Triimidazolium tris­(pyridine-2,6-di­carboxyl­ato)dysprosate(III) trihydrate

Lingzong Meng; Chaowen Duan

doi:10.1107/S1600536810036421

. 2010 Sep 25;66(Pt 10):m1291–m1292. doi: 10.1107/S1600536810036421

Triimidazolium tris(pyridine-2,6-dicarboxylato)dysprosate(III) trihydrate

Lingzong Meng ^a,^*, Chaowen Duan ^a

PMCID: PMC2983370 PMID: 21587433

Abstract

The structure of the title compound, (C₃N₂H₅)₃[Dy(C₇H₃NO₄)₃]·3H₂O, contains a mononuclear Dy^III complex with the rare earth metal cation in a distorted tricapped trigonal–prismatic environment. The Dy^III ion is in each case O,N,O′-chelated by three tridentate pyridine-2,6-dicarboxylate anions. Three protonated imidazole molecules act as counter-cations and three lattice water molecules are also present. Numerous N—H⋯O and O—H⋯O hydrogen bonding interactions, some of which are bifurcated, help to stabilize the packing of the structure.

Related literature

For background to pyridine-2,6-dicarboxylic acid (H₂pda) and structures of metal complexes with (pda²⁻) ligands, see: Ghosh & Bharadwaj (2005 ▶); Huang et al. (2008 ▶); Kjell et al. (1993 ▶); Song et al. (2005 ▶); Wu et al. (2008 ▶); Yue et al. (2005 ▶); Zhao et al. (2005 ▶, 2007 ▶).

Experimental

Crystal data

(C₃H₅N₂)₃[Dy(C₇H₃NO₄)₃]·3H₂O
M _r = 919.13
Triclinic,
a = 10.939 (2) Å
b = 12.099 (2) Å
c = 14.070 (3) Å
α = 88.57 (3)°
β = 85.64 (3)°
γ = 67.28 (3)°
V = 1712.7 (6) Å³
Z = 2
Mo Kα radiation
μ = 2.27 mm⁻¹
T = 296 K
0.35 × 0.25 × 0.25 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.504, T _max = 0.601
27464 measured reflections
7447 independent reflections
7223 reflections with I > 2σ(I)
R _int = 0.022

Refinement

R[F ² > 2σ(F ²)] = 0.022
wR(F ²) = 0.060
S = 1.10
7447 reflections
505 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.69 e Å⁻³
Δρ_min = −0.77 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: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810036421/wm2398sup1.cif

e-66-m1291-sup1.cif^{(33.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810036421/wm2398Isup2.hkl

e-66-m1291-Isup2.hkl^{(364.4KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Dy2—O5	2.3745 (19)
Dy2—O1	2.4032 (17)
Dy2—O7	2.4072 (18)
Dy2—O3	2.4167 (19)
Dy2—O11	2.420 (2)
Dy2—O9	2.426 (2)
Dy2—N2	2.482 (2)
Dy2—N1	2.492 (2)
Dy2—N3	2.506 (2)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N4—H4A⋯O14ⁱ	0.94 (2)	2.50 (3)	3.286 (4)	141 (4)
N5—H5⋯O12ⁱ	0.86	2.27	3.121 (5)	171
N8—H8A⋯O10ⁱⁱ	0.96 (2)	2.29 (2)	3.241 (4)	172 (4)
N7—H7A⋯O10ⁱⁱⁱ	0.87 (2)	1.82 (2)	2.695 (4)	177 (4)
N7—H7A⋯O9ⁱⁱⁱ	0.87 (2)	2.60 (3)	3.127 (3)	120 (3)
N6—H6⋯O14^iv	0.86	1.89	2.731 (4)	167
O13—H2W⋯O15^iv	0.85	2.02	2.828 (4)	159
O13—H1W⋯O11	0.85	2.05	2.896 (3)	174
O13—H1W⋯O12	0.85	2.61	3.192 (4)	127
O14—H3W⋯O4	0.85	1.91	2.756 (3)	178
O14—H4W⋯O6^v	0.85	2.06	2.842 (3)	153
O15—H5W⋯O2^vi	0.85	2.22	3.061 (4)	169
O15—H6W⋯O4	0.85	2.00	2.845 (4)	172

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

supplementary crystallographic information

Comment

In recent years, the interaction of pyridine-2,6-dicarboxylic acid (H₂pdc) with several metal ions has been extensively studied due to its unique ability to form stable chelates in diverse coordination modes such as bidentate, meridian and bridging (Kjell et al., 1993). A considerable number of metal—pdc complexes have been synthesized and their structures determined over the past decade (Huang et al., 2008; Ghosh et al., 2005; Song et al., 2005; Wu et al., 2008; Yue et al., 2005; Zhao et al., 2005, 2007). Here we present the structure of the title compound (C₃N₂H₅)₃[Dy(C₇H₃NO₄)₃]^.(H₂O)₃, which includes pyridinedicarboxylate (pdc^2-) anions and imidazolium (im) counter cations.

The crystal structure is composed of a mononuclear Dy^III complex with the rare earth metal cation in a distorted tricapped trigonal-prismatic environment (Fig. 1, Table 1). The Dy^III ion is in each case O,N,O-chelated by three tridentate pyridine-2,6-dicarboxylate (pda^2-) ligands. Three imidazolium molecules act as counter cations. Moreover, three lattice water molecules are present. Numerous N—H···O, O—H···O and O—H···N hydrogen bonding interactions (Table 2), part of which are bifurcated, lead to a three-dimensional assembly of the structural building blocks.

Experimental

The title compound was synthesized under solvothermal conditions. A mixture of pyridine-2,6-dicarboxylic acid (0.0334 g, 0.2 mmol), Dy(NO₃)₃^.6H₂O (0.0245 g, 0.06 mmol), imidazole (0.0340 g, 0.5 mmol) and H₂O / C₂H₅OH (v / v = 1: 1, 2.5 ml) was sealed in a 6 ml glass tube and heated to 393 K for 72 h. After cooling to room temperature, colorless block-like crystals were obtained.