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

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Reaction of pentaphenylantimony and penta(para-tolyl)antimony with b-diketones in benzene (100 °C, 1 h) forms tetraarylantimony b-diketonates Ph4Sb[MeC(O)CHC(O)Ph] (1), p-Tol4Sb[MeC(O)CEtC(O)Me] ∙ 1½PhH (2), p-Tol4Sb[MeC(O)CHC(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; a = 99.03(3)°, β = 101.50(6)°, g = 111.02(4)°, V = 1438(3) Å3, Z = 2; rcal = 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; a = 107.818(14)°, β = 90.292(18)°, g = 105.33(2)°, V = 1929,7(16) Å3, Z = 2; rcal = 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; rcal = 1.430 g/cm3]. The obtained tetraarylantimony b-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.

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Tetraarylantimony b-diketonates, synthesis, structure, ir spectra, x-ray diffraction analysis

Короткий адрес: https://sciup.org/147244640

IDR: 147244640   |   DOI: 10.14529/chem240210

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