Synthesis and structural study of [{Pd(C6H4CH2N(CH3)2)}2(μ-Br)(μ-X)] complexes (X = hydroxide, amide or thiolate)

Article abstract of DOI:10.1016/S0022-328X(96)06520-5

The mixed hydroxo-bromo bridged complex [{Pd(C₆H₄CH₂NMe₂)}₂(μ-Br)(μ-OH)] (1) (C₆H₄CH₂NMe₂ = 2-[(dimethylamino)methyl]phenyl) has been prepared by addition of one equivalent of NBu₄OH to [{Pd(C₆H₄CH₂NMe₂)(μ-O₂CMe)}₂] in acetone-water solution, followed by addition of one equivalent of LiBr. Complex 1 reacts with arylamines or thiols in 1:1 mole ratio to yield the corresponding amido-or thiolato-bromo complexes [{Pd(C₆H₄CH₂NMe₂)}2(μ-Br)(μ-NHR)] (R = C₆H₅ (2), p-MeOC₆H₄ (3), p-MeOC₆H₄ (4)) or [{Pd(C₆H₄CH₂NMe₂)}₂(μ-Br)(μ-SR)] (R = Et (5), ^tBu (6), C₆H₅ (7), p-MeC₆H₄ (8)). The ₁H NMR data indicate a cis arrangement of the C₆H₄CH₂NMe₂ ligands. The crystal structure of compound 1 has been determined by X-ray diffraction. It crystallizes in the orthorhombic space group Pbca with a = 12.445(3), b = 18.029(3), c = 17.436(3) A. Final R = 0.039 and R_w = 0.040 based on 2692 reflections.