[M(bpy)3] (M = Fe, Ru, Os): New Crystalline Materials from the reductive electrocrystallization of [M(bpy)3](PF6)2

Eduardo Pérez‐Cordero; Rosanna Buigas; Nancy Brady; Luis Echegoyen; Claudia Arana; Jean‐Marie Lehn

doi:10.1002/hlca.19940770504

[M(bpy)₃] (M = Fe, Ru, Os): New Crystalline Materials from the reductive electrocrystallization of [M(bpy)₃](PF₆)₂

Eduardo Pérez‐Cordero
, Rosanna Buigas
, Nancy Brady
, Luis Echegoyen
, Claudia Arana
, Jean‐Marie Lehn

Research output: Journal Publications and Reviews › RGC 21 - Publication in refereed journal › peer-review

24 Citations (Scopus)

Abstract

Reductive electrocrystallization at a constant current density (11.0–11.5 μA/cm2) of millimolar solutions of [M(bpy)3](PF6)2, where M = Fe, Ru, or Os, and bpy = 2,2′‐bipyridine in acetonitrile containing 0.1M Bu4NPF6 results in the formation of dark crystals on the Pt cathode. The crystals grow as long, thin, and shiny needles having a hexagonal cross section of 0.1–0.5 mm in diameter. Combustion microanalyses results are consistent with the composition for [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. In addition, the chromophores are conserved, as confirmed by recording both the electronic and the 1H‐NMR spectra after reoxidation of the electrocrystals in humid air. The spectra are identical to those for authentic samples of [Fe(bpy)3]2+, [Ru(bpy)3]2+, and [Os(bpy)3]2+. A ratio of 2.0 ± 0.1 e−/molecule is observed upon completion of the controlled potential electrolysis of a solution of [M(bpy)3]2+, which results in the precipitation of a dark solid and the almost complete fading of the color of the original solution. Unexpectedly, the crystals do not exhibit an ESR signal. These data indicate the formation of novel materials, crystalline [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. Copyright © 1994 Verlag GmbH & Co. KGaA, Weinheim

Original language	English
Pages (from-to)	1222-1228
Journal	Helvetica Chimica Acta
Volume	77
Issue number	5
DOIs	https://doi.org/10.1002/hlca.19940770504
Publication status	Published - 10 Aug 1994
Externally published	Yes

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@article{73c21ed5043f4c439e44e9effb2ac300,

title = "[M(bpy)3] (M = Fe, Ru, Os): New Crystalline Materials from the reductive electrocrystallization of [M(bpy)3](PF6)2",

abstract = "Reductive electrocrystallization at a constant current density (11.0–11.5 μA/cm2) of millimolar solutions of [M(bpy)3](PF6)2, where M = Fe, Ru, or Os, and bpy = 2,2′‐bipyridine in acetonitrile containing 0.1M Bu4NPF6 results in the formation of dark crystals on the Pt cathode. The crystals grow as long, thin, and shiny needles having a hexagonal cross section of 0.1–0.5 mm in diameter. Combustion microanalyses results are consistent with the composition for [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. In addition, the chromophores are conserved, as confirmed by recording both the electronic and the 1H‐NMR spectra after reoxidation of the electrocrystals in humid air. The spectra are identical to those for authentic samples of [Fe(bpy)3]2+, [Ru(bpy)3]2+, and [Os(bpy)3]2+. A ratio of 2.0 ± 0.1 e−/molecule is observed upon completion of the controlled potential electrolysis of a solution of [M(bpy)3]2+, which results in the precipitation of a dark solid and the almost complete fading of the color of the original solution. Unexpectedly, the crystals do not exhibit an ESR signal. These data indicate the formation of novel materials, crystalline [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. Copyright {\textcopyright} 1994 Verlag GmbH \& Co. KGaA, Weinheim",

author = "Eduardo P{\'e}rez‐Cordero and Rosanna Buigas and Nancy Brady and Luis Echegoyen and Claudia Arana and Jean‐Marie Lehn",

note = "Publication details (e.g. title, author(s), publication statuses and dates) are captured on an “AS IS” and “AS AVAILABLE” basis at the time of record harvesting from the data source. Suggestions for further amendments or supplementary information can be sent to [email protected].",

year = "1994",

month = aug,

day = "10",

doi = "10.1002/hlca.19940770504",

language = "English",

volume = "77",

pages = "1222--1228",

journal = "Helvetica Chimica Acta",

issn = "0018-019X",

publisher = "Wiley-Blackwell",

number = "5",

}

TY - JOUR

T1 - [M(bpy)3] (M = Fe, Ru, Os)

T2 - New Crystalline Materials from the reductive electrocrystallization of [M(bpy)3](PF6)2

AU - Pérez‐Cordero, Eduardo

AU - Buigas, Rosanna

AU - Brady, Nancy

AU - Echegoyen, Luis

AU - Arana, Claudia

AU - Lehn, Jean‐Marie

N1 - Publication details (e.g. title, author(s), publication statuses and dates) are captured on an “AS IS” and “AS AVAILABLE” basis at the time of record harvesting from the data source. Suggestions for further amendments or supplementary information can be sent to [email protected].

PY - 1994/8/10

Y1 - 1994/8/10

N2 - Reductive electrocrystallization at a constant current density (11.0–11.5 μA/cm2) of millimolar solutions of [M(bpy)3](PF6)2, where M = Fe, Ru, or Os, and bpy = 2,2′‐bipyridine in acetonitrile containing 0.1M Bu4NPF6 results in the formation of dark crystals on the Pt cathode. The crystals grow as long, thin, and shiny needles having a hexagonal cross section of 0.1–0.5 mm in diameter. Combustion microanalyses results are consistent with the composition for [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. In addition, the chromophores are conserved, as confirmed by recording both the electronic and the 1H‐NMR spectra after reoxidation of the electrocrystals in humid air. The spectra are identical to those for authentic samples of [Fe(bpy)3]2+, [Ru(bpy)3]2+, and [Os(bpy)3]2+. A ratio of 2.0 ± 0.1 e−/molecule is observed upon completion of the controlled potential electrolysis of a solution of [M(bpy)3]2+, which results in the precipitation of a dark solid and the almost complete fading of the color of the original solution. Unexpectedly, the crystals do not exhibit an ESR signal. These data indicate the formation of novel materials, crystalline [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. Copyright © 1994 Verlag GmbH & Co. KGaA, Weinheim

AB - Reductive electrocrystallization at a constant current density (11.0–11.5 μA/cm2) of millimolar solutions of [M(bpy)3](PF6)2, where M = Fe, Ru, or Os, and bpy = 2,2′‐bipyridine in acetonitrile containing 0.1M Bu4NPF6 results in the formation of dark crystals on the Pt cathode. The crystals grow as long, thin, and shiny needles having a hexagonal cross section of 0.1–0.5 mm in diameter. Combustion microanalyses results are consistent with the composition for [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. In addition, the chromophores are conserved, as confirmed by recording both the electronic and the 1H‐NMR spectra after reoxidation of the electrocrystals in humid air. The spectra are identical to those for authentic samples of [Fe(bpy)3]2+, [Ru(bpy)3]2+, and [Os(bpy)3]2+. A ratio of 2.0 ± 0.1 e−/molecule is observed upon completion of the controlled potential electrolysis of a solution of [M(bpy)3]2+, which results in the precipitation of a dark solid and the almost complete fading of the color of the original solution. Unexpectedly, the crystals do not exhibit an ESR signal. These data indicate the formation of novel materials, crystalline [Fe(bpy)3], [Ru(bpy)3], and [Os(bpy)3]. Copyright © 1994 Verlag GmbH & Co. KGaA, Weinheim

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U2 - 10.1002/hlca.19940770504

DO - 10.1002/hlca.19940770504

M3 - RGC 21 - Publication in refereed journal

SN - 0018-019X

VL - 77

SP - 1222

EP - 1228

JO - Helvetica Chimica Acta

JF - Helvetica Chimica Acta

IS - 5

ER -