Triarylantimony dicarboxylates Ph3Sb[OC(O)CF2CF2CF3]2,(3-FC6H4)3Sb[OC(O)C6F5)]2· 1?PhH, p-Tol3Sb[OC(O)CF2Br]2

The oxidative addition reaction between triphenylantimony, tris(3-fluorophenyl)antimony and tris(para-tolyl)antimony and carboxylic acid in the presence of t-butyl hydroperoxide in diethyl ether leads to high-yield synthesis of bis(heptafluorobutanato)triphenylantimony (1), bis(pentafluorobenzoato)tris(3-fluorophenyl)antimony (2), and bis(bromodifluoroacetato)tris(para-tolyl)antimony (3) . The compounds have been identified by X-ray structural analysis. According to the X-ray diffraction data, crystal 1 consists of four types of crystallographically independent molecules, target product 2 is a solvate with benzene, and 3 contains two types of crystallographically independent molecules. In the molecules of compounds 1-3, antimony atoms have a distorted trigonal-bipyramidal coordination with the oxygen atoms of the carboxylate ligands in the axial positions. The ranges in the Sb-C bond length changes are 2.083(6)-2.117(6) Å (1), 2.095(4) -2.111(3) Å (2), 2.03(3)-2.12(2) Å (3). The Sb-O distances (2.142(4), 2.128(5) Å (1), 2.108(3), 2.116(3) Å (2), 2.156(16), 2.140(15) Å (3)) are longer than the Sb-С bonds, which is typical for triarylantimony dicarboxylates, structurally characterized earlier. The CSbC angles are 111.9(2)°-124.7(2)° (1), 111.69(13)°-130.72(14)° (2), 114.2(6)°-131.6(11)° (3). The OSbО axial angles are 172.66(10)°-179.08(18)° (1), 175.53(10)° (2) and 174.6(7)° (3). Molecules 1-3 contain intramolecular contacts between antimony and the oxygen atoms of carboxylate ligands (3.210(8)-3.235(8) Å (1), 3.048(4), 3.250(4) Å (2), 3.239(17)-3.254(18) Å (3), which is less than the sum of the van der Waals radii of antimony and oxygen (3.70 Å). The formation of a spatial network in crystals of compounds 1-3 is due to the presence of weak hydrogen bonds with the participation of carbonyl oxygen atoms O∙∙∙H (2.69, 2.70 Å) (1), 2.50 Å (2), fluorine F∙∙∙H 2.49, 2.57, 2.65 Å (2) and bromine atoms Br∙∙∙H (2.89, 2.94 Å) (3). Complete tables of atomic coordinates, bond lengths and bond angles have been deposited with the Cambridge Crystallographic Data Center (No. 2089436 for 1; No. 1919922 for 2; No. 1851632 for 3, deposit@ccdc.cam.ac.uk or http: //www.ccdc. cam.ac.uk/data_request/cif).