The structures of five organoantimony compounds Ph4SbOCH2Ph (1), p-Tol4SbBr (2), [Ph4Sb][I3] (3), [Ph3PCH2СHMe2][I3] (4) and [Ph3P(CH2)3PPh3]+2 [I]2  I2 (5) were determined by X-ray diffraction analysis. X-ray diffraction of the compounds was carried out on an automatic four-circle diffractometer D8 Quest Bruker (МоКα, λ = 0,71073 Å, 293 К. (1), crystal size 0.3 × 0.18 × 0.1 mm, P21/c, a = 14.512(7), b = 10.554(4), c = 17.209(9) Å, β = 106.91(2) deg., V = 2522(2) Å3, Z = 4, R1 = 0.0206, wR2 = 0.0457. (2), crystal size 0.38 × 0.22 × 0.18 mm, P21/n, a = 9.896(6), b = 23.349(11), c = 12.149(6) Å, β = 113.393(18) deg., V = 2576(2) Å3, Z = 4, R1 = 0.0321, wR2 = 0.0673. (3), crystal size 0.3×0.21×0.13 mm, P2/n, a = 10.679(18), b = 8.178(14), c = 15.07(3) Å, β = 92.89(11) deg., V = 1315(4) Å3, Z = 2, R1 = 0.0297, wR2 = 0.0589. (4), crystal size 0.27×0.14×0.05 mm, P21/c, a = 10.199(5), b = 17.886(11), c = 13.300(9) Å, β = 91.77(2), deg., V = 2425(2) Å3, Z = 4, R1 = 0.0531, wR2 = 0.1331. (5), crystal size 0.46×0.29×0.18 мм, P21, a = 8.613(3), b = 15.509(6), c = 14.875(5) Å, β = 93.349(11), deg., V = 1940(6) Å3, Z = 2, R1 = 0.0297, wR2 = 0.0678.