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Three new 3D metal-organic porous frameworks based on Co(II) and 2,2′-bithiophen-5,5′-dicarboxylate (btdc 2− ) [Co 3 (btdc) 3 (bpy) 2 ]·4DMF,  1 ; [Co 3 (btdc) 3 (pz)(dmf) 2 ]·4DMF·1.5H 2 O,  2 ; [Co 3 (btdc) 3 (dmf) 4 ]∙2DMF∙2H 2 O,  3  (bpy = 2,2′-bipyridyl, pz = pyrazine, dmf =  N , N -dimethylformamide) were synthesized and structurally characterized. All compounds share the same trinuclear carboxylate building units {Co 3 (RCOO) 6 }, connected either by btdc 2–  ligands ( 1 ,  3 ) or by both btdc 2–  and pz bridging ligands ( 2 ). The permanent porosity of  1  was confirmed by N 2 , O 2 , CO, CO 2 , CH 4  adsorption measurements at various temperatures (77 K, 273 K, 298 K), resulted in BET surface area 667 m 2 ⋅g −1  and promising gas separation performance with selectivity factors up to 35.7 for CO 2 /N 2 , 45.4 for CO 2 /O 2 , 20.8 for CO 2 /CO, and 4.8 for CO 2 /CH 4 . The molar magnetic susceptibilities χ p ( T ) were measured for  1  and  2  in the temperature range 1.77–330 K at magnetic fields up to 10 kOe. The room-temperature values of the effective magnetic moments for compounds  1  and  2  are μ eff  (300 K) ≈ 4.93 μ B . The obtained results confirm the mainly paramagnetic nature of both compounds with some antiferromagnetic interactions at low-temperatures  T  < 20 K in  2  between the Co(II) cations separated by short pz linkers. Similar conclusions were also derived from the field-depending magnetization data of  1  and  2 .

3D Metal–Organic Frameworks Based on Co(II) and Bithiophendicarboxylate: Synthesis, Crystal Structures, Gas Adsorption, and Magnetic Properties