Chloridobis(ethyl­enediamine-κ2 N,N′)(n-pentyl­amine-κN)cobalt(III) dichloride monhydrate

K Anbalagan; M Tamilselvan; S Nirmala; L Sudha

doi:10.1107/S1600536809022764

. 2009 Jun 27;65(Pt 7):m836–m837. doi: 10.1107/S1600536809022764

Chloridobis(ethylenediamine-κ² N,N′)(n-pentylamine-κN)cobalt(III) dichloride monhydrate

K Anbalagan ^a,^*, M Tamilselvan ^a, S Nirmala ^b, L Sudha ^c

PMCID: PMC2969482 PMID: 21582753

Abstract

The title complex, [CoCl(C₅H₁₃N)(C₂H₈N₂)₂]Cl₂·H₂O, comprises one chloridobis(ethylenediamine)(n-pentylamine)cobalt(III) cation, two chloride counter-anions and a water molecule. The Co^III atom of the complex is hexacoordinated by five N and one Cl atoms. The five N atoms are from two chelating ethylenediamine and one n-pentylamine ligands. Neighbouring cations and anions are connected by N—H⋯Cl and N—H⋯O hydrogen bonds to each other and also to the water molecule.

Related literature

For the potential applications of metal–chelate complexes, see: Tweedy (1964 ▶); Kralova et al. (2004 ▶); Parekh et al. (2005 ▶); Rajevel et al. (2008 ▶). For cobalt(III) complexes, see: Bailer & Clapp (1945 ▶); Bailer & Rollinson (1946 ▶). For a related structure, see: Ou et al. (2007 ▶).

Experimental

Crystal data

[CoCl(C₅H₁₃N)(C₂H₈N₂)₂]Cl₂·H₂O
M _r = 390.67
Monoclinic,
a = 10.5214 (3) Å
b = 7.2294 (2) Å
c = 23.6225 (6) Å
β = 96.117 (2)°
V = 1786.58 (8) Å³
Z = 4
Mo Kα radiation
μ = 1.41 mm⁻¹
T = 293 K
0.25 × 0.20 × 0.15 mm

Data collection

Bruker Kappa-APEX2 CCD diffractometer
Absorption correction: multi-scan (Blessing, 1995 ▶) T _min = 0.719, T _max = 0.816
23262 measured reflections
5510 independent reflections
4506 reflections with I > 2σ(I)
R _int = 0.029

Refinement

R[F ² > 2σ(F ²)] = 0.030
wR(F ²) = 0.090
S = 1.10
5510 reflections
181 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.52 e Å⁻³
Δρ_min = −0.35 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: APEX2 and SAINT (Bruker, 2004 ▶); data reduction: SAINT and XPREP (Bruker, 2004 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: PLATON (Spek, 2009 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809022764/bq2142sup1.cif

e-65-0m836-sup1.cif^{(20.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809022764/bq2142Isup2.hkl

e-65-0m836-Isup2.hkl^{(264.4KB, 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
N1—H1C⋯Cl3	0.90	2.39	3.2589 (14)	162
N1—H1D⋯O1	0.90	2.12	3.018 (3)	174
N3—H3C⋯Cl3	0.90	2.56	3.3641 (14)	150
N4—H4D⋯Cl3ⁱ	0.90	2.36	3.2597 (14)	179
N4—H4C⋯Cl2ⁱⁱ	0.90	2.51	3.3731 (15)	161
N5—H5C⋯Cl3ⁱⁱⁱ	0.90	2.51	3.3605 (15)	158
N5—H5D⋯Cl3ⁱ	0.90	2.56	3.3784 (15)	151

Open in a new tab

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

Acknowledgments

KA thanks the Department of Science and Technology, Goverment of India, for financial assistance and the Council of Scientific & Industrial Research–Human Resource Development Group, New Delhi, for support through a major research project.

supplementary crystallographic information

Comment

Metal-chelate complexes find potential applications in the research fields (Tweedy, 1964; Kralova et al., 2004) of antitumor activity, enzyme catalysis, functioning of micro organisms and in the respiration processes of biological systems (Parekh et al., 2005; Rajevel et al., 2008). Chelating ligand such as ethylenediamine has been widely used to prepare a number of cobalt(III) complexes (Bailer & Clapp, 1945; Bailer & Rollinson, 1946). A structural analogue of the cobalt(III)-alkyl amine complex, such as chloro(n-pentyl amine)bis(ethylenediamine)cobalt(III) chloride, [Co^III(en)₂(nPentNH₂) Cl]Cl₂, is studied. Cobalt(III) complex consisting of n-PentNH₂ligand, is an interesting complex showing some novel reactivity. Hence, single-crystal X-ray study of the above compound has been carried out.

The molecular structure of the title compound is shown in Fig. 1. The title compound, Cis-[Co^III(en)₂(nPentNH₂)Cl]Cl₂.H₂O, is a mononuclear cobalt(III) complex. The Co(III) atom is hexa-coordinated by six ligating atoms (five N and one Cl) forming two chelating ethylenediamine ligands, leading to a slightly distorted octahedral configuration. The two chloride ions act as counter-ions. The average Co— N bond length is 1.963 (4) Å and agrees well with related literature (Ou et al., 2007).

The crystal structure is stabilized by intramolecular N—H···O and N—H···Cl interactions. The molecules are linked into three-dimensional framework by N—H···Cl and C—H···Cl intermolecular interactions (Fig. 2, Table 1).

Experimental

A modified method of synthesize of cis-[Co^III(en)₂(nPentNH₂)Cl]Cl₂.H₂O was developed by substituting chloride ligand with AnalaR n-pentyl amine in trans-[Co(en)₂Cl₂]Cl. AnalaR n-pentyl amine (2–3 ml) was added in drops to a paste of 2 g of the trans-dichlorobis(1,2-diamino ethane)cobalt(III) chloride suspended in 1 ml of water. The mixture was ground for an hour until the solid becomes rosy red, and allowed overnight. The complex was recrystallized from acidified water. Single crystal was grown by adding the metal complex in triply distilled water containing few drops of conc. HCl and kept at 0°C for 2–3 weeks.