The reactions of organoantimony chlorides L
1,2SbCl
2 1 and
2 ([2,6-(ROCH
2)
2C
6H
3]
−, R = Me; L
1 and R =
t-Bu; L
2) with silver salts of selected carboxylic acids resulted to corresponding organoantimony carboxylates L
1,2Sb(OOCR′)
2,
1a–
c (for L
1) and
2a–
c (for L
2), where R′ = CH
3 for
1a,
2a; R′ = CH
![]()
CH
2 for
1b,
2b and R′ = CF
3 for
1c,
2c. All compounds were characterized by the help of elemental analysis, ESI–MS,
1H and
13C NMR spectroscopy. The solid state structure investigation using single crystal X-ray diffraction techniques (
2a,
c) and IR spectroscopy revealed significant differences in coordination mode of both O,C,O chelating ligand and carboxylic groups in this set of compounds. The structure of all compounds in solution of non-coordinating solvent (CDCl
3) was determined by means of variable temperature
1H,
13C,
19F NMR spectroscopy and IR spectroscopy.