Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L)

Beissel T, Glaser T, Kesting F, Wieghardt K, Nuber B (1996)
Inorganic Chemistry 35(13): 3936-3947.

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Abstract
The hexadentate, pendant arm macrocycle 1,4,7-tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacylononane (H(3)L) has been synthesized and isolated as its trihydrochloride, H(3)L . 3HCl, or sodium salt, Na(3)L, and its coordination chemistry with first-row transition metals has been studied. Mononuclear complexes of the type [LM(III)] (M Ga (1), In (2), V (3), Cr (4), Mn (5), Fe,Co (6)) have been isolated as have the one-electron-oxidized forms [LM]PF6 (M = V-IV (3a), Mn-IV (5a)). The crystal structure of 6 has been determined by single-crystal X-ray crystallography. Complex 6 crystallizes in the orthorhombic space group Iba2, with cell constants a = 14.206(8) Angstrom, b = 22.53(1) Angstrom, c = 26.07(1) Angstrom, V = 8344.0(3) Angstrom(3), and Z = 8. The cobalt(III) ion is in a distorted octahedral fac-N3S3 donor set. The reaction of L with divalent metal chlorides in a 1:2 ratio in methanol affords the homodinuclear complexes [LM(2)(II)Cl] (M = Mn (7), Co (8), Ni (9), Zn (10), Cd (11)) where one metal is six(N(3)MS(3)) and the other is four-coordinate (S(3)MCl); the two polyhedra are linked by three Lcp-thiolato bridges. Heterodinuclear complexes of the type [LM(1)M(2)Cl] have been obtained from [LM(2)Cl] species by abstraction of the four-coordinate metal ion and replacement by a different metal ion. The complexes [LZn(II)M(II)Cl] (M = Fe (12), Co (13), Ni (14)), [LNi(II)M(II)Cl] (M = Co (15), Zn (16)), and [LMn(II)M(II)Cl] (M = Fe (17), Co (18), Ni (19), Zn (20), Cd (21), Hg (22)) have been isolated as solid materials. The crystal structure of 14 has been determined by X-ray crystallography. Complex 14 crystallizes in the orthorhombic space group P2(1)2(1)2(1), with cell constants a = 15.45(1) Angstrom, b = 17.77(1) Angstrom, c = 17.58(1) Angstrom, V = 4826.5(4) Angstrom(3), and Z = 4. The linkage isomers 14 and 16 show characteristic electronic spectra for octahedrally and tetrahedrally coordinated Ni(II), respectively. The electronic structures of new complexes have been investigated by UV-vis spectroscopy; their magnetochemistry and electrochemistry are reported.
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Beissel T, Glaser T, Kesting F, Wieghardt K, Nuber B. Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L). Inorganic Chemistry. 1996;35(13):3936-3947.
Beissel, T., Glaser, T., Kesting, F., Wieghardt, K., & Nuber, B. (1996). Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L). Inorganic Chemistry, 35(13), 3936-3947.
Beissel, T., Glaser, T., Kesting, F., Wieghardt, K., and Nuber, B. (1996). Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L). Inorganic Chemistry 35, 3936-3947.
Beissel, T., et al., 1996. Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L). Inorganic Chemistry, 35(13), p 3936-3947.
T. Beissel, et al., “Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L)”, Inorganic Chemistry, vol. 35, 1996, pp. 3936-3947.
Beissel, T., Glaser, T., Kesting, F., Wieghardt, K., Nuber, B.: Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L). Inorganic Chemistry. 35, 3936-3947 (1996).
Beissel, T, Glaser, Thorsten, Kesting, F, Wieghardt, K, and Nuber, B. “Mono- and dinuclear transition metal complexes of the hexadentate ligand tris(4-tert-butyl-2-mercaptobenzyl)-1,4,7-triazacyclononane (L)”. Inorganic Chemistry 35.13 (1996): 3936-3947.
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Chemisorption of exchange-coupled [Ni2L(dppba)]+ complexes on gold by using ambidentate 4-(diphenylphosphino)benzoate co-ligands.
Golecki M, Lach J, Jeremies A, Lungwitz F, Fronk M, Salvan G, Zahn DR, Park J, Krupskaya Y, Kataev V, Klingeler R, Buchner B, Mahns B, Knupfer M, Siles PF, Grimm D, Schmidt OG, Reis A, Thiel WR, Breite D, Abel B, Kersting B., Chemistry 19(24), 2013
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