A new rigid angular bridging ligand, 7-oxa-dibenzofluorene-3,11-dicarboxylic acid (H2L), was synthesized by cyanation of known rac-6,6'-dibromo-1,1'-bi-2-naphthoI followed by ring closure and hydrolysis with concentrated sulfuric acid and used for the self-assembly of nanoscopic molecular rectangle [Cu-4(L)(4)(Py)(8)].2DMF.10H(2)O, 1, and 1-D coordination polymer [Co-2(L)(2)(PY)(4)].2DMF.2H(2)O, 2. Both 1 and 2 contain open channels occupied by DMF and water guest molecules. Crystal data for 1: triclinic, space group P (1) over bar, a = 8.869(2) Angstrom, b = 16.437(3) Angstrom, c = 21.586(4) Angstrom, alpha = 78.18(3)degrees, beta = 79.19(3)degrees, gamma = 83.66(3)degrees, U = 3017.0(11) Angstrom(3), and Z = 1. Crystal data for 2: triclinic, space group P (1) over bar, a = 8,254(2) Angstrom, b 12,154(2) Angstrom, c = 15.348(3) Angstrom, alpha = 95.34(3)degrees, beta = 93.38(3)degrees, gamma = 94.37(3)degrees, U = 1525.1(5) Angstrom(3), and Z = 1.