Structure of bis(5,6,11,12-tetrahydro-2,8-dimethylphenhomazine)-nickel(II) perchlorate

An X-ray diffraction study of the title compound, [NiL₂][ClO₄]₂·3CH₃NO ₂, was carried out to investigate the stereochemistry of the mesocyclic ligand complexed to nickel(II). The compound crystallizes in space group Pbnb with lattice constants a = 10.289(1), b = 18.471(3), c = 22.271(4) Å, and Z = 4. The intensity data were collected on a CAD-4 automated diffractometer and the structure was refined to a final R value of 0.068 for 1 339 unique reflections. The structure consists of discrete [NiL₂]²⁺ cations, ClO₄^- anions, and CH₃NO₂ molecules of crystallization. The axial positions are shielded by the hydrogen atoms of the rings, thus preventing octahedral co-ordination. The average Ni-N distance is 1.912(7) Å and the chelate bite angle N(1)-Ni-N(2) is 86.6(2)°.