Poly[[μ2-acetato-aquadi-μ3-isonicotinato-dysprosium(III)silver(I)] perchlorate]

Li-Cai Zhu

doi:10.1107/S1600536809046637

. 2009 Nov 18;65(Pt 12):m1595–m1596. doi: 10.1107/S1600536809046637

Poly[[μ₂-acetato-aquadi-μ₃-isonicotinato-dysprosium(III)silver(I)] perchlorate]

Li-Cai Zhu ^a,^*

PMCID: PMC2972040 PMID: 21578624

Abstract

In the title three-dimensional heterometallic complex, {[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄}_n, the Dy(III) ion is eight-coordinated by four O atoms from four different isonicotinate ligands, three O atoms from two different acetate ligands and one O atom of water molecule. The two-coordinate Ag^I ion is bonded to two N atoms from two different isonicotinate anions. These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network. The coordinated water molecules link the carboxylate group and the acetate ligand by O—H⋯O hydrogen bonding. The perchlorate anion is disordered over two sites with site occupancy factors 0.508 (12) and 0.492 (12) and the methyl group of the acetate ligand is disordered over two positions of equal occupancy.

Related literature

For the applications of lanthanide–transition metal heterometallic complexes with bridging multifunctional organic ligands in ion exchange, magnetism, bimetallic catalysis and as luminescent probes, see: Cheng et al. (2006 ▶); Kuang et al. (2007 ▶); Peng et al. (2008 ▶); Zhu et al. (2009 ▶). graphic file with name e-65-m1595-scheme1.jpg

Experimental

Crystal data

[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄
M _r = 691.08
Monoclinic,
a = 16.1682 (15) Å
b = 15.1020 (14) Å
c = 7.9846 (7) Å
β = 92.845 (1)°
V = 1947.2 (3) Å³
Z = 4
Mo Kα radiation
μ = 5.01 mm⁻¹
T = 296 K
0.23 × 0.20 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.328, T _max = 0.386
9904 measured reflections
3486 independent reflections
3112 reflections with I > 2σ(I)
R _int = 0.025

Refinement

R[F ² > 2σ(F ²)] = 0.023
wR(F ²) = 0.056
S = 1.04
3486 reflections
322 parameters
158 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.66 e Å⁻³
Δρ_min = −0.76 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: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809046637/zq2015sup1.cif

e-65-m1595-sup1.cif^{(21.4KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809046637/zq2015Isup2.hkl

e-65-m1595-Isup2.hkl^{(171KB, 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—H2W⋯O2ⁱ	0.79 (3)	2.21 (4)	2.925 (4)	150 (5)
O1W—H1W⋯O5ⁱⁱ	0.79 (3)	2.05 (4)	2.813 (4)	161 (5)

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

Acknowledgments

The author acknowledges South China Normal University for supporting this work.

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; Peng et al., 2008; Zhu et al., 2009). As an extension of this research, the structure of the title compound, a new heterometallic coordination polymer, (I), has been determined which is presented in this article.

In the title compound (Fig. 1), there are one Dy(III) ion, one Ag(I) ion, two halves of acetate ligand, two isonicotinate ligands, one coordinated water molecule, and one perchlorate anion in the asymmetric unit. Each Dy(III) ion is eight-coordinated by four O atoms from four different isonicotinate ligands [Dy—O distances ranging from 2.297 (3) to 2.348 (3) Å], and three O atoms from two different acetate ligands [Dy—O distances ranging from 2.394 (3) to 2.484 (3) Å], and one O atom of water molecule [Dy—O distances 2.414 (3) Å]. The O—Dy—O bond angles are in the range from 52.70 (10) to 155.05 (10) °. The Dy center can be described as having a bicapped trigonal prism coordination geometry. The two-coordinate Ag(I) ion is bonded to two N atoms from two different isonicotinate anions [Ag—N distances 2.163 (4) Å]. Thus the Ag(I) ion is in a somewhat linear configuration with N1—Ag1—N2 angle 165.40 (17) °. These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network (Fig. 2).The coordinated water molecules link the carboxylate group and acetate ligand by O—H···O hydrogen bonding (Table 1). The perchlorate anion is disordered over two sites with site occupancy factors 0.508 (12) and 0.492 (12). The methyl group of the acetate ligand is disordered over two positions of equal occupancy (0.5:0.5).

Experimental

A mixture of AgNO₃(0.057 g, 0.33 mmol), Dy₂O₃(0.116 g, 0.33 mmol), isonicotinic acid (0.164 g, 1.33 mmol), CH₃COONa(0.057 g, 0.7 mmol), H₂O(7 ml), and HClO₄(0.257 mmol)(pH 2) was sealed in a 20 ml Teflon-lined reaction vessel at 443 K for 6 days then slowly cooled to room temperature. The product was collected by filtration, washed with water and air-dried. Colorless block crystals suitable for X-ray analysis were obtained.