In this thesis, an orthopalladated dimeric complex [Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 }(µ-Cl)] 2 ( A ) has been synthesized by reaction of PdCl 2 , NaCl, NaOAc and 2-phenylaniline in acetone for 1 week at room temperature. The chloro bridge in the dimeric orthopalladated complex (A) is easily cleaved by various neutral ligands including 1,10-phenanthroline, 4-methyl-1,10-phenanthroline, thiourea, pyridine and bipyridine to afford mononuclear complexes: ( 1 )L-L = 1,10-phen), ( 2 ) L-L = 4-Me-phen) 2 , ( 3 )L = tu, ( 4 )L = py, ( 5 )L-L = bipy. These complexes were fully characterized by elemental analysis, IR and NMR spectroscopies. In addition, the crystal structure of 5 was determined by single- crystal X-ray diffraction analysis. In this structure, the palladium atom shows a slightly distorted square-planar geometry. The disappearance of the protons of 2-phenylaniline in the aromatic region in 1 H-NMR spectrum shows bidentate 4-methyl-1,10-phenanthroline ligand coordinated to the both sides of Pd atom. In the second part of the project, the 1:2 and 1:4 insertion reactions have been done at room temperature with symmetrical and unsymmetrical alkynes including diphenylacethylene, ethylphenylacetylene carboxylate and dimethyl acetylene dicarboxylate to afford inserted dimeric and monomeric complexes ( 6 ) [Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 }(µ-Cl)(PhC=CPh)] 2 ( 7 )Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 }(PhC=CPh) 2 Cl ( 8 ) [Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 }(µ-Cl) (PhC=CO 2 CH 2 CH 3 )] 2 ( 9 )Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 (PhC=CO 2 CH 2 CH 3 ) 2 Cl ( 10 )[Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 }(µ-Cl)(CH 3 O 2 C=CO 2 CH 3 )] 2 These complexes were characterized by FT-IR, NMR and elemental analysis. The disappearance of strong peak of C?C and appearance of C=C peak in the range of 1600-1640 cm -1 frequency in IR spectra of inserted complexes shows that acetylene group in alkynes convert to C=C group. In the last part of the project, the inserted mononuclear complexes ( 7 ) and ( 8 ) have been reacted with monodentate ligand PPh 3 to give complexes:( 11 ) [Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 (PhC=CO 2 CH 2 CH 3 ) 2 PPh 3 ]Cl ( 12 )[Pd{( C,N )-(2?-NH 2 C 6 H 4 )C 6 H 4 }(PhC=CPh) 2 PPh 3 ]Cl 31 P-{ 1 H} NMR spectra of the final complexes show a single peak at 25.50 ppm correspond to the coordination of PPh 3 group.