Preparation and characterization of [RhCl2(edpp)2]+ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl2(edpp)2]Cl·2C2H5OH and cis(Cl,Cl),trans(P,P)-[RhCl2(edpp)2]Cl·4H2O

Frode GalsbØl; Masaaki Kojima; Toshio Ishii; Shigeru Ohba; Yoshihiko Saito; Junnosuke Fujita

doi:10.1246/bcsj.59.1701

Preparation and characterization of [RhCl₂(edpp)₂]⁺ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl·2C₂H₅OH and cis(Cl,Cl),trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O

Frode GalsbØl, Masaaki Kojima, Toshio Ishii, Shigeru Ohba, Yoshihiko Saito, Junnosuke Fujita

Department of Humanities and Social Sciences

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

8 Citations (Scopus)

Abstract

Two of the five possible geometrical isomers of [RhCl₂(edpp)₂]⁺ were formed by reaction of RhCl₃ · 2H₂0 with edpp (edpp=(2-aminoethyl)diphenylphosphine) in 1:2 molar ratio in ethanol. The chlorides of the isomers were separated by fractional crystallization from ethanol. The structures of the more soluble (main product) and the less soluble (minor product) complexes were determined by X-ray analyses to have the trans(Cl,Cl), cis(P,P) and cis(Cl,Cl), trans(P,P) configurations, respectively. Crystal data are: for trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl-2C₂H₅OH, triclinic, space group P1, with a= 10.024(3), b=18.865(3), c=9.833(2) Å, α=97.66(l), β=103.92(2), γ=82.30(2)°, and Z=2, and for cic(Cl,Cl), trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O, triclinic, space group P1, with a= 11.341(4), b=17.780(6), c=8.712(3) Å, α=95.60(4), β=112.31(3), γ=82.56(4)°, and Z=2. The trans influence of the P atom on the Rh-N and Rh-P bond lengths is observed. The mean Rh-N and Rh-P bond lengths (2.125(4) and 2.300(1)Å) in the trans(Cl,Cl), cis(P,P) isomer are respectively longer and shorter than those of the cis(Cl,Cl), trans(P,P) isomer (2.078(12) and 2.336(3)Åt). ¹³C NMR and absorption spectra of the isomers were recorded and are discussed.

Original language	English
Pages (from-to)	1701-1707
Number of pages	7
Journal	Bulletin of the Chemical Society of Japan
Volume	59
Issue number	6
DOIs	https://doi.org/10.1246/bcsj.59.1701
Publication status	Published - 1986 Jun

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Chemistry(all)

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GalsbØl, F., Kojima, M., Ishii, T., Ohba, S., Saito, Y., & Fujita, J. (1986). Preparation and characterization of [RhCl₂(edpp)₂]⁺ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl·2C₂H₅OH and cis(Cl,Cl),trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O. Bulletin of the Chemical Society of Japan, 59(6), 1701-1707. https://doi.org/10.1246/bcsj.59.1701

Preparation and characterization of [RhCl₂(edpp)₂]⁺ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl·2C₂H₅OH and cis(Cl,Cl),trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O. / GalsbØl, Frode; Kojima, Masaaki; Ishii, Toshio; Ohba, Shigeru; Saito, Yoshihiko; Fujita, Junnosuke.

In: Bulletin of the Chemical Society of Japan, Vol. 59, No. 6, 06.1986, p. 1701-1707.

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

GalsbØl, F, Kojima, M, Ishii, T, Ohba, S, Saito, Y & Fujita, J 1986, 'Preparation and characterization of [RhCl₂(edpp)₂]⁺ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl·2C₂H₅OH and cis(Cl,Cl),trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O', Bulletin of the Chemical Society of Japan, vol. 59, no. 6, pp. 1701-1707. https://doi.org/10.1246/bcsj.59.1701

GalsbØl F, Kojima M, Ishii T, Ohba S, Saito Y, Fujita J. Preparation and characterization of [RhCl₂(edpp)₂]⁺ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl·2C₂H₅OH and cis(Cl,Cl),trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O. Bulletin of the Chemical Society of Japan. 1986 Jun;59(6):1701-1707. https://doi.org/10.1246/bcsj.59.1701

GalsbØl, Frode ; Kojima, Masaaki ; Ishii, Toshio ; Ohba, Shigeru ; Saito, Yoshihiko ; Fujita, Junnosuke. / Preparation and characterization of [RhCl₂(edpp)₂]⁺ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl₂(edpp)₂]Cl·2C₂H₅OH and cis(Cl,Cl),trans(P,P)-[RhCl₂(edpp)₂]Cl·4H₂O. In: Bulletin of the Chemical Society of Japan. 1986 ; Vol. 59, No. 6. pp. 1701-1707.

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title = "Preparation and characterization of [RhCl2(edpp)2]+ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl2(edpp)2]Cl·2C2H5OH and cis(Cl,Cl),trans(P,P)-[RhCl2(edpp)2]Cl·4H2O",

abstract = "Two of the five possible geometrical isomers of [RhCl2(edpp)2]+ were formed by reaction of RhCl3 · 2H20 with edpp (edpp=(2-aminoethyl)diphenylphosphine) in 1:2 molar ratio in ethanol. The chlorides of the isomers were separated by fractional crystallization from ethanol. The structures of the more soluble (main product) and the less soluble (minor product) complexes were determined by X-ray analyses to have the trans(Cl,Cl), cis(P,P) and cis(Cl,Cl), trans(P,P) configurations, respectively. Crystal data are: for trans(Cl,Cl), cis(P,P)-[RhCl2(edpp)2]Cl-2C2H5OH, triclinic, space group P1, with a= 10.024(3), b=18.865(3), c=9.833(2) {\AA}, α=97.66(l), β=103.92(2), γ=82.30(2)°, and Z=2, and for cic(Cl,Cl), trans(P,P)-[RhCl2(edpp)2]Cl·4H2O, triclinic, space group P1, with a= 11.341(4), b=17.780(6), c=8.712(3) {\AA}, α=95.60(4), β=112.31(3), γ=82.56(4)°, and Z=2. The trans influence of the P atom on the Rh-N and Rh-P bond lengths is observed. The mean Rh-N and Rh-P bond lengths (2.125(4) and 2.300(1){\AA}) in the trans(Cl,Cl), cis(P,P) isomer are respectively longer and shorter than those of the cis(Cl,Cl), trans(P,P) isomer (2.078(12) and 2.336(3){\AA}t). 13C NMR and absorption spectra of the isomers were recorded and are discussed.",

author = "Frode Galsb{\O}l and Masaaki Kojima and Toshio Ishii and Shigeru Ohba and Yoshihiko Saito and Junnosuke Fujita",

year = "1986",

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doi = "10.1246/bcsj.59.1701",

language = "English",

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T1 - Preparation and characterization of [RhCl2(edpp)2]+ (edpp=(2-aminoethyl)-diphenylphosphine). Crystal Structures of trans(Cl,Cl), cis(P,P)-[RhCl2(edpp)2]Cl·2C2H5OH and cis(Cl,Cl),trans(P,P)-[RhCl2(edpp)2]Cl·4H2O

AU - GalsbØl, Frode

AU - Kojima, Masaaki

AU - Ishii, Toshio

AU - Ohba, Shigeru

AU - Saito, Yoshihiko

AU - Fujita, Junnosuke

PY - 1986/6

Y1 - 1986/6

N2 - Two of the five possible geometrical isomers of [RhCl2(edpp)2]+ were formed by reaction of RhCl3 · 2H20 with edpp (edpp=(2-aminoethyl)diphenylphosphine) in 1:2 molar ratio in ethanol. The chlorides of the isomers were separated by fractional crystallization from ethanol. The structures of the more soluble (main product) and the less soluble (minor product) complexes were determined by X-ray analyses to have the trans(Cl,Cl), cis(P,P) and cis(Cl,Cl), trans(P,P) configurations, respectively. Crystal data are: for trans(Cl,Cl), cis(P,P)-[RhCl2(edpp)2]Cl-2C2H5OH, triclinic, space group P1, with a= 10.024(3), b=18.865(3), c=9.833(2) Å, α=97.66(l), β=103.92(2), γ=82.30(2)°, and Z=2, and for cic(Cl,Cl), trans(P,P)-[RhCl2(edpp)2]Cl·4H2O, triclinic, space group P1, with a= 11.341(4), b=17.780(6), c=8.712(3) Å, α=95.60(4), β=112.31(3), γ=82.56(4)°, and Z=2. The trans influence of the P atom on the Rh-N and Rh-P bond lengths is observed. The mean Rh-N and Rh-P bond lengths (2.125(4) and 2.300(1)Å) in the trans(Cl,Cl), cis(P,P) isomer are respectively longer and shorter than those of the cis(Cl,Cl), trans(P,P) isomer (2.078(12) and 2.336(3)Åt). 13C NMR and absorption spectra of the isomers were recorded and are discussed.

AB - Two of the five possible geometrical isomers of [RhCl2(edpp)2]+ were formed by reaction of RhCl3 · 2H20 with edpp (edpp=(2-aminoethyl)diphenylphosphine) in 1:2 molar ratio in ethanol. The chlorides of the isomers were separated by fractional crystallization from ethanol. The structures of the more soluble (main product) and the less soluble (minor product) complexes were determined by X-ray analyses to have the trans(Cl,Cl), cis(P,P) and cis(Cl,Cl), trans(P,P) configurations, respectively. Crystal data are: for trans(Cl,Cl), cis(P,P)-[RhCl2(edpp)2]Cl-2C2H5OH, triclinic, space group P1, with a= 10.024(3), b=18.865(3), c=9.833(2) Å, α=97.66(l), β=103.92(2), γ=82.30(2)°, and Z=2, and for cic(Cl,Cl), trans(P,P)-[RhCl2(edpp)2]Cl·4H2O, triclinic, space group P1, with a= 11.341(4), b=17.780(6), c=8.712(3) Å, α=95.60(4), β=112.31(3), γ=82.56(4)°, and Z=2. The trans influence of the P atom on the Rh-N and Rh-P bond lengths is observed. The mean Rh-N and Rh-P bond lengths (2.125(4) and 2.300(1)Å) in the trans(Cl,Cl), cis(P,P) isomer are respectively longer and shorter than those of the cis(Cl,Cl), trans(P,P) isomer (2.078(12) and 2.336(3)Åt). 13C NMR and absorption spectra of the isomers were recorded and are discussed.

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