V. Ermakova, O. Sharutina
2018
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Chem
Abstract
The interaction of tris(5-bromo-2-methoxyphenyl)bismuth with bromodifluoroacetic acid in the presence of hydrogen peroxide in diethyl ether at the molar ratio (1: 2: 1) leads to the formation of tris(5-bromo-2-methoxyphenyl)bismuth bis(bromodifluoroacetate) ( 1 ) with 80 % yield after recrystallization from the benzene-petroleum ether mixture. The use of tert-butyl hydroperoxide as the oxidizing agent does not lead to the formation of the desired prod-uct. Compound 1 is characterized by IR spectroscopy and X-ray diffraction analysis. Accord-ing to X-ray diffraction data, there are two types of crystallographically independent mole-cules in the crystal, the geometric characteristics of which differ slightly. The bismuth atom in the molecule has distorted trigonal-bipyramidal coordination with oxygen atoms of car-boxylate substituents in axial positions and carbon atoms of the aryl groups at equatorial positions. The angles between the axial and equatorial substituents OBi(1,2)O and CBi(1,2)C are 169.3(5)°, 170.6(7)° and 113.1(8)° –123.5(8)°, 118.1(7)°– 123.1(8)°. The bond lengths of Bi(1,2)–O and Bi(1,2)–C are 2.256(16), 2.276(19) Å; 2.261(14), 2.316(16) Å and 2.15(2)– 2.23(2) Å; 2.18(2)– 2.19(2) Å. The intramolecular distances between the valence-free non-bound atoms are Bi(1,2) ⋅⋅⋅ O(=C) (3.16(2), 3.57(4) Å, 3.11(2), 3.18(2) Å) and Bi(1,2) ⋅⋅⋅ OMe (3.00(2) – 3.17(2) Å, 3.04(2) – 3.14(2) Å) are less than the sum of the Van-der-Waals radii of Bi and O atoms. Crystallographic characteristics of 1 : the space group (cid:1842)1 ; cell parameters: a = 12.775(14) Å, b = 15.999(12) Å, c = 17.196(16) Å; α = 88.09(3) degrees, β = 68.67(5) degrees, γ = 87.92 (4) degrees; V = 3271 (5) Å 3 . Full tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data Bank (no. 1833279; deposit@ccdc.cam.ac.uk; http: //www.ccdc. Cam.ac.uk).