Poly[[μ-ethane-1,2-diyl bis­(pyridine-3-carboxyl­ate)](μ-tetra­fluorido­borato)silver(I)]

Javier Vallejos; Iván Brito; Alejandro Cárdenas; Michael Bolte

doi:10.1107/S1600536812018399

. 2012 Apr 28;68(Pt 5):m705. doi: 10.1107/S1600536812018399

Poly[[μ-ethane-1,2-diyl bis(pyridine-3-carboxylate)](μ-tetrafluoridoborato)silver(I)]

Javier Vallejos ^a, Iván Brito ^a,^*, Alejandro Cárdenas ^b, Michael Bolte ^c

PMCID: PMC3344420 PMID: 22590182

Abstract

In the title compound, [Ag(BF₄)(C₁₄H₁₂N₂O₄)]_n, the coordination of the Ag⁺ ion is trigonal–bipyramidal with the N atoms of two ethane-1,2-diyl bis(pyridine-3-carboxylate) ligands in the apical positions and three F atoms belonging to different tetrafluoridoborate anions in the equatorial plane. The material consists of infinite chains of [Ag(C₁₄H₁₂N₂O₄)] units running along [001], held together by BF₄ ⁻ bridging anions.

Related literature

For the crystal structure of the ethane-1,2-diyl bis(pyridine-3-carboxylate) ligand, see: Brito et al. (2010 ▶). For background to coordination chemistry, see: Blake et al. (1999 ▶); Brito et al. (2011 ▶).

Experimental

Crystal data

[Ag(BF₄)(C₁₄H₁₂N₂O₄)]
M _r = 466.94
Orthorhombic,
a = 15.2667 (11) Å
b = 6.7170 (4) Å
c = 30.8598 (16) Å
V = 3164.6 (3) Å³
Z = 8
Mo Kα radiation
μ = 1.34 mm⁻¹
T = 173 K
0.16 × 0.04 × 0.04 mm

Data collection

Stoe IPDS-II two-circle diffractometer
Absorption correction: multi-scan (MULABS; Spek, 2009 ▶; Blessing, 1995 ▶) T _min = 0.814, T _max = 0.948
27909 measured reflections
2772 independent reflections
1605 reflections with I > 2σ(I)
R _int = 0.115

Refinement

R[F ² > 2σ(F ²)] = 0.058
wR(F ²) = 0.144
S = 0.93
2772 reflections
235 parameters
H-atom parameters constrained
Δρ_max = 1.75 e Å⁻³
Δρ_min = −1.14 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2001 ▶); cell refinement: X-AREA; data reduction: X-AREA; 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 datablock(s) I, global. DOI: 10.1107/S1600536812018399/ff2064sup1.cif

e-68-0m705-sup1.cif^{(18.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812018399/ff2064Isup2.hkl

e-68-0m705-Isup2.hkl^{(136.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Ag1—N11	2.145 (6)
Ag1—N23ⁱ	2.155 (6)
Ag1—F1ⁱⁱ	3.168 (9)
Ag1—F2	2.832 (8)
Ag1—F2ⁱⁱⁱ	2.972 (7)

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

Acknowledgments

Thanks are given to the Consejo Superior de Investigaciones Científicas (CSIC) of Spain for the award of a licence for the use of the Cambridge Structural Database (CSD). JV thanks the Universidad de Antofagasta for a PhD fellowship.

supplementary crystallographic information

Comment

The design of polymeric organic-inorganic materials with novel topologies and structural motifs is of current interest in the field of coordination chemistry (Blake et al., 1999). This paper forms part of our continuing study of the synthesis, structural characterization and physical properties of coordination polymers (Brito et al., 2011). We report here the crystal structure of the title compound (Fig.1). It crystallizes as colorless needles, which were found to be stable to air and light. In the title compound, the coordination of the Ag^I atom is a trigonal bipyramid with the N atoms of two 1,2-diyl-bis(pyridine-3-carboxylate)ethane ligands in the apical positions and three F atoms belonging to different tetrafluoroborate anions in the equatorial plane. The Ag–N distances are 2.145 (6) and 2.155 (6) Å and the Ag–F distances are 2.832 (8) Å, 2.972 (7) Å and 3.168 (9) Å. The N–Ag–N angle [168.8 (3)°] is not far from being linear and the Ag—N vectors are almost perpendicular to the Ag—F vectors [76.7 (3)° to 103.1 (3)°]. The F–Ag–F angles are 106.4 (2)°, 120.7 (2)° and 127.4 (2)°. The molecular dimensions of the 1,2-bis(3-pyridyl)ethane ligand are within normal ranges and the ethylene moiety retains the gauche conformation (Brito et al., 2010). The material consists of infinite chains of [Ag(C₁₄H₁₂N₂O₄)] moieties running along [001] held together by BF₄^- bridging anions (Fig. 2).

Experimental

A solution of AgBF₄ (19.4 mg, 0.1 mmol) in water was slowly added to a solution of the ligand (27.2 mg, 0.1 mmol) in THF (4 ml). Colorless single crystals suitable for X-ray were obtained after a few days (82%).The FT—IR (KBr, cm^-1): 1724 s, 1609, 1434 m, 1280 s, 742 m.