Structural features of pentaphenyl antimony, penta(para-tolyl)antimony, and their solvates with organic solvents

The structures of pentaphenylantimony, penta( para -tolyl)antimony, as well as their solvates with benzene, dioxane, tetrahydrofuran, and xylene were determined by X-ray diffraction analysis. According to the X-ray diffraction analysis carried out at 293 K on an automatic four-circle D8 Quest Bruker diffractometer (two-coordinate CCD detector, MoKα radiation, λ = 0.71073 Å, graphite monochromator) in pentaphenylantimony crystals Ph5Sb (1) [C30H25Sb, M 507.25; triclinic system, P-1 symmetry group; cell parameters: a = 10.286(3), b = 10.510(4), c = 13.590(4) Å; a = 68.29(2)°, β = 79.364(14)°, g = 61.272(12)°; V = 1196.9(7) Å3; Z 2; crystal size 0.5 ´ 0.38 ´ 0.29 mm; reflection index intervals -21 ≤ h ≤ 21, -21 ≤ k ≤ 21, -28 ≤ l ≤ 28; total reflections 177843; independent reflections 22858; R int 0.0446; GOOF 1.067; R 1 = 0.0440, wR 2 = 0.0848; residual electron density 1.09/-0.86 e/Å3, solvate of pentaphenylantimony with benzene Ph5Sb ∙ 0.5PhH (2) [C66H56Sb2, M 1092.61; triclinic system, P -1 symmetry group; cell parameters: a = 13.165(11), b = 14.394(16), c = 15.193(13) Å; a = 90.22(3)°, β = 113.71(2)°, g = 94.23(5)°; V = 2627(4) Å3; Z 2; crystal size 0.49 x 0.38 x 0.33 mm; reflection index intervals -16 ≤ h ≤ 16, -18 ≤ k ≤ 18, -19 ≤ l ≤ 19; total reflections 61668; independent reflections 11757; R int 0.0395; GOOF 1.022; R 1 = 0.0270, wR 2 = 0.0585; residual electron density 0.43/-0.63 e/Å3, solvate of pentaphenylantimony with dioxane Ph5Sb ∙ 0,5C4H8O2 (3) [C32H29OSb, M 551.30; triclinic system, P- 1 symmetry group; cell parameters: a = 10.451(5), b = 10.462(4), c = 13.323(5) Å; a = 75.647(11)°, β = 69.648(19)°, g = 86.300(19)°; V = 1322.8(9) Å3; Z 2; crystal size 0.43 ´ 0.35 ´ 0.27 mm; reflection index intervals -18 ≤ h ≤ 18, -18 ≤ k ≤ 18, -23 ≤ l ≤ 23; total reflections 99009; independent reflections 15054; R int 0.0505; GOOF 1.036; R 1 = 0.0554, wR 2 = 0.1038; residual electron density 1.04/-0.58 e/Å3, penta( para -tolyl)antimony p -Tol5Sb (4) [C35H35Sb, M 577.38; monoclinic system, P 21/ n symmetry group; cell parameters: a = 14.472(6), b = 12.084(7), c = 17.009(6) Å; β = 102.934(14); V = 2899(2) Å3; Z 4; crystal size 0.38 ´ 0.26 ´ 0.24 mm; reflection index intervals -19 ≤ h ≤ 19, -16 ≤ k ≤ 16, -22 ≤ l ≤ 22; total reflections 106229; independent reflections 7238; R int 0,0296; GOOF 1.081; R 1 = 0.0239, wR 2 = 0.0548; residual electron density 0.59/-0.69 e/Å3. Complete tables of atomic coordinates, bond lengths, and bond angles for the structure have been deposited with the Cambridge Crystallographic Data Center (Nos. 2124594 (1), 2121835 (2), 2124972 (3), 2124962 (4); deposit@ccdc.cam.ac). uk; https://www.ccdc.cam.ac.uk).