Benzene solvates of tris(4-fluorophenyl)antimony diaryloxides (4-FC6H4)3Sb(OAr)2 • 1/2PhH (Ar = C6H4Cl-4, C6H4Br-4, C6H3Br2-2,4). Synthesis and structure

Resumo

The solvates of tris(4-fluorophenyl)antimony diaryloxides with benzene, (4-FC₆H₄)₃Sb(OAr)₂ • 1/2PhH (Ar = C₆H₄Cl-4 (I), C₆H₄Br-4 (II), and C₆H₃Br₂-2,4 (III)), were prepared by the reaction of tris(4-fluorophenyl)antimony with 4-chlorophenol, 4-bromophenol, and 2,4-dibromophenol in diethyl ether in the presence of tert-butyl hydroperoxide followed by recrystallization from a benzene–heptane mixture (2: 1). The antimony atoms in I, II, and III form a distorted trigonal-bipyramidal coordination with oxygen atoms in axial positions (CIF files CCDC nos. 1047500 (I), 1048172 (II), 1048212 (III)). The OSbO angles are 177.23(8)° (I), 177.34(12)° (II), and 179.47(16)° (III). The Sb–O and Sb–C bond lengths are 2.0519(16), 2.0508(18), and 2.105(2)–2.121(2) Å (I); 2.045(3), 2.055(3), and 2.105(4)–2.126(4) Å (II); and 2.066(3), 2.058(3), and 2.100(6)–2.107(5) Å (III). The structural organization in crystals I–III is formed by weak intermolecular C−H•••F hydrogen bonds (H•••F 2.52 Å (I), 2.52 Å (II), and 2.61 and 2.51Å (III)).