The crystal structure of 1,3-bis(3,5-dibromosalicylideneamino)-2-propanol was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the monoclinic space group P2(1)/n with a = 16.5374(17)angstrom, b = 18.1164(19)angstrom, c = 19.330(2)angstrom, beta = 93.608(3)degrees, V = 5779.9(10)angstrom(3), D-x = 2.117 g/cm(3), and Z = 12. The R1 [I > 2 sigma(I)] and wR2 (all data) values are 0.0743 and 0.1541, respectively, for all 13203 independent reflections. The crystal contains three crystallographically independent Schiff-base molecules. Each molecule takes a bended structure at the central carbon atom with a dihedral angle of between the two 3,5-dibromosalicylideneaminomethyl planes of 79.68, 84.52, or 89.72 degrees. The three Schiff-base molecules are connected one another by intermolecular hydrogen bonds between an alcohol-oxygen atom and a phenolato-oxygen atom of a neighboring Schiff-base molecule.
The crystal structure of a hydrolyzed product of the cobalt(III) complex with 1-(3,5-dichlorosalicylideneamino)-3-amino2-propanol (H(2)dcsalapr) was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the triclinic space group P (1) over bar with a = 9.2242(15)angstrom, b = 9.3391(16) angstrom, c = 9.5525(16)angstrom, alpha = 75.574(3)degrees, beta = 85.550(3)degrees, beta = 69.154(3)degrees, V = 744.7(2)angstrom(3), D-x = 1.634 g/cm(3), and Z = 1. The R1 [I > 2 sigma(I)] and wR2 (all data) values are 0.0489 and 0.1093, respectively, for all 3319 independent reflections. The X-ray structure analysis revealed a centrosymmetric octahedral Co(III) complex with two hydrolyzed Schiff-base ligands, Hdcsalapr(-), in a facial mode, one chloride ion, two acetonitrile molecules, and two water molecules in the unit cell, which was formed from the reaction solution of cobalt(II) chloride hexahydrate with 1,3-bis(3,5-dichlorosalicylideneamino)-2-propanol in the presence of triethylamine in acetonitrile.
A dinuclear Cu(II) complex, [Cu-2(OAc)(2)(tpxn)(H2O)(2)](PF6)(2) [tpxn = N,N,N',N'-tetrakis(2-pyridylmethyl)-1,4-xylenediamine], was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in the monoclinic space group P2(1)/c with a = 9.310(4), b = 10.880(4), c = 20.628(8)angstrom, beta = 91.581(6)degrees, V = 2088.6(14)angstrom(3), D-caled = 1.704 g/cm(3), and Z = 4. The R1 [I > 2 sigma(I)] and wR2 (all data) values are 0.0343 and 0.0923, respectively, for all 4731 independent reflections. The complex contains two square-pyramidal Cu(II) ions bound to both terminal tridentate sites of tpxn.
The title compound of [Ru-2(O2CCH2CH2CH3)(4)Br](n) was prepared and the crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the tetragonal space group I (4) over bar 2d with a = 13.2222(10)angstrom, c = 24.0779(18)angstrom, V = 4209.5(7)angstrom(3), D-x = 1.990 g/cm(3), and Z = 8. The R1 [I > 2 sigma(I)] and wR2 (all data) values are 0.0310 and 0.0572, respectively, for all 2430 independent reflections. The two ruthenium atoms are bridged by four n-butyrato ligands in the syn-syn mode with the Ru-Ru distance of 2.2897(9)angstrom. Both of the axial sites of the dinuclear ruthenium units are bridged by bromido ligands with the Ru-Br distance of 2.7078(7)angstrom to form an alternated zig-zag chain molecule with Ru-Ru-Br and Ru-Br-Ru angles of 172.68(2) and 117.21(3)degrees, repectively. The temperature-dependent profile of the magnetic moment was simulated with g = 2.14, D = 67 cm(-1), zJ = 0.38 cm(-1) values. The g and D values are similar to those of other tetracarboxylato Ru-2(5+) complexes.
