Iminoacylation. 3. Formation of platinum(IV)-based metallaligands due to facile one-end addition of vic-dioximes to coordinated organonitriles1-3

Author(s)
Vadim Yu Kukushkin, Tatyana B. Pakhomova, Nadezhda A. Bokach, Gabriele Wagner, Maxim L. Kuznetsov, Mathea Sophia Galanski, Armando J L Pombeiro
Abstract

The reaction of vic-dioximes with the organonitrile platinum(IV) complexes trans-[PtCl4(RCN)2] (R = Me, CH2- Ph, Ph, vic-dioxime = dimethylglyoxime; R = Me, vic-dioxime = cyclohexa-, cyclohepta-, and cyclooctanedione dioximes) proceeds rapidly under relatively mild conditions and affords products of one-end addition of the dioximes to the nitrile carbon, i.e. [PtCl4(NH = C(R)ON = {spacer} = NOH)2] (1-6) (R = Me, CH2Ph, Ph, spacer = C(Me)C-(Me) for dimethylglyoxime; R = Me, spacer = C{C4H8}C, C{C5H(10)}C, C{C6H(12)}C for the other dioximes), giving a novel type of metallaligand. All addition compounds were characterized by elemental analyses (C, H, N, Cl, Pt), FAB mass spectrometry, and IR and 1H, (13)C{1H}, and (195)Pt NMR spectroscopy. X-ray structure determination of the dimethylformamide bis-solvate [PtCl4(NH = C(Me)ON = C(Me)C(Me) = NOH)2]ž2DMF (1a) disclosed its overall trans geometry with the dimethylglyoxime part in anti configuration and the amidine one-end (rather than N,N-bidentate) coordination mode of the N-donor ligands. When a mixture of cis- and trans-[PtCl4(MeCN)2] in MeCN was treated with dimethylglyoxime, the formation of, correspondingly, cis- and trans-[PtCl4(NH = C(Me)ON = C(Me)C(Me) = NOH)2] (1) was observed and cis-to-trans isomerization in DMSO-d6 solution was monitored by 1H, 2D [1H, 15)N] HMQC, and (195)Pt NMR spectroscopies. Although performed ab initio calculations give evidence that the trans geometry is the favorable one for the iminoacylated species [PtCl4- (ligand)2], the platinum(IV) complex [PtCl4(NH = C(Me)ON = C{C4H8}C = NOH)2] (4) was isolated exclusively in cis configuration with the two metallaligand 'arms' held together by intramolecular hydrogen bonding between the two peripheral OH groups, as it was proved by single-crystal X-ray diffractometry. The classic substitution products, e.g. [PtCl2(N,N-dioximato)2] (12-15), are formed in the addition reaction as only byproducts in minor yield; two of them, [PtCl2(C7H11N2O2)2] (14) and [PtCl2(C8H13N2O2)2] (15), were structurally characterized. Complexes (12-15) were also prepared by reaction of the vic-dioximes with [PtCl4L(Me2SO)] (L = Me2SO, MeCN), but monoximes (Me2C = NOH, {C4H8}C = NOH, {C5H(10)}C = NOH, PhC(H) = NOH, (OH)C6H4C(H) = NOH) react differently adding to [PtCl4(MeCN)(Me2SO)] to give the corresponding iminoacylated products [PtCl4- (NH = C(Me)ON = CRR')(Me2SO)] (7-11).

Organisation(s)
Department of Inorganic Chemistry
External organisation(s)
Saint Petersburg State University, Peter the Great St.Petersburg Polytechnic University, University of Surrey, Anuchin Research Institute and Museum of Anthropology, Instituto Superior Técnico
Journal
Inorganic Chemistry
Volume
39
Pages
216-225
No. of pages
10
ISSN
0020-1669
Publication date
2000
Peer reviewed
Yes
Austrian Fields of Science 2012
1040 Chemistry
Portal url
https://ucrisportal.univie.ac.at/en/publications/a1ba06df-ed8c-456e-b53f-8c5c20da3ab9