Bis(pyridine-3-carboxylic acid-κN)silver(I) perchlorate

Xiao-Yan Nie; Qian-Zhu Li

doi:10.1107/S1600536808044206

. 2009 Jan 8;65(Pt 2):m148. doi: 10.1107/S1600536808044206

Bis(pyridine-3-carboxylic acid-κN)silver(I) perchlorate

Xiao-Yan Nie ^a, Qian-Zhu Li ^a,^*

PMCID: PMC2968163 PMID: 21581761

Abstract

In the title compound, [Ag(C₆H₅NO₂)₂]ClO₄, the Ag^I atom shows an almost linear coordination geometry, defined by two N atoms from two pyridine-3-carboxylic acid ligands. The complex cations are linked by hydrogen bonds between the carboxyl groups into a chain. The chains are further connected through C—H⋯O hydrogen bonds and a weak Ag⋯O interaction [2.757 (8) Å] into a layer. Another Ag⋯O interaction [2.899 (2) Å] and a C—H⋯O hydrogen bond connect the layers into a three-dimensional network.

Related literature

For general background on coordination polymers and open-framework materials, see: James (2003 ▶); Serre et al. (2004 ▶); Yaghi et al. (1998 ▶, 2003 ▶). For related structures, see: Evans & Lin (2001 ▶); Luo et al. (2004 ▶).

Experimental

Crystal data

[Ag(C₆H₅NO₂)₂]ClO₄
M _r = 453.54
Monoclinic,
a = 8.0139 (4) Å
b = 26.3288 (15) Å
c = 7.6891 (4) Å
β = 110.728 (1)°
V = 1517.36 (14) Å³
Z = 4
Mo Kα radiation
μ = 1.55 mm⁻¹
T = 273 (2) K
0.29 × 0.25 × 0.21 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.649, T _max = 0.731
7763 measured reflections
2729 independent reflections
2150 reflections with I > 2σ(I)
R _int = 0.029

Refinement

R[F ² > 2σ(F ²)] = 0.043
wR(F ²) = 0.123
S = 0.87
2729 reflections
219 parameters
H-atom parameters constrained
Δρ_max = 1.26 e Å⁻³
Δρ_min = −0.57 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); 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/S1600536808044206/hy2176sup1.cif

e-65-0m148-sup1.cif^{(15.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808044206/hy2176Isup2.hkl

e-65-0m148-Isup2.hkl^{(134KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Ag1—N1	2.178 (4)
Ag1—N2	2.185 (4)

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N1—Ag1—N2

165.65 (15)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯O5ⁱ	0.93	2.51	3.244 (8)	136
C4—H4⋯O7ⁱⁱ	0.93	2.52	3.266 (8)	139
C6—H6⋯O7	0.93	2.52	3.248 (8)	136
C7—H7⋯O8ⁱ	0.93	2.49	3.287 (9)	144
C12—H12⋯O7	0.93	2.38	3.228 (9)	152
O2—H2⋯O4ⁱⁱⁱ	0.82	1.84	2.649 (5)	169
O3—H3⋯O1^iv	0.82	1.87	2.689 (5)	175

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

Acknowledgments

The authors kindly acknowledge Bijie University for supporting this work.

supplementary crystallographic information

Comment

The use of multifunctional organic linker molecules in the preparation of coordination polymers and open-framework materials has led to the development of a rich field of chemistry owing to the potential applications of these materials in catalysis, separation, gas storage and molecular recognition (James, 2003; Serre et al., 2004; Yaghi et al., 1998, 2003). In our investigations we used nicotinic acid ligands for the preparation of new coordination polymers, because it can act as a multidentate ligand with versatile binding and coordination modes (Evans & Lin, 2001; Luo et al., 2004). In this paper, we report the crystal structure of the title compound, a new Ag^I complex obtained by the reaction of nicotinic acid, AgNO₃ and perchloric acid in water.

As shown in Fig. 1, the title compound consists of a [Ag(C₆H₅NO₂)₂]⁺ cation and a perchlorate anion. The Ag^I atom exhibits a linear coordination geometry, defined by two N atoms from two pyridine-3-carboxylic acid ligands (Table 1). The complex cations are linked by hydrogen bonds between the carboxyl groups into a chain (Table 2). The chains are further connected by C—H···O hydrogen bonds involving C1, C6, C7 and C12 atoms and the perchlorate anions, and by a weak Ag1···O5(x-1, y, z) interaction [2.757 (8) Å] into a layer (Fig. 2). Another Ag1···O1(x, 3/2-y, z-1/2) interaction [2.899 (2) Å] and a C4—H4···O7(x, 3/2-y, 1/2+z) hydrogen bond connect the layers into a three-dimensional network.

Experimental

A mixture of AgNO₃ (0.169 g, 1 mmol), perchloric acid (0.12 ml), nicotinic acid (0.123 g, 1 mmol) and H₂O (10 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 433 K for 3 d and then cooled to room temperature at a rate of 10 K h^-1. The crystals obtained were washed with water and dried in air.