Bis(5-chloro­salicylato-κO)bis­(1,10-phenanthroline-κ2 N,N′)cadmium(II)

Decai Wen; Jing Xie; Xiurong Jiang

doi:10.1107/S1600536808015687

. 2008 Jun 7;64(Pt 7):m851–m852. doi: 10.1107/S1600536808015687

Bis(5-chlorosalicylato-κO)bis(1,10-phenanthroline-κ² N,N′)cadmium(II)

Decai Wen ^a,^*, Jing Xie ^a, Xiurong Jiang ^a

PMCID: PMC2961793 PMID: 21202730

Abstract

In the title complex, [Cd(C₇H₄ClO₃)₂(C₁₂H₈N₂)₂], the Cd atom is coordinated by two 5-chlorosalicylate ligands and two 1,10-phenanthroline ligands, displaying a distorted octahedral coordination geometry. The crystal structure is stabilized by O—H⋯O and C—H⋯O hydrogen bonds and π–π interactions between the 1,10-phenanthroline ligands and 5-chlorosalicylate ligands, with a centroid–centroid distance between neighbouring aromatic rings of 3.730 (1) Å.

Related literature

For related literature, see: Lemoine et al. (2004 ▶); Melnik et al. (2001 ▶); Wen, Liu & Ribas (2007 ▶); Wen & Ying (2007 ▶); Wen, Ta et al. (2007 ▶); Yin et al. (2004 ▶); Zhu et al. (2003 ▶).

Experimental

Crystal data

[Cd(C₇H₄ClO₃)₂(C₁₂H₈N₂)₂]
M _r = 815.91
Orthorhombic,
a = 10.812 (3) Å
b = 16.495 (4) Å
c = 18.862 (5) Å
V = 3363.9 (14) Å³
Z = 4
Mo Kα radiation
μ = 0.86 mm⁻¹
T = 293 (2) K
0.25 × 0.23 × 0.22 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer
Absorption correction: none
32955 measured reflections
7696 independent reflections
5812 reflections with I > 2σ(I)
R _int = 0.086

Refinement

R[F ² > 2σ(F ²)] = 0.045
wR(F ²) = 0.086
S = 1.01
7696 reflections
461 parameters
H-atom parameters constrained
Δρ_max = 0.64 e Å⁻³
Δρ_min = −0.55 e Å⁻³
Absolute structure: Flack (1983 ▶), with 3402 Friedel pairs
Flack parameter: 0.00 (19)

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

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808015687/wn2261sup1.cif

e-64-0m851-sup1.cif^{(30.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808015687/wn2261Isup2.hkl

e-64-0m851-Isup2.hkl^{(376.5KB, hkl)}

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

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

Cd1—O4	2.261 (3)
Cd1—O1	2.336 (4)
Cd1—N4	2.400 (3)
Cd1—N2	2.400 (4)
Cd1—N1	2.422 (3)
Cd1—N3	2.423 (3)

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O4—Cd1—O1	82.14 (12)
O4—Cd1—N4	125.46 (12)
O1—Cd1—N4	83.28 (13)
O4—Cd1—N2	86.00 (13)
O1—Cd1—N2	156.59 (12)
N4—Cd1—N2	87.33 (12)
O4—Cd1—N1	84.29 (12)
O1—Cd1—N1	129.12 (13)
N4—Cd1—N1	141.39 (12)
N2—Cd1—N1	69.12 (12)
O4—Cd1—N3	164.68 (11)
O1—Cd1—N3	97.76 (14)
N4—Cd1—N3	69.51 (11)
N2—Cd1—N3	98.95 (13)
N1—Cd1—N3	83.98 (12)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O2	0.82	1.76	2.504 (6)	149
O6—H6⋯O5	0.82	1.83	2.553 (6)	147
C15—H15A⋯O2	0.93	2.45	3.181 (6)	136
C36—H36A⋯O5	0.93	2.34	3.134 (6)	143
C24—H24A⋯O3ⁱ	0.93	2.42	3.185 (6)	140

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Symmetry code: (i) Inline graphic .

Acknowledgments

This work was supported financially by the Education Department of Fujian Province (grant No. JA02261) and Longyan Science and Technology Bureau (grant No. 2003LY03).

supplementary crystallographic information

Comment

Salicylic acid and its derivatives continue to attract attention because of their versatile coordination modes (Zhu et al., 2003; Yin et al., 2004; Wen, Liu & Ribas, 2007) and biological applications (Lemoine et al., 2004). We report here the structure of a Cd (II) complex with the 5-chlorosalicylate ligand (Melnik et al., 2001; Wen & Ying, 2007; Wen, Ta et al., 2007). The title complex, Cd(C₇H₄ClO₃)₂ (C₁₂H₈N₂)₂, was synthesized under hydrothermal conditions.

The Cd atom is coordinated in a distorted octahedral coordination geometry by two O atoms from two 5-chlorosalicylate ligands and four N atoms from two 1,10-phenanthroline ligands (Fig. 1 and Table 1). The crystal structure is stabilized by O—H···O and C—H···O hydrogen bonds (Table 2), and π–π interactions between the 1,10-phenanthroline ligands and 5-chlorosalicylate ligands, with a centroid–centroid distance between neighbouring aromatic rings of 3.730 (1) Å (Fig. 2).

Experimental

A mixture of Cd(NO₃)₂.6H₂O (0.1 mmol), 1,10-phenanthroline (0.1 mmol), 5-chlorosalicylic acid (0.2 mmol) and distilled water (10 ml) was put into a Teflon-lined autoclave (20 ml) and then heated at 130 °C for 48 h. Colorless, block-like crystals of the title compound suitable for X-ray analysis were collected from the reaction mixture.