Tributylstannyl ester of polymeric silicic acid (PTBS) was used for the preparation of a mesoporous organic-inorganic hybrid gel. Reactions of PTBS and polyhalosilane 1 such as methyltrichlorosilane (la), dichlorodimethylsilane (lb) or bis(chlorodimethylsilyl)alkanes, used as cross-linker, proceeded efficiently with elimination of tributylstannyl chloride to afford silylated gels containing the corresponding organic groups. Specific surface areas of obtained gels measured by BET method were from 510 m 2 g-1 to 608 m 2 g-1. Maximum pore volume of0.377 mL g-1 and average pore size of 33 A. were recorded on the gel obtained from 1,2-bis(chlorodimethylsilyl)ethane (le) and PTBS. Plots of pore size distribution of gels obtained from la, lb, and le showed sharp single peaks in mesopore range, indicating pore size to be controlled by the steric effects of organic groups of 1. In using 1,6-bis(chlorodimethylsilyl)hexane (ld), the results of BET analysis indicated the formation of nonporous gel.