Molecular and crystal structures of tri- and tetraarylantimony carboxylates

Triarylantimony interaction with a carboxylic acid in ether medium in the presence of hydrogen peroxide (1:2:1 mol.) has synthesized triarylantimony dicarboxylates: Ph3Sb[OC(O)C6H4OMe-2]2 (I), Ph3Sb[OC(O)CH2C6H4NO2-4]2 (II), Ph3Sb[OC(O)cyclo-C3H5]2 (III), Ph3Sb[OC(O)C6H4NO2-2]2 (IV), (3-MeC6H4)3Sb[OC(O)C6H4OMe-2]2 (V). Tetraphenylantimony carboxylates: Ph4SbOC(O)C6H4OMe-2 (VI), Ph4SbOC(O)CH2C6H4NO2-4 (VII), Ph4SbOC(O)cyclo-C3H5 (VIII) и Ph4SbOC(O)C6H4NO2-2 (IX) have been obtained from pentaphenylantimony and triphenylantimony dicarboxylates (1:1 mol.) in toluene. According to the X-ray diffraction analysis, antimony atoms in the molecules I, II, III, V have a distorted trigonal-bipyramidal coordination with the oxygen atoms of the carboxyl groups in axial positions. Axial OSbO angles in I-III, V are equal to 173.30(6)° (I), 173.35(11)° (II), 176.46(4)° (III), 173.58(19)° (V), CSbC angles are 104.30(5)°, 104.30(5) °, 151.39(10)° (I); 110.04(9)°, 110.04(9)°, 139.91(17)° (II); 104.44(6)°, 106.38( 5)°, 149.18(6)° (III); 105.3(3)°, 105.9(3)°, 148.8(3)° (V). Ranges of Sb-O and Sb-C bond lengths are 2.106(2)-2.137(5) A and 2.082(2)-2.1258(16) A. Intramolecular distances Sb???O=C are equal to 2.611(3)-3.012 (3) A. In the molecules of tetraphenylantimony carboxylates (VII, IX), which have a distorted trigonal-bipyramidal configuration, the axial CSbO angles, Sb-C and Sb-O bond lengths and intramolecular contacts Sb???O =C are 176.26(8)°, 2.115(2 )-2.168 (3), 2.220(2) and 3.247 (3) A (VII); 176.39(8)°, 2.115(3)-2.167(2), 2.325(2) and 3.318 (3) A (IX).