Dichloridotetrakis(3-methoxyaniline)nickel(II)

The complex sits in a general position. Each NiII ion has an N4Cl2 coordination sphere. Weak hydrogen bonding exists between three of the amino groups and the chloride ions of an adjacent molecule. Chains of molecules, linked by the hydrogen bonding and short Cl⋯Cl contacts, are well separated by the 3-methoxyaniline ligands.

It is also noteworthy that the conformations of the anisidine rings are such that three of the rings have their methoxy substituents tipped toward, and above, the Cl2 side of the NiN 4 plane.The O33-C33 methoxy group is also tipped in that direction, but due to the orientation of the N31-C31 bond, the methoxy group itself lies on the opposite side of the NiN 4 plane.

Figure 1
The molecular structure of the title compound with displacement ellipsoids drawn at the 50% probability level.Hydrogen atoms are shown as spheres of arbitrary size.Only those hydrogen atoms whose positions were refined are labeled.Hydrogen-bond geometry (A ˚, � ).

Figure 2
Chain formation via hydrogen bonding (b axis horizontal).

Synthesis and crystallization
Synthesis: 0.5035 g of 3-methoxyaniline were dissolved in 18 ml of EtOH, creating a red solution.NiCl 2 hexahydrate was dissolved in 25 ml of EtOH, creating a green solution.Both solutions were heated until they began to boil, at which point the methoxyaniline solution was poured into the nickel chloride solution, resulting in a peach-colored solution that quickly became cloudy.The mixture was repeatedly decanted to remove the majority of the precipitate over the course of two hours and then allowed to cool.The next day, a green powdery precipitate was collected using vacuum filtration and washed using DI water.The filtrate was collected and allowed to evaporate slowly.The next day, small dark-yellow crystals were observed and collected by vacuum filtration, 0.002 g (0.2%).

Refinement
Crystal data, data collection and structure refinement details are summarized in Table 3.

data reports
3 of 3

Special details
Geometry.All esds (except the esd in the dihedral angle between two l.s.planes) are estimated using the full covariance matrix.The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry.An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s.planes.

Table 3
Experimental details.