Resolution and characterization of helicate dimer and trimer complexes of 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i)

Luis Lemus; Juan Guerrero; Juan Costamagna; Romina Lorca; Danilo H. Jara; Guillermo Ferraudi; Allen Oliver; A. Graham Lappin

doi:10.1039/c3dt50971k

Resolution and characterization of helicate dimer and trimer complexes of 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i)

Luis Lemus, Juan Guerrero, Juan Costamagna, Romina Lorca, Danilo H. Jara, Guillermo Ferraudi, Allen Oliver, A. Graham Lappin

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

16 Scopus citations

Abstract

Complexation of copper(i) with the binucleating ligand, 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane, mphenpr, result in formation of helical dimers, [Cu₂(mphenpr)₂]²⁺. The resolution of the enantiomeric forms of the dimers has been carried out with Δ-[As(cat)₃]^- as resolving agent and X-ray structures for two compounds, P-[Cu₂(mphenpr)₂](Δ- [As(cat)₃])₂ and P-[Cu₂(mphenpr) ₂](Δ-[As(cat)₃])₂·4(CH ₃CN), are reported. The rate of racemization in poorly-coordinating solvents has been examined by ¹H NMR, and is slow. At saturating concentrations of [[Cu₂(mphenpr)₂]²⁺] in acetonitrile, crystals of the helical trimeric complex [Cu₃(mphenpr) ₃](ClO₄)₃ are obtained. The X-ray structure of the trimer is reported. This species has also been resolved. As with the helical dimer, racemization in poorly-coordinating solvents is slow, and circular dichroism and ¹H NMR spectra are reported. The absolute configuration of the resolved complex, P-[Cu₃(mphenpr)₃](Δ- [As(cat)₃])₃, has been determined by X-ray crystallography.

Original language	English
Pages (from-to)	11426-11435
Number of pages	10
Journal	Dalton Transactions
Volume	42
Issue number	32
DOIs	https://doi.org/10.1039/c3dt50971k
State	Published - 28 Sep 2013
Externally published	Yes

Access to Document

10.1039/c3dt50971k

Cite this

@article{a19320088eea4bd5adc2a19ba266cf9a,

title = "Resolution and characterization of helicate dimer and trimer complexes of 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i)",

abstract = "Complexation of copper(i) with the binucleating ligand, 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane, mphenpr, result in formation of helical dimers, [Cu2(mphenpr)2]2+. The resolution of the enantiomeric forms of the dimers has been carried out with Δ-[As(cat)3]- as resolving agent and X-ray structures for two compounds, P-[Cu2(mphenpr)2](Δ- [As(cat)3])2 and P-[Cu2(mphenpr) 2](Δ-[As(cat)3])2·4(CH 3CN), are reported. The rate of racemization in poorly-coordinating solvents has been examined by 1H NMR, and is slow. At saturating concentrations of [[Cu2(mphenpr)2]2+] in acetonitrile, crystals of the helical trimeric complex [Cu3(mphenpr) 3](ClO4)3 are obtained. The X-ray structure of the trimer is reported. This species has also been resolved. As with the helical dimer, racemization in poorly-coordinating solvents is slow, and circular dichroism and 1H NMR spectra are reported. The absolute configuration of the resolved complex, P-[Cu3(mphenpr)3](Δ- [As(cat)3])3, has been determined by X-ray crystallography.",

author = "Luis Lemus and Juan Guerrero and Juan Costamagna and Romina Lorca and Jara, {Danilo H.} and Guillermo Ferraudi and Allen Oliver and Lappin, {A. Graham}",

year = "2013",

month = sep,

day = "28",

doi = "10.1039/c3dt50971k",

language = "English",

volume = "42",

pages = "11426--11435",

journal = "Dalton Transactions",

issn = "1477-9226",

publisher = "Royal Society of Chemistry",

number = "32",

}

TY - JOUR

T1 - Resolution and characterization of helicate dimer and trimer complexes of 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i)

AU - Lemus, Luis

AU - Guerrero, Juan

AU - Costamagna, Juan

AU - Lorca, Romina

AU - Jara, Danilo H.

AU - Ferraudi, Guillermo

AU - Oliver, Allen

AU - Lappin, A. Graham

PY - 2013/9/28

Y1 - 2013/9/28

N2 - Complexation of copper(i) with the binucleating ligand, 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane, mphenpr, result in formation of helical dimers, [Cu2(mphenpr)2]2+. The resolution of the enantiomeric forms of the dimers has been carried out with Δ-[As(cat)3]- as resolving agent and X-ray structures for two compounds, P-[Cu2(mphenpr)2](Δ- [As(cat)3])2 and P-[Cu2(mphenpr) 2](Δ-[As(cat)3])2·4(CH 3CN), are reported. The rate of racemization in poorly-coordinating solvents has been examined by 1H NMR, and is slow. At saturating concentrations of [[Cu2(mphenpr)2]2+] in acetonitrile, crystals of the helical trimeric complex [Cu3(mphenpr) 3](ClO4)3 are obtained. The X-ray structure of the trimer is reported. This species has also been resolved. As with the helical dimer, racemization in poorly-coordinating solvents is slow, and circular dichroism and 1H NMR spectra are reported. The absolute configuration of the resolved complex, P-[Cu3(mphenpr)3](Δ- [As(cat)3])3, has been determined by X-ray crystallography.

AB - Complexation of copper(i) with the binucleating ligand, 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane, mphenpr, result in formation of helical dimers, [Cu2(mphenpr)2]2+. The resolution of the enantiomeric forms of the dimers has been carried out with Δ-[As(cat)3]- as resolving agent and X-ray structures for two compounds, P-[Cu2(mphenpr)2](Δ- [As(cat)3])2 and P-[Cu2(mphenpr) 2](Δ-[As(cat)3])2·4(CH 3CN), are reported. The rate of racemization in poorly-coordinating solvents has been examined by 1H NMR, and is slow. At saturating concentrations of [[Cu2(mphenpr)2]2+] in acetonitrile, crystals of the helical trimeric complex [Cu3(mphenpr) 3](ClO4)3 are obtained. The X-ray structure of the trimer is reported. This species has also been resolved. As with the helical dimer, racemization in poorly-coordinating solvents is slow, and circular dichroism and 1H NMR spectra are reported. The absolute configuration of the resolved complex, P-[Cu3(mphenpr)3](Δ- [As(cat)3])3, has been determined by X-ray crystallography.

UR - http://www.scopus.com/inward/record.url?scp=84883253318&partnerID=8YFLogxK

U2 - 10.1039/c3dt50971k

DO - 10.1039/c3dt50971k

M3 - Article

AN - SCOPUS:84883253318

SN - 1477-9226

VL - 42

SP - 11426

EP - 11435

JO - Dalton Transactions

JF - Dalton Transactions

IS - 32

ER -

Resolution and characterization of helicate dimer and trimer complexes of 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i)

Abstract

Access to Document

Fingerprint

Cite this