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

Wang, Xue; Zhao, Ke Qing; Elsegood, Mark R.J.; Redshaw, Carl

Authors

Xue Wang

Ke Qing Zhao

Mark R.J. Elsegood

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Professor Carl Redshaw C.Redshaw@hull.ac.uk
Professor of Inorganic Materials Chemistry and REF Lead for Chemistry



Abstract

The ‘one-pot’ reaction of 2-hydroxy-3,5-di-tert-butylsalicylaldehyde with in situ generated ‘amino calixarene’ (from {Mo[(2-NC 6 H 4 ) 2 CH 2 CH 2 ]Cl 2 (DME)}, KOtBu and p-tert-butylcalix[4]areneH 4 LH 4 ) afforded, after work-up, the heterobimetallic salt K(NCMe) 2 [Mo(NCMe)(OEt)(2-C 6 H 4 CH 2 CH 2 C 6 H 4 NH 2 -2)L] (1∙2MeCN). By constrast, use of the ‘amino calixarene’ [Mo(NCMe)(2-C 6 H 4 CH 2 CH 2 C 6 H 4 NH 2 -2)L] afforded the potassium/ethoxide-free complex [Mo(NCMe)(2-C 6 H 4 CH 2 CH 2 C 6 H 4 N-2-CHC 6 H 2 -2′-(OH)-3′,5′-tBu)L] (2∙2MeCN). Reaction of the ‘amino calixarene’ (two equivalents) with the dialdehyde [1,3-(CHO) 2 -5-MeC 6 H 3 OH-2] led, following work-up, to the isolation of the cation-anion pair [C 46 H 42 N 4 O 2 ] 2+ [Mo 6 O 19 ] 2− ·C 2 H 3 N (3∙MeCN). 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 O 5 N 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 O 4 N 2 coordination environment. In 3, a protonated macrocyclic cation, formed via hydrolysis, has weak intermolecular interactions with the polyoxomolybdate anion.

Citation

Wang, X., Zhao, K. Q., Elsegood, M. R., & Redshaw, C. (2018). Molybdocalix[4]arene N,O-Schiff-base ligands. Supramolecular chemistry, 30(5-6), 404-410. https://doi.org/10.1080/10610278.2017.1403608

Journal Article Type Article
Acceptance Date Nov 6, 2017
Online Publication Date Nov 27, 2017
Publication Date 2018
Deposit Date Nov 15, 2017
Publicly Available Date Mar 28, 2024
Journal Supramolecular Chemistry
Print ISSN 1061-0278
Electronic ISSN 1029-0478
Publisher Taylor and Francis
Peer Reviewed Peer Reviewed
Volume 30
Issue 5-6
Pages 404-410
DOI https://doi.org/10.1080/10610278.2017.1403608
Keywords Molybdenum; Calixarene; Schiff base; Molecular structures
Public URL https://hull-repository.worktribe.com/output/456508
Publisher URL http://www.tandfonline.com/doi/full/10.1080/10610278.2017.1403608
Additional Information Peer Review Statement: The publishing and review policy for this title is described in its Aims & Scope.; Aim & Scope: http://www.tandfonline.com/action/journalInformation?show=aimsScope&journalCode=gsch20

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