Study of the structure of tetraarylantimony <greek>b</greek>-diketonates Ph4Sb[MeC(O)CHC(O)Ph], p-Tol4Sb[MeC(O)CEtC(O)Me] ∙ 1½PhH, p-Tol4Sb[MeC(O)СHC(O)NHPh]

Abstract

Reaction of pentaphenylantimony and penta(para-tolyl)antimony with -diketones in benzene (100 °C, 1 h) forms tetraarylantimony -diketonates Ph4Sb[MeC(O)CHC(O)Ph] (1), p-Tol4Sb[MeC(O)CEtC(O)Me] ∙ 1½PhH (2), p-Tol4Sb[MeC(O)СHC(O)NHPh] (3), characterized by IR spectra and X-ray diffraction analysis. Crystals 1 [C34H29O2Sb, M 591.32; triclinic system, symmetry group P–1; cell parameters: a = 9.524(13) Å, b = 9.827(10) Å, c = 17.350(18) Å;  = 99.03(3), β = 101.50(6),  = 111.02(4), V = 1438(3) Å3, Z = 2; cal = 1.365 g/cm3], 2 [C44H48O2Sb, M 730.57; triclinic system, symmetry group P–1; cell parameters: a = 9.740(5) Å, b = 14.283(6) Å, c = 15.174(6) Å;  = 107.818(14), β = 90.292(18),  = 105.33(2), V = 1929,7(16) Å3, Z = 2; cal = 1.257 g/cm3], 3 [C34H30NO2Sb, M 606.34; monoclinic system, symmetry group P21/n; cell parameters: a = 9.396(17) Å, b = 10.23(2) Å, c = 29.45(6) Å; β = 95.91(6), V = 2817(10) Å3, Z = 4; cal = 1.430 g/cm3]. The obtained tetraarylantimony -diketonates are crystalline compounds with a distinct melting point, resistant to moisture and atmospheric oxygen, and highly soluble in aromatic solvents and polyhalide solvents. Complex 2 is a solvate and contains 1½ benzene molecules. According to the X-ray diffraction data, the antimony atoms in complexes 1–3 have a distorted octahedral coordination, with the chelate ring and two aryl substituents located in the equatorial plane, while two aryl ligands occupy axial positions.