catena-Poly[[{N,N-dimethyl-N′-[1-(pyridin-2-yl)ethyl­idene]ethane-1,2-diamine-κ3 N,N′,N′′}(thio­cyanato-κN)cadmium]-μ-thio­cyanato-κ2 S:N]

Nura Suleiman Gwaram; Hamid Khaledi; Hapipah Mohd Ali

doi:10.1107/S1600536811010063

. 2011 Mar 26;67(Pt 4):m480. doi: 10.1107/S1600536811010063

catena-Poly[[{N,N-dimethyl-N′-[1-(pyridin-2-yl)ethylidene]ethane-1,2-diamine-κ³ N,N′,N′′}(thiocyanato-κN)cadmium]-μ-thiocyanato-κ² S:N]

Nura Suleiman Gwaram ^a, Hamid Khaledi ^a,^*, Hapipah Mohd Ali ^a

PMCID: PMC3099776 PMID: 21753992

Abstract

In the title compound, [Cd(NCS)₂(C₁₁H₁₇N₃)]_n, the Cd^II atom is octahedrally coordinated by the N,N′,N′′-tridentate Schiff base ligand and one terminal thiocyanate N atom. Two trans-N:S-bridging thiocyanates complete the N₅S donor set around the Cd atom. In the crystal, adjacent Cd^II ions are linked by the thiocyanate N:S-bridges into polymeric chains along the c axis.

Related literature

For the structures of some cadmium thiocyanate complexes with nitrogen-based ligands, see: Banerjee et al. (2005 ▶). For a singly bridged cadmium thiocyanate complex, see: Bose et al. (2004 ▶). For a triply bridged cadmium thiocyanate complex, see: Chen et al. (2002 ▶). For an S-bound terminal thiocyanate cadmium complex, see: Nfor et al. (2006 ▶).

Experimental

Crystal data

[Cd(NCS)₂(C₁₁H₁₇N₃)]
M _r = 419.84
Monoclinic,
a = 14.602 (2) Å
b = 9.5827 (14) Å
c = 12.8714 (19) Å
β = 107.483 (2)°
V = 1717.9 (4) Å³
Z = 4
Mo Kα radiation
μ = 1.51 mm⁻¹
T = 100 K
0.35 × 0.29 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.619, T _max = 0.889
19975 measured reflections
3756 independent reflections
3298 reflections with I > 2σ(I)
R _int = 0.047

Refinement

R[F ² > 2σ(F ²)] = 0.023
wR(F ²) = 0.056
S = 1.07
3756 reflections
193 parameters
H-atom parameters constrained
Δρ_max = 0.54 e Å⁻³
Δρ_min = −0.73 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: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811010063/om2412sup1.cif

e-67-0m480-sup1.cif^{(17.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811010063/om2412Isup2.hkl

e-67-0m480-Isup2.hkl^{(184.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Cd1—N4	2.2406 (18)
Cd1—N5	2.3008 (19)
Cd1—N2	2.3345 (17)
Cd1—N1	2.3801 (18)
Cd1—N3	2.3820 (19)
Cd1—S2	2.7803 (6)

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors thank the University of Malaya for funding this study (FRGS grant No. FP004/2010B).

supplementary crystallographic information

Comment

Thiocyanate anion is known to bind the cadmium ion in different modes: terminal N-bound, terminal S-bound (Nfor et al. 2006) or N:S-bridging ligand. As a bridging ligand, it may give rise to a singly bridged (Bose et al. 2004), doubly bridged or triply bridged (Chen et al. 2002) cadmium complex. The title compound is a mixed-ligand cadmium complex with thiocyanate and the Schiff base N,N-dimethyl-N'-[methyl(2-pyridyl)methylene]ethane-1,2-diamine. Similar to what was observed in the cadmium thiocyanate adduct of the similar Schiff base, N,N-diethyl-N'-[methyl(2-pyridyl)methylene]ethane-1,2-diamine (Banerjee et al. 2005), the thiocyanate ions act as either bridging or terminal ligands. However, different from the doubly bridged dimeric structure of the former, in the present structure the bridging thiocyanate ligands singly bridge the adjacent metal centers, related by symmetry x, –y+1/2, z - 1/2, into infinite chains along the c axis. Within this coordination polymer, the Cd^II ions are separated by the distance of 8.0234 (9) Å. Two thiocyanate N:S-bridges, one terminal thiocyanate N atom and the N,N',N"-tridentate Schiff base make a distorted octahedral geometry around the Cd(II) atoms.

Experimental

A mixture of 2-acetylpyridine (0.2 g, 1.65 mmol) and N,N-dimethylethyldiamine (0.15 g, 1.65 mmol) in ethanol (20 ml) was refluxed for 2 hr followed by addition of a solution of cadmium(II) acetate dihydrate (0.44 g, 1.65 mmol) and sodium thiocyanate (0.27 g, 3.3 mmol) in a minimum amount of water. The resulting solution was refluxed for 30 min, then set aside at room temperature. The crystals of the title compound were obtained in a few days.