Thirteen Ni(II) and Co(II) coordination polymers based on the organic linker 1H,1'H-4,4'-bipyrazole (H 2 BPZ) were synthesized and characterized using single crystal X-ray diffraction, namely Ni(H 2 BPZ)(acac) 2(1), 11), Ni(BPZ) • (DMF) 0.65 (12), and Ni(BPZ) (13). In order to study the structural correlations of 1D-3D, 2D-3D, and 3D-3D phase transitions the structures were investigated by means of thermal analysis. In addition, the role of charge-balancing anions with respect to their coordination strength on structure, framework dimension, and crystal properties is discussed in detail. This work exemplifies the function of anions as structure directing agents and how they, as well as thermal activation, can influence framework topology, dimensionality, and crystal size.