Novel nickel(II) coordination polymers have been constructed from asymmetric semi-rigid V-shaped multicarboxylate ligands with the help of 4,4′-bipyridine (4,4′-bpy) ligand. The hydrothermal reaction between 3-(4-carboxy-phenoxy)-phthalic acid (H₃L¹) and Ni(OAc)₂·4H₂O led to the formation of [Ni₃(L¹)₂(μ-4,4′-bpy)₃(H₂O)₂]_n·(4,4′-bpy)_n·(H₂O)_5n (1). In contrast, the same reaction using 3-(2-carboxy-phenoxy)-phthalic acid (H₃L²) as a starting material instead of H₃L¹ resulted in [Ni₃(L²)₂(H₂O)₄(μ-4,4′-bpy)₃]_n·(H₂O)_2n (2) and [Ni₃(L²)₂(H₂O)₄(μ-4,4′-bpy)₄]_n·(H₂O)_2n (3) at 120 and 150 °C, respectively, revealing the effect of reaction temperature on the structure of the coordination polymer formed from the semi-rigid V-shaped ligand of L². Single-crystal X-ray diffraction analysis reveals that complex 1 shows a 3D framework structure assembled from right- and left-handed helices together with isolated tubes. This compound represents the first metal–organic hybrid tube constructed from an asymmetric semi-rigid V-shaped multicarboxylate ligand. Compound 2 also exhibits a 3D network composed of discontiguous trinuclear Ni(II) clusters, while the 3D architecture of 3 consisting of isolated Ni(II) ions separated in a long distance is constructed by two kinds of 2D (6,3) networks. Magnetic studies reveal the overall antiferromagnetic interaction between the neighbouring Ni(II) ions in 1–3.