Two related lithium calixarene complexes, [p-tert-butyl-calix[4]arene(OMe) (OH)2(OLi)]2·4MeCN and {p-tert-butyl-calix[4] arene(OH)2(OLi)[OLi(NCMe)2]}2·8MeCN, determined using synchrotron radiation

Lee, Darren S.; Elsegood, Mark R.J.; Redshaw, Carl; Zhan, Shuzhong

Abstract

The crystal structures of acetonitrile solvates of two related lithium calixarene complexes have been determined by low-temperature single-crystal X-ray diffraction using synchrotron radiation. Bis(μ-5,11,17,23-tetra-tert- butyl-26,28-dihydr-oxy-25-meth-oxy-27-oxido-calix[4]arene)dilithium(I) acetonitrile tetra- solvate, [Li2(C45H57O 4)2]·4C2H3N or [p-tert-butyl-calix[4]arene-(OMe)(OH) 2 (OLi)]2·4MeCN, (I), crystallizes with the complex across a centre of symmetry and with four mol-ecules of unbound aceto-nitrile of crystallization per com-plex. Tetra-acetonitrile-bis(μ-5,11,17,23-tetra-tert-butyl-26,28-dihydr-oxy-25, 27-dioxidocalix[4]arene)tetra-lithium(I) acetonitrile octa-solvate, [Li 4 (C44H54O4)2(C 2H3N) 4]·8C2H3N or {p-tert-butyl-calix[4]arene(OH)2(OLi)[OLi(NCMe) 2]} 2·8MeCN, (II), also crystallizes with the complex lying across a centre of symmetry and contains eight mol-ecules of unbound acetonitrile per complex plus four more directly bound to two of the lithium ions, two on each ion. The cores of both complexes are partially supported by O- H⋯O hydrogen bonds. The meth-oxy methyl groups in (I) prevent the binding of any more than two Li+ ions, while the corresponding two O-atom sites in (II) bind an extra Li+ ion each, making four in total. The calixarene cone adopts an undistorted cone conformation in (I), but an elliptical one in (II).

Citation

Lee, D. S., Elsegood, M. R., Redshaw, C., & Zhan, S. (2009). Two related lithium calixarene complexes, [p-tert-butyl-calix[4]arene(OMe) (OH)2(OLi)]2·4MeCN and {p-tert-butyl-calix[4] arene(OH)2(OLi)[OLi(NCMe)2]}2·8MeCN, determined using synchrotron radiation. Acta Crystallographica Section C: Crystal Structure Communications, 65(8), m291-m295. https://doi.org/10.1107/S0108270109025311

• Journal Article Type: Article
• Publication Date: Aug 19, 2009
• Deposit Date: Jun 8, 2022
• Journal: Acta Crystallographica Section C: Crystal Structure Communications
• Print ISSN: 0108-2701
• Electronic ISSN: 0108-2701
• Publisher: International Union of Crystallography
• Peer Reviewed: Peer Reviewed
• Volume: 65
• Issue: 8
• Pages: m291-m295
• DOI: https://doi.org/10.1107/S0108270109025311
• Public URL: https://hull-repository.worktribe.com/output/3622530