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Two new metal–organic frameworks [Mn 3 (MMA) 2 (INA) 2 ] n ( 1 ) and [Cu 2 (FA)(INA) 3 (H 2 O)] n ( 2 , FA = formate) were prepared solvothermally by using mixed methylmalonic acid (H 2 MMA) and isonicotinic acid (HINA) as the initial reactants. Single-crystal X-ray diffraction analyses reveal that complex 1 has a 3D framework structure consisting of 2D [Mn 3 ] layer units and INA connector, and 2 owns a 2D pillar-layered structure constituted of mononuclear-Cu(II)-based 2D layer unit and paddle-wheel dinuclear Cu(II) cluster-based pillared linker, which further interspersed with each other to form a 3-fold interpenetrated framework with a (4 8 .6 2 )- SP topology. The magnetic studies show that 1 displays antiferromagnetic ordering at low temperature, and a strong antiferromagnetic interaction exists in 2 . [ABSTRACT FROM AUTHOR]