New binuclear aryl compounds of antimony: [Ph3SbOC(O)(CF2)3CF3]2O and [Ph3SbOC(O)(CF2)5CF3]2O

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The interaction of equimolar amounts of triphenylantimony, perfluoropentanoic and perfluoroheptanoic acids, and tert-butyl hydroperoxide in ether led to formation of compounds [Ph3SbOC(O)(CF2)3CF3]2O (1) and [Ph3SbOC(O)(CF2)5CF3]2O (2), yielding 69% and 98%, respectively, the structures were confirmed by X-ray diffraction analysis. The X-ray diffraction analysis was performed on a D8 Quest Bruker automatic four-circle diffractometer (Mo Kα radiation, λ = 0.71073 Å, graphite monochromator) at 293 K. Crystals (1) C92H60F36O10Sb4, M = 2496.40; triclinic syngony, symmetry group P-1; cell parameters: a = 10.924(10), b = 19.090(15), c = 23.22(2) Å;  = 93.03(3), β = 90.44(4),  = 90.42(4); V = 4834(7) Å3; Z = 2; calc = 1.715 g/cm3; 2 5.59454.932 deg.; total reflections 119542; independent reflections 21610; number of refined parameters 1256; Rint = 0.0560; GOOF 1.094; R1 = 0.0586, wR2 = 0,1410; residual electron density (max/min); 1.32/0.82 e/Å3], (2) C50H30F26O5Sb2, M = 1448.24; triclinic syngony, symmetry group P-1; cell parameters: a = 10.667(4), b = 16.972(9), c = 17.450(9) Å;  = 62.93(2), β = 77.977(17),  = 83.18(2) deg, V = 2750(2) Å3, Z = 2; calc = 1.749 g/cm3; 2 5.39454.294 deg; total reflections 42645; independent reflections 11288; number of refined parame-ters 737; Rint = 0.0590; GOOF 1.645; R1 = 0.1283, wR2 = 0.3459; residual electron density (max/min); 2.47/2.50 e/Å3]. The antimony atoms in 1 and 2 exhibit a distorted trigonal-bipyramidal coordination geometry with a bridging oxygen atom and a monodentate carboxylate ligand in the axial positions.

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Structure, binuclear, phenyl, carboxyl, antimony, X-ray structural analysis

Короткий адрес: https://sciup.org/147251988

IDR: 147251988   |   УДК: 546.86+547.53.024+546.16+548.312.5   |   DOI: 10.14529/chem250312