catena-Poly[[bis­(nitrato-κO)cadmium]bis­[μ-1,4-bis­(pyridin-3-yl­meth­oxy)benzene-κ2 N:N′]]

Shuang Zhang; Ying-Hui Yu; Ying Liu; Guang-Feng Hou; Jin-Sheng Gao

doi:10.1107/S1600536811032697

. 2011 Aug 17;67(Pt 9):m1263. doi: 10.1107/S1600536811032697

catena-Poly[[bis(nitrato-κO)cadmium]bis[μ-1,4-bis(pyridin-3-ylmethoxy)benzene-κ² N:N′]]

Shuang Zhang ^a, Ying-Hui Yu ^a,^b, Ying Liu ^b, Guang-Feng Hou ^a,^b, Jin-Sheng Gao ^a,^b,^*

PMCID: PMC3200741 PMID: 22064823

Abstract

In the title compound, [Cd(NO₃)₂(C₁₈H₁₆N₂O₂)₂]_n, the six-coordinated Cd^II ion is located on an inversion center and has a distorted octahedral environment defined by four N atoms from four 1,4-bis(pyridin-3-ylmethoxy)benzene ligands and two O atoms from two nitrate anions. The ligands link the Cd^II ions into a ribbon-like structure running along [201]. One O atom of the nitrate anion is disordered over two positions with site-occupancy factors of 0.59 (2) and 0.41 (2).

Related literature

For the synthesis and background to metal complexes with pyridyl-based aromatic ligands, see: Liu et al. (2010a ▶,b ▶). For isotypic compounds, see: Liu et al. (2011 ▶); Zou et al. (2011 ▶).

Experimental

Crystal data

[Cd(NO₃)₂(C₁₈H₁₆N₂O₂)₂]
M _r = 821.08
Monoclinic,
a = 8.4034 (17) Å
b = 16.914 (3) Å
c = 13.436 (5) Å
β = 114.23 (2)°
V = 1741.5 (8) Å³
Z = 2
Mo Kα radiation
μ = 0.70 mm⁻¹
T = 293 K
0.20 × 0.19 × 0.17 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.871, T _max = 0.890
16413 measured reflections
3952 independent reflections
3277 reflections with I > 2σ(I)
R _int = 0.028

Refinement

R[F ² > 2σ(F ²)] = 0.029
wR(F ²) = 0.077
S = 1.08
3952 reflections
251 parameters
12 restraints
H-atom parameters constrained
Δρ_max = 0.45 e Å⁻³
Δρ_min = −0.30 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811032697/hy2453sup1.cif

e-67-m1263-sup1.cif^{(24.7KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811032697/hy2453Isup2.hkl

e-67-m1263-Isup2.hkl^{(193.7KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Cd1—N1	2.3793 (17)
Cd1—N2ⁱ	2.3064 (17)
Cd1—O3	2.3778 (17)

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors thank the Project of Innovation Service Platform of Heilongjiang Province (PG09J001) and Heilongjiang University for supporting this work.

supplementary crystallographic information

Comment

The bridging compounds with rigid and flexible pyridyl-containing bidentate or multidentate organic spacers have assembled numerous interesting topology structures by coordination with metals and intermolecular supramolecular interactions. Our group focused attention on study of flexible pyridyl-based aromatic ligands, and obtained some isolated molecules, chain, two- and three-dimensional network structures (Liu et al., 2010a, b). Herein, as a continuing work for pyridyl ligands, we report the synthesis and crystal structure of the title compound, which is a isostructural compound of our previous reports (Liu et al., 2011; Zou et al., 2011).

In the title compound, the Cd^II ion lies on an inversion center and is six-coordinated in a distorted octahedral geometry defined by four N atoms of the pyridine derivatives and two O atoms of the nitrate anions (Fig. 1, Table 1). One O atom of the nitrate anion has a badly thermal ellipsoid, which is split over two positions with site-occupancy factors of 0.59 (2) and 0.41 (2). In the crystal, ribbon-like structures along [2 0 1] are built up by the N-heterocyclic ligands linking the Cd^II ions (Fig. 2).

Experimental

The 1,4-bis(pyridin-3-ylmethoxy)benzene ligand was synthesized as the reference method (Liu et al., 2010a). A mixture of 1,4-dihydroxybenzene (1.10 g, 10 mmol), 3-chloromethylpyridine hydrochloride (3.28 g, 20 mmol) and NaOH (1.60 g, 40 mmol) in acetonitrile (50 ml) was refluxed under nitrogen with stirring for 24 h. After cooling to room temperature, the solution was filtered and the residue was washed with acetonitrile for several times. The mixed filtrate was dropped into a 300 ml water solution, giving a powder crude product. A total of 2.51 g (yield 86%) pure product was obtained by recrystallizing from a mixed solution of 10 ml water and 10 ml methanol. The title compound was synthesized by the reaction of 1,4-bis(pyridin-3-ylmethoxy)benzene (0.29 g, 1.0 mmol) and Cd(NO₃)₂.4H₂O (0.31 g, 1.0 mmol) in a mixed solution of 5 ml water and 5 ml methanol. The mixture was filtered after stirring for about 1 h. The filtate was allowed to stand for 4 d under room temperature to give block-like colorless crystals suitable for X-ray analysis.