A new charge transfer complex of bis (ethylenedithio) tetrathiafulvalene, (BEDT-TTF) ₄ ·H₂O ·Fe(C₂O₃) ₃ · C₆H₅NO₂, were prepared, and its crystal structure and physical properties were determined. The crystal structure of the complex has been refined in the C2/c space group, the unit cell parameters: a = 1.031 (8) nm, b =2.014(8) nm, c = 3. 534(4) nm, β=92. 21(9)°, Z = 4, R = 0. 065. Successive layers of BEDT-TTF and layers of and approximately hexoganal geometry containing alternating H₂O and Fe(C₂O₄) ₃^-3- were formed, with C₆H₅NO₂ lying within the hexagonal cavities. The BEDT-TTF adopts the β packing, the charge of BEDT-TTF estimated from the C = C and C-S bond lengths is + 3/4. The complex is a semiconductor with σ_r.t..=10 S ·cm^-1. The ESR spectra of the complex shows only one signal with the line width ΔH = 38. 1 × 10^-4 T, which indicates that there may be some interaction between the conduction electrons and the 3d⁵ electrons of Fe³⁺.