Spectroscopic Analysis of IIJ

The P NMR chemical shifts of IIJ appeared as a singlet at 8 11.8-12.5 ppm. Their chemical shifts moved upheld approximately 11-12 ppm compared with that of the corresponding 0,0-dimethyl phosphonates (at —23 ppm). The spectmm of IIJ-16 (R =Me, Y =2-F,4-C1) is shown in Fig. 3.13. 

An X-ray single-crystal stmcture of IU-24 (R =Me, Y =2,4-Cl2) is shown in Fig. 3.14. Packing diagrams of IU-24 are shown in Fig. 3.15. Selected bond lengths and angles are presented in Table 3.33. Analysis of the crystal stmcture 

There are many hydrogen bonds in the molecular, which make every two molecules with the same configuration to bind and form dimers. For example, three ammonium H atoms participate in N-H-O hydrogen bonds (Table 3.34), which stabilize the crystal packing (Fig. 3.15) along with weak intermolecular interactions of C-H-0 (Table 3.34). 

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