Synthesis, structure and reactivity of SalanH(2)-metal complexes

The present work is an exploration into synthesis of complexes of general formula LH(2)M (where M = Mn, Fe, Cu, and Al). The results obtained for L = Salophan (M = Fe (1), Cu (2)); Salomphan (M = Mn(3), Fe(4), Cu(5); Salpan (M = Fe(6), Cu(7)) and L = Salean (M = AlCl) (8) are reported. When 8 is dissolved in MeOH, [SaleanH(2)AlOMe](2) (9) is formed. In MeOH, and in the presence of air, 1 and 4 undergo oxidation of both the ligand and metal (Fe(II) to Fe(III) to form the ''half'' Schiff base complexes, [SalophanHFeOMe](2) (10) and [SalomphanHFeOMe](2) (11). Compounds 9-11 were structurally characterized. Crystal Data: (9) C36H46Al2N4O7, Space Group P-1 (no. 2) with a = 7.536(1) Angstrom, b = 10.513(2) Angstrom, c = 11.997(2) Angstrom, alpha = 97.72(1), beta = 94.040(10)degrees, gamma = 102.73(1), V = 914.8(3) Angstrom(3) and Z = 2. With 226 parameters refined on 1226 reflections having F>6.0 sigma(F), the final R values were R = 0.0540 and R(w) = 0.0565; (10), C46H46Fe2N4O8, Space Group P-1 (no. 2) with a = 9.400(2) Angstrom, b = 10.718(4) Angstrom, c = 12.354(3) Angstrom, alpha = 76.28(3), beta = 67.89(2)degrees, gamma = 86.63(3), V = 1119.7(7) Angstrom(3) and Z = 2. With 289 parameters refined on 1327 reflections having F>6.0 sigma(F), the final R values were R = 0.0672 and R(w) = 0.0749; (11) C48H54Fe2N4O8, Space Group P-1 (no. 2) with a = 9.047(2) Angstrom, b = 11.723(2) Angstrom, c = 12.419(3) Angstrom, alpha = 80.14(2), beta = 68.68(3)degrees, gamma = 85.88(2), V = 1208.8(4) Angstrom(3) and Z = 2. With 307 parameters refined on 2171 reflections having F>4.0 sigma(F), the final R values were R = 0.0546 and R(w) = 0.0573.