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Starting from two low-nuclearity linear synthesised Co 3 precursors {[Co 3 L' 2 (H 2 O) 6 ]·2NO 3 ·4H 2 O} (1) and {[Co 3 L' 2 (H 2 O) 6 ]·2NO 3 } (2) (here, H 2 L = bis((pyridine-2-yl)-1,2,4-triazol-5-yl)methane, H 2 L' = bis((pyridine-2-yl)-1,2,4-triazol À5-yl)ketone), a series of Co3-substituted complexes and two higher-nuclearity Co(II) clusters {[Co 8 L 6 (m 3 -O) 2 ]·5H 2 O} (3) and [Co 6 L 4 (MeOH) 6 (OAc) 4 ] (4) have been synthesized and characterized through regulating solvent, anion, and pH conditions. For tracking the formation of higher-nuclearity clusters, the single-crystal X-ray diffraction (SXRD), powder X-ray diffraction (PXRD) and electrospray ionization mass spectrometry (ESI-MS) analyses for the solidliquid phase at different times, revealed that [Co 2 L 2 ] and [Co 2 L] species can combine together to form [Co 4 L 3 ] species, which bridged each other through two [m 3 -O] 2À ions in strong alkaline conditions, to get [Co 8 (m 3 -O) 2 L 6 ] units in 3; which or combined [Co 2 L] species in weak alkaline conditions, to get [Co 6 L 4 ] species in 4. And the antiferromagnetic coupling in 1-4 has been briefly investigated.