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

In the title compound, [CoCl(CH5N)(C3H10N2)2]Cl2·H2O, the CoIII ion has an octahedral coordination environment and is surrounded by four N atoms of two propane-1,3-diamine ligands in the equatorial plane, with another N atom of the methylamine ligand and a Cl atom occupying the axial positions. The crystal packing is stabilized by intermolecular N—H⋯O, N—H⋯Cl, and O—H⋯Cl interactions, generating a three-dimensional network.

In the title compound, [CoCl(CH 5 N)(C 3 H 10 N 2 ) 2 ]Cl 2 ÁH 2 O, the Co III ion has an octahedral coordination environment and is surrounded by four N atoms of two propane-1,3-diamine ligands in the equatorial plane, with another N atom of the methylamine ligand and a Cl atom occupying the axial positions. The crystal packing is stabilized by intermolecular N-HÁ Á ÁO, N-HÁ Á ÁCl, and O-HÁ Á ÁCl interactions, generating a three-dimensional network.
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) The interest in understanding the outer-sphere electron-transfer (OSET) reactions of transition metal complexes in mixed solvents has increased significantly in recent years. It was established that the method of linear solvation energy relationship (LSER) is a generalized treatment of solvation effects and can very well be used to understand the influence of solvent on reaction rates (Anbalagan et al., 2003). The present research is the design and synthesis of cobalt(III) complexes with an objective to understand the structure-reactivity correlation. Substituting an amino ligand for the MeNH 2 moiety can yield complexes of similar structure, but with differing electron transfer rate (Anbalagan, 2011;Anbalagan et al., 2011).
Such complexes can offer a clear correlation between structure and spectral characteristics, reactions in particular. The optical properties and mechanism of electron transfer reaction can be understood through the structure of these complexes.
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, antibiotics and antimicrobial activities, as well as their multiple applications in fields such as medicine and drug delivery (Chang et al.,2010). Against this background and to ascertain the molecular structure and conformation, the X-ray crystal structure determination of the title compound has been carried out.
The ORTEP plot of the molecule is shown in Fig. 1. The molecular structure is symmetric with respect to cobalt, the Co III ion has an octahedral coordination environment and 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 a axis is shown in Fig. 2. The molecules are stabilized by N-H···Cl, N-H···O and O-H···Cl intermolecular interactions generating a three-dimensional network.

Experimental
Two grams of trans-[CoIII(tn) 2 Cl 2 ]Cl solid was made in to paste using 3-4 drops of water. To the solid mass, about 0.12M methyl amine (MeNH 2 ) was added in drops for 20 min and mixed by grinding (Bailar & Work 1946). The grinding of the resulting dull green paste was continued to obtain red mass. The reaction mixture was set aside until no further change occurred and the product was allowed to stand overnight. Finally, the solid was washed and recrystallized using acidified water pre-heated to 70°C. The pure crystals were filtered, washed with ethanol and dried over vacuum. The microcrystalline solid obtained was pink colored and the yield was estimated to be 0.85 g (85%). X-ray quality crystals supplementary materials sup-2 Acta Cryst. (2013). E69, m205-m206 were grown after repeated recrystallization and using hot acidified water.

Refinement
N and C-bound H atoms were positioned geometrically (N-H =0.90 Å, C-H =0.93-0.97 Å) and allowed to ride on their parent atoms, with U iso (H) =1.5U eq (C) for methyl H atoms and 1.2U eq (C,N) for all other H atoms. The water H atoms were freely refined.

Figure 1
The molecular structure of the title compound, showing the atomic numbering and displacement ellipsoids drawn at 30% probability level.  The packing of the molecules viewed down a axis. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.