The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions,...

Simon R. Drake; David J. Otway; Michael B. Hursthouse; K. M.Abdul Malik

doi:10.1016/S0277-5387(00)83154-X

The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions,...

Simon R. Drake
, David J. Otway
, Michael B. Hursthouse
, K. M.Abdul Malik

Imperial College London
University of Wales

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

Abstract

Title full: The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions, [M(OAr′)₂]₂, and the adducts [M(OAr′)₂(L)_x]·L (M = Ca, Sr, Ba; Ar′= 2,4,6,-tri-t-butyl-phenol; L THF, x = 3; M = Ba; L = DME, x = 2; and L = HMPA, x = 3); and the X-ray structure of [Sr(OAr′)₂(THF)₃]· 0.5THF. The homoleptic group IIA phenoxides, [M(OAr′)₂]₂ (M = Ca, Sr and Ba), have been synthesized by the reaction of the bulk metal and 2,4,6,-tri-t-butyl-phenol in a mixed ammonia-toluene solution at -40°C. Ammonia adducts are initially obtained, [M(OAr′)₂(NH₃)_x]_n, which may be readily converted to the homoleptic dimers by the toluene reflux method. The dimeric complexes [M(OAr′)₂]₂ react with a range of Lewis bases to yield the monomeric adducts [M(OAr′)₂(L)_x]· L. All complexes have been characterized by IR, ¹H and ¹³C NMR spectroscopy, solution cryoscopy (in selected cases) and microanalysis. The X-ray structure of [Sr(OAr′)₂(THF)₃]· (THF) reveals that it has a monomeric distorted trigonal bipyramidal structure with two THF ligands in apical positions, while the fourth THF molecule is present as a hemi-solvate.

Original language	English
Pages (from-to)	1995-2007
Number of pages	13
Journal	Polyhedron
Volume	11
Issue number	16
DOIs	https://doi.org/10.1016/S0277-5387(00)83154-X
Publication status	Published - 1992
Externally published	Yes

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10.1016/S0277-5387(00)83154-X

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@article{684dc9a693ec49e9bf381ed28546a6fc,

title = "The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions,...",

abstract = "Title full: The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions, [M(OAr′)2]2, and the adducts [M(OAr′)2(L)x]·L (M = Ca, Sr, Ba; Ar′= 2,4,6,-tri-t-butyl-phenol; L THF, x = 3; M = Ba; L = DME, x = 2; and L = HMPA, x = 3); and the X-ray structure of [Sr(OAr′)2(THF)3]· 0.5THF. The homoleptic group IIA phenoxides, [M(OAr′)2]2 (M = Ca, Sr and Ba), have been synthesized by the reaction of the bulk metal and 2,4,6,-tri-t-butyl-phenol in a mixed ammonia-toluene solution at -40°C. Ammonia adducts are initially obtained, [M(OAr′)2(NH3)x]n, which may be readily converted to the homoleptic dimers by the toluene reflux method. The dimeric complexes [M(OAr′)2]2 react with a range of Lewis bases to yield the monomeric adducts [M(OAr′)2(L)x]· L. All complexes have been characterized by IR, 1H and 13C NMR spectroscopy, solution cryoscopy (in selected cases) and microanalysis. The X-ray structure of [Sr(OAr′)2(THF)3]· (THF) reveals that it has a monomeric distorted trigonal bipyramidal structure with two THF ligands in apical positions, while the fourth THF molecule is present as a hemi-solvate.",

author = "Drake, \{Simon R.\} and Otway, \{David J.\} and Hursthouse, \{Michael B.\} and Malik, \{K. M.Abdul\}",

year = "1992",

doi = "10.1016/S0277-5387(00)83154-X",

language = "English",

volume = "11",

pages = "1995--2007",

journal = "Polyhedron",

issn = "0277-5387",

publisher = "Elsevier Ltd",

number = "16",

}

TY - JOUR

T1 - The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions,...

AU - Drake, Simon R.

AU - Otway, David J.

AU - Hursthouse, Michael B.

AU - Malik, K. M.Abdul

PY - 1992

Y1 - 1992

N2 - Title full: The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions, [M(OAr′)2]2, and the adducts [M(OAr′)2(L)x]·L (M = Ca, Sr, Ba; Ar′= 2,4,6,-tri-t-butyl-phenol; L THF, x = 3; M = Ba; L = DME, x = 2; and L = HMPA, x = 3); and the X-ray structure of [Sr(OAr′)2(THF)3]· 0.5THF. The homoleptic group IIA phenoxides, [M(OAr′)2]2 (M = Ca, Sr and Ba), have been synthesized by the reaction of the bulk metal and 2,4,6,-tri-t-butyl-phenol in a mixed ammonia-toluene solution at -40°C. Ammonia adducts are initially obtained, [M(OAr′)2(NH3)x]n, which may be readily converted to the homoleptic dimers by the toluene reflux method. The dimeric complexes [M(OAr′)2]2 react with a range of Lewis bases to yield the monomeric adducts [M(OAr′)2(L)x]· L. All complexes have been characterized by IR, 1H and 13C NMR spectroscopy, solution cryoscopy (in selected cases) and microanalysis. The X-ray structure of [Sr(OAr′)2(THF)3]· (THF) reveals that it has a monomeric distorted trigonal bipyramidal structure with two THF ligands in apical positions, while the fourth THF molecule is present as a hemi-solvate.

AB - Title full: The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions, [M(OAr′)2]2, and the adducts [M(OAr′)2(L)x]·L (M = Ca, Sr, Ba; Ar′= 2,4,6,-tri-t-butyl-phenol; L THF, x = 3; M = Ba; L = DME, x = 2; and L = HMPA, x = 3); and the X-ray structure of [Sr(OAr′)2(THF)3]· 0.5THF. The homoleptic group IIA phenoxides, [M(OAr′)2]2 (M = Ca, Sr and Ba), have been synthesized by the reaction of the bulk metal and 2,4,6,-tri-t-butyl-phenol in a mixed ammonia-toluene solution at -40°C. Ammonia adducts are initially obtained, [M(OAr′)2(NH3)x]n, which may be readily converted to the homoleptic dimers by the toluene reflux method. The dimeric complexes [M(OAr′)2]2 react with a range of Lewis bases to yield the monomeric adducts [M(OAr′)2(L)x]· L. All complexes have been characterized by IR, 1H and 13C NMR spectroscopy, solution cryoscopy (in selected cases) and microanalysis. The X-ray structure of [Sr(OAr′)2(THF)3]· (THF) reveals that it has a monomeric distorted trigonal bipyramidal structure with two THF ligands in apical positions, while the fourth THF molecule is present as a hemi-solvate.

UR - https://www.scopus.com/pages/publications/0013149686

U2 - 10.1016/S0277-5387(00)83154-X

DO - 10.1016/S0277-5387(00)83154-X

M3 - Article

AN - SCOPUS:0013149686

SN - 0277-5387

VL - 11

SP - 1995

EP - 2007

JO - Polyhedron

JF - Polyhedron

IS - 16

ER -

The synthesis and characterization of the group IIA homoleptic aryloxides under mild conditions,...

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