catena-Poly[[aqua­(1,10-phenanthroline)cadmium(II)]-μ-benzene-1,4-di­carboxyl­ato]

Hongping Hu

doi:10.1107/S1600536808041913

. 2008 Dec 17;65(Pt 1):m90. doi: 10.1107/S1600536808041913

catena-Poly[[aqua(1,10-phenanthroline)cadmium(II)]-μ-benzene-1,4-dicarboxylato]

Hongping Hu ^a,^*

PMCID: PMC2967922 PMID: 21581553

Abstract

The title compound, [Cd(C₈H₄O₄)(C₁₂H₈N₂)(H₂O)]_n, is a new coordination polymer of benzene-1,4-dicarboxylate with cadmium(II) and 1,10-phenanthroline. The Cd^II ion is coordinated by two N atoms from the 1,10-phenanthroline molecule, three O atoms from two crystallographically independent benzene-1,4-dicarboxylate ligands and the O atom of a coordinated water molecule, forming a heavily distorted octahedron. The 1,10-phenanthroline ligand is approximately planar within 0.073 (4) Å. The two different benzene-1,4-dicarboxylate ligands each coordinate to two Cd^II ions in bidentate and monodentate modes, forming an infinite zigzag chain. Adjacent chains are packed tightly by strong π–π interactions [centroid–centroid distances = 3.851 (2) and 3.859 (2) Å] between the aromatic rings of the benzene-1,4-dicarboxylate ligand and the 1,10-phenanthroline of a neighboring chain, forming a sheet parallel to (011). Different sheets are linked together via O—H⋯O hydrogen bonds between the coordinated water molecules and the O atoms of the carboxylate groups, forming a three-dimensional network.

Related literature

For related literature, see: Go et al. (2004 ▶); Sun et al. (2001 ▶).

Experimental

Crystal data

[Cd(C₈H₄O₄)(C₁₂H₈N₂)(H₂O)]
M _r = 474.74
Triclinic,
a = 9.1831 (5) Å
b = 9.6550 (6) Å
c = 11.3600 (7) Å
α = 104.6310 (8)°
β = 104.0390 (9)°
γ = 101.8920 (7)°
V = 906.28 (9) Å³
Z = 2
Mo Kα radiation
μ = 1.24 mm⁻¹
T = 298 (2) K
0.10 × 0.08 × 0.04 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.888, T _max = 0.952
5387 measured reflections
3939 independent reflections
3428 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.033
wR(F ²) = 0.081
S = 1.07
3939 reflections
261 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.44 e Å⁻³
Δρ_min = −0.49 e Å⁻³

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; 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 global, I. DOI: 10.1107/S1600536808041913/ez2152sup1.cif

e-65-00m90-sup1.cif^{(22.6KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808041913/ez2152Isup2.hkl

e-65-00m90-Isup2.hkl^{(193KB, 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
O5—H5A⋯O1ⁱ	0.81 (4)	1.91 (4)	2.697 (4)	163 (4)
O5—H5B⋯O4ⁱⁱ	0.75 (4)	2.07 (4)	2.782 (4)	159 (4)

Open in a new tab

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

supplementary crystallographic information

Comment

The title compound (I) was obtained by chance when the synthesis of its polymorph RAMJAQ (Sun et al., 2001) was repeated for a fluorescence study. A single-crystal suitable for X-ray diffraction of I was crystallized from an H₂O-EtOH (1:1) solvent mixture at room temperature.

The Cd^II ion is coordinated by two N atoms from the 1,10-phenanthroline, three O atoms from two crystallographically independent benzene-1,4-dicarboxylate ligands, and one O atom of a water molecule (Fig. 1). The 1,10-phenanthroline ligand is approximately planar, the maximum deviation of the C10 atom from the mean plane being 0.073 (4) Å. The geometries of the two crystallographically independent benzene-1,4-dicarboxylate ligands in (I) are similar to those observed by Go et al. (2004). The two different benzene-1,4-dicarboxylate ligands each coordinate to two Cd^II ions in chelate bidentate and monodentate modes, respectively, forming an infinite zigzag chain. All the bond distances and bond angles in the ligand are comparable to those values in its polymorph (Sun et al., 2001). Adjacent chains are packed tightly by strong π-π interactions between the aromatic rings of the 1,10-phenanthroline and benzene-1,4-dicarboxylate ligands to form a sheet along the (011) direction. Strong π-π interactions between the aromatic rings are indicated by the short distance between C2 and C12 of 3.580 (6) Å. Different sheets are linked together though hydrogen bonds (Table 1) between coordinated the water molecules and O atoms of the carboxylate groups to form a three-dimensional network (Fig. 2).

Experimental

Cd(NO₃)₂.4H₂O (0.5 mmol, 154 mg), benzene-1,4-dicarboxylate acid (0.5 mmol, 84 mg), and 1,10-phenanthroline (0.5 mmol 90 mg) were added into 30 ml of the mixed solvent water and EtOH (1:1). The mixture was stirred at room temperature for 30 minutes and the pH value was adjusted to 7 by 1M NaOH to get a clear solution. The solution was allowed to evaporate in the air. Plate crystals of the title compound were obtained after 2 days. The crystals were filtered, washed by cold MeOH and dried in air. Crystals of (I) suitable for single-crystal X-ray diffraction were selected directly from the sample as prepared.