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

The mixed hydroxo-bromo bridged complex [{Pd(C(6)H(4)CH(2)NMe(2))}(2)(mu-Br)(mu-OH)] (1) (C(6)H(4)CH(2)NMe(2) = 2-[(dimethylamino)methyl]phenyl) has been prepared by addition of one equivalent of NBu(4)OH to [{Pd(C(6)H(4)CH(2)NMe(2))(mu-O(2)CMe)}(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(C(6)H(4)CH(2)NMe(2))}(2)(mu-Br)(mu-NHR)] (R = C6H5 (2), p-MeOC(6)H(4) (3), p-MeOC(6)H(4) (4)) or [{Pd(C(6)H(4)CH(2)NMe(2))}(2)(mu-Br)(mu-SR)] (R = Et (5), (t)Bu (6), C6H5 (7), p-MeC(6)H(4) (8)), The H-1 NMR data indicate a cia arrangement of the C(6)H(4)CH(2)NMe(2) 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) Angstrom. Final R = 0.039 and R(w) = 0.040 based on 2692 reflections.