Poly[aqua­[μ3-4-carb­oxy-2-(pyridin-4-yl)-1H-imidazole-5-carboxyl­ato-κ5 N 1,O 5:N 3,O 4:N 2]nickel(II)]

Xue-Min Jing; Shu-zhe Gong; Li-Wei Xiao

doi:10.1107/S1600536812001900

. 2012 Jan 21;68(Pt 2):m187. doi: 10.1107/S1600536812001900

Poly[aqua[μ₃-4-carboxy-2-(pyridin-4-yl)-1H-imidazole-5-carboxylato-κ⁵ N ¹,O ⁵:N ³,O ⁴:N ²]nickel(II)]

Xue-Min Jing ^a,^*, Shu-zhe Gong ^b, Li-Wei Xiao ^a

PMCID: PMC3274911 PMID: 22346858

Abstract

The water-coordinated Ni²⁺ cation in the title compound, [Ni(C₁₀H₅N₃O₄)(H₂O)]_n, assumes an octahedral NiN₃O₃ coordination mode and is N,O-chelated by two deprotonated 2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylic acid (HPyImDC²⁻) ligands, forming a layer structure extending in the bc plane. The chains are arranged along the b-axis direction, forming a layer structure extending in the bc plane. O—H⋯O hydrogen bonding between the layers results in the formation of a three-dimensional supramolecular framework. The structure is isotypic with the Zn analogue [Li et al. (2009). Cryst. Growth Des. 6, 3423–3431].

Related literature

For the isotypic Zn compound, see: Li et al. (2009 ▶). The HPyImDC²⁻ anion behaves as a T-shaped linker, see: Jing et al. (2010 ▶).

Experimental

Crystal data

[Ni(C₁₀H₅N₃O₄)(H₂O)]
M _r = 307.88
Monoclinic,
a = 7.5117 (15) Å
b = 11.400 (2) Å
c = 12.896 (4) Å
β = 109.04 (3)°
V = 1043.9 (4) Å³
Z = 4
Mo Kα radiation
μ = 1.88 mm⁻¹
T = 293 K
0.21 × 0.16 × 0.13 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.216, T _max = 0.422
10075 measured reflections
2377 independent reflections
1951 reflections with I > 2σ(I)
R _int = 0.067

Refinement

R[F ² > 2σ(F ²)] = 0.051
wR(F ²) = 0.118
S = 1.04
2377 reflections
200 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.55 e Å⁻³
Δρ_min = −1.09 e Å⁻³

Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812001900/hp2024sup1.cif

e-68-0m187-sup1.cif^{(16.1KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812001900/hp2024Isup2.hkl

e-68-0m187-Isup2.hkl^{(116.8KB, hkl)}

Supplementary material file. DOI: 10.1107/S1600536812001900/hp2024Isup4.cdx

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
O1—H1⋯O3	0.94 (7)	1.57 (7)	2.501 (4)	171 (7)
O1W—H1A⋯O3ⁱ	0.78 (9)	1.95 (9)	2.726 (5)	174 (9)
O1W—H1B⋯O1ⁱⁱ	0.73 (6)	2.35 (6)	3.007 (5)	150 (5)

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

Acknowledgments

This work was supported by the Second Self-financing Project of Langfang Scientific and Technological Research and the Development Program of Hebei Province of the People’s Republic of China (grant No. 2011011037).

supplementary crystallographic information

Comment

Li et al. (2009) described the structure of [Zn(C₁₀H₅N₃O₄)H₂O] as a stairway-like two-dimensional 3,3-connected layer held together via hydrogen-bonding interactions involving the carboxylic acid and water H atoms to be a three-dimensional network. The HPyImDC^2- anion behaves as a T-shaped linker (Jing et al., 2010) with one N atoms and bis-N,O-bridging modes chelating the Ni(II) atoms. The present centrosymmetric Ni analogue, (Fig. 1) is isomorphous, the two compounds having nearly identical unit-cell parameters.

As shown in Fig. 2a, the {NiN₃O₃} octahedra connect with the T-shaped HPyImDC^2- anions to be a one-dimensional chain structure extending in the c direction. Then these one-dimensional chains arrange along the b direction to be a two-dimensional layer structure extending in the bc plane (Fig. 2 b), which are further connected through the hydrogen bonds occurred between O(1 W)—H(1 A)···O(3) (-x + 1,-y,-z) and O(1 W)—H(1B)···O(1)(x-1, y, z), respectively, to construct a three-dimensional supramolecular framework (Fig. 2c and Table 1).

Experimental

Preparation of the complex.

A solution of NiCl₂6H₂O (0.012 g, 0.5 mmol) and H₃PyImDC (0.012 g, 0.05 mmol) in DMF (1 ml) and H₂O (0.5 ml) was sealed into a 15 ml Teflon-lined stainless autoclave and heated at 433 K for 4 days and then cooled to room temperature gradually to afford well formed green block crystals in about 60% yield (based on Zn). Elemental analysis found (%): C, 39.06; H, 2.30; N, 13.72; Ni, 19.01. H₇C₁₀N₃O₅Ni requires (%): C, 39.01; H, 2.29; N, 13.65; Ni, 19.06. IR (KBr, cm^-1): 3571 (s), 3083 (m), 2560 (w), 1675 (w), 1565 (versus), 1271 (s), 842 (m), 567 (w).