A new trinuclear cluster [Co3(ib)6(phen)2] (where Hib = isobutyric acid, phen = 1,10′-phenanthroline) has been obtained and characterized by elemental analysis, IR spectroscopy, ESI-MS spectrometry, and thermogravimetric studies. This can be achieved simultaneously by synthesis methods such as stirring and ultrasonic irradiation. The structure of the trinuclear Co(II) cluster has been solved by single-crystal X-ray diffraction measurements, revealing a centrosymmetric linear arrangement of three Co(II) atoms bridged by six isobutyrate moieties. Four of these moieties act in a bidentate syn-syn fashion, bridging two Co atoms, while the remaining two serve as bidentate chelate-bridging units. The central Co atom resides at the crystallographic center of symmetry and is coordinated by six O atoms from six isobutyrates, resulting in an octahedral O6 surrounding. The coordination sphere of the peripheral Co atoms is completed by three isobutyrate ligands, two of which coordinate in a monodentate fashion and one in a chelate bidentate mode, and 1,10′-phenanthroline, providing a distorted octahedral N2O4 surrounding. Hirshfeld surface analysis was performed to elucidate the intermolecular interactions contributing to the stabilization of the crystal structure. Magnetic measurements show ferromagnetic exchange interactions between the high spin Co(II) centers.