Aqua{N,N-dimethyl-N′-[1-(2-pyridyl)ethylidene]ethane-1,2-diamine-κ3 N,N′,N′′}bis(thiocyanato-κN)nickel(II)

In the title compound, [Ni(NCS)2(C11H17N3)(H2O)], the NiII ion is six-coordinated by the N,N′,N"-tridentate Schiff base N atoms, two cis-positioned N-bound isothiocyanate groups and one water molecule. In the crystal, O—H⋯S hydrogen bonds link adjacent molecules into infinite layers parallel to the ac plane. The layers are further connected into a three-dimensional network via C—H⋯π interactions. The –CH2–N(CH3)2 fragment is disordered over two sets of sites in a 0.556 (5):0.444 (5) ratio.

In the title compound, [Ni(NCS) 2 (C 11 H 17 N 3 )(H 2 O)], the Ni II ion is six-coordinated by the N,N 0 ,N"-tridentate Schiff base N atoms, two cis-positioned N-bound isothiocyanate groups and one water molecule. In the crystal, O-HÁ Á ÁS hydrogen bonds link adjacent molecules into infinite layers parallel to the ac plane. The layers are further connected into a threedimensional network via C-HÁ Á Á interactions. The -CH 2 -N(CH 3 ) 2 fragment is disordered over two sets of sites in a 0.556 (5):0.444 (5) ratio.

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 h followed by addition of a solution of nickel(II) acetate tetrahydrate (0.41 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. Brown crystals of the title compound were obtained by slow evaporation of the resulting reaction mixture.

Refinement
The C-bound H atoms were placed at calculated positions at distances C-H = 0.95, 0.98 and 0.99 Å for aryl, methyl and methylene type H-atoms, respectively. The O-bound H atoms were placed in a difference Fourier map, and were refined with distance restraint of O-H 0.84 (2) Å. For all hydrogen atoms Uiso(H) were set to 1.2-1.5 times Ueq(carrier atom).
C9, C10 and C11 were found to be disordered with two positions being resolved for each of the atoms. From anisotropic refinement, the major component of the disorder had a site occupancy factor of 0.556 (5). The N3-C methyl bond distances were restrained to be 1.470±0.001 Å. The N3-C9 and N3-C9' bond distances were refined with the distance restraint of 1.480±0.001 Å. The C8-C9 and C8-C9' bond distances were refined with the distance restraint of 1.52±0.001 Å.
The corresponding bond distances involving the disordered atoms were restrained to be equal with the SADI command in SHELXL97 (Sheldrick, 2008). An absolute structure was established using anomalous dispersion effects; 1798 Friedel pairs were not merged.
supplementary materials sup-2 Figures Fig. 1. Thermal ellipsoid plot of the title compound at the 50% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. Only the major disordered component is shown.