摘要 在这项工作中,我们旨在合成和表征一种包括三个邻苯二酚基团的新型三向配体及其新型三向三核三嗪核心配合物。为此,我们使用三聚氰胺 (2,4,6-triamino-1,3,5-triazine) ( MA ) 作为起始材料。2,4,6-三(4-羧基苯并氨基)-1,3,5-三嗪(II)由等量三聚氰胺(I)与三当量4-羧基苯甲醛反应合成。4,4',4"-((1E,1'E,1"E)-((1,3,5-triazine-2,4,6-triyl)tris(azanylylidene))tris(methanylylidene))tris (N-(3,4-二羟基苯乙基)苯甲酰胺)L(IV)是由一当量(II)和三当量多巴胺(3,4-二羟基苯乙胺)(DA)通过两种不同的方法反应合成的。( II, III, IV ) 和九种新型三核 Cr(III), (IV)的Mn(III)和Fe(III)配合物通过元素分析、
Multinuclear Paramagnetic NMR Spectra and Solid State X-ray Crystallographic Characterization of Manganese(III) Schiff-Base Complexes
摘要:
The H-1 NMR spectra of symmetrically substituted paramagnetic [(R,R'-SALOPHEN)Mn-III](+) and [(R,R'-SALOPHEN)Mn-III](2)(mu-O) complexes (SALOPHEN is 1,3-bis(salicylideneamino)benzene) were obtained. All of the monomers and dimers yielded well-resolved but isotropically shifted H-1 NMR spectra. A diamagnetic suppression routine was applied to the H-1 NMR spectra that allowed observation of all rapidly relaxing resonances. The binding of axial ligands, acetate, methanol, water, and pyridine was also observable by H-1 NMR. Two X-ray crystal structures were obtained: [(3,3'-17-crown-6-SALOPHEN)Mn-III].(CH3C(O)O). BaTf2 . 2H(2)O, [9b]-OAc . OAc . BaTf2 . 2H(2)O, crystallized in the triclinic space group P (1) over bar; with a = 10.747(2) Angstrom, b = 12.271(8) Angstrom, c = 16.206(6) Angstrom, alpha = 106.10(4)degrees, beta = 103.07(2)degrees, gamma = 106.06(3), and Z = 2, while [(3,3',6,6'-(CH3)(4)-SALOPHEN)-Mn-III]PF6 . H2O, [6b]PF6 . H2O, crystallized in the monoclinic space group P2(1)/n, with a = 12.465(1) Angstrom, b = 13.366(2) Angstrom, c = 15.240(1) Angstrom, beta = 103.051(7)degrees, and Z = 2. [9b]OAc . BaTf2 . 2H(2)O has the Mn(III) center ligated in the axial positions by one oxygen of the acetate group and an oxygen from one SO3CF3-. The second oxygen of the acetate is bound to the Ba2+ residing in the crown ether. The water molecule in [6b]PF6 . H2O is O-bound to the Mn(III) center and also hydrogen bonded to one of the fluorine atoms of the PF6 counterion, O-F 3.01 Angstrom. H-1 and F-19 NMR spectra revealed that the hydrogen bond in [6b]PF6 . H2O was preserved in CD3OD.
The synthesis and characterization of [M(salen/salophen/saldeta)] [M=Cr(III), Mn(III) or Fe(III)] capped s-triazine cored tripodal trinuclear Schiff bases complexes
作者:Berkman İşçi、Şaban Uysal
DOI:10.1007/s10847-018-0844-7
日期:2018.12
bases complexes were synthesized with the reaction of 8 and/or 9 and ligand complexes. The complexes have been characterized as low-spin (S = 1/2) distorted octahedral Fe(III)Salen/Salophen, low-spin (S = 1) distorted octahedral Mn(III)Salen/Salophen, high-spin (S = 5/2) distorted octahedral Fe(III)Saldeta, high-spin (S = 2) distorted octahedral Mn(III)Saldeta and (S = 3/2) distorted octahedral Cr(II