NDLI: Synthesis and physicochemical study of Ni$^{II}$ complexes with tetradentate acyclic and macrocyclic N$_{2}$S$

Content Provider	Springer Nature Link
Author	Butin, K. P. Moiseeva, A. A. Beloglazkina, E. K. Chudiv, Yu. B. Chizhevskii, A. A. Mirov, A. V. Tarasevich, B. N. Lalov, A. V. Zyk, N. V.
Copyright Year	2005
Abstract	N,N’-Polymethylenebis(thiosalicylidene)iminate and macrocyclic dithiadiazadibenzocycloalkadiene complexes of nickel(II) were synthesized and their electrochemical and spectroscopic properties were studied. Dithiadiazadibenzocycloalkadiene complexes containing two DMSO molecules coordinated to Ni$^{2+}$ and two outer-sphere ClO$_{4}$ $^{−}$ anions were synthesized by the reaction of the corresponding macrocyclic ligands with Ni(ClO$_{4}$)$_{2}$·6H$_{2}$O. The structure of 3,6-dithia-10,14-diazadibenzo[a,g]cyclopentadeca-9,14-dienylnickel(II)[bis(dimethyl sulfoxide) bis-perchlorate] was established by X-ray diffraction. The UV-Vis spectroscopic data are consistent with octahedral structures of diiminobis(sulfide) complexes, a square-planar structure of the thiosalen complex, and distorted tetrahedral structures of other diiminodithiolate complexes. The reaction of S-tert-butylthiosalicylaldehyde with hydrazine hydrate afforded di(ortho-tert-butylthiobenzal)azine. The reaction of the latter with anhydrous NiCl$_{2}$ produced a colored complex with the simplest molecular formula Ni(C$_{16}$H$_{12}$N$_{2}$S$_{2}$) in 15% yield. Semiempirical PM3(tm) calculations and the results of UV-Vis, ESR, and $^{1}$H NMR spectroscopy demonstrate that this complex has most probably a dimeric structure, in which two Ni centers adopt a nearly square-planar configuration. The complexes are clearly divided into two types according to their electrochemical behavior in DMF solutions. The type 1 is characterized by reversibility of the first reduction steps. The type 2 is characterized by irreversible two-electron reduction as the first step accompanied by deposition of Ni metal on the electrode surface. Rapid electrochemically initiated alkylation occurs in the presence of various alkylating agents (Bu$^{n}$I, Bu$^{n}$Br, (DmgH)$_{2}$CoCH$_{3}$) in a solution of complex 1 in DMF.
Starting Page	173
Ending Page	188
Page Count	16
File Format	PDF
ISSN	10665285
Journal	Russian Chemical Bulletin
Volume Number	54
Issue Number	1
e-ISSN	15739171
Language	English
Publisher	Kluwer Academic Publishers-Consultants Bureau
Publisher Date	2005-01-01
Publisher Place	New York
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	nickel(II) thiosalen homoleptic thiosalen complexes diiminobis(sulfide) complexes macrocyclic S,S-alkylidenethiosalicylimines electrochemistry UV-Vis spectroscopy 3,6-dithia-10,14-diazadibenzo[a,g]cyclopentadeca-9,14-dienylnickel(II) bis-dimethyl sulfoxide bis-perchlorate crystal and molecular structures Inorganic Chemistry Organic Chemistry Chemistry/Food Science
Content Type	Text
Resource Type	Article
Subject	Chemistry

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