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Preparation of mesoporous molecular sieve MCM-41 with complementary textural porosity and high thermal stability that results from thicker wall has been achieved by decreasing surfactant/silicon ratio of synthesis gel. MCM-41 material obtained by using the surfactant/silicon molar ratio of 0.10 consists of large and well-defined spherical particles. A further decrease in the ratio results in the formation of MCM-41 silica with the bimodal framework meopores and complementary textural porosity. The textural porosity results from the loose aggregate structure. The resultant materials retain ordered channels and large BET surface area even after thermal treatment at 1273 K for 1 h in air. The complementary textural porosity decreases the length of the one-dimensional mesopores and provides the facilitating framework access for the diffusion of mass.