The electrical conductivity, photoconductivity, and electrical and magneto-optical properties of the films of new polycomplexes of 4-methacryloyloxy-(4 ′ -carboxy-3 ′ -oxy)-azobenzene with nickel and cobalt have been investigated. The electrical conductivity and photoconductivity in the visible region of light are determined by the orientation effects of azobenzene groups as well as by generation and transfer of charge carriers between them. A change in the spatial orientation of photoinduced dipole moments of azobenzene groups in an external electric or magnetic field is attributed to the appearance of forces acting on electrically charged magnetic ions of a metal and that are rigidly connected with these groups.Introduction. Films of polymeric compositions with the monomers of azo dyes [1-3] or containing azobenzene side groups chemically bound with the base by a polymer chain [4][5][6] are of interest as optically active media. Under the action of a linearly polarized light, an induced polarization appears in them which at room temperature may persist for a rather long time. The induced polarization can change under the action of an external thermal or mechanical effect, on irradiation by light, and on superposition of an external electric or magnetic field. In an external field, rotation of the dipole moments occurs, and sometimes the effect of photoconductivity is observed, owing its origin to the photogeneration of charge carriers, which makes it possible to use such materials in xerography [6]. To enhance the influence of the magnetic field, polymeric compositions are prepared either on the basis of metal-containing monomers [7] or with addition of magnetic nanoparticles [8,9]. Since the mechanism of the effect of the electric and magnetic field is associated with the appearance of forces that rotate the dipole moments of azo compounds [10,11], an assumption suggests itself that the electro-optical and magneto-optical effects must manifest themselves in polymers with azo groups and ions of magnetic metals that are chemically bound with the polymer. Therefore, the aim of the present work is investigation of the electro-and photophysical properties of the films of such polycomplexes.Objects, Specimens, and Experimental Technique. For investigations we have synthesized for the first time the polymer poly-4-methacryloyloxy-(4 ′ -carboxy-3 ′ -oxy)azobenzene (PA) and polycomplexes 4-methacryloyloxy-(4 ′ -carboxy-3 ′ -oxy)azobenzene with nickel (PA-Ni) and cobalt (PA-Co), the structural formulas of which have the form