The carboxylatonickel(II) compounds, (RCO2)2 NiL, xH2O [R = C6F5, ρ- MeOC6F4, or ρ-EtOC6F4; L = 2, 2'-bipyridyl (bipy), x = 2, or L = 1, 10-phen-anthroline (phen), x = 1], have been obtained from reactions of nickel carbonate, the appropriate carboxylio acids, and the bidentate nitrogen ligands in aqueous ethanol. Nickel has octahedral stereochemistry, and possible structures are discussed. Decomposition of the complexes in boiling toluene, except for C6F5CO2)2Ni(phen), H2O when boiling benzene with added benzoyl peroxide was used, gave the corresponding organonickel compounds, R2NiL. The formation of the α-substituted phenanthroline derivatives, R2NiL’[R = ρ-MeOC6F4 or ρ-EtOC6F4; L’ = 2-(ρ-alkoxytetrafluorophenyl)-1, 10-phenanthroline] and (ρ-MeOC6F4), NiL’' [L’' = 2, 9-bis(ρ-methoxytetrafluorophenyl)-1, 10-phenanthroline], accompanied the preparations of the appropriate R2NiL compounds. The stereochemistry of nickel in the organonickel derivatives is approximately planar.