Synthesis and structural characterization of tetradentate (N2O2) ligand complexes of zinc

The potentially tetradentate-N2O2 ligands, N,N'-bis(o-hydroxybenzyl)-1,2-diaminoethane (SaleanH(4)), N,N'-bis(o-hydroxybenzyl)-1,3-diaminopropane (SalpanH(4)), N,N'-bis(o-hydroxybenzyl)-1,4-diaminobutane (SalbanH(4)), N,N'-bis(o-hydroxybenzyl)-1,6-diaminohexane (SalhanH(4)), N,N'-bis(o-hydroxybenzyl)-1,2-diaminobenzene (SalophanH(4)), and N, N'-bis(o-hydroxybenzyl)-1,2-diamino-4,5-dimethylbenzene (SalomphanH(4)), have been synthesized and used to prepare the series of zinc complexes, [SaleanH(2)Zn](2) (1), [Salpan H2Zn](2) (2), [SalbanH(2)Zn](2) (3), [SalhanH(2)Zn](2) (4), [SalophanH(2)Zn], (5), and [Salomphan H2Zn](2) (6), Compounds (2) and (5) have been structurally characterized with single-crystal x-ray diffractometry. The molecules consist of oxygen-bridged zinc dimers. Unique structures for (5) were determined from crystals grown from MeOH (5a) and DMF (5b). The structures possess varying numbers of solvent molecules in the unit cell. Crystal Data: (2) Space Group P (1) over bar with a = 13.076(3) Angstrom, b = 13.137(3) Angstrom, c = 13.228(3) Angstrom, alpha = 72.09(3)degrees, beta = 69.18(3)degrees, gamma = 70.71(3)degrees, V = 1957.5(8) Angstrom(3) and Z = 2. With 478 parameters refined on 3899 reflections having F > 4.0 sigma(F), the final R factors were R = 0.0733 and R-w = 0.0796; (5a) Space Group P (1) over bar with a = 10.271(3) Angstrom, b = 10.447(4) Angstrom, c = 11.950(2) Angstrom, alpha = 64.510(0)degrees, beta = 73.310(0)degrees, gamma = 85.520(0)degrees, V = 1107.1(7) Angstrom(3) and Z = 2. With 271 parameters refined on 2190 reflections having F > 4.0 sigma(F), the final R factors were R = 0.0678 and R-w = 0.0787; (5b) Space Group P (1) over bar with a = 13.109(3) Angstrom, b = 13.577(2) Angstrom, c = 16.540(4) Angstrom, alpha = 93.45(2)degrees, beta = 105.04(2)degrees, gamma = 92.85(2)degrees, V = 2830.8(10) Angstrom(3) and Z = 2. With 661 parameters refined on 3082 reflections having F > 4.0 sigma(F), the final R factors were R = 0.0575 and R-w = 0.0626.