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(4E)-5-(3-Chlorophenyl)-N-(4-chlorophenyl)-2-diazo-3-oxopent-4-enoic acid amide (5) was synthesized from p-chloroaniline to N-(4-chlorophenyl)-2-diazo-3-oxo-butyramide (4) with 3-chlorobenzaldehyde. The yielded product 5 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 5 (C17H11Cl2N3O2, Formula wt = 360.19), crystallizes in the monoclinic space group P21/c with unit cell parameters a = 10.516(2), b = 17.996(4), c = 8.902(2) Å, α = 90.00, β = 105.36(3), γ = 90.00∘. V = 1624.5(6) Å3, Z = 4, Dx = 1.473 Mg m−3. The final R was 0.0511.