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Download fileMolybdocalix[4]arene N,O-Schiff base ligands
journal contribution
posted on 2017-11-16, 13:51 authored by Xue Wang, Ke-Qing Zhao, Mark ElsegoodMark Elsegood, Carl RedshawThe ‘one-pot’ reaction of 2-hydroxy-3,5-di-tert-butylsalicylaldehyde with in-situ generated
‘amino calixarene’ (from {Mo[(2-NC6H4)2CH2CH2]Cl2(DME)}, KOtBu and tbutylcalix[4]areneH4 LH4) afforded, after work-up, the heterobimetallic salt K(NCMe)2[Mo(NCMe)(OEt)(2-C6H4CH2CH2C6H4NH2-2)L] (1∙2MeCN). By constrast, use of the ‘amino calixarene’ [Mo(NCMe)(2-C6H4CH2CH2C6H4NH2-2)L]
afforded the potassium/ethoxide-free complex [Mo(NCMe)(2-C6H4CH2CH2C6H4N-2-CHC6H2-2/-(OH)-3/,5/-tBu)L] (2∙2MeCN). Reaction of 2 (two equivalents) with the dialdehyde [1,3-(CHO)2-5-MeC6H3OH-
2] led, following work-up, to the isolation of the cation-anion pair [C46H42N4O2]
2+[Mo6O19]2-·C2H3N (3). The molecular structures of 1·2MeCN, 2·2MeCN and 3·MeCN are reported, for which it was necessary to
use synchrotron radiation for data collection. Complex 1 contains an eliptical calixarene conformation as a result of π-interactions between the K+ and the arene groups and a distorted O5N octahedral geometry at the
molybdenum centre, whereas in ‘K+
/ethoxide-free’ 2, the calixarene retains the cone conformation and the metal possesses a distorted octahedral O4N2 coordination environment. In 3, a protonated macrocyclic
cation, formed via hydrolysis, has weak intermolecular interactions with the polyoxomolybdate anion.
Funding
Sichuan Normal University and the National Natural Science Foundation of China (grants 51443004 and 51273133) are thanked for financial support
History
School
- Science
Department
- Chemistry
Published in
Supramolecular ChemistryCitation
WANG, X. ...et al., 2018. Molybdocalix[4]arene N,O-Schiff base ligands. Supramolecular Chemistry, 30(5-6), pp. 404-410.Publisher
Taylor & FrancisVersion
- AM (Accepted Manuscript)
Publisher statement
This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/Acceptance date
2017-11-06Publication date
2017-11-27Notes
This is an Accepted Manuscript of an article published by Taylor & Francis in Supramolecular Chemistry on 27 November 2017, available online: http://www.tandfonline.com/10.1080/10610278.2017.1403608.ISSN
1061-0278Publisher version
Language
- en