Tris(phenyl 2-pyridyl ketone oxime-κ2 N,N′)cadmium(II) dinitrate

Juan Yan; Guang-Xiang Liu

doi:10.1107/S1600536809017073

. 2009 May 14;65(Pt 6):m641. doi: 10.1107/S1600536809017073

Tris(phenyl 2-pyridyl ketone oxime-κ² N,N′)cadmium(II) dinitrate

Juan Yan ^a, Guang-Xiang Liu ^a,^*

PMCID: PMC2969799 PMID: 21583008

Abstract

The Cd atom in the title compound, [Cd(C₁₂H₁₀N₂O)₃](NO₃)₂, adopts a distorted octahedral geometry, being ligated by six N atoms from three different phenyl-2-pyridyl ketone oxime ligands. In the crystal structure, intermolecular O—H⋯O and C—H⋯O hydrogen bonds link the molecules into a chain structure propagating along [100]. The chains are further linked into a three-dimensional supramolecular structure via van der Waals forces.

Related literature

For related structures, see: Korpi et al. (2005 ▶); Pearse et al. (1989 ▶); Afrati et al. (2005 ▶); Stamatatos et al. (2006 ▶). For related literature on 2-pyridyl-substituted oximes, see: Papatriantafyllopoulou et al. (2007 ▶).

Experimental

Crystal data

[Cd(C₁₂H₁₀N₂O)₃](NO₃)₂
M _r = 831.08
Triclinic,
a = 10.618 (3) Å
b = 11.687 (4) Å
c = 15.279 (5) Å
α = 101.263 (4)°
β = 100.166 (4)°
γ = 101.807 (4)°
V = 1773.3 (10) Å³
Z = 2
Mo Kα radiation
μ = 0.68 mm⁻¹
T = 293 K
0.24 × 0.22 × 0.18 mm

Data collection

Bruker SMART Apex CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T _min = 0.853, T _max = 0.887
13329 measured reflections
6526 independent reflections
4387 reflections with I > 2σ(I)
R _int = 0.041

Refinement

R[F ² > 2σ(F ²)] = 0.046
wR(F ²) = 0.077
S = 1.08
6526 reflections
490 parameters
H-atom parameters constrained
Δρ_max = 0.45 e Å⁻³
Δρ_min = −0.54 e Å⁻³

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); 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, New_Global_Publ_Block. DOI: 10.1107/S1600536809017073/at2779sup1.cif

e-65-0m641-sup1.cif^{(31.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809017073/at2779Isup2.hkl

e-65-0m641-Isup2.hkl^{(319.4KB, 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
C32—H32⋯O8	0.93	2.48	3.355 (6)	157
C27—H27⋯O9ⁱ	0.93	2.58	3.191 (6)	123
C14—H14⋯O5ⁱⁱ	0.93	2.49	3.261 (6)	141
C4—H4⋯O3ⁱⁱⁱ	0.93	2.42	3.285 (5)	155
C3—H3A⋯O2ⁱⁱⁱ	0.93	2.56	3.461 (5)	164
O3—H3⋯O6	0.82	2.34	2.892 (4)	126
O3—H3⋯O4	0.82	2.00	2.820 (5)	176
O2—H2⋯O8	0.82	2.04	2.800 (5)	154
O2—H2⋯O7	0.82	2.21	2.939 (6)	149
O1—H1⋯O6	0.82	1.81	2.585 (4)	158

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

Acknowledgments

This work was supported by the National Natural Science Foundation of China (No. 20731004), the Natural Science Foundation for Outstanding Scholars of Anhui Province, China (grant No. 044-J-04011) and the Natural Science Foundation of Education Commission of Anhui Province, China (No. KJ2008B004).

supplementary crystallographic information

Comment

Pyridine-2-carbaldehyde oxime ligands usually bind to metals in a bidentate fashion, either chelating one metal center or bridging two metals. Their complexes find application in diverse areas such as functional supramolecular design, magnetic materials and catalysis (Korpi et al., 2005; Pearse et al., 1989; Afrati et al., 2005; Stamatatos et al., 2006). The title compound is a new cadmium complex from the reaction of Cd(NO₃)₂.4H₂O with phenyl-2-pyridyl ketone oxime (ppo). The compound consists of three N,N-chelating ligands and two nitrate anion. The three ppo ligands are coordinated to nickel to form three five-membered CdC₂N₂ rings.

The central cadmium atom adopts a distorted octahedral geometry (Fig. 1), which are ligated by six N atoms from three different phenyl-2-pyridyl ketone oxime ligands. The bond distances Cd—N, are in the expected ranges of 2.320 (3)–2.402 (3) Å, and the coordination angles around Ni atom are in the range 68.00 (11)–172.80 (12)°. In the crystal structure, intermolecular C—H···O hydrogen bonds link the molecules into one-dimensional chain structure, which are further linker into three-dimensional supramolecular structure via van der Waals forces.

Experimental

A colourless solution of phenyl-2-pyridyl ketone oxime (0.394 g, 2.00 mmol) in MeOH (10 ml) was slowly added to a solution of Cd(NO₃)₂.4H₂O (0.308 g, 1.00 mmol) in MeOH (10 ml) and the resulting colourless solution was stirred for 1 h at room temperature. A small quantity of undissolved material was removed by filtration. The filtrate was allowed to stand undisturbed in a closed flask for a period of 7–8 d. Colourless block crystals appeared which were collected by filtration, washed with cold MeOH (1 ml) and ice-cold Et₂O (2 ml), and dried in air [yield: 70%].