Synthesis and structure of bis[(3-trifluoromethyl)phenyl]bismuth bromide

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Tris[(3-trifluoromethyl)phenyl]bismuth was synthesized by the interaction of (3-trifluoromethyl)phenylmagnesium bromide with bismuth trichloride in diethyl ether. Treatment of tris[(3-trifluoromethyl)phenyl]bismuth with hydrobromic acid under mild conditions (ether, 20°C, 24 h) led to formation of bis[(3-trifluoromethyl)phenyl]bismuth bromide (1). According to X-ray diffraction data, crystals of 1 are a coordination polymer [C14H8BiBrF6, M 579.09, monoclinic syngony, symmetry group P21/c, cell parameters: a = 9.80642(7), b = 8.95563(6), c = 18.60999(13) Å, = 90.00, β = 102.0811(7), = 90.00, V = 1598.183(19) Å3, Z = 4, cal = 2.407 g/cm3, crystal size 0.10.070.05 mm, 2 9.222139.97, index range –11 ≤ h ≤ 11, –10 ≤ k ≤ 10, –22 ≤ l ≤ 22, total reflections 25622, independent reflections 3026, number of refined parameters 209, Rint = 0.0445, GOOF 1.084, R1 = 0.0193, wR2 = 0.0485, residual electron density (max/min): 1.11/1.04 e/Å3], in which the Ar2BiBr trigonal bipyramidal molecules are linked to each other by bridging bromine atoms, forming 1D poly-mer chains oriented along the crystallographic b axis. In the equatorial plane at the central metal atom there are two aryl ligands (CBiC 95.16(13)) and a lone electron pair. The Bi−C bond lengths are 2.246(4) and 2.249(3) Å; the BrBiC bond angles are 84.99(9)–92.20(10)°. Fluorine atoms do not form any H∙∙∙F hydrogen bonds, however, in 1 the F∙∙∙Bi intermolecular contact is observed (3.462 Å), which is less than the sum of the Van der Waals radii of fluorine and bismuth atoms (3.54 Å). Complete tables of atomic coordinates, bond lengths, and valence angles for the structures have been deposited with the Cambridge Crystallographic Data Centre (No. 2449619, deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).

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Tris[(3-trifluoromethyl)phenyl]bismuth, bis[(3-trifluoromethyl)phenyl]bismuth bromide, hydrobromic acid, synthesis, structure, X-ray diffraction analysis

Короткий адрес: https://sciup.org/147251979

IDR: 147251979   |   УДК: 546.87+547.53.024+546.14+548.312.4   |   DOI: 10.14529/chem250302