A novel type of organic-inorganic hybrid zeolite with organic lattice (ZOL) is studied in detail by solidstate C-13 magic angle spinning nuclear magnetic resonance (MAS NMR). The 13C MAS NMR measurements employing several pulse sequences quantitatively demonstrate that methylene groups are really incorporated in the framework, although they are partially cleaved into methyl groups. The organic species in ZOL materials are open for adsorbates, which is evidenced by the 13C MAS NMR measurements for an n-hexane-adsorbing ZOL material. This finding strongly suggests that organic moieties are incorporated as a zeolite framework, indicating that ZOL is not a physical mixture of a carbon-containing amorphous aggregate and a conventional zeolite but a true organic -inorganic hybrid zeolite.