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Molybdocalix[4]arene N,O-Schiff base ligands

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journal contribution
posted on 16.11.2017, 13:51 authored by Xue Wang, Ke-Qing Zhao, Mark ElsegoodMark Elsegood, Carl Redshaw
The ‘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 Chemistry

Citation

WANG, X. ...et al., 2018. Molybdocalix[4]arene N,O-Schiff base ligands. Supramolecular Chemistry, 30(5-6), pp. 404-410.

Publisher

Taylor & Francis

Version

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

06/11/2017

Publication date

2017-11-27

Notes

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

1061-0278

Language

en