Novel microporous polymers were synthesized through Yamamoto polymerization of selectively brominated spirofluorene-bridged N-heterotriangulenes. Extensive characterization, including combustion analysis, ToF-SIMS, IR, and Raman spectroscopy, confirmed the elemental composition and integrity of the polymers. The amorphous polymers, observed by scanning electron microscopy as globular particles aggregating into larger structures, exhibited remarkable thermal stability (decomposition …