Abstract
Pentaphenylantimony reacts with 1,2,3,4-tetrahydroacridine-9-carboxylic and coumarin-3-carboxylic acids in benzene at room temperature to form tetraphenylantimony carboxylates Ph4SbOC(O)R, R = C13H12N (1), C9H5O2 (2), the structure of which has been determined by X-ray diffraction analysis (XRD). According to the X-ray diffraction data, the antimony atoms in molecules 1 and 2 have a distorted trigonal bipyramidal coordination with three phenyl substituents in the equatorial plane, the CSbO axial angles are 175.85(7) and 177.6(6), the sum of the angles between equatorial bonds are 356.31(8) and 356.5(6). The SbC equatorial bonds (2.112(2)–2.125(2) Å for 1 and 2.128(16)–2.131(16) Å for 2 are shorter than the axial ones (2.174(2) Å for 1 and 2.224(12) Å for 2. The SbO bond lengths (2.2793(18) Å in 1 and 2.204(13) Å in 2) exceed the sum of the covalent radii of antimony and oxygen atoms. It has been established that the geometric characteristics of the free coumarin-3-carboxylic acid molecule (3) and the acid residue included in complex 2 differ significantly. The X-ray diffraction data: a D8 Quest diffractometer from Bruker (MoKα radiation, λ = 0.71073 Å, graphite monochromator, at 293(2) K. [(1) C38H32NO2Sb, M = 656.40; monoclinic system, space group Р21/c; crystal size 0.480.230.18 mm; cell parameters: a = 9.063(4) Å, b = 15.911(8) Å, c = 21.495(11) Å; β = 94.719(16), V = 3089(3) Å3, Z = 4; calc = 1.411 g/cm3; = 0.927 mm–1; F(000) = 1336.0; collection region for 2q: 5.66–62.12; –13 ≤ h ≤ 10, –23 ≤ k ≤ 23, –31 ≤ l ≤ 31; total reflections 146090; independent reflections 9883 (Rint = 0.0591); GOOF = 1.052; R-factor is 0.0338; (2) C34H24O4Sb, M = 619.29; triclinic system, space group P–1; crystal size 0.610.420.29 mm; cell parameters: a = 9.533(4) Å, b = 10.560(4) Å, c = 16.397(6) Å; = 97.431(13), β = 98.49(2), = 108.962(12), V = 1516.1(9) Å3, Z = 2; calc = 1.357 g/cm3; = 0.944 mm–1; F(000) = 624.0; collection region at 2q: 5.7–55.64; –12 ≤ h ≤ 12, –13 ≤ k ≤ 13, –21 ≤ l ≤ 21; total reflections 19837; independent reflections 12162 (Rint = 0.0707); GOOF = 1.087; R-factor is 0.0543; (3) 3 C10H6O4, M = 190.15; monoclinic system, space group Р21/n; crystal size 0.11 0.24 0.29 mm; cell parameters: a = 11.390(6) Å, b = 5.534(3) Å, c = 13.890(8) Å; = 90.00, β = 106.33(3), = 90.00, V = 840.1(7) Å3, Z = 4; calc = 1.503 g/cm3; = 0.118 mm –1; F(000) = 392.0; collection region at 2q: 6.12–55.04; –14 ≤ h ≤ 14,7 ≤ k ≤ 7, –18 ≤ l ≤ 17; total reflections 23991; independent reflections 1917 (Rint = 0.0263); GOOF = 1.072; R-factor is 0.0406].
Published Version
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