Synthesis and structure of tetrachloro(o-phenanthroline)zirconium and product of its partial hydrolysis

By interaction of anhydrous ZrCL4 with acetonitrile solution of o-phenanthroline (o-Phen) compound ZrCl4·(o-Phen) (1) has been prepared. Using the method of X-ray diffraction analysis its molecular and crystal structure is determined. Zr atom has a distorted octahedral coordination by four Cl atoms and two N atoms. Parameters of monoclinic lattice of 1 are as follows: a=7.551, b=10.603, c=19.763 A, γ=108.10 deg, Z=4, sp.gr.P21/b. Thermal stability and structural characteristics of 1 and ZrCl4·(2,2-bipy) are compared. As a result of partial hydrolysis of 1 compound [o-PhenH]6[ZrCl6]Cl4 (2) has been prepared. Zr atom in ZrCl62- ion has almost regular octahedral surrounding by six Cl atoms. For 2 triclinic lattice parameters are: a=8.038, b=9.285, c=23.13 A, α=96.22, β=92.27, γ=77.85 deg, Z=1, sp.gr. P1