A new crystal of 2-methylpropan-2-aminium methyl （（4-fluorobenzamido）（4- fluorophenyl）methyl）phosphonate has been prepared at room temperature and characterized by ZH- NMR, 13C NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic space, group C2/c with a = 20.719（2）, b = 11.8559（13）, c = 18.176（2） A,β = 94.434（2）°, V= 4451.4（9） A3, Dc = 1.317 Mg/m3, Z= 8, F（000） = 1864 and μ= 0.174 mm-1. The crystal packing is stabilized by intermolecular N-H……O and O-H……O hydrogen bonds, as well as by weak π-π stacking interactions.
A new crystal of 4-fluoro-N-（2-methyl-5-（（2-（p-tolyloxy）acetamido）methyl）pyrimi- din-4-yl）benzamide has been prepared at room temperature and characterized by 1H NMR, 13C- NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic, space group P21 /c with a = 17.226（5）, b = 13.934（4）, c = 17.262（5）, μ= 92.180（5）°, V = 4140（2） ？3, Dc = 1.311 g/cm3, Z = 8, F（000） = 1712 and ？？= 0.095 mm-1. The molecular packing in the crystal is the result of N-H…ydrogen bonds.
A new crystal of N,N＇-bis（4-nitrophenylcarbamothioyl）isophthalamide DMF solva-te has been prepared at room temperature and characterized by elemental analysis and IR,MS,1H NMR spectra and X-ray single-crystal determination.The complex crystallizes in monoclinic,space group P21/c with a = 11.2093（12）,b = 22.081（2）,c = 13.9640（15） ,β= 112.128（2）°,V = 3201.8（6） 3,C28H30N8O8S2,Mr = 670.72,Dc = 1.391 Mg/m3,Z = 4,μ= 0.228 mm-1,F（000） = 1400,the final R = 0.0483 and wR = 0.1411（I 2σ（I））.The molecular packing in the crystal is the result of N-H…O hydrogen bonding.
