X-ray powder diffraction data for new metal-organic compounds: tetrakis(3-ethylanilinium) octamolybdate Mo8O26(C8H12N)4 [a = 10.682(4), b = 16.589(5), c = 7.307(2) Å, α = 92.79(2)°, β = 97.99(3)°, γ = 103.89(3)°, V = 1240.27 Å3, Z = 1, space group P−1]; tetrakis(3-ethylanilinium) octamolybdate tetrahydrate Mo8O26(C8H12N)4·(H2O)4 [a = 18.801(7), b = 17.943(6), c = 7.334(3) Å, β = 98.50(5)°, V = 2446.99 Å3, Z = 2, space group P21/m] and bis(3-ethylanilinium) pentamolybdate Mo5O16(C8H12N)2 [a = 34.643(6), b = 5.5796(7), c = 14.200(3) Å, β = 96.20(2)°, V = 2728.69 Å3, Z = 4, space group I2/a] are reported in this paper. The investigated compounds were synthesized from molybdic acid and 3-ethylaniline in acidic solution. In the first two cases, we obtained octamolybdates, while the last compound crystallized as pentamolybdate.