We have obtained three layered hybrid materials from the hydrothermal reaction of 4-cyclohexene-1,2-dicarboxylic acid with Co and Mn salts: Co(C₈H₈O₄) [1], Mn(H₂O)(C₈H₈O₄) [2], and Mn₄(H₂O)(C₈H₈O₄)₄·0.3(H₂O) [3]. The structures for all materials were solved by single-crystal XRD ([1] P, a = 4.805(2) Å, b = 6.650(3) Å, c = 12.960(6) Å, α = 98.285(7)°, β = 98.986(7)°, γ = 95.689(7)°, V = 401.6(3) ų, R₁ = 0.0438; [2] P2₁/c, a = 11.151(2) Å, b = 11.330(2) Å, c = 7.6560(15) Å, β = 108.813(3)° , V = 915.6(3) ų, R₁ = 0.0412; [3] P, a = 11.412(3) Å, b = 12.136(4) Å, c = 13.809(4) Å, α = 104.703(6)°, β = 103.207(6)°, γ = 92.468(5)°, V = 1790.6(9) ų, R₁ = 0.1056). While all three structures are two-dimensional overall, the metal–oxygen–metal dimensionality within the layers varies from isolated metal atoms in the case of [1] to 1D ribbons of vertex sharing MnO₆ octahedra [2] and 2D arrays of edge- and vertex-sharing polyhedra in [3].