Two 2-D inorganic-organic hybrid layered network materials Zn(BDG) (C_3H_3N_2)·(DMF) (1) and Go_2-(BDG)_2(C_5H_5N)_4·2(DMF)(C_5H_5N)(2) were synthesized under mild synthesis condition. Their crystal structures were determined by using single crystal X-ray diffraction. Crystal structures were solved by direct method and refined by fullmatrix least-square method. Compound 1 is monoclinic, space group C2/c with a = 2.1059(4) nm, b = 1.0316(2) nm, c = 1.4836(3) ran, β = 99.09(3)°, F = 3.1826(11) nm3, Z = 4, Dx = 1.543 Mg/m~3, C_(14)H_(14) N_3O_5Zn, Mr = 369.65, μ = 1.571 mm~(-1), F(000) = 1512, R =0.0697, R_W = 0.2018, and compounds is monoclinic, space group P2(l)/n with a = 1.0829(2) nm, 6 = 1.5431(3) ran, c = 1.4428(3) nm, β= 101.65(3)°, V = 2.3612(8) nm~3, Z = 2, D_x = 1.391 Mg/m~3, C_(47)H_(47)N_7O_(10) Co_2, M_r = 987.78, μ =0.767 mm~(-1), F(000) = 1024, 72 = 0.0652, R_W = 0.1888. They are layered networks with 0.9 nm*0.9 nm pore.

Key words: CRYSTAL STRUCTURE, HYBRID MATERIALS, GLYOXALINE, PYRIDINE, STRUCTURE CHARACTERISTICS, ZINC COMPLEX, COBALT COMPLEX