Poly[diaqua­(μ5-1H-imidazole-4,5-di­carboxyl­ato)(μ4-1H-imidazole-4,5-di­carboxyl­ato)tris­ilver(I)ytterbium(III)]

Si-Ming Zhu

doi:10.1107/S1600536812031303

. 2012 Jul 18;68(Pt 8):m1073–m1074. doi: 10.1107/S1600536812031303

Poly[diaqua(μ₅-1H-imidazole-4,5-dicarboxylato)(μ₄-1H-imidazole-4,5-dicarboxylato)trisilver(I)ytterbium(III)]

Si-Ming Zhu ^a,^*

PMCID: PMC3414133 PMID: 22904740

Abstract

The asymmetric unit of the title compound, [Ag₃Yb(C₅HN₂O₄)₂(H₂O)₂]_n, contains three Ag^I ions, one Yb^III ion, two imidazole-4,5-dicarboxylate ligands and two coordinating water molecules. The Yb^III atom is eight-coordinated, in a bicapped trigonal prismatic coordination geometry, by six O atoms from three imidazole-4,5-dicarboxylate ligands and two coordinating water molecules. The two-coordinated Ag^I ions exhibit three types of coordination environments. One Ag^I atom is bonded to two N atoms from two different imidazole-4,5-dicarboxylate ligands. The other two Ag^I atoms are each coordinated by one O atom and one N atom from two different imidazole-4,5-dicarboxylate ligands. These metal coordination units are connected by bridging imidazole-4,5-dicarboxylate ligands, generating a two-dimensional heterometallic layer. These layers are stacked along the a axis via O—H⋯O hydrogen-bonding interactions to generate a three-dimensional framework.

Related literature

For the application of lanthanide–transition metal heterometallic complexes with bridging multifunctional organic ligands, see: Cheng et al. (2006 ▶); Kuang et al. (2007 ▶); Sun et al. (2006 ▶); Zhu et al. (2010 ▶).

Experimental

Crystal data

[Ag₃Yb(C₅HN₂O₄)₂(H₂O)₂]
M _r = 838.84
Monoclinic,
a = 12.6850 (7) Å
b = 8.6643 (5) Å
c = 28.4015 (16) Å
β = 97.686 (1)°
V = 3093.5 (3) Å³
Z = 8
Mo Kα radiation
μ = 9.80 mm⁻¹
T = 295 K
0.20 × 0.18 × 0.17 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.162, T _max = 0.189
7613 measured reflections
2794 independent reflections
2629 reflections with I > 2σ(I)
R _int = 0.026

Refinement

R[F ² > 2σ(F ²)] = 0.024
wR(F ²) = 0.055
S = 1.19
2794 reflections
265 parameters
4 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.58 e Å⁻³
Δρ_min = −1.29 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); 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: SHELXL97.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812031303/rk2366sup1.cif

e-68-m1073-sup1.cif^{(19.3KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812031303/rk2366Isup2.hkl

e-68-m1073-Isup2.hkl^{(137.3KB, 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
O1W—H1W⋯O8ⁱ	0.82 (2)	2.11 (5)	2.751 (5)	136 (6)
O1W—H2W⋯O2ⁱⁱ	0.81 (2)	2.03 (3)	2.823 (5)	165 (6)
O2W—H4W⋯O1ⁱⁱⁱ	0.81 (2)	1.88 (4)	2.634 (5)	154 (8)

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

Acknowledgments

This work was supported by the Fundamental Research Funds for the Central Universities of South China University of Technology (grant No. 2012ZM0072).

supplementary crystallographic information

Comment

In the past few years, lanthanide-transition metal heterometallic complexs with bridging multifunctionnal organic ligands are of increasing interest, not only because of their impressive topological structures, but also due to their versatile applications in ion exchange, magnetism, bimetallic catalysis and luminescent probe (Cheng et al., 2006; Kuang et al., 2007; Sun et al., 2006; Zhu et al., 2010). As an extension of this research, the structure of the title compound, a new heterometallic coordination polymer, has been determined which is presented in this artcle.

The asymmetric unit of the title compound (Fig. 1), contains three Ag^I ions, one Yb^III ion, two imidazole-4,5-dicarboxylate ligands, and two coordinated water molecules. The Yb^III are eight-coordinated, in a bicapped trigonal prismatic coordination geometry, by six O atoms from three imidazole-4,5-dicarboxylate ligands and two coordinated water molecules. The two-coordinated Ag^I ions exhibit three types of coordination environment. One Ag^I ion is linear bonded to two N atoms from two different imidazole-4,5-dicarboxylate ligands with N2^iv-Ag3-N3 angle 176.23 (17)°. The other two Ag^I ions are coordinated in a bow-like conformation each by one O atom and one N atom from two different imidazole-4,5-dicarboxylate ligands with N-Ag-O angle 157.45 (14)° and 159.80 (14)°, respectively. These metal coordination units are connected by bridging imidazole-4,5-dicarboxylate ligands, generating a two-dimensional heterometallic layer. The two-dimensional layers are stacked along a axis via O–H···O hydrogen-bonding interactions to generate the three-dimensional framework (Table 1 and Fig. 2). Symmetry code: (iv) -x, y, -z+3/2.

Experimental

A mixture of AgNO₃ (0.102 g, 0.6 mmol), Yb₂O₃ (0.118 g, 0.3 mmol), imidazole-4,5-dicarboxylic acid (0.188 g, 1.2 mmol), H₂O (10 ml), and HClO₄ (0.385 mmol) was sealed in a 20 ml teflon-lined reaction vessel at 443 K for 5 days then slowly cooled to room temperature. The product was collected by filtration, washed with water and air-dried. Colourless block crystals suitable for X-ray analysis were obtained.