The new giant MO36 polyoxomolybdate formulated as K-10 [Mo36O110(OH)(6) (H2O)(12)].38 H2O (1) was isolated by conventional solution method by the reaction of K2MoO4 and KNO3 in aqueous solution (pH = 1.8), at room temperature, and structurally characterized by single-crystal X-ray diffraction methods. The title compound crystallized in the monoclinic system, space group P2(1)/n with unit a = 16.5180 (0) <(A)over circle >, b = 18.4485 (0) <(A)over circle >, c = 24.2424 (0) <(A)over circle >, alpha = 90.00 degrees , beta = 99.51 degrees , gamma = 90.00 degrees , V = 7285.79 (0) <(A)over circle >(3), and Z = 2. The refinement of the structure led to a residual factor R = 0.061 for 15,676 reflections.