Isup2.hkl^{(256.9KB, 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—H11⋯O4wⁱ	0.84	1.66	2.49 (1)	170
O1w—H12⋯O2wⁱⁱ	0.84	1.88	2.60 (1)	143
O2w—H21⋯N2	0.84	2.00	2.83 (1)	168
O2w—H22⋯N2ⁱⁱⁱ	0.84	2.28	2.83 (1)	124
O3w—H31⋯N3	0.84	2.34	2.95 (1)	129
O3w—H32⋯O6w^iv	0.84	1.85	2.68 (1)	174
O4w—H41⋯O3w^v	0.84	2.03	2.84 (2)	161
O5w—H51⋯O1w^v	0.84	2.31	2.75 (1)	113
O6w—H61⋯O4^vi	0.84	1.99	2.76 (1)	152
O6w—H62⋯O8	0.84	2.09	2.86 (1)	152
N1—H1⋯O1w	0.88	1.93	2.80 (1)	168
N4—H4⋯O4w	0.88	1.99	2.86 (1)	167

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

Acknowledgments

We thank the Scientific Research Foundation of the Education Department of Heilongjiang Province (No. 11544005), the Scientific Research Innovation Foundation for young teachers of Zhoukou Normal University (No. zknuqn201044B) and the University of Malaya for supporting this study.

supplementary crystallographic information

Comment

The 1H-benzimidazole-5,6-dicarboxylate dianion affords a large number of metal salts; most of the crystal structure studies involve rare earth metals. The crystal structures of only few main group derivatives have been reported. The Sr^II derivative exists as a monohydrate; the metal atom is also coordinated by two water ligands in an eight-coordinate square-antiprismatic geometry. The dianion functions in a \m4 bridging mode (Song et al., 2009). The Ba^II analog has 4.5 lattice water molecules (Scheme I). Polymeric Ba₂(H₂O)(C₉H₄NO₄)₂^.4.5H₂O adopts a layer structure in which adjacent Ba^II atoms are connected by two benzimidazole-5,6-dicarboxylate dianions, one functioning in a µ₄ bridging mode and the other in a µ₅ bridging mode. The Ba atom having water in its coordination environment as well as the Ba atom without water exist in a nine-coordinate polyhedron of O atom; the geometry is undefined. Lattice water molecules occupy the space between layers, and interact with the layers through O–H···O and N–H···O hydrogen bonds to generate a three-dimensional network (Table 1).

Experimental

Barium chloride (0.0416 g, 0.20 mmol) and 1H-benzimidazole-5,6-dicarboxylic acid (0.0412 g, 0.20 mmol) were placed in water (35 ml); the reactants dissolved upon addition of several drops of dilute sodium hydroxide to a pH of 7. The solution was set aside for the growth of crystals over several weeks; yield 60% based on Ba.