Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- benzoic aicd) with CH 2 Cl 2 and triethylamine in 1∶1 molar ratio and characterized by elemental analysis, IR and 1 H NMR . Their crystal structures were determined by X-ray single crystal diffractometry, the crystal(Ⅰ) belongs to orthorhombic with a=0 699 43(14) nm, b=1 348 9(3 ) nm, c=1 668 9(3) nm, V= 1 574 5(6) nm 3 , Z=4, D c =1 336 Mg/m 3 , μ=0 259 mm -1 , R 1 =0 033 4, wR 2 =0 080 6, F(000)=672. The crystal(Ⅱ) belongs to triclinic with a=0 788(12) nm, b=1 239(19) nm, c=2 18(3) nm, α= 89 2°, β =89 6°, γ=76 9°, V=2 078(55) nm 3 , Z=4, D c=1 457 Mg/m 3 , μ=0 414 mm -1 , R 1 =0 062 0, wR 2 =0 151 6, F(000)=960.
