J. Ruiz et al., SYNTHESIS AND STRUCTURAL STUDY OF [(PD(C6H4CH2N(CH3)(2)))(2)(MU-BR)(MU-X)] COMPLEXES (X EQUALS HYDROXIDE, AMIDE OR THIOLATE), Journal of organometallic chemistry, 526(1), 1996, pp. 67-72
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]phe
nyl) 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, fo
llowed by addition of one equivalent of LiBr. Complex 1 reacts with ar
ylamines 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-N
HR)] (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 b
een determined by X-ray diffraction. It crystallizes in the orthorhomb
ic space group Pbca with a = 12.445(3), b = 18.029(3), c = 17.436(3) A
ngstrom. Final R = 0.039 and R(w) = 0.040 based on 2692 reflections.