Cobalt(III) coordination compounds showed remarkable biological activities and found applications as antiviral and antibacterial agents [1]. Two new Co(III)-containing compounds [CoIII(NH3)6]Cl(L)*4H2O (1) and [CoIII(NH3)6]2(L)3*EtOH*3H2O (2) have been obtained from the reaction of [CoIII(NH3)6]Cl3with 4-sulfobenzoic acid potassium salt (H2L) in the presence of triethanolamine in mixture of EtOH and H2O (1:1) under solvothermal (1) and ultrasonic (2) treatment. The compounds have been characterized by a single-crystal X-ray diffraction studies and IR spectroscopy. The IR spectra of the synthesized compounds showstrong and broad bands at 1591 cm^–1 and 1544 cm^–1 corresponding to the asymmetric and symmetric stretching vibrations of the deprotonated carboxylic group of the 4-sulfobenzoic acid. The asymmetric and symmetric C–H stretching vibrations were localized in the regions of 2989 –2854 cm^–1. The hydroxyl groups of solvent EtOH and H2O molecules as well as vibrations of NH3 groups result in broad bands 3500 –3251cm^–1. The stretching vibrations (asymmetric/symmetric) of sulfonic groups in both compounds are founded in the region of 1394 – 1331 cm^–1 and 1174 – 1143 cm^–1, respectively. Compound 1 crystallizes in triclinic P1/n space group, a = 7.652(1), b = 10.243(1), c = 13.028(1) Å, a = 76.309(5), b = 85.404(6), y= 87.888(5)º, V = 988.8(1) Å3; where as compound 2 crystallizes in monoclinic P21/n space group, a = 13.538(2), b = 25.260(3), c = 13.727(2)Å, b=112.56(2)º, V=4435(1)Å3. The asymmetric unit in the structure of 1 contains [CoIII(NH3)6]3+ cation, C^l– anion,4-sulfobenzoicdianions (L^2–) and four water molecules, while the compound 2 involves two [CoIII(NH3)6]3+ cations, three L^2– anions, solvate ethanol, and three water molecules. In the crystal structures the deprotonated carboxylic and sulfonic groups are involved in 3D hydrogen bonding network between the complex cations and anions as well as with solvent EtOH and water molecules, Figure 1.Figure 1. Fragments of the structure of 1 (a) and 2 (b).