Complex salts of the composition [Co(NH 3 ) 6 ](ReO 4 ) 3 ⋅2H 2 O (I), [Co(en) 3 ](ReO 4 ) 3 (II), [Co(NH 3 ) 5 H 2 O](ReO 4 ) 3 ⋅2H 2 O (III), and [Co(NH 3 ) 5 Cl](ReO 4 ) 2 ⋅0.5H 2 O (IV) are obtained. Their crystal structures are determined by single crystal XRD. Crystallographic characteristics: (I) a = 9.9797(3) Å, b = 12.6994(3) Å, c = 14.7415(4) Å, β = 102.870(1)°, C2/c space group; (II) a = 8.0615(3) Å, b = 8.4483(4) Å, c = 8.8267(4) Å, α = 61.923(2)°, β = 89.552(2)°, γ = 72.295(2)°, P1 space group; (III) a = 8.0086(4) Å, b = 12.9839(6) Å, c = 17.5122(7) Å, β=91.858(1)°, P2 1 /n space group; (IV) a = 14.9446(3) Å, b = 14.6562(4) Å, c = 12.2434(4) Å, Cmc2 1 space group. Compounds consisting of complex cations and anions (double complex salts) are considered as precursors of various nanoscale bimetallic powders [1, 2]. Complex salts in which one of the metals is rhenium are of interest, in particular, the compounds in which the cationic part is a complex ion of any metal and the anionic part consists of the perrhenate ion. Therefore, complex compounds of the composition [M(NH 3 ) 5 Cl](ReO 4 ) 2 , where M = Ir, Rh, Ru, Cr, Co [3], [M(NH 3 ) 4 ](ReO 4 ) 2 (M = Pd, Pt) [4, 5], [Pt(NH 3 ) 5 Cl](ReO 4 ) 3 ⋅2H 2 O [6], [Au(dien)Cl](ReO 4 ) 2 , where dien is diethylenetriamine C 4 H 13 N 3 [7] have previously been studied.The purpose of this work is to synthesize and structurally investigate some amine complexes of cobalt(III) with a ratio Co:Re = 1:3, such as [Co(NH 3 ) 6 ](ReO 4 ) 3 ⋅2H 2 O (I), [Co(en) 3 ](ReO 4 ) 3 (II), where en is ethylenediamine C 2 Н 8 N 2 , [Co(NH 3 ) 5 H 2 O](ReO 4 ) 3 ⋅2H 2 O (III), and also to determine the crystal structure of [Co(NH 3 ) 5 Сl](ReO 4 ) 2 ⋅0,5H 2 O (IV) (metal ratio is 1:2). For the first time, compound IV was obtained in the synthesis of a series of complex compounds [M(NH 3 ) 5 Cl]× (ReO 4 ) 2 , where M = Ir, Rh, Ru, Cr, Co [3]. However, the diffraction pattern of the polycrystalline sample was indexed using the structural data for [Rh(NH 3 ) 5 Cl](ReO 4 ) 2 complex salt, and their isostructurality was established. The description of the crystal structure of [Co(NH 3 ) 5 Сl](ReO 4 ) 2 ⋅0.5H 2 O (IV) determined by single crystal XRD is given in the present work. EXPERIMENTAL In the work, we used NaReO 4 (chemically pure), [Co(en) 3 ]Cl 3 [8], [Co(NH 3 ) 5 Cl]Cl 2 , and [Co(NH 3 ) 6 ]Cl 3 [9] complexes obtained by the known procedures.