188547-60-6Relevant articles and documents
Synthesis and spectroscopic characterization of five-coordinate complexes of Ni2+ based on N3-macrocycles and salicylaldiminates. Crystal structure of [Ni(9-Me-N3-mc)(OC6H4CH=NC6H 5-o)](ClO4) (9-Me-N3-mc=2,4,4,9-tetramethyl-1,5,9-triazacyclododec-1-ene)
Santana, M. Dolores,Rufete, Antonio,Sánchez, Gregorio,García, Gabriel,López, Gregorio,Casabó, Jaume,Molins, Elíes,Miravitlles, Carles
, p. 21 - 27 (2008/10/08)
Five-coordinate nickel(II) complexes of the type [Ni(N3-macrocycle)(OC6H4CH=NR-o)]+ (N3-macrocycle=2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene, N3-mc, or its 9-methyl derivative, 9-Me-N3-mc) have been prepared by reaction between [{Ni(N3-macrocycle)(μ-OH)}2]+ and the appropriate arylsalicylaldimine. An X-ray diffraction study carried out with the complex [Ni(9-Me-N3-mc)(OC6H4CH=NC6H 5-o)](ClO4) has established that the Ni atom presents a square pyramidal coordination and is displaced 0.30 A? out of the basal plane towards the apical N1 atom (a=8.552(2), b=33.398(3), c=9.630(3) A?, β=91.67(1)°, monoclinic, space group P21/a, V=2749(1) A?3, Z=4, Dcalc=1.40 g cm-3, R=0.058, Rw=0.066). These paramagnetic species have been studied by 1H NMR. The characteristic pattern of N3-mc and 9-Me-N3-mc has been established and the specific assigment of salicylaldimine resonances has been achieved by NOE measurements. The solution electronic spectra of the complexes are also suggestive of five-coordinate geometry in solution.
