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

Darren S. Lee; Mark R. J. Elsegood; Carl Redshaw; Shu-Zhong Zhan

doi:10.1107/S0108270109025311

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

Darren S. Lee, Mark R. J. Elsegood, Carl Redshaw, Shu-Zhong Zhan

Research output: Contribution to journal › Article › peer-review

1 Citation (Scopus)

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(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25-methoxy-27-oxidocalix[4]arene)dilithium(I) acetonitrile tetrasolvate, [Li₂(C₄₅H₅₇O₄)₂]·4C₂H₃N or [p-tert-butylcalix[4]arene(OMe)(OH)₂(OLi)]₂·4MeCN, (I), crystallizes with the complex across a centre of symmetry and with four molecules of unbound acetonitrile of crystallization per complex. Tetraacetonitrilebis(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25,27-dioxidocalix[4]arene)tetralithium(I) acetonitrile octasolvate, [Li₄(C₄₄H₅₄O₄)₂(C₂H₃N)₄]·8C₂H₃N or {p-tert-butylcalix[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 molecules 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-HO hydrogen bonds. The methoxy 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).

Formula: [Li₂(C₄₅H₅₇O₄)₂]·4C₂H₃N and [Li₄(C₄₄H₅₄O₄)₂(C₂H₃N)₄]·8C₂H₃N

Original language	English
Pages (from-to)	m291-m295
Number of pages	5
Journal	Acta Crystallographica Section C
Volume	65
Issue number	8
DOIs	https://doi.org/10.1107/S0108270109025311
Publication status	Published - Aug 2009

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10.1107/S0108270109025311

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@article{88ca9d31b6384b5c9e5778e131bccb7d,

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

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(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25-methoxy-27-oxidocalix[4]arene)dilithium(I) acetonitrile tetrasolvate, [Li2(C45H57O4)2]·4C2H3N or [p-tert-butylcalix[4]arene(OMe)(OH)2(OLi)]2·4MeCN, (I), crystallizes with the complex across a centre of symmetry and with four molecules of unbound acetonitrile of crystallization per complex. Tetraacetonitrilebis(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25,27-dioxidocalix[4]arene)tetralithium(I) acetonitrile octasolvate, [Li4(C44H54O4)2(C2H3N)4]·8C2H3N or {p-tert-butylcalix[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 molecules 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-HO hydrogen bonds. The methoxy 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).Formula: [Li2(C45H57O4)2]·4C2H3N and [Li4(C44H54O4)2(C2H3N)4]·8C2H3N",

author = "Lee, {Darren S.} and Elsegood, {Mark R. J.} and Carl Redshaw and Shu-Zhong Zhan",

year = "2009",

month = aug,

doi = "10.1107/S0108270109025311",

language = "English",

volume = "65",

pages = "m291--m295",

journal = "Acta Crystallographica Section C: Crystal Structure Communications",

issn = "0108-2701",

publisher = "International Union of Crystallography",

number = "8",

}

In: Acta Crystallographica Section C, Vol. 65, No. 8, 08.2009, p. m291-m295.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Two related lithium calixarene complexes, [p-tert-butylcalix[4]arene(OMe)(OH)2(OLi)]2·4MeCN and {p-tert-butylcalix[4]arene(OH)2(OLi)[OLi(NCMe)2]}2·8MeCN, determined using synchrotron radiation

AU - Lee, Darren S.

AU - Elsegood, Mark R. J.

AU - Redshaw, Carl

AU - Zhan, Shu-Zhong

PY - 2009/8

Y1 - 2009/8

N2 - 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(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25-methoxy-27-oxidocalix[4]arene)dilithium(I) acetonitrile tetrasolvate, [Li2(C45H57O4)2]·4C2H3N or [p-tert-butylcalix[4]arene(OMe)(OH)2(OLi)]2·4MeCN, (I), crystallizes with the complex across a centre of symmetry and with four molecules of unbound acetonitrile of crystallization per complex. Tetraacetonitrilebis(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25,27-dioxidocalix[4]arene)tetralithium(I) acetonitrile octasolvate, [Li4(C44H54O4)2(C2H3N)4]·8C2H3N or {p-tert-butylcalix[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 molecules 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-HO hydrogen bonds. The methoxy 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).Formula: [Li2(C45H57O4)2]·4C2H3N and [Li4(C44H54O4)2(C2H3N)4]·8C2H3N

AB - 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(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25-methoxy-27-oxidocalix[4]arene)dilithium(I) acetonitrile tetrasolvate, [Li2(C45H57O4)2]·4C2H3N or [p-tert-butylcalix[4]arene(OMe)(OH)2(OLi)]2·4MeCN, (I), crystallizes with the complex across a centre of symmetry and with four molecules of unbound acetonitrile of crystallization per complex. Tetraacetonitrilebis(-5,11,17,23-tetra-tert-butyl-26,28-dihydroxy-25,27-dioxidocalix[4]arene)tetralithium(I) acetonitrile octasolvate, [Li4(C44H54O4)2(C2H3N)4]·8C2H3N or {p-tert-butylcalix[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 molecules 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-HO hydrogen bonds. The methoxy 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).Formula: [Li2(C45H57O4)2]·4C2H3N and [Li4(C44H54O4)2(C2H3N)4]·8C2H3N

U2 - 10.1107/S0108270109025311

DO - 10.1107/S0108270109025311

M3 - Article

VL - 65

SP - m291-m295

JO - Acta Crystallographica Section C: Crystal Structure Communications

JF - Acta Crystallographica Section C: Crystal Structure Communications

SN - 0108-2701

IS - 8

ER -