The designed synthesis of heterobimetallic microporous coordination polymers (MCPs) is reported by a strategy employing the selective replacement of a single metal in homometallic MCPs with two unique metal coordination environments: octahedral and tetrahedral. This strategy is successful in the preparation of six mixed-metal MCPs, where Co/Zn and Ni/Zn versions of MOF-4 MOF-39, and a Zn-BTEC MCP are reported.