cis-Chlorido(ethyl­amine)­bis­(propane-1,3-diamine)­cobalt(III) dichloride

Velusamy Maheshwaran; Viswanathan Thiruselvam; Munisamy Manjunathan; Krishnamoorthy Anbalagan; Mondikalipudur Nanjappa Gounder Ponnuswamy

doi:10.1107/S1600536813004650

. 2013 Feb 23;69(Pt 3):m170–m171. doi: 10.1107/S1600536813004650

cis-Chlorido(ethylamine)bis(propane-1,3-diamine)cobalt(III) dichloride

Velusamy Maheshwaran ^a, Viswanathan Thiruselvam ^a, Munisamy Manjunathan ^b, Krishnamoorthy Anbalagan ^b, Mondikalipudur Nanjappa Gounder Ponnuswamy ^a,^*

PMCID: PMC3588535 PMID: 23476511

Abstract

In the title compound, [CoCl(C₂H₇N)(C₃H₁₀N₂)₂]Cl₂, the Co^III ion has a distorted octahedral coordination environment and is surrounded by four N atoms in the equatorial plane, with the other N and Cl atoms occupying the axial positions. The crystal packing is stabilized by N—H⋯Cl hydrogen bonds, forming a layered arrangement parallel to (1-10).

Related literature

For supramolecular structures, see: Desiraju (1995 ▶); Khlobystov et al. (2001 ▶); Lehn (1995 ▶); Seo et al. (2000 ▶). For Co^III complexes, see: Chang et al. (2010 ▶). For related and comparable structures, see: Anbalagan et al. (2009 ▶); Lee et al. (2007 ▶); Ramesh et al. (2008 ▶); Ravichandran et al. (2009 ▶). For the preparation of (1,3-diaminopropane)cobalt(III), see: Bailar & Work (1946 ▶).

Experimental

Crystal data

[CoCl(C₂H₇N)(C₃H₁₀N₂)₂]Cl₂
M _r = 358.63
Triclinic,
a = 7.8847 (4) Å
b = 8.0627 (4) Å
c = 12.6526 (5) Å
α = 102.780 (3)°
β = 99.936 (4)°
γ = 92.580 (4)°
V = 769.76 (6) Å³
Z = 2
Mo Kα radiation
μ = 1.62 mm⁻¹
T = 293 K
0.45 × 0.35 × 0.35 mm

Data collection

Oxford Diffraction Xcalibur Eos diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009 ▶) T _min = 0.600, T _max = 1.000
4965 measured reflections
2711 independent reflections
2299 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.025
wR(F ²) = 0.060
S = 0.99
2711 reflections
194 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.30 e Å⁻³
Δρ_min = −0.35 e Å⁻³

Data collection: CrysAlis CCD (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2009 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: PLATON.

Supplementary Material

Click here for additional data file.^{(19.8KB, cif)}

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536813004650/bt6888sup1.cif

e-69-0m170-sup1.cif^{(19.8KB, cif)}

Click here for additional data file.^{(133.1KB, hkl)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813004650/bt6888Isup2.hkl

e-69-0m170-Isup2.hkl^{(133.1KB, 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
N2—H2D⋯Cl2ⁱ	0.84 (2)	2.77 (2)	3.5033 (19)	145.6 (18)
N3—H3C⋯Cl2ⁱ	0.79 (2)	2.49 (2)	3.275 (2)	168 (2)
N1—H1D⋯Cl2ⁱⁱ	0.82 (2)	2.52 (2)	3.3278 (19)	173.2 (18)
N3—H3D⋯Cl2ⁱⁱ	0.87 (2)	2.72 (2)	3.472 (2)	145.6 (18)
N4—H4C⋯Cl3ⁱⁱⁱ	0.88 (2)	2.40 (2)	3.261 (2)	163.7 (19)
N5—H5D⋯Cl3ⁱⁱⁱ	0.82 (2)	2.57 (2)	3.329 (2)	154 (2)

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

Acknowledgments

KA is thankful to the CSIR, New Delhi (Lr: No. 01 (2570)/12/EMR-II/3.4.2012) for financial support through a major research project. The authors are thankful to the Department of Chemistry, Pondicherry University, for the single-crystal XRD instrumentation facility.

supplementary crystallographic information

Comment

In recent years, considerable effort has been dedicated to the design and synthesis of supramolecular architectures of coordination complexes (Lehn, 1995; Khlobystov et al.,2001). The primary reason for the interest in such complexes is their new and versatile topologies and potential applications in functional materials (Desiraju, 1995; Seo et al., 2000).

The interaction of transition metal polyamine complexes of cobalt(III) with DNA has received considerable attention in the recent years. Using mixed ligand complexes, it is possible to systematically vary parameters of interest by changing the properties of the interacting units either by the use of suitable substituents or simply by changing the nature of ancillary ligand.

In addition, cobalt(III) complexes have received a sustained high level of attention due to their relevance in various redox processes in biological systems and act as promising agents for antitumor, anthelmintic, antiparasitic, antibiotic and antimicrobial activities, as well as their multiple applications in fields of medicine and drug delivery (Chang et al., 2010). Against this background and to ascertain the molecular structure and conformation of the title compound, the crystal structure determination has been carried out.

The ORTEP plot of the molecule is shown in Fig. 1. The molecular geometry is not a perfect octahedron. The metal centre is surrounded by four N atoms in an equatorial plane, with the other N and Cl atoms occupying the axial positions.

The bond lengths [Co—N] and [Co—Cl] are comparable with the values reported in the literature (Lee et al., 2007; Ramesh et al., 2008; Anbalagan et al., 2009; Ravichandran et al., 2009).

The packing of the molecules viewed down the a axis is shown in Fig. 2. The packing is stabilized by N—H···Cl and N—H···N types of inter- and intramolecular interaction.

Experimental

2 grams of trans-[Co^III(tn)2Cl₂]Cl solid was made in the path using 3–4 drops of water. To the solid mass, about 0.12M ethyl amine (EtNH₂) was dropped for 20 min and mixed well. The grinding was continued until the colour turned dull green to red (Bailar & Work, 1946). The reaction mixture was set aside until no further change was observed and the product was allowed to stand overnight. Finally, the solid was washed. The final solid was dissolved in 5–10 ml of water pre-heated to 70°C and allowed to crystallize using hot acidified water. Finally Microcrystalline pink color crystal was retrieved (yield 0.85 g). The crystals were filtered, washed with ethanol and dried over vacuum. X-ray quality crystals were obtained by recrystallization from hot acidified distilled water.