Rhenium(V)salen complexes: configurational control and ligand exchange

Kjeld J.C. Bommel, Willem Verboom, Huub Kooijman, Anthony L. Spek, David N. Reinhoudt

Research output: Contribution to journalArticleAcademicpeer-review

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Abstract

Reactions of ReO(PPh3)2Cl3 with tetradentate bis(salicylideneamine) ligands, H2salpd (1) and H2salbd (2), in different alcohols gave the novel mixed-ligand rhenium complexes ReO(sal)OAlk (OAlk = variety of alkoxy ligands). Configurational studies show that the rhenium complexes ReO(salpd)OAlk (1a−f) display either a symmetrical or a nonsymmetrical configuration, depending on the size of the alcohol and its boiling point. The rhenium complexes ReO(salbd)OAlk (2a−d) are all nonsymmetrical due to the number of carbons that bridge the imine nitrogens. In the case of the symmetrical ReO(salpd)OMe (1a) complex the methoxy ligand can be exchanged for a number of ligands of different types (OAlk, OPh, SAlk, OC(O)Alk). In the newly formed complexes the original configuration was retained except for the ReO(salpd)SAlk (1i,j) complexes which were isolated in the nonsymmetrical configuration. Starting from the nonsymmetrical ReO(salpd)OPr (2c) complex, ligand exchange led to a mixture of the symmetrical and nonsymmetrical complexes, with ratios depending on the reaction time. The crystal structures of ReO(salbd)OPr (2c), and ReO(salpd)OPhOMe (1g) have been determined. ReO(salbd)OPr crystallizes in the triclinic space group P1̄, Z = 2, with a = 10.0344(16) Å, b = 10.647(2) Å, c = 11.481(2) Å, α = 86.551(15)°, β = 86.998(14)°, γ = 80.112(15)°, V = 1205.1(4) Å3, and final R = 0.0460. Crystals of ReO(salpd)OPhOMe are orthorhombic, space group P212121, Z = 4, with a = 10.6222(15) Å, b = 12.442(3) Å, c = 16.354(3) Å, V = 2161.4(7) Å3, and final R = 0.0371. Under the influence of traces of water a number of symmetrical complexes react to a “dimeric” structure, consisting of two ReO(salpd) moieties bridged by an oxygen atom with the bridging Re−O−Re angle symmetrically imposed at 180°. [ReO(salpd)]2O (3) crystallizes in the monoclinic, space group P21/c, Z = 4, with a = 14.860(2) Å, b = 12.545(2) Å, c = 16.5111(17) Å, β = 95.030(10)°, V = 3066.1(7) Å3, and final R = 0.0439.
Original languageEnglish
Pages (from-to)4197-4203
JournalInorganic chemistry
Volume37
Issue number37
DOIs
Publication statusPublished - 1998

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Rhenium
rhenium
Ligands
ligands
alcohols
configurations
Alcohols
Imines
Boiling point
reaction time
boiling
imines
disalicylaldehyde ethylenediamine
oxygen atoms
Nitrogen
Carbon
Crystal structure
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Oxygen
nitrogen

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Bommel, Kjeld J.C. ; Verboom, Willem ; Kooijman, Huub ; Spek, Anthony L. ; Reinhoudt, David N. / Rhenium(V)salen complexes : configurational control and ligand exchange. In: Inorganic chemistry. 1998 ; Vol. 37, No. 37. pp. 4197-4203.
@article{f4fabd0cd43c43e38801b0acd3e218d9,
title = "Rhenium(V)salen complexes: configurational control and ligand exchange",
abstract = "Reactions of ReO(PPh3)2Cl3 with tetradentate bis(salicylideneamine) ligands, H2salpd (1) and H2salbd (2), in different alcohols gave the novel mixed-ligand rhenium complexes ReO(sal)OAlk (OAlk = variety of alkoxy ligands). Configurational studies show that the rhenium complexes ReO(salpd)OAlk (1a−f) display either a symmetrical or a nonsymmetrical configuration, depending on the size of the alcohol and its boiling point. The rhenium complexes ReO(salbd)OAlk (2a−d) are all nonsymmetrical due to the number of carbons that bridge the imine nitrogens. In the case of the symmetrical ReO(salpd)OMe (1a) complex the methoxy ligand can be exchanged for a number of ligands of different types (OAlk, OPh, SAlk, OC(O)Alk). In the newly formed complexes the original configuration was retained except for the ReO(salpd)SAlk (1i,j) complexes which were isolated in the nonsymmetrical configuration. Starting from the nonsymmetrical ReO(salpd)OPr (2c) complex, ligand exchange led to a mixture of the symmetrical and nonsymmetrical complexes, with ratios depending on the reaction time. The crystal structures of ReO(salbd)OPr (2c), and ReO(salpd)OPhOMe (1g) have been determined. ReO(salbd)OPr crystallizes in the triclinic space group P1̄, Z = 2, with a = 10.0344(16) {\AA}, b = 10.647(2) {\AA}, c = 11.481(2) {\AA}, α = 86.551(15)°, β = 86.998(14)°, γ = 80.112(15)°, V = 1205.1(4) {\AA}3, and final R = 0.0460. Crystals of ReO(salpd)OPhOMe are orthorhombic, space group P212121, Z = 4, with a = 10.6222(15) {\AA}, b = 12.442(3) {\AA}, c = 16.354(3) {\AA}, V = 2161.4(7) {\AA}3, and final R = 0.0371. Under the influence of traces of water a number of symmetrical complexes react to a “dimeric” structure, consisting of two ReO(salpd) moieties bridged by an oxygen atom with the bridging Re−O−Re angle symmetrically imposed at 180°. [ReO(salpd)]2O (3) crystallizes in the monoclinic, space group P21/c, Z = 4, with a = 14.860(2) {\AA}, b = 12.545(2) {\AA}, c = 16.5111(17) {\AA}, β = 95.030(10)°, V = 3066.1(7) {\AA}3, and final R = 0.0439.",
author = "Bommel, {Kjeld J.C.} and Willem Verboom and Huub Kooijman and Spek, {Anthony L.} and Reinhoudt, {David N.}",
year = "1998",
doi = "10.1021/ic980125t",
language = "English",
volume = "37",
pages = "4197--4203",
journal = "Inorganic chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "37",

}

Rhenium(V)salen complexes : configurational control and ligand exchange. / Bommel, Kjeld J.C.; Verboom, Willem; Kooijman, Huub; Spek, Anthony L.; Reinhoudt, David N.

In: Inorganic chemistry, Vol. 37, No. 37, 1998, p. 4197-4203.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - Rhenium(V)salen complexes

T2 - configurational control and ligand exchange

AU - Bommel, Kjeld J.C.

AU - Verboom, Willem

AU - Kooijman, Huub

AU - Spek, Anthony L.

AU - Reinhoudt, David N.

PY - 1998

Y1 - 1998

N2 - Reactions of ReO(PPh3)2Cl3 with tetradentate bis(salicylideneamine) ligands, H2salpd (1) and H2salbd (2), in different alcohols gave the novel mixed-ligand rhenium complexes ReO(sal)OAlk (OAlk = variety of alkoxy ligands). Configurational studies show that the rhenium complexes ReO(salpd)OAlk (1a−f) display either a symmetrical or a nonsymmetrical configuration, depending on the size of the alcohol and its boiling point. The rhenium complexes ReO(salbd)OAlk (2a−d) are all nonsymmetrical due to the number of carbons that bridge the imine nitrogens. In the case of the symmetrical ReO(salpd)OMe (1a) complex the methoxy ligand can be exchanged for a number of ligands of different types (OAlk, OPh, SAlk, OC(O)Alk). In the newly formed complexes the original configuration was retained except for the ReO(salpd)SAlk (1i,j) complexes which were isolated in the nonsymmetrical configuration. Starting from the nonsymmetrical ReO(salpd)OPr (2c) complex, ligand exchange led to a mixture of the symmetrical and nonsymmetrical complexes, with ratios depending on the reaction time. The crystal structures of ReO(salbd)OPr (2c), and ReO(salpd)OPhOMe (1g) have been determined. ReO(salbd)OPr crystallizes in the triclinic space group P1̄, Z = 2, with a = 10.0344(16) Å, b = 10.647(2) Å, c = 11.481(2) Å, α = 86.551(15)°, β = 86.998(14)°, γ = 80.112(15)°, V = 1205.1(4) Å3, and final R = 0.0460. Crystals of ReO(salpd)OPhOMe are orthorhombic, space group P212121, Z = 4, with a = 10.6222(15) Å, b = 12.442(3) Å, c = 16.354(3) Å, V = 2161.4(7) Å3, and final R = 0.0371. Under the influence of traces of water a number of symmetrical complexes react to a “dimeric” structure, consisting of two ReO(salpd) moieties bridged by an oxygen atom with the bridging Re−O−Re angle symmetrically imposed at 180°. [ReO(salpd)]2O (3) crystallizes in the monoclinic, space group P21/c, Z = 4, with a = 14.860(2) Å, b = 12.545(2) Å, c = 16.5111(17) Å, β = 95.030(10)°, V = 3066.1(7) Å3, and final R = 0.0439.

AB - Reactions of ReO(PPh3)2Cl3 with tetradentate bis(salicylideneamine) ligands, H2salpd (1) and H2salbd (2), in different alcohols gave the novel mixed-ligand rhenium complexes ReO(sal)OAlk (OAlk = variety of alkoxy ligands). Configurational studies show that the rhenium complexes ReO(salpd)OAlk (1a−f) display either a symmetrical or a nonsymmetrical configuration, depending on the size of the alcohol and its boiling point. The rhenium complexes ReO(salbd)OAlk (2a−d) are all nonsymmetrical due to the number of carbons that bridge the imine nitrogens. In the case of the symmetrical ReO(salpd)OMe (1a) complex the methoxy ligand can be exchanged for a number of ligands of different types (OAlk, OPh, SAlk, OC(O)Alk). In the newly formed complexes the original configuration was retained except for the ReO(salpd)SAlk (1i,j) complexes which were isolated in the nonsymmetrical configuration. Starting from the nonsymmetrical ReO(salpd)OPr (2c) complex, ligand exchange led to a mixture of the symmetrical and nonsymmetrical complexes, with ratios depending on the reaction time. The crystal structures of ReO(salbd)OPr (2c), and ReO(salpd)OPhOMe (1g) have been determined. ReO(salbd)OPr crystallizes in the triclinic space group P1̄, Z = 2, with a = 10.0344(16) Å, b = 10.647(2) Å, c = 11.481(2) Å, α = 86.551(15)°, β = 86.998(14)°, γ = 80.112(15)°, V = 1205.1(4) Å3, and final R = 0.0460. Crystals of ReO(salpd)OPhOMe are orthorhombic, space group P212121, Z = 4, with a = 10.6222(15) Å, b = 12.442(3) Å, c = 16.354(3) Å, V = 2161.4(7) Å3, and final R = 0.0371. Under the influence of traces of water a number of symmetrical complexes react to a “dimeric” structure, consisting of two ReO(salpd) moieties bridged by an oxygen atom with the bridging Re−O−Re angle symmetrically imposed at 180°. [ReO(salpd)]2O (3) crystallizes in the monoclinic, space group P21/c, Z = 4, with a = 14.860(2) Å, b = 12.545(2) Å, c = 16.5111(17) Å, β = 95.030(10)°, V = 3066.1(7) Å3, and final R = 0.0439.

U2 - 10.1021/ic980125t

DO - 10.1021/ic980125t

M3 - Article

VL - 37

SP - 4197

EP - 4203

JO - Inorganic chemistry

JF - Inorganic chemistry

SN - 0020-1669

IS - 37

ER -