New benzoyl thiourea derivatives and their nickel and copper complexes were synthesized. The structure of the synthesized compounds were confirmed by elemental analysis, FT-IR, and H-1 NMR techniques. Four of the synthesized compounds are analyzed by X-ray single crystal diffraction technique. Whereas N,N-dimethyl-N'-(4-fluorobenzoyl) thiourea, N, N-diethyl-N'-(4-fluorobenzoyl)thiourea, and N,N-di-n-butyl-N'-(4-fluorobenzoyl)thiourea crystallize in the monoclinic system, bis(N,N-di-n-propyl-N'-(4-fluorobenzoyl)thioureato) nickel(II) complex crystallizes in the triclinic system. These ligandmolecules formdimers through strong intermolecular hydrogen bonds such as N-H center dot center dot center dot S, C-H center dot center dot center dot, and N-H center dot center dot center dot O. Moreover, there are different types of intramolecular interactions in the crystal structures. Bis(N,N-dimethyl-N'-(4-fluorobenzoyl)thioureato) nickel(II) complex has a nearly square-planar coordination. The distance of nickel atom from the best plane through the coordination sphere is 0.029 angstrom.