catena-Poly[[aqua­[1,4-bis­(1H-imidazol-4-yl)benzene]cadmium]-μ3-5-methyl­isophthalato]

Sen-Lin Yang; De-Hai Wang; Shui-Sheng Chen

doi:10.1107/S1600536811030509

. 2011 Aug 2;67(Pt 9):m1174–m1175. doi: 10.1107/S1600536811030509

catena-Poly[[aqua[1,4-bis(1H-imidazol-4-yl)benzene]cadmium]-μ₃-5-methylisophthalato]

Sen-Lin Yang ^a, De-Hai Wang ^a, Shui-Sheng Chen ^a,^*

PMCID: PMC3200974 PMID: 22065019

Abstract

In the title coordination polymer, [Cd(C₉H₆O₄)(C₁₂H₁₀N₄)(H₂O)]_n, the Cd^II atom has a NO₆ donor set and is coordinated by five carboxylate O atoms from three different 5-methyl-1,3-phenylenediacetate (pda²⁻) anions, one O atom from a water molecule and one N atom from a 1,4-bis(1H-imidazol-4-yl)benzene (L) ligand, displaying a highly distorted pentagonal–bipyramidal geometry. Each pda²⁻ anion acts as a μ₃-bridge, linking Cd^II atoms to form one-dimensional slabs extending parallel to [010]. In the crystal, adjacent molecules are linked through N—H⋯N and N—H⋯O hydrogen bonds into a three-dimensional network.

Related literature

For background to metal-organic hybrid materials, see: Bradshaw et al. (2005 ▶); Ockwig et al. (2005 ▶). For structures containing mixed ligands, see: Liu et al. (2007 ▶); Chen et al. (2006 ▶); Choi & Jeon (2003 ▶). For related structures, see: Chen et al. (2010 ▶; 2011 ▶).

Experimental

Crystal data

[Cd(C₉H₆O₄)(C₁₂H₁₀N₄)(H₂O)]
M _r = 518.80
Triclinic,
a = 6.9407 (9) Å
b = 9.8231 (13) Å
c = 15.506 (2) Å
α = 74.091 (2)°
β = 85.963 (2)°
γ = 70.707 (2)°
V = 959.4 (2) Å³
Z = 2
Mo Kα radiation
μ = 1.18 mm⁻¹
T = 296 K
0.18 × 0.16 × 0.12 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.815, T _max = 0.871
15863 measured reflections
4376 independent reflections
4161 reflections with I > 2σ(I)
R _int = 0.022

Refinement

R[F ² > 2σ(F ²)] = 0.026
wR(F ²) = 0.128
S = 1.09
4376 reflections
281 parameters
H-atom parameters constrained
Δρ_max = 0.86 e Å⁻³
Δρ_min = −0.80 e Å⁻³

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); 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 ▶) and DIAMOND (Brandenburg, 2000 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811030509/wm2517sup1.cif

e-67-m1174-sup1.cif^{(24.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811030509/wm2517Isup2.hkl

e-67-m1174-Isup2.hkl^{(214.4KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Cd1—N1	2.222 (3)
Cd1—O1ⁱ	2.315 (3)
Cd1—O3ⁱⁱ	2.380 (3)
Cd1—O4ⁱⁱ	2.404 (2)
Cd1—O2ⁱ	2.473 (3)
Cd1—O5	2.520 (3)
Cd1—O3	2.539 (3)

Open in a new tab

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

Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2A⋯N4ⁱⁱⁱ	0.86	2.17	2.975 (4)	157
N3—H3⋯O4^iv	0.86	2.03	2.815 (4)	151

Open in a new tab

Symmetry codes: (iii) Inline graphic ; (iv) .

Acknowledgments

This work was supported by the Natural Science Foundation of Anhui Provincial Education Commission (No. KJ2011B128).

supplementary crystallographic information

Comment

The rational design and synthesis of metal-organic frameworks (MOFs) has attracted considerable attention, which is stimulated by their intriguing aesthetic structures and topological features as well as their potential applications as materials (Bradshaw et al., 2005; Ockwig et al., 2005). The choice of suitable ligands is a key factor that greatly affects the structure and stabilization of the coordination architecture (Choi & Jeon 2003). For a more tunable ligand design mixed polycarboxylate and N-containing compounds (Liu et al., 2007; Chen et al., 2006) are favourable. Therefore we have focused on constructing complexes based on the organic ligand 1,4-di(1H-imidazol-4-yl)benzene (L) and polycarboxylate anions (Chen et al., 2010; 2011). As an extension of our work, we report the synthesis and structure of a new Cd^II complex (I), which was obtained by solvothermal reaction of CdI₂ with L and 5-methylisophthalic acid (H₂pda).

The asymmetric unit of (I) consists of one Cd^II atom, one L ligaqnd, one pda^2- anion and one coordinated water molecule. Each Cd^II atom has a NO₆ donor set and is coordinated by five carboxylate oxygen atoms from three different pda^2- anions, one water oxygen atom and one nitrogen atom from L, displaying a highly distorted pentagonal-bipyramidal geometry (Fig. 1). The pda^2- ligand acts as a µ₃– bridge with two monodentate carboxylate groups to form one-dimensional slabs parellel to [010] (Fig. 2). In the crystal, adjacent molecules are linked through N—H···N and N—H···O hydrogen bonding interactions into a three-dimensional network (Fig. 3).

Experimental

All reagents and solvents were used as obtained commercially without further purification. A mixture containing CdI₂ (36.6 mg, 0.1 mmol), L (21.0 mg, 0.1 mmol), H₂pda (18.0 mg, 0.1 mmol), DMF (N:N'- dimethylformamide, 1 ml), 10 ml H₂O was sealed in a 16 ml Teflon-lined stainless steel container and heated at 453 K for 72 h. After cooling to room temperature within 12 h, colorless crystals of (I) suitable for X-ray diffraction analysis were obtained in 48% Yield.