The new (CH2FC(O)NH)P(O)(NHC6H4-4-CH3)2 compound was crystallized in the space group C2/c and characterized by 1H, 13C, 31P, 19F NMR and IR spectroscopies, mass spectrometry and by single crystal X-ray diffraction analysis. The asymmetric unit is composed of one complete molecule. The P═O, C═O and P―N bond lengths and P―N―C angles are within the expected values observed for analogous structures.1 The anti orientation of P═O with respect to C═O is reflected in the [O―P―N―C] 170.5(9)° torsion angle. Moreover, the C―F bond adopts an anti orientation with respect to the C═O bond with the torsion angle of [O═C―C―F] 173.4(14)°. The P atom has a distorted tetrahedral environment with the bond angles at the P atom within 100.8 (5)° [O1-P1-N2] to 117.5 (5)° [O1-P1-N3]. The N atoms bonded to P atom have mainly sp2 character tending towards a planar environment. In the crystal structure, molecules are linked via N—H⋯O═P and N—H⋯O═C hydrogen bonds, into a one dimensional arrangement along the b axis, which includes the (10) ring motifs.2 The aggregation of chains formed through C—H⋯π interactions leads to a 2D array. In the 13C NMR spectrum, the signal of CFH2 carbon atom appears as a doublet of doublet due to the coupling with fluorine and phosphorus nuclei (1JF–C & 3JP–C). In the 31P{1H} NMR spectrum, a singlet negative peak is observed at –6.82 ppm. The 19F siganl reveals at –74.31 ppm.

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