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N,N′-Tetramethyl-N″-p-chlorobenzoylphosphoryltriamide (I), N,N′-tetramethyl-N″-o-fluorobenzoylphosphoryltriamide (II) and their sodium salts were synthesized and characterized by means of IR and  1 H ,  31 P NMR spectroscopy. The structures of both compounds were determined by X-ray diffraction (I triclinic, space group P1̄ with a = 12.073(2), b = 12.869(3), c = 12.854(4) Å, α = 56.93(2), β = 62.45(2), γ = 66.34(2)° V = 1453.7(6)Å 3 , ρ(caled.) = 1.324 mg/cm 3 , Z = 4 and R = 0.0545, wR2 = 0.1425; II monoclinic, space group P2(1)/n with a = 10.051(2), b = 13.093(2), c = 10.856(2) Å, β = 108.36(2)°, V = 1355.9(4) Å 3 , ρ(caled.) = 1.339 mg/cm 3 , Z = 4 and R = 0.0533, wR2 = 0.1263). In both structures the molecules are associated into dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups. In I the unit cell consists of two independent molecules connected into non-symmetric dimers, in II of centrosymmetric dimer molecules.

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Carbacylamidophosphates: Synthethis and Structure of N,N'-Tetramethyl-N''-p-chlorobenzoyIphosphoryltriamide and N,N'-Tetramethyl-NM-o-fluorobenzoylphosphoryltriamide