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The preparation of two types of molecular sieves AlPO4-11 and MAPO-11 is reported. The particle size of the latter is hundreds of microns, about 10 times larger than that of the former. The XRD, IR and DTA spectra have demonstrated that magnesium has been introduced into the framework of AlPO4-11. The successful preparation of large single crystal of MAPO-11 will open up a new area for the preparation of large molecular sieves crystals in the future. The large MAPO-11 crystal compound is a promising host for the host-guest assembly of composite materials.