Monoclinic single crystals of Co[(C6H10)(NH3)2][C6H2(COO)4] · 2H2O have been prepared inaqueous solution at 80 °C. Space group C2/c (no. 15), a = 1065.92(8), b = 1568.97(9), c =1140.88(9) pm, β = 90.101(6)°, V = 1.9080(2) nm3, Z = 4. Co2+, which is situated on atwofold crystallographic axis, is coordinated in a moderately distorted tetrahedral fashion byfour oxygen atoms stemming from the pyromellitate anions (Co-O 197.87(12) and 200.64(12)pm). A three-dimensionally connected coordination polymer is made up by Co2+ andC6H2(COO)44- featuring channel-like voids, which accomodate water molecules and(C6H10)(NH3)22+ cations compensating for the negative excess charge of the three-dimensionalframework. Thermogravimetric analysis in air showed that the dehydrated compound wasstable between 198 and 361 °C. Further decomposition yielded CoO.Zn[(C6H12)(NH3)2][C6H2(COO)4]·1/2H2O (2) was prepared analogously to 1 employing 1, 6-diaminohexane. Space group P21/n (no. 14), a = 1087.78(8), b = 1515.18(11), c = 1162.21(10)pm, β=96.249(7)°, V = 1.9042(3) nm3, Z = 4. Zn2+ is coordinated tetrahedrally like Co2+ byoxygen atoms of the pyromellitate anions (Zn—O 195.0(4) - 197.8(4)). The connection ofZn2+ with the anions leads similar to 1 to a three-dimensional framework with voidsaccomodating (C6H12)(NH3)22+-cations and water molecules. 2 was stable anhydrouslybetween approx. 120 and 340 °C, the further decomposition was completed at 700 °C yieldingZnO.